USEPA Contract Laboratory Program
Statement of Work for Organics Analysis
Multi-media, Multi-concentration
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54OR995O7
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK
FOR
ORGANICS ANALYSIS
Multi-Media, Multi-Concentration
OLM04.2
May 1999
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STATEMENT OF WORK
TABLE OF CONTENTS
EXHIBIT A: SUMMARY OF REQUIREMENTS
EXHIBIT B: REPORTING AND DELIVERABLES REQUIREMENTS
EXHIBIT C: TARGET COMPOUND LIST (TCL) AND CONTRACT REQUIRED QUANTISATION
LIMITS (CRQLs)
EXHIBIT D: ANALYTICAL METHODS
EXHIBIT E: QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES AND REQUIREMENTS
EXHIBIT F: CHAIN-OF-CUSTODY, DOCUMENT CONTROL, AND WRITTEN STANDARD OPERATING
PROCEDURES
EXHIBIT G: GLOSSARY OF TERMS
EXHIBIT H: AGENCY STANDARD IMPLEMENTATION
OLM04.2
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EXHIBIT A
SUMMARY OF REQUIREMENTS
A-l OLM04.2
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Exhibit A - Summary of Requirements
Table of Contents
Section Page
1.0 PURPOSE 3
2.0 DESCRIPTION OF SERVICE 3
3.0 DATA USES 3
4.0 SUMMARY OF REQUIREMENTS 3
4 .1 Introduction to the SOW 3
4.2 Overview of Major Task Areas 4
4.3 Technical and Management Capability 9
A-2 OLM04.2
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Exhibit A -- Sections 1-4
Summary of Requirements
1.0 PURPOSE
The purpose of the multi-media, multi-concentration organic analytical
service is to provide analytical data for use by the U.S. Environmental
Protection Agency (EPA) in support of its investigation and clean-up
activities under the Comprehensive Environmental Response, Compensation,
and Liability Act of 1980 (CERCLA) and the Superfund Amendments and
Reauthorization Act of 1986 (SARA). Other EPA Program Offices that have
similar analytical data needs also use this service.
2.0 DESCRIPTION OF SERVICE
The organic analytical service provides a contractual framework for
laboratories to apply EPA Contract Laboratory Program (CLP) analytical
methods for the isolation, detection, and quantitative measurement of 48
volatile, 65 semivolatile, and 28 pesticide/Aroclor target compounds in
water and soil/sediment environmental samples. The analytical service
provides the methods to be used, and the specific contractual
requirements by which EPA will evaluate the data. This service uses gas
chromatography/mass spectrometry (GC/MS) and gas chromatography/electron
capture (GC/EC) methods to analyze the target compounds.
3.0 DATA USES
This analytical service provides data which EPA uses for a variety of
purposes, such as determining the nature and extent of contamination at
a hazardous waste site, assessing priorities for response based on risks
to human health and the environment, determining appropriate cleanup
actions, and determining when remedial actions are complete. The data
may be used in all stages in the investigation of a hazardous waste
site, including site inspections, Hazard Ranking System scoring,
remedial investigations/feasibility studies, remedial design,
treatability studies, and removal actions. In addition, this service
provides data that are available for use in Superfund
enforcement/litigation activities.
4.0 SUMMARY OF REQUIREMENTS
4.1 Introduction to the SOW. This SOW is designed as part of the
documentation for a contract between EPA and a commercial laboratory
performing analyses in support of EPA Superfund programs. The SOW is
comprised of eight exhibits. Exhibit A provides an overview of the SOW
and its general requirements.. Exhibit B contains a description of the
reporting and deliverables requirements, in addition to the data
reporting forms and the forms instructions. Exhibit C specifies the
target compound list for this SOW with the contract-required
quantitation limits for sample matrices. Exhibit D details.the specific
analytical procedures to be used with this SOW and resulting contracts.
Exhibit E provides descriptions of required quality assurance/quality
control (QA/QC), standard operating procedures, and procedures used for
evaluating analytical methodologies, QA/QC performance, and the
reporting of data. Exhibit F contains chain-of-custody -and sample
documentation requirements which the Contractor shall follow. To ensure
proper understanding of the terms utilized in this SOW, a glossary can
A-3 OLMO'4.2
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Exhibit A -- Section 4
Summary of Requirements
be found in Exhibit G (when a term is used in the text without
explanation, the glossary meaning shall be applicable). Specifications
for reporting data in computer-readable form appear in Exhibit H.
4.2 Overview of Major Task Areas. For each sample, the Contractor shall
perform the tasks described in this section. Specific requirements for
each task are detailed in the exhibits as referenced.
4.2.1 Task I: Chain-of-Custody
4.2.1.1 Chain-of-Custody. The Contractor shall receive and maintain
samples under proper chain-of-custody procedures. All associated
document control and inventory procedures shall be developed and
followed. Documentation, as described therein, shall be required
to show that all procedures are being strictly followed. This
documentation shall be reported as the Complete Sample Delivery
Group File (CSF) (see Exhibit B). The Contractor shall establish
and use appropriate procedures to handle confidential information
received from the Agency. See Exhibit F for specific
requirements.
4.2.1.2 Sample Scheduling/Shipments. Sample shipments to the Contractor's
facility will be scheduled and coordinated by the CLP Sample
Management Office (SMO). The Contractor shall communicate with
SMO personnel by telephone, as necessary throughout the .process of
sample scheduling, shipment, analysis, and data reporting, to
ensure that samples are properly processed. At the time of sample
scheduling, the Contractor will be notified if the Modified SW-846
Method 5035 is to be used in the preparation and analysis of low
level soil samples for volatiles.
4.2.1.2.1 Samples will be shipped routinely to the Contractor through an
overnight delivery service. However, as necessary, the
Contractor shall be responsible for any handling or processing
required for the receipt of sample shipments, including pick-up
of samples at the nearest servicing airport, bus station, or
other carrier service within the Contractor's geographical
area. The Contractor shall be available to receive sample
shipments at any time the delivery service is operating,
including Saturdays.
4.2.1.2.2 If there are problems with the samples (e.g., mixed media,
containers broken or leaking) or sample documentation/paperwork
(e.g., Traffic Reports not with shipment, sample and Traffic
Report numbers do not correspond), the Contractor shall
immediately contact SMO for resolution. The Contractor shall
immediately notify SMO regarding any problems and laboratory
conditions that affect the timeliness of analyses and data
reporting. In particular, the Contractor shall notify SMO
personnel in advance regarding sample data that will be
delivered late and shall specify the estimated delivery date.
4.2.1.2.3 To effectively monitor the temperature of the sample shipping
cooler, each USEPA Regional office may include a sample
A-4 OLM04.2
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Exhibit A -- Section 4
Summary of Requirements
shipping cooler temperature blank with each cooler shipped.
The temperature blank will be clearly labeled:- USEPA COOLER
TEMPERATURE INDICATOR.
4.2.1.2.3.1 When the USEPA Regional office supplies a cooler temperature
indicator bottle in the sample shipping cooler, the
Contractor shall use the USEPA supplied cooler temperature
indicator bottle to determine the cooler temperature. The
temperature of the cooler shall be measured at the time of
sample receipt by the Contractor.
4.2.1.2.3.2 The temperature of the sample shipping cooler-shall be
measured and recorded immediately upon opening the cooler,
and prior to unpacking the samples or removing the packing
material.
4.2.1.2.3.3 To determine the temperature of the cooler, the contractor
shall locate the cooler temperature indicator bottle in the
sample shipping cooler, remove the cap, and insert a
calibrated thermometer into the cooler temperature indicator
bottle. Prior to recording the temperature, the Contractor
shall allow a minimum of 3 minutes, but not greater than 5
minutes, for the thermometer to equilibrate with the liquid
in the bottle. At a minimum, the calibrated thermometer
(±1°C) shall have a measurable range of 0 to 50 degrees
Celsius. Other devices which can measure temperature may be
used if they can be calibrated to ±1°C and have a range of 0
to 20°C. Jf a temperature indicator bottle is not present
in the cooler, an alternative means of determining cooler
temperature shall be used. However, under no circumstances
shall a thermometer or any other device be inserted into a
sample bottle for the purpose of determining cooler
temperature. The Contractor shall contact SMO and inform
them that a temperature indicator bottle was not present in
the cooler. The Contractor shall document the alternative
technique used to determine cooler temperature in the SDG
Narrative.
4.2.1.2.3.4 If the temperature of the sample shipping cooler's
temperature indicator exceeds 10 degrees Celsius, the
Contractor shall contact SMO and inform them of the
temperature deviation. The SMO will contact the Region from
which the samples were shipped for instructions on how to
proceed. The Region will either require that no sample
analysis(es) be performed or that the Contractor proceed
with the analysis(es). The SMO will in turn notify the
Contractor of the Region's decision. The Contractor shall
document the Region's decision in the SDG Narrative. Also
in the SDG Narrative, the Contractor shall list by fraction,
the USEPA sample-number of all samples which were shipped in
a cooler which exceeded 10 degrees Celsius.
A-5 OLM04.2
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Exhibit A -- Section 4
Summary of Requirements
4.2.1.2.3.5 The Contractor shall record the temperature of the cooler on
the DC-1 Form, under Remark #9 - Cooler Temperature, and in
the SDG Narrative.
4.2.1.2.4 . The Contractor shall accept all samples scheduled by SMO,
provided that the total number of samples received in any
calendar month does not exceed the monthly limitation expressed
in the contract. Should the Contractor elect to accept
additional samples, the Contractor shall remain bound by all
contract requirements for analysis of those samples accepted.
4.2.1.2.5 The Contractor shall be required to routinely return sample
shipping containers (e.g., coolers) to the appropriate sampling
office within 14 calendar days.following shipment receipt '(see
Clause entitled Government Furnished Supplies and Materials).
4.2.2 Task II: Analysis of Samples
4.2.2.1 Overview. Sample.analyses will be scheduled by groups of samples,
each defined as a Case and identified by a unique EPA Case number
assigned by SMO. A Case signifies a group of samples collected at
one site or geographical area over a finite time period, and will
include one or more field samples with associated blanks. Samples
may be shipped to the Contractor in a single shipment or multiple
shipments over a period of time, depending on the size of the
Case.
4.2.2.1.1 A Case consists of one or more Sample Delivery Group(s). A
Sample Delivery Group (SDG) is defined by the following,
whichever is most frequent:
Each Case of field samples received, OR
Each 20 field samples (excluding PE samples) within a Case,
OR
Each 7 calendar day period (excluding Sundays and
Government holidays) during which field samples in a Case
are received (said period beginning with the receipt of the
first sample in the SDG).
In addition, all samples and sample fractions assigned to an
SDG must have been scheduled under the same contractual
turnaround time.
4.2.2.1.2 Samples may be assigned to SDGs by matrix (i.e., all soils in
one SDG, all waters in another), at the discretion of the
laboratory. However, PE samples received within a Case shall
be assigned to an SDG containing field samples for that Case.
Such assignment shall be made at the time the samples are
received, and shall not be made retroactively.
4.2.2.2 Preparation Techniques. The Contractor will prepare samples as
described in Exhibit D. For semivolatile and pesticide/Aroclor
A-6 OLM04.2
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Exhibit A -- Section 4
Summary of Requirements
samples, an aliquot is extracted with a solvent and concentrated.
The concentrated extract is subjected to fraction-specific cleanup
procedures and then analyzed by GC/MS for semivolatile or GC/EC
for the pesticide/Aroclor target compounds listed in Exhibit C.
For volatile samples, an aliquot is purged with an inert gas,
trapped on a solid sorbent, and then desorbed onto the GC/MS for
analysis of the target compounds listed in Exhibit C.
4.2.2.3 Analytical Techniques. The target compounds listed in Exhibit C
shall be identified as described in the methodologies given in
Exhibit D. Automated computer programs may be used to facilitate
the identification of compounds.
4.2.2.4 Qualitative Verification of Compounds. The volatile and
semivolatile compounds identified by GC/MS techniques shall be
verified by an analyst competent in the interpretation of mass
spectra by comparison of the suspect mass spectrum to the mass
spectrum of a standard of the suspected compound. This procedure
requires the use of multiple internal standards.
4.2.2.4.1 If a compound initially identified by GC/MS techniques cannot
be verified, but in the technical judgment of the mass spectral
interpretation specialist the identification is correct, then
the Contractor shall report that identification and proceed
with quantitation.
4.2.2.4.2 The pesticide/Aroclor compounds identified by GC/EC techniques
shall be verified by an analyst competent in the interpretation
of gas chromatograms and by comparison of the retention times
of the suspected unknowns with the retention times of
respective standards of the suspected compounds. Compounds
shall also be confirmed by GC/MS techniques if the compounds
are of sufficient concentration to be detected by the GC/MS.
4.2.2.5 Quantitation of Verified Compounds. The Contractor shall
quantitate components identified by GC/MS techniques by the
internal standard method stipulated in Exhibit D. Where multiple
internal standards are required by EPA, the Contractor shall
perform quantitation utilizing the internal standards specified in
Exhibit D. The Contractor shall quantitate components analyzed -by
GC/EC techniques by the external standard method stipulated in
Exhibit D. The Contractor shall also perform an initial three-
point calibration, verify its linearity, determine the breakdown
of labile components, and determine calibration factors for all
standards analyzed by GC/EC techniques as described in Exhibit D.
4.2.2.6 Tentative Identification of Non-Target Sample Components. For
each analysis of a sample, the Contractor shall conduct mass
spectral library searches to determine tentative compound
identifications as follows: For each volatile sample, the
Contractor shall'conduct a search to determine the possible
identity of up to 30 organic compounds of greatest concentration
.which are not system monitoring compounds or internal standards
and are not listed in Exhibit C under volatiles or semivolatiles.
A-7 OLM04.2
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Exhibit A -- Section 4
Summary of Requirements
For each semivolatile sample, the Contractor shall conduct a
search to determine the possible identification of up to 30
organic compounds of greatest concentration which are not
surrogates or internal standards and are not listed in Exhibit C
under volatiles or semivolatiles. In performing searches, the
NIST/EPA/NIH (May 1992 release or later) and/or Wiley (1991
release or later), or equivalent, mass spectral library shall be
used.
NOTE: Substances with responses less than 10% of the nearest
internal standard are not required to be searched in this fashion.
4.2.2.7 Quality Assurance/Quality Control Procedures. The Contractor
shall strictly adhere to all specific QA/QC procedures prescribed
in Exhibits D and E. Records documenting the use of the protocol
shall be maintained in accordance with the document control
procedures prescribed in Exhibit F, and shall be reported in
accordance with Exhibit B and Exhibit H.
4.2.2.7.1 The Contractor shall maintain a Quality Assurance Plan (QAP)
with the objective of providing sound analytical chemical
measurements. This program shall incorporate the quality
control procedures, any necessary corrective action, and all
documentation required during data collection as well as the
quality assessment measures performed by management to ensure
acceptable data production.
4.2.2.7.2 Additional quality control shall be conducted in the form of
the analysis of laboratory evaluation samples submitted to the
laboratory by the Agency. The results of all such quality
control or laboratory evaluation samples may be used as the
basis for an equitable adjustment to reflect the reduced value
of the data to the Agency or rejection of data for: sample(s),
a fraction within an SDG, or the entire SDG, and/or may be used
as the basis for contract action. "Compliant performance" is
defined as that which yields correct compound identification
and concentration values as determined by the Agency, as well
as meeting the contract requirements for analysis (Exhibit D),
quality assurance/quality control (Exhibit E), data reporting
and other deliverables (Exhibits B and H) , and sample custody,
sample documentation, and standard operating procedure
documentation (Exhibit F).
4.2.2.8 The Contractor may be requested by EPA to perform modified
analyses. These modifications may include, but are not limited
to, additional compounds, sample matrices other than soil/sediment
or water, and lower guantitation limits. These requests will be
made by the EPA Administrative Project Officer and Contracting
Officer in writing, prior to sample scheduling. If the Contractor
voluntarily elects to perform these modified analyses, these
analyses will be performed with no increase in per sample price.
In addition, all applicable contract requirements specified in the
Statement of Work/Specifications will remain in effect.
A-8 OLM04.2
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Exhibit A -- Section 4
Summary of Requirements
4.2.3 Task III: Reporting Requirements
4.2.3.1 EPA has provided the Contractor with formats for the reporting of
data (Exhibits B and H). The Contractor shall be responsible for
completing and submitting analysis data sheets and computer-
readable data on diskette (or via an alternate means of electronic
transmission approved in advance by the EPA) in the format
specified in this SOW and within the time specified in the
Contract Performance/DeliverySchedule in Exhibit B.
4.2.3.2 Use of formats other than those designated by EPA will be deemed
as noncompliant. Such data are unacceptable. Resubmission in the
specified format at no additional cost to the Agency shall be
required.
4.2.3.3 Computer-generated forms may be submitted in the hardcopy data
package(s) provided that the forms are in exact EPA format. This
means that the order of data elements is the same as on each EPA-
required form, including form numbers and titles, page numbers,
and header information.
4.2.3.4 The data reported by the Contractor on the hardcopy data forms and
the associated computer-readable data submitted by the Contractor
shall contain identical information. If discrepancies are found
during government inspection, the Contractor shall be required to
resubmit either the hardcopy forms or the computer-readable data,
or both sets of data, at no additional cost to the Agency.
4.3 Technical and Management Capability
4.3.1 Personnel. The Contractor shall have adequate personnel at all times
during the performance of the contract to ensure that EPA receives
data that meet the terms and conditions of the contract.
4.3.2 Instrumentation. The Contractor shall have sufficient gas
chromatograph/electron capture/data system (GC/EC/DS), gas
chromatograph/mass spectrometer/data system (GC/MS/DS), including
magnetic tape storage devices, and gel permeation chromatography
system (GPC) capability to meet all the terms and conditions of the
contract.
4.3.3 Facilities. The Contractor shall maintain a facility suitable for
the receipt, storage, analysis, and delivery of the product meeting
the terms and conditions of the contract.
A-9 OLM04.2
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EXHIBIT B
REPORTING AND DELIVERABLES REQUIREMENTS
B-l OLM04.2
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Exhibit B - Reporting and Deliverables Requirements
Table of Contents
Section Page
1.0 CONTRACT REPORTS/DELIVERABLES DISTRIBUTION 3
1.1 Report Deliverable Schedule 3
1.2 Distribution 6
2.0 REPORTING REQUIREMENTS AND ORDER OF DATA DELIVERABLES 7
2.1 Introduction 7
2.2 Resubmission of Data 7
2.3 Quality Assurance Plan and Standard Operating Procedures ... 8
2.4 Sample Traffic Reports 8
2 . 5 Sample Data Summary Package 9
2.6 Sample Data Package 9
2.7 Complete SDG File 25
2.8 Data in Computer-Readable Form 26
2.9 Preliminary Results 27
2.10 GC/MS and GC/EC Tapes 27
2.11 Extracts 27
3.0 FORMS INSTRUCTIONS 28
3.1 Introduction 28
3.2 General Information 28
3.3 Header Information 29
3.4 Organic Analysis Data Sheet (Form I, All Fractions) 33
3.5 Organic Analysis Data Sheet: Tentatively Identified Compounds
(Form I VOA-TIC and Form I SV-TIC) 38
3.6 System Monitoring Compound Recovery (Form II, VOA-1, VOA-2) . . 39
3.7 Surrogate Recovery (Form II, SV-1, SV-2 and Form II, PEST-1,
PEST-2) 39
3.8 Matrix Spike/Matrix Spike Duplicate Recovery (Form III, All
Fractions) 41
3.9 Method Blank Summary (Form IV, All Fractions) 42
3.10 GC/MS Instrument Performance Check and Mass Calibration
(Form V VOA and Form V SV) '. 44
3.11 GC/MS Initial Calibration Data (Form VI, VOA-1, VOA-2 and
Form VI, SV-1, SV-2) 45
3.12 GC/EC Initial Calibration Data (Form VI, PEST-1, PEST-2) ... 46
3.13 GC/MS Continuing Calibration Data (Form VII, VOA-1, VOA-2
and Form VII, SV-1, SV-2) 48
3.14 GC/EC Calibration Verification Summary (Form VII, PEST-1,
PEST-2) 49
3.15 Internal Standard Area and RT Summary (Form VIII VOA and Form
VIII, SV-1, SV-2) 50
3.16 Pesticide Analytical Sequence (Form VIII PEST) 52
3.17 Pesticide Cleanup Summary (Form IX, PEST-1, PEST-2) 53
3.18 Pesticide/Aroclor Identification (Form X, PEST-1, PEST-2) ... 54
3.19 Sample Log-In Sheet (Form DC-1) 56
3.20 Document Inventory Sheet (Form DC-2) 57
4.0 DATA REPORTING FORMS 59
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Exhibit B--Section 1
Contract Reports/Deliverables Distribution
1.0 CONTRACT REPORTS/DELIVERABLES DISTRIBUTION
1.1 Report Deliverable Schedule. The following table reiterates the
contract reporting and deliverable requirements specified in the
Contract Schedule (Performance/Delivery Schedule) and specifies the
distribution that is required for each deliverable. The turnaround
times for items B through E listed below are 7, 14, and 21 days.
NOTE: Specific recipient names and addresses are subject to change
during the term of the contract. The Administrative Project Officer
(APO) will notify the Contractor in writing of such changes when they
occur.
Table 1
Distribution
Item
No. of
Copies*
Delivery Schedule
o
2
W
O
H
01
0)
A.
1. 3
F.'
Sample Traffic
Reports
Sample Data
Summary
Package
Sample Data
Package0
Data in
Computer
Readable
Format
Complete SDG
File
Preliminary
Results (VOA
Analyses)
Preliminary
Results (SV
and Pest
Analyses)
3 working days
after receipt of
last sample in
Sample Delivery
Group (SDG).2
XXs days after
receipt of last
sample in SDG.
XXs days after
receipt of last
sample in SDG.
XXs days after
receipt of last
sample in SDG.
XX3 days after
receipt- of last
sample in SDG.
Within 48 hours
after receipt of
last sample in SDG
at laboratory, if
requested.
Within 72 hours
after receipt of
last sample in SDG
at laboratory, if
requested.
X X
X
X X
B-3
OLM04.2
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Exhibit B--Section 1
Contract Reports/Deliverables Distribution
Distribution
Item
No. of
Copies
Delivery
Schedule
o
w
o
cn
0)
Standard
Operating
Procedures--
Technical and
Evidentiary
.Revise within 60
days after
contract award.
Submit within 7
days of receipt
of written
request to
recipients as
directed.
-As directed
Quality
Assurance Plan
Revise within 60
days after
contract award.
GC/MS and GC/EC
Tapes
Lot
Submit within 7
days of receipt
of written
request to
recipients as
directed.
Retain for 365
days after data
submission.
As directed
As directed
Extracts
Lot
Submit within 7
days after
receipt of
written request
by APO.
Retain for 365
days after data
submission.
As directed
Submit within 7
days after
receipt of
written request
by APO or SMO,
at the Agency's
direction.
B-4
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Exhibit B--Section 1
Contract Reports/Deliverables Distribution
Footnotes:
AThe number of copies specified are the number of copies required to be
delivered to each recipient.
BThe number of days associated with these elements will be provided in
the associated laboratory contract document, and will also be provided at the
time of the sample scheduling by the SMO' Contractor.
cContractor-concurrent delivery to EPA designated recipient (e.g., QATS)
may be required upon request by the APO. Retain for 365 days after data
submission, and submit as directed within 7 days after receipt of written
request by the APO.
Also required in the Sample Data Summary Package.
A sample delivery group (SDG) is a group of samples within a Case,
received over a period of 7 days or less and not exceeding 20 samples
(excluding PE samples) . Data, for all samples in the SDG are due
concurrently. The date of delivery of the SDG or any samples within the
SDG is the date that the last sample in the SDG is received. See Exhibit
A for further description.
DELIVERABLES ARE TO BE REPORTED TOTAL AND COMPLETE. Concurrent delivery
required. Delivery shall be made such that all designated recipients
receive the item on the same calendar day. This includes resubmission of
both the hardcopy and electronic deliverable. The date of delivery of
the SDG, or any sample within the SDG, is the date all samples have been
delivered. If the deliverables are due on a Saturday, Sunday, or Federal
holiday, then they shall be delivered on the next business day.
Deliverables delivered after this time will be considered late.'
Complete SDG File will contain the originalsample data package plus all
of the original documents described under Section .2.7.
See Exhibit E and Exhibit F for a more detailed description.
If requested at the time of sample scheduling, the Contractor shall
provide Preliminary Results, consisting of Form I and Form I TIC
analytical results, by fraction, for field and QC sample analyses via
telefacsimile (fax) 'or other electronic means. The Contractor will be
notified of the fax number or E-mail address at the time of sample
scheduling. Sample Traffic Reports and SDG cover sheets shall be
submitted with the Preliminary Results. The Contractor shall contact SMO
after confirming transmission. The Contractor shall document all
communication in a telephone contact log.
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Exhibit B--Section 1
Contract Reports/Deliverables Distribution
Footnotes (con't):
Preliminary Results Delivery Schedule:
If the last sample in the SDG arrives before 5 p.m., the Preliminary
Results are due within the required turnaround time. If the last sample
in the SDG is received after 5 p.m., the Preliminary Results are due
within the required turnaround time beginning at 8 a.m. the following
day. DELIVERABLES ARE TO BE REPORTED TOTAL AND COMPLETE. Concurrent
delivery is required. Delivery shall be made such that all designated
recipients receive the item on the same calendar day.
If the deliverables are due on a Saturday, Sunday, or Federal holiday,
then they shall be delivered on the next business day. Deliverables
delivered after this time will be considered late.
NOTE: As specified in the Contract Schedule (Government Furnished Supplies
and Materials), unless otherwise instructed by the CLP Sample Management
Office based on a Regional decision, the Contractor shall dispose of unused
sample volume and used sample bottles/containers no earlier than sixty (60)
days following submission of the reconciled Complete SDG File. Sample
disposal and disposal of unused sample bottles/containers is the
responsibility of the Contractor, and should be done in accordance with all
applicable laws and regulations governing disposal of such materials.
1.2- Distribution. The following addresses correspond to the "Distribution"
column in Table 1 of Section 1.1.
SMO: USEPA Contract Laboratory Program
Sample Management Office (SMO)1
2000 Edmund Halley Drive
Reston, VA 20191-3436
Region: USEPA Region: The Sample Management Office will provide the
Contractor with the list of addresses for the 10 EPA Regions.
SMO will provide the Contractor with updated Regional
address/name lists as necessary throughout the period of the
contract and identify other client recipients on a
case-by-case basis.
QATS: USEPA Contract Laboratory Program
Quality Assurance Technical Support (QATS) Laboratory2
2700 Chandler Avenue, Building C
Las Vegas, NV 89120
Attn: Data Audit Staff
xThe Sample Management Office (SMO) is a contractor operated facility
operating under the CLASS contract awarded and administered by the EPA.
2The Quality Assurance Technical Support (QATS) Laboratory is a
contractor operated facility operating under the QATS contract awarded and
administered by the EPA.
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
2.0 REPORTING REQUIREMENTS AND ORDER OF DATA DELIVERABLES
2.1 Introduction. The Contractor shall provide reports and other
deliverables as specified in the Contract Schedule (Performance/Delivery
Schedule). The required content and form of each deliverable is
described in this exhibit. All reports and documentation must be:
Legible,
. Clearly labeled and completed in accordance with instructions in
this exhibit,
Arranged in the order specified in this section,
Paginated consecutively in ascending order starting from the SDG
Narrative, and
Copies must be legible and double-sided.
NOTE: Complete SDG files need not be double-sided. (The CSF is
composed of original documents.) However, sample data packages
delivered to SMO must be double-sided.
2.1.1 Requirements for each deliverable item cited in the Contract
Schedule (Contract Performance/Delivery Schedule) are specified in
Sections 2.3 through 2.11. Prior to submission, the Contractor
shall arrange items and the components of each item in the order
listed in these sections.
2.1.2 The Contractor shall use EPA Case numbers (including SDG numbers)
and EPA sample numbers to identify samples received under this
contract, both verbally and in reports/correspondence. The
contract number shall be specified in all correspondence.
2.2 Resubmission of Data. If submitted documentation does not conform to
the above criteria, the Contractor shall resubmit such documentation
with deficiency(ies) corrected, at no additional cost to the Agency.
2.2.1 The Contractor shall respond within seven (7) days to written
requests from data recipients for additional information or
explanations that result from the Government's inspection
activities unless otherwise specified in the contract.
2.2.2 Whenever the Contractor is required to submit or resubmit data as a
result of an on-site laboratory evaluation, or through an
Administrative Project Officer/Technical Project Officer action, or
through a Regional data reviewer's request, the data shall be
clearly marked as ADDITIONAL DATA and shall be sent to both
contractual data recipients (SMO and the Region; and to the EPA
.designated recipient (e.g., QATS) when a written request for the
sample data package has been made). .The Contractor shall include a
cover letter which describes which data are being delivered, to
which EPA Case(s) the data pertain, and who requested the data.
2.2.3 Whenever the Contractor is required to submit or resubmit data as a
result of Contract Compliance Screening (CCS) review by SMO, the
B-7 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
data shall be sent to both contractual data recipients (SMO and the
Region; and to the EPA designated recipient (e.g., QATS) when a
written request for the sample data package has been made). In all
instances, the Contractor shall include a color-coded COVER SHEET
(Laboratory Response To Results of Contract Compliance Screening)
provided by SMO.
2.3 Quality Assurance Plan and Standard Operating Procedures. The Contractor
shall adhere to the requirements in Exhibits E and F.
2.4 Sample Traffic Reports. Each sample received by the Contractor will be
labeled with an EPA sample number, and will be accompanied by a Sample
Traffic Report (TR) bearing the sample number and descriptive information
regarding the sample. The Contractor shall complete the TR (marked "Lab
Copy for Return to SMO"), recording the date of sample receipt and sample
condition upon receipt for each container, and shall sign the TR.
Information shall be recorded for each sample in the SDG.
2.4.1 The Contractor shall submit TRs in SDG sets (i.e., TRs for all
samples in an SDG shall be clipped together), with an SDG cover
sheet attached. The SDG cover sheet shall contain the following
items:
Laboratory name,
Contract number,
Sample analysis price (full sample price from the contract),
Case number, and
List of EPA sample numbers of all samples in the SDG,
identifying the first and last samples received, and their
dates of receipt (LRDs).
NOTE: When more than one sample is received in the first or last
SDG shipment, the "first" sample received would be the lowest
sample number (considering both alpha and numeric designations);
the "last" sample received would be the highest sample number
(considering both alpha and numeric designations).
2.4.2 Each TR shall be clearly marked with the SDG number, entered below
the laboratory receipt date on the TR. The TR for the last sample
received in the SDG shall be clearly marked "SDG--FINAL SAMPLE."
The SDG number is the EPA sample number of the first sample
received in the SDG. When several samples are received together in
the first SDG shipment, the SDG number shall be the lowest sample
number (considering both alpha and numeric designations) in the
first group of samples received under the SDG.
2.4.3 If samples are received at the laboratory with multi-sample TRs,
all the samples on one multi-sample TR may not necessarily be in
the same SDG. In this instance, the Contractor shall make the
appropriate number of photocopies of the TR, and submit one copy
with each SDG cover sheet.
B-8 OLM04.2
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Exhibit B--Section 2
Reporting Requirements.and Order of Data Deliverables
2.5 Sample Data Summary Package. The sample data.summary package shall be
ordered as follows and shall be submitted separately (i.e., separated by
rubber bands, clips, or other means) directly preceding the sample data
package. Sample data forms shall be arranged in increasing EPA sample
number order, considering both letters and numbers. For example, BE400
is a lower sample number than BF100, as E precedes F in the alphabet.
The SDG number shall be reported on all data reporting forms. The sample
data summary package shall be arranged in the same manner as the sample
data package. The sample data summary package shall contain data for all
samples in one SDG of the Case, as follows: (See Section 2.6 for a
detailed description of each item.)
2.5.1 SDG Narrative.
2.5.2 Arranged by fraction and by sample within each fraction: tabulated
target compound results (Form I) for the volatile, semivolatile,
and pesticide fractions and tentatively identified compounds (Form
I TIC) for the volatile and semivolatile fractions only.
2.5.3 Arranged by fraction: system monitoring compound or surrogate
spike analysis results (Form II) by matrix (water and/or soil) for
the volatile, semivolatile, and pesticide fractions; and for soil,
by concentration (low or medium), for volatile and semivolatile
fractions.
2.5.4 Arranged by fraction: matrix spike/matrix spike duplicate results
.(Form III) for the volatile, semivolatile, and pesticide fractions.
2.5.5 Arranged by fraction: blank data (Form IV) and tabulated results
(Form I) for the volatile, semivolatile, and pesticide fractions
including tentatively identified compounds (Form I TIC) for the
volatile and semivolatile fractions only.
2.5.6 Arranged by fraction: internal standard area data (Form VIII) for
the volatile and semivolatile fractions only.
2.6 Sample Data Package. The sample data package is divided into the five
major units described in this section. The last three units are each
specific to an analytical fraction (volatiles, semivolatiles, and
pesticides/Aroclors). If the analysis of a fraction is not required,
then that fraction-specific unit is not required as a deliverable. The
sample data package shall include data for the analyses of all samples in
one SDG, including: field samples, dilutions, reanalyses, blanks, matrix
spikes, and matrix spike duplicates. The Contractor shall retain a copy
of the sample data package for 365 days after final acceptance of data.
After this time, the Contractor may dispose of the package.
2.6.1 SDG Narrative. This document shall be clearly labeled "SDG
Narrative" and shall contain: laboratory name; Case number; EPA
sample numbers in the SDG, differentiating between initial analyses
and reanalyses; SDG number; Contract number,- and detailed
documentation of any quality control, sample, shipment, and/or
analytical problems encountered in processing the samples reported in
the data package. All volatile low level soil samples prepared
B-9 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
according to the Modified SW-846 Method 5035 must be noted in the SDG
Narrative. When using the Modified SW-846 Method 5035, all
discrepancies between sample weights determined in the field and in
the laboratory shall be documented in the SDG Narrative.
All GC columns used for analysis shall be documented here, by
fraction. List- the GC column identification--brand name, the
internal diameter, in mm, and the length, in meters, packing/coating
material and film thickness. The trap used for volatile analysis
shall be described here. List trap name, when denoted by the
manufacturer, its composition (packing material/brand name, amount of
packing material, in length, cm). All tentatively identified alkanes
and their estimated concentrations are to be reported here. The EPA
sample number, the CAS number, when available, the alkane compound
(or series) name, and its estimated concentration shall be provided
in a tabular format. The Contractor shall include any technical and
administrative problems encountered, the corrective actions taken,
the resolution, and an explanation for all flagged edits (e.g.,
manual edits) on quantitation lists. The Contractor shall document
in the SDG Narrative all instances of manual integration.
The SDG Narrative shall contain the following statement, verbatim:
"I certify that this data package is in compliance with the terms and
conditions of the contract, both technically and for completeness,
for other than the conditions detailed above. Release of the data
contained in this hardcopy data package and in the computer-readable
data submitted on diskette has been authorized by the laboratory
manager or his/her designee, as verified by the following signature."
This statement shall be directly followed by an original signature'of
the laboratory manager or his/her designee with a typed line below it
containing the signer's name and title, and the date of signature.
2.6.1.1 Whenever data from sample reanalyses are submitted, the Contractor
shall state in the SDG Narrative for each reanalysis whether the
reanalysis is billable, and if so, why.
2.6.1.2 The Contractor shall list the pH determined for each water sample
submitted for volatiles analysis. This information may appear as
a simple list or table in the SDG Narrative. The purpose of this
pH determination is to ensure that all water volatiles samples
were acidified in the field. No pH adjustment is to be performed
by the Contractor on water samples for volatiles analysis.
2.6.2 Traffic Reports. The Contractor shall include a copy of the TRs
submitted in Section 2.4 for all of the samples in the SDG. The TRs
shall be arranged in increasing EPA sample number order, considering
both letters and numbers. Copies of the SDG cover sheet are to be
included with the copies of the TRs. (See Section 2.4 for more
detail on reporting requirements for TRs.) In the case of multi-
sample TRs, the Contractor shall make the appropriate number of
photocopies of the TR so that a copy is submitted with each
applicable data package. In addition, in any instance where samples
from more than one multi-sample TR are in the same data package, the
Contractor shall submit a copy of the SDG cover- sheet with copies of
the TRs.
B-10 OLM04.2
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Exhibit B--Section 2
Reporting Requirements.and Order of Data Deliverables
Volatiles
2.6.3 Volatiles Data
2.6.3.1 Volatiles QC Summary
2.6.3.1.1 System Monitoring Compound Summary (Form II, VOA-1, VOA-2).
2.6.3.1.2 Matrix Spike/Matrix Spike Duplicate Summary (Form III, VOA-1,
VOA-2).
2.6.3.1.3 Method Blank Summary (Form IV VOA): If more than a single form
is necessary, forms shall be arranged in chronological order by
date of analysis of the blank, by instrument.
2.6.3.1.4 GC/MS instrument performance check (Form V VOA): If more than
a single form is necessary, forms shall be arranged in
chronological order, by instrument.
2.6.3.1.5 Internal Standard Area and RT Summary (Form VIII VOA): If more
than a single form is necessary, forms shall be arranged in
chronological order, by instrument.
2.6.3.2 Volatiles Sample Data. Sample data shall be arranged in packets
with the Organic Analysis Data Sheet (Form I, VOA-1, VOA-2,
including Form I VOA-TIC), followed by the raw data for volatile
samples. These sample packets shall be placed in order of
increasing EPA sample number order, considering both letters and
numbers.
2.6.3.2.1 Target Compound Results, Organic Analysis Data Sheet (Form I,
VOA-1, VOA-2). Tabulated results (identification and
quantitation) of the specified target compounds (Exhibit C,
Volatiles) shall be included. The validation and release of
these results are authorized by a specific, signed statement in
the SDG Narrative (see Section 2.6.1). In the event that the
laboratory manager cannot verify all data reported for each
sample, the laboratory manager shall provide a detailed
description of the problems associated with the sample in the
SDG Narrative.
2.6.3.2.2 Tentatively Identified Compounds (Form I VOA-TIC). Form I
VOA-TIC is the tabulated list of the highest probable match for
up to 30 organic compounds that are not system monitoring
compounds or internal standard compounds and are not listed in
Exhibit C. It includes the Chemical Abstracts Service (CAS)
registry number (if applicable), tentative identification, and
estimated concentration. This form shall be included even if
no compounds are found. If no compounds are found, indicate
this on the form by entering "0" in the field for "Number
Found."
2.6.3.2.3 Reconstructed Total Ion Chromatograms (for each sample or
sample extract, including dilutions and reanalyses).
Reconstructed ion chromatograms shall be normalized to the
B-ll OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Volatiles
largest nonsolvent component and shall contain the following
header information:
EPA sample number,
Date and time of analysis,
GC/MS instrument identifier,
Lab file identifier, and
Analyst ID.
2.6.3.2.3.1 Internal standards and system monitoring compounds shall be
labeled with the names of compounds, either directly out
from the peak or on a printout of retention times if
retention times are printed over the peak.
2.6.3.2.3.2 If automated data system procedures are used for preliminary
identification and/or quantitation of the target compounds,
the complete data system report shall be included in all
sample data packages, in addition to the reconstructed ion
chromatogram. The complete data system report shall include
all of the information listed below. For laboratories which
do not use the automated data system procedures, a
laboratory "raw data sheet" containing the following
information shall be included in the sample data package, in
addition to the chromatogram:
EPA sample number,
Date and time of analysis,
Retention time or scan number of identified target
compounds,
Ion used for quantitation with measured area,
Copy of area table from data system,
GC/MS instrument identifier,
Lab file identifier, and
Analyst ID.
2.6.3.2.3.3 In all instances where the data system report has been
edited, or where manual integration or quantitation has been
performed, the GC/MS operator shall identify such edits or
manual procedures by initialing and dating the changes made
to the report, and shall include the integration scan range.
In addition, a hardcopy printout of the EICP of the
quantitation ion displaying the manual integration shall be
included in the raw data. This applies to all compounds
B-12 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Volatiles
listed in Exhibit C (Volatiles),:internal standards and
system monitoring compounds.
EICPs displaying each manual integration.
2.6.3.2.4 Other Required Information. For each sample, by each compound
identified, the following items shall be included in the data
package.
Copies of raw spectra and copies of background-subtracted
mass spectra of target compounds listed in Exhibit C
(Volatiles) that are identified in the sample and
corresponding background-subtracted target compound
standard mass spectra. Spectra shall be labeled with EPA
sample number, lab file identifier, date and time of
analysis, and GC/MS instrument identifier. Compound names
shall be clearly marked on all spectra.
Copies of mass spectra of organic compounds not listed in
Exhibit C with associated best-match spectra (minimum of
one, maximum of three best matches). Spectra shall be
labeled with EPA sample number, lab file identifier, date
and time of analysis, and GC/MS instrument identifier.
Compound names shall be clearly marked on all spectra.
2.6.3.3 Volatiles Standards Data
2.6.3.3.1 Initial calibration data (Form VI, VOA-1, VOA-2) shall be
included in order by instrument, if more than one instrument is
used.
Volatile standard(s) reconstructed ion chromatograms and
quantitation reports for the initial (five-point)
calibration, labeled as in Section 2.6.3.2.3. Spectra are
not required.
All initial calibration data that pertain to samples in the
data package shall be included, regardless of when it was
performed and for which Case. When more than one initial
calibration is performed, the data shall be in
chronological order, by instrument.
EICPs displaying each manual integration.
2.6.3.3.2 Continuing calibration data (Form VII, VOA-1, VOA-2) shall, be
included in order by instrument, if more than one instrument is
used.
Volatile standard(s) reconstructed ion chromatograms and
quantitation reports for all continuing (12-hour)
calibrations, labeled as in Section 2.6.3.2.3. Spectra are
not required.
B-13 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Volatiles
When more than one continuing calibration is performed,
forms shall be in chronological order, by instrument.
EICPs displaying each manual integration.
2.6.3.3.3 In all instances where the data system report has been edited,
or where manual integration or quantitation has been performed,
the GC/MS operator shall identify such edits or manual
procedures by initialing and dating the changes made to the
report, and shall include the integration scan range. In
addition, a hardcopy printout of the EICP of the quantitation
ion displaying the manual integration shall be included in the
raw data. This applies to all compounds listed in Exhibit C
(Volatiles), internal standards and system monitoring
compounds.
2.6.3.4 Volatiles Raw QC Data
2.6.3.4.1 BFB data shall be arranged in chronological order by instrument
for each 12-hour period, for each GC/MS system utilized.
Bar graph spectrum, labeled as in Section 2.6.3.2.3.
Mass listing, labeled as in Section 2.6.3.2-. 3.
Reconstructed total ion chromatogram, labeled as in Section
2.6.3.2.3.
2.6.3.4.2 Blank data shall be arranged by type of blank (method, storage,
instrument) and shall be in chronological order by instrument.
NOTE: This order is different from that used for samples.
Tabulated results (Form I, VOA-1, VOA-2).
Tentatively identified compounds (Form I VOA-TIC) even if
none are found.
Reconstructed ion chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.3.2.3.
Target compound spectra with laboratory-generated standard,
labeled as in Section 2.6.3.2.4. Data systems which are
incapable of dual display shall provide spectra in the
following order:
Raw target compound spectra.
Enhanced or background-subtracted spectra.
Laboratory-generated standard spectra.
GC/MS library search spectra for tentatively identified
compounds, labeled as in Section 2.6.3.2.4.
B-14 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Semivolatiles
Quantitation/calculation of tentatively identified compound
concentrations.
2.6.3.4.3 Volatiles Matrix Spike Data
Tabulated results (Form I, VOA-1, VOA-2) of target
compounds. Form I VOA-TIC is not required.
Reconstructed ion'chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.3.2.3. Spectra are
not required.
2.6.3.4.4 Volatiles Matrix Spike Duplicate Data
Tabulated results (Form I, VOA-1, VOA-2) of target
compounds. Form I VOA-TIC is not required.
Reconstructed ion chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.3.2.3. Spectra are
not required.
2.6.4 Semivolatiles Data
2.6.4.1 Semivolatiles QC Summary
2.6.4.1.1 Surrogate Percent Recovery Summary (Form II, SV-1, SV-2).
2.6.4.1.2 Matrix Spike/Matrix Spike Duplicate Summary (Form III, SV-1,
SV-2)
2.6.4.1.3 Method Blank Summary (Form IV SV): If more than a single form
is necessary, forms shall be.arranged in chronological order by
date of analysis of the blank, by instrument.
2.6.4.1.4 GC/MS Instrument Performance Check (Form V SV): If more than a
single form is necessary, forms shall be arranged in
chronological order, by instrument.
2.6.4.1.5 Internal Standard Area and RT Summary (Form VIII, SV-1, SV-2):
If more than a single form is necessary, forms shall be
arranged in chronological order, by instrument.
2.6.4.2 Semivolatiles Sample Data. Sample data shall be arranged in
packets with the Organic Analysis Data Sheet (Form I, SV-1, SV-2,
including Form I SV-TIC), followed by the raw data for
semivolatile samples. These sample packets shall be placed in
increasing EPA sample number order, considering both letters and
numbers.
2.6.4.2.1 Target Compound Results, Organic Analysis Data Sheet (Form I
SV-1, SV-2). Tabulated results (identification and
quantitation) of the specified target compounds (Exhibit C,
Semivolatiles) shall be .included. The validation and release
of these results are authorized by a specific, signed statement
B-15 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Semivolatiles
in the SDG Narrative (see Section. 2.6.1) . In the event that
the laboratory manager cannot verify all data reported for each
sample, the laboratory manager shall provide a detailed
description of the problems associated with the sample in the
SDG Narrative.
2.6.4.2.2 Semivolatile Tentatively Identified Compounds (Form I SV-TIC).
Form I SV-TIC is the tabulated list of the highest probable
match for up to 30 of the non-surrogate/non-internal standard
organic compounds that are not listed in Exhibit C (Volatiles,
Semivolatiles). It includes the CAS registry number (if
applicable), tentative identification, and estimated
concentration. This form shall be included even if no
compounds are found. If no compounds are found, indicate this
on the form by entering "0" in the field for "number found."
2.6.4.2.3 Reconstructed Total Ion Chromatograms (for each sample,
including dilutions and reanalyses). Reconstructed ion
chromatograms shall be normalized to the largest nonsolvent
component and shall contain the following header information:
EPA sample number,
Date and time of analysis,
GC/MS instrument identifier,
Lab file identifier, and
Analyst ID.
2.6.4'. 2.3.1 Internal standards and surrogate compounds shall be labeled
with the names of compounds, either directly out from the
peak or on a printout of retention times if retention times
are printed over the peak.
2.6.4.2.3.2 If automated data system procedures are used for preliminary
identification and/or quantitation of the target compounds,
the complete data system report shall be included in all
sample data packages, in addition to the reconstructed ion
chromatogram. The complete data system report shall include
all of the information listed below. For laboratories which
do not use the automated data system procedures, a
laboratory "raw data sheet" containing the following
information shall be included in the sample data package, in
addition to the chromatogram.
EPA sample number,
Date and time of analysis,
Retention time or scan number of identified target
compounds,
B-16 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Semivolatiles
Ion used for quantitation with.measured area,
Copy of area table from data system,
GC/MS instrument identifier, and
Lab file identifier.
2.6.4.2.3.3 In all instances where the data system report has been
edited, or where manual integration or quantitation has been
performed, the GC/MS operator shall identify such edits or
manual procedures by initialing and dating the changes made
to the report, and shall include the integration scan range.
In addition, a hardcopy printout of the EICP of the
quantitation ion displaying the manual integration shall be
included in the raw data. This applies to all compounds
listed in Exhibit C (Semivolatiles), internal standards, and
system monitoring compounds.
EICPs displaying each manual integration.
2.6.4.2.4 Other Required Information. For each sample, by each compound
identified, the following shall be included in the data
package.
Copies of raw spectra and copies of background-subtracted
mass spectra of target compounds listed in Exhibit C
(Semivolatiles) that are identified in the sample and
corresponding background-subtracted target compound
standard mass spectra. Spectra shall be labeled with EPA
sample number, lab file identifier, date and time of
analysis, and GC/MS instrument identifier compound names
shall be clearly marked on all spectra.
Copies of mass spectra of non-surrogate/non-internal
standard organic compounds not listed in Exhibit C
(Volatiles and Semivolatiles) with associated best-match
spectra (maximum of three best matches). This includes the
mass spectra for tentatively identified alkanes. Spectra
shall be labeled with EPA sample number, lab file
identifier, date and time of analysis, and GC/MS instrument
identifier compound names shall be clearly marked on all
spectra.
2.'6.4. 3 Semivolatiles Standards Data
2.6.4.3.1 Initial calibration data (Form VI SV-1, SV-2) shall be included
in order by instrument, if more than one instrument used.
Semivolatile standard(s) reconstructed ion chromatograms
and quantitation reports for the initial (five-point)
calibration, labeled as in Section 2.6.4.2.3. Spectra are
not required.
B-17 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Semivolatiles
All initial calibration data that pertain to samples in the
data package shall be included, regardless of when it was
performed and for which Case. When more than one initial
calibration is performed, the data shall be in
chronological order, by instrument.
EICPs displaying each manual integration.
2.6.4.3.2 Continuing calibration data (Form VII SV-1, SV-2) shall be
included in order by instrument, if more than one instrument is
used.
Semivolatile standard(s) reconstructed ion chromatograms
and quantitation reports for all continuing (12-hour)
calibrations, labeled as in Section 2.6.4.2.3. Spectra are
not required.
When more than one continuing calibration is performed,
forms shall be in chronological order, by instrument.
EICPs displaying each manual integration-.
2.6.4.3.3 In all instances where the data system report has been edited,
or where manual integration or quantitation has been performed,
the GC/MS operator shall identify such edits or manual
procedures by initialing and dating the changes made to the
report, and shall include the integration scan range. In
addition, a hardcopy printout of the EICP of the quantitation
ion displaying the manual integration shall be included in the
raw data. This applies to all compounds listed in Exhibit C
(Semivolatiles), internal standards, and system monitoring
compounds.
2.6.4.4 Semivolatiles Raw QC Data
2.6.4.4.1 DFTPP data shall be arranged in chronological order by
instrument for each 12-hour period, for each GC/MS system
utilized.
Bar graph spectrum, labeled as in Section 2.6.4.2.3.
Mass listing, labeled as in Section 2.6.4.2.3.
Reconstructed total ion chromatogram, labeled as in Section
2.6.4.2.3.
2.6.4.4.2 Blank data shall be included in chronological order by
extraction date.
NOTE: This order is different from that used for samples.
Tabulated results (Form I SV-1, SV-2).
B-18 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Semivolatiles
Tentatively identified compounds (Form I SV-TIC) even if
none are found.
Reconstructed ion chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.4.2.3.
Target compound spectra with laboratory-generated standard,
labeled as in Section 2.6.4.2.4. Data systems which are
incapable of dual display shall provide spectra in the
following order:
Raw target compound spectra.
Enhanced or background-subtracted spectra.
Laboratory-generated standard spectra.
GC/MS library search spectra for tentatively identified
compounds, labeled as in Section 2.6.4.2.4.
Quantitation/calculation of tentatively identified compound
concentrations.
2.6.4.4.3 Semivolatiles Matrix Spike Data
. Tabulated results (Form I SV-1, SV-2) of target compounds.
Form I SV-TIC is not required.
Reconstructed ion chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.4.2.3. Spectra are
not required.
2.6.4.4.4 Semivolatiles Matrix Spike Duplicate Data
Tabulated results (Form I SV-1, SV-2) of target compounds.
Form I SV-TIC is not required.
Reconstructed ion chromatogram(s) and quantitation
report(s), labeled as in Section 2.6.4.2.3. Spectra are
not required.
| 2.6.4.4.5 Semivolatile GPC Data. The two most recent UV traces of the
j GPC calibration solution, and the reconstructed ion
chromatogram and data system reports for the GPC blank shall be
arranged in chronological order by GPC for the GPC calibration.
UV traces labeled with the GPC column identifier, date of
calibration, and compound names. Compound names shall be
placed directly out from the peak, or on the printout of
retention times when the retention times are printed
directly over the peak.
B-19 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Pesticides/Aroclors
Reconstructed ion chromatogram and data system report(s)
labeled as specified in Section 2.6.4.2.3 for GPC blank
analysis.
Reconstructed ion chromatogram and data system report(s)
for all standards used to quantify compounds in the GPC
blank labeled as specified in Section 2.6.4.2.3 (continuing
calibration standard).
2.6.5 Pesticide/Aroclor Data
2.6.5.1 Pesticide/Aroclor QC Summary
2.6.5.1.1 Surrogate Percent Recovery Summary (Form II, PEST-1, PEST-2).
2.6.5.1.2 Matrix Spike/Matrix Spike Duplicate Summary (Form III, PEST-1,
PEST-2).
2.6.5.1.3 Method Blank Summary (Form IV PEST): If more than a single
form is necessary, forms shall be arranged in chronological
order by date of analysis of the blank.
2.6.5.2 Pesticide/Aroclor Sample Data. Sample data shall be arranged in
packets with the Organic Analysis Data Sheet (Form I PEST),
followed by the raw data for pesticide samples. These sample
packets should then be placed in order of increasing' EPA sample
number, considering both letters and numbers.
2.6.5.2.1 Target Compound Results, Organic Analysis Data Sheet (Form I
PEST). Tabulated results (identification and quantitation) of
the specified target compounds (Exhibit C, Pesticides/Aroclors)
shall be included. The validation and release of these results
is authorized by a specific, signed statement in the SDG
Narrative (see Section 2.'6.1). In the event that the
laboratory manager cannot verify all data reported for each
sample, the laboratory manager shall provide a detailed
description of the problems associated with the sample in the
SDG Narrative.
2.6.5.2.2 Copies of Pesticide Chromatograms. Positively identified
compounds shall be labeled with the names of compounds, either
directly out from the peak on the chromatogram, or on a
printout of retention times on the data system printout if
retention times are printed over the peak on the chromatogram.
All chromatograms shall meet the acceptance criteria in Exhibit
D PEST, and shall be labeled with the following information:
EPA sample number,
Volume injected (fj.Ii) ,
Date and time of injection,
B-20 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Pesticides/Aroclors
GC column identifier (by stationary-phase and internal
diameter),
GC instrument identifier, and
f Scaling factor (label the x and y axes using a numerical
scale).
2.6.5.2.3 Copies of pesticide chromatograms from the second GC column
shall be included and labeled as in Section 2.6.5.2.2.
2.6.5.2.4 Data System Printout. A printout of retention time and
corresponding peak height or peak area shall accompany each
chromatogram. The printout shall be labeled with the EPA
sample number. In all instances where the data system report
has been edited, or where manual integration or quantitation
has been performed, the GC/EC operator must identify such edits
or manual procedures by initialing and dating the changes made
to the report, and shall include the integration time range.
2.6.5.2.5 All manual work sheets shall be included in the sample data
package.
2.6.5.2.6 Other Required Information. If pesticides/Aroclors are
confirmed by GC/MS, the Contractor shall submit copies of
reconstructed ion chromatograms, raw spectra, and background-
subtracted mass spectra of target compounds listed in Exhibit C
(Pesticides/Aroclors) that are identified in the sample and
corresponding background-subtracted TCL standard mass spectra.
Compound names shall be clearly marked on all spectra. For
multicomponent pesticides/Aroclors confirmed by GC/MS, the
Contractor shall submit mass spectra of three major peaks of
multicomponent compounds from samples and standards.
2.6.5.3 Pesticide/Aroclor Standards Data
2.6.5.3.1 Initial Calibration of Single Component Analytes (Form VI PEST-
1, PEST-2): for all GC columns, all instruments, in
chronological order by GC column and instrument.
2.6.5.3.2 Initial Calibration of Multicomponent Analytes (Form VI PEST-
3): for all GC columns, all instruments, in chronological
order by GC column and instrument.
2.6.5.3.3 Analyte Resolution Summary (Form VI PEST-4): for all GC
columns and instruments, in chronological, order by GC column
and instrument.
2.6.5.3.4 Performance Evaluation Mixture (Form VI PEST-5): for all GC
columns and instruments, in chronological order by GC column
and instrument. .
B-21 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order"of Data Deliverables
Pesticides/Aroclors
2.6.5.3.5 Individual-Standard Mixture A (Form VI PEST-6): for all GC
columns and instruments, in chronological order by GC column
and instrument.
2.6.5.3.6 Individual Standard Mixture B (Form VI PEST-7): for all GC
columns and instruments, in chronological order by GC column
and instrument.
2.6.5.3.7 Calibration Verification Summary (Form VII PEST-1): for all
performance evaluation mixtures and instrument, blanks, on all
GC columns and instruments, in chronological order by GC column
and instrument.
2.6.5.3.8 Calibration Verification Summary (Form VII PEST-2): for all
mid-point concentrations of Individual Standard Mixtures A and
B and instrument blanks used for calibration verification, on
all GC columns and instruments, in chronological order-by GC
column and instrument.
2.6.5.3.9 Analytical Sequence (Form VIII PEST): for all GC columns and
instruments, in chronological order by GC column and
instrument.
2.6.5^-3.10 Florisil Cartridge Check (Form IX PEST-1): for all lots of
-:- cartridges used to process samples in the SDG.
2.6.5/3.11 Pesticide GPC Calibration Verification (Form IX PEST-2): for
all GPC columns, in chronological order by calibration
verification date.
2.6.5^3.12 Pesticide Identification Summary for Single Component Analytes
Ti (Form X PEST-1): for all samples with positively identified
single component analytes, in order by increasing EPA sample
number.
2.6.5.3.13 Pesticide Identification Summary for Multicomponent Analytes
(Form X PEST-2): for all samples with positively identified
multicomponent analytes, in order by increasing EPA sample
number.
2.6.5.3.14 Chromatograms and data system printouts shall be included for
all standards including the following:
Resolution check mixture.
Performance evaluation mixtures, all.
Individual Standard Mixture A, at three concentrations,
each initial calibration.
Individual Standard Mixture B, at three concentrations,
each initial calibration.
B-22 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
Pesticides/Aroclors
All multicomponent analytes (toxaphene and Aroclors), each
initial calibration.
All mid-point concentrations of Individual Standard
Mixtures A and B used for calibration verification.
All multicomponent analyte standards analyzed for
confirmation.
2.6.5.3.15 A printout of retention time and corresponding peak height or
peak area shall accompany each chromatogram. The printout
shall be labeled with the EPA sample number. In addition, all
chromatograms shall meet the acceptance criteria in Exhibit D
PEST, and shall be labeled with the following:
EPA sample number for the standard. (e.g., INDAL1, INDAM2,
etc.). See Section 4 for details.
Label all standard peaks for all individual compounds
either directly out from the peak on the chromatogram or on
the printout of retention times on the data system printout
if retention times are printed over the peak on the
chromatogram.
Total nanograms injected for each standard. When total
nanograms injected appear on the printout, it is not
necessary to include them on the chromatogram.
Date and time of injection.
GC column identifier (by stationary phase and internal
diameter).
GC instrument identifier:
Scaling factor (label the x and y axes using a numerical
scale).
NOTE: In all instances where the data system report has been
edited, or where manual integration or quantitation has been
performed, the GC/EC operator must identify such edits or
manual procedures by initialing and dating the changes made to
the report, and shall include the integration time range.
2.6.5.4 Pesticide/Aroclor Raw QC Data
2.6.5.4.1 Blank data shall be arranged by type of blank (method,
instrument, sulfur cleanup) and shall be in chronological order
by instrument.
NOTE: This order is different from that used for samples.
Tabulated results (Form I PEST).
; B-23 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverabies
Pesticides/Aroclors
Chromatogram(s) and data system printout(s) for each GC
column and instrument used for analysis, labeled as in
Sections 2.6.5.2.2 and 2.6.5.2.4.
2.6.5.4.2 Matrix Spike Data
Tabulated results (Form I PEST) of target compounds.
Chromatogram(s) and data system printout(s), labeled as in
Sections 2.6.5.2.2 through 2.6.5.2.4.
2.6.5.4.3 Matrix Spike Duplicate Data
Tabulated results (Form I PEST) of target compounds.
Chromatogram(s) and data system printout(s), labeled as in
Sections 2.6.5.2.2 through 2.6.5.2.4.
2.6.5.5 Raw GPC Data
2.6.5.5.1 GPC Calibration. The UV traces for the GPC calibration
solution, chromatograms, and the data system reports for the
GPC blank shall be arranged in chronological order for the GPC
calibration.
UV traces labeled with the GPC column identifier, date of
calibration, and compound names. Compound names shall be
placed directly out from the peak, or on the printout of
retention times when the retention times are printed '
directly over the peak.
Chromatogram and data system report(s) labeled as specified
in Sections 2.6.5.2.2 and 2.6.5.2.4 for GPC blank analyses.
Chromatogram and data system report(s) for all standards
used to quantify compounds in the GPC blank labeled as
specified in Section 2.6.5.3.15 (i.e., Individual Standard
Mixture A, Individual Standard Mixture B, and the
Aroclor/toxaphene standards).
2.6.5.5.2 GPC Calibration Verification. The Chromatogram and the data
system report(s) shall be arranged in chronological order for
the GPC calibration check.
Chromatograms and data system printouts labeled as
specified in Sections 2.6.5.2.2 and 2.6.5.2.4 for the GPC
calibration verification solution analyses.
Chromatogram and data system report(s) for standards used
to quantify compounds in the GPC calibration verification
solution or used to assess the Aroclor pattern labeled as
specified in Section 2.6.5.3.15 (i.e., Individual Standard
Mixtures A and B and Aroclor Standard Mixture 1016/1260
from the initial calibration sequence).
B-24 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
2.6.5.6 Raw Florisil Data. The chromatogram and data system report(s)
shall be arranged in chronological order by Florisil cartridge
performance check analyses.
Chromatograms and data system reports labeled as specified in
Sections 2.6.5.2.2 and 2.6.5.2.4 for the florisil cartridge
performance check analyses.
Chromatograms and data system reports for standard analyses
used to quantify compounds in the Florisil cartridge
performance check analysis, labeled as specified in Section
2.6.5.3.15 (i.e., Individual Standard Mixture A and Individual
Standard Mixture B and the 2,4,5 Trichlorophenol solution).
2.7 Complete SDG File. As specified in Section 1, the Contractor shall
deliver one Complete SDG File (CSF) including the original sample data
package to the Region concurrently with delivery of the sample data
package to SMO. Delivery to EPA designated recipient (e.g., QATS) is
only required upon written request.
2.7.1 The CSF will contain all original documents specified in Sections 3
and 4 and in Form DC-2 (see Section 4). No photocopies of original
documents will be placed in the CSF unless the original data was
initially written in a bound notebook, maintained by the Contractor,
or the originals were previously submitted to the Agency with another
Case/SDG in accordance with the requirements described in Exhibit F.
The contents of the CSF shall be numbered according to the
specifications described in Section 3.20.
2.7.2 The CSF will consist of the following original documents in addition
to the documents in the sample data package.
NOTE: All SDG-related documentation may be used or admitted as
evidence in subsequent legal proceedings. Any other SDG-specific
documents generated after the CSF is sent to EPA, as well as copies
that are altered in any fashion, are also deliverables to EPA.
Deliver the original to the Region and a copy to SMO. Delivery to
EPA designated recipient (e.g., QATS) is only .upon written request.
2.7.2.1 The original sample data package.
2.7.2.2 A completed and signed document inventory sheet (Form DC-2).
2.7.2.3 All original shipping documents including, but not limited to, the
following documents:
EPA Chain-of-Custody Record,
Airbills (if an airbill is not received, include a hardcopy
receipt requested from the shipping company or a printout of
the shipping company's electronic tracking information),
EPA Traffic Reports, and
Sample tags (if present) sealed in plastic bags.
,B-25 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
2.7.2.4 All original receiving documents including, but not limited to,
the following documents:
Form DC-1,
Other receiving forms or copies of receiving logbooks, and
SDG cover sheet.
2.7.2.5 All original laboratory records, not already submitted in the
sample data package, of sample transfer, preparation, and analysis
including, but not limited to, the following documents:
Original preparation and analysis forms or copies of
preparation and analysis logbook pages,
Internal sample and sample extract transfer chain-of-custody
records,
Screening records, and
All instrument output, including strip charts from screening
activities.
2.7.2.6 All other original SDG-specific documents in the possession of the
Contractor including, but not limited to, the following documents:
Telephone contact logs,
Copies of personal logbook pages,
All handwritten SDG-specific notes, and
Any other SDG-specific documents not covered by the above.
2.7.3 If the Contractor does submit SDG-specific documents to EPA after
submission of the CSF, the documents should be identified with unique
accountable numbers, a revised Form DC-2 should be submitted, and the
unique accountable numbers and locations of the documents in the CSF
should be recorded in the "Other Records" section on the revised Form
DC-2. Alternatively, the Contractor may number the newly submitted
SDG-specific documents to EPA as a new CSF and submit a new Form DC-
2. The revised Form DC-2 or new Form DC-2 should be submitted to the
EPA Regions only.
2.8 Data in Computer-Readable Format. The Contractor shall provide a
computer-readable copy of the data on data reporting Forms I-X for all
samples in the SDG as specified in Exhibit H, and delivered as specified
in the Contract Schedule (Contract Performance/Delivery Schedule).
Computer-readable data deliverables shall be submitted on IBM or
IBM-compatible, 3.5-inch high-density 1.44 M-byte diskette (or via an
alternate means of electronic transmission approved in advance by the
EPA) .
B-26 OLM04.2
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Exhibit B--Section 2
Reporting Requirements and Order of Data Deliverables
2.8.1 When submitted, the diskette(s) shall be packaged and shipped in such
a manner that the diskette(s) cannot be bent or folded, and will not
be exposed to extreme heat or cold or any type of electromagnetic
radiation. The diskette(s) shall be included in the same shipment as
the hardcopy data and shall, at a minimum, be enclosed in a diskette
mailer. The diskette(s) shall be labeled as specified in Exhibit H,
Section 8.4.
2.8.2 The data shall be recorded in ASCII, text file format, and shall
adhere to the file, record, and field specifications listed in
Exhibit H.
2.9 Preliminary Results. The Form I data results shall be submitted for all
samples in one SDG of a Case. This includes tabulated target compound
results (Form I) for the volatile, semivolatile, and pesticide
fractions, and tentatively identified compounds (Form I TIC) for the
volatile and semivolatile fractions. The Contractor shall clearly
identify the Preliminary Results by labeling each Form I and Form I TIC
as "Preliminary Results" under each form title (e.g., under Volatile
Organics Analysis Data Sheet, Volatile Organics Analysis Data Sheet
Tentatively Identified Compounds).
2.10 GC/MS and GC/EC Tapes. The Contractor shall adhere to the requirements
in Exhibit E.
2.11 Extracts. The Contractor shall preserve sample extracts at 4° C (± 2°C)
in bottles/vials with Teflon-lined septa. Extract bottles/vials shall
be labeled with EPA sample number. Case number, and SDG number. The
Contractor shall maintain a logbook of stored extracts, listing EPA
sample numbers and associated Case and SDG numbers. The Contractor
shall retain extracts for 365 days following submission of the
reconciled complete sample data package. During that time, the
Contractor shall submit extracts and associated logbook pages within
seven days following receipt of a written request from the
Administrative Project Officer or Technical Project Officer.
B-27 OLM04.2
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Exhibit B--Section 3
Forms Instructions
General Information
3.0 FORMS INSTRUCTIONS
3.1 Introduction. This"section includes specific instructions for
completing the data reporting forms required under this contract. Each
of the forms are specific to a given fraction (volatile, semivolatile,
or pesticide/Aroclor) and, in some instances, specific to a given matrix
(water or soil) within each fraction. The Contractor shall submit only
those forms pertaining to the fractions analyzed for a given sample(s).
For instance, if a sample is scheduled for volatiles analysis only, the
Contractor shall provide only forms for the volatile fraction. NOTE:
There are two pages relating to the volatile fraction for Forms I, VI,
and VII. There are also two pages relating to the semivolatile fraction
for Forms I, VI, VII, and VIII. Whenever volatiles or semivolatiles are
analyzed and one of these forms is required, both pages (VOA-1 and VOA-
2; SV-1 and SV-2) shall be submitted.
3.2 General Information. The Contractor shall report values on the hardcopy
forms according to the individual form instructions in this section.
For example, results for concentrations of volatile target compounds
shall be reported to two significant figures if the value is greater
than or equal to 10. Values that exceed the maximum length allowed
shall be reported to the maximum possible, maintaining the specified
decimal place.
3.2.1 The data reporting forms presented in Section 4 have been designed in
conjunction with the computer-readable data format specified in
Exhibit H. The specific length of each variable for
computer-readable data transmission purposes is also given in Exhibit
H. Information entered on these forms shall not exceed the size of
the field given on the form, including such laboratory-generated
items as lab name and lab sample identifier.
NOTE: The space provided for entries on the hardcopy forms (Section
4) is greater in some instances than the length prescribed for the
variable as written to the electronic deliverable (see Exhibit H).
Greater space is provided on the hardcopy forms for visual clarity.
3.2.2 When submitting data, the Contractor shall reproduce all characters
that appear on the data reporting forms in Section 4. The format of
the forms submitted shall be identical to that shown in the contract.
No information may be added, deleted, or moved from its specified
position without prior written approval of the Administrative Project
Officer. The names of the various fields and compounds (e.g., "Lab
Code," "Chloromethane") shall appear as they do on the forms in the
contract, including the options specified in the form (e.g., "Matrix:
(soil/water)" shall appear, not just "Matrix"). For items appearing
on the uncompleted forms (Section 4), the use of uppercase and
lowercase letters is optional.
3.2.3 Alphabetical entries made on the forms by the Contractor shall be in
ALL UPPERCASE letters (e.g., "LOW", not "Low" or "low"). If an entry
does not fill the entire blank space provided on the form, null
characters shall be used to remove the remaining underscores that
comprise the blank line. See Exhibit H for more detailed
B-28 OLM04.2
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Exhibit B--Section 3
. Forms Instructions
General Information
instructions. However, the Contractor shall not remove the
underscores or vertical bars that delineate "boxes" on the forms.
The only exception would be those underscores at the bottom of a
"box" that are intended as a data entry line. (For instance, on Form
2A, line 30, if data is entered on line 30, it will replace the
underscores.)
3.3 Header Information. Six pieces of information are common to the header
section of each data reporting form: lab name, contract, lab code, case
number, SAS number, and SDG number. Except as noted for SAS number,
this information shall be entered on every form and shall match on every
form.
3.3.1 Lab Name. The lab name shall be the name chosen by the Contractor to
identify the laboratory. It shall not exceed 25 characters.
3.3.2 Contract. Contract refers to the number of the EPA contract under
which the analyses were performed.
3.3.3 Lab Code. The lab code is an alphabetical abbreviation of up to six
letters, as assigned by EPA, to identify the laboratory and aid in
data processing. This lab code will be assigned by EPA at .the time a
contract is awarded, and shall not be modified by the Contractor,
except at the direction of EPA. If a change of name or ownership
occurs at the laboratory, the lab code will remain the same until the
Contractor is directed by EPA to use another lab code.
3.3.4 Case Number. The Case number is the EPA-assigned Case number
associated with the sample. This number is reported on the Traffic
Report.
3.3.5 SAS Number. The SAS number is the EPA-assigned number for analyses
performed under Special Analytical Services. If samples are td be
analyzed under SAS only and reported on these forms, then enter the
SAS number'and leave the Case number blank. If samples are analyzed
according to the Routine Analytical Services (RAS) protocols and have
additional SAS requirements, list both the Case number and the SAS
number on all forms. If there are no SAS requirements, leave the
"SAS No." field blank.
NOTE: Some samples in an SDG may have a SAS number while others may
not.
3.3.6 SDG Number. The "SDG No." field is for the sample delivery group
number. It is the EPA sample number of a field sample assigned to
the SDG and shall be unique for each SDG within a Case. If fractions
of the same field samples are scheduled under different turnaround
times, thus creating separate SDGs containing the same sample
numbers, a different sample number shall be utilized in the
assignment of the SDG number for each sample delivery group. If a
situation arises where there are an insufficient number of samples
for assignment of SDG numbers (i.e., 1 sample with a 7 day turnaround
for volatile analyses and a 14 day turnaround for semivolatile and
B-29 OLM04.2
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Exhibit B--Section 3
Forms Instructions
General Information
pesticide/Aroclor analyses), the Contractor shall contact SMO for the
assignment of an SDG number.
3.3.7 Sample Number. This number appears either in the header information
of the form, or as the left column of a table summarizing data from a
number of samples. When the EPA sample number is entered in the
triple-spaced box in the upper righthand corner of Form I, Form IV,
or Form X, it should be entered on the middle line of the three lines
.that comprise the box.
3.3.7.1 The Contractor shall identify all samples, including: dilutions,
reanalyses, matrix spikes, matrix spike duplicates, blanks, and
standards with an EPA sample number. For field samples, matrix
spikes and matrix spike duplicates, the EPA sample number is the
unique identifying number given in the Traffic Report that
accompanied that sample. In order to facilitate data assessment,
the Contractor shall use the following sample suffixes:
XXXXX = EPA sample number
XXXXXMS = Matrix spike sample
XXXXXMSD = Matrix spike duplicate sample
XXXXXRE = Re-extracted and reanalyzed sample
XXXXXDL = The suffix DL is appended to the EPA
sample number to indicate that the
analytical results are a result of a
dilution of the original analysis ,
(reported as EPA sample XXXXX). See
Exhibit D for requirements for
dilutions.
3.3.7.2 There may be instances when all samples analyzed must be listed on
the form, regardless of whether or not they are part of the SDG
being reported (e.g., Form VIII PEST). In these instances, use
ZZZZZ as the EPA sample number for any sample analysis not
associated with the SDG being reported.
3.3.7.3 For blanks, the Contractor shall use the following identification
scheme for the EPA sample number:
Volatile method blanks shall be identified as VBLK##.
Volatile instrument blanks shall be identified as VIBLK##.
Volatile storage blanks shall be identified as VHBLK##.
Semivolatile-method blanks shall be identified as SBLK##.
Pesticide/Aroclor method blanks and/or sulfur cleanup blanks
shall be identified as PBLK##.
Pesticide/Aroclor instrument blanks shall be identified as
PIBLKtftf.
B-30 OLM04.2
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3.3.7.4
3.3.7.5
3.3.7.6
Exhibit B--Section 3
Forms Instructions
General Information
The EPA sample number shall be unique for each blank within an
SDG. Within a fraction, the Contractor shall achieve this by
replacing the two-character terminator (##) of the identifier with
one or two characters or numbers, or a combination of both. For
example,, possible identifiers for volatile blanks would be VBLK1,
VBLK2, VBLKA1, VBLKB2, VBLK10, VBLKAB, etc. If the method blank
is analyzed on multiple instruments, then an additional two-
character suffix shall be added to make the blank EPA sample
number unique.
Volatile and semivolatile standards shall be identified as
FSTD***##, where
STD =
*** _
Fraction code (V for volatiles; S for semivolatiles).
Standard.
Concentration of volatile standards in ug/L (e.g.,
010, 020, 050, 100, and 200) or the amount injected in
ng for semivolatile standards (e.g., 020, 050, 080,
120, and 160).
One,or two characters, numbers, or combinations of
both to create a unique EPA sample number within an
SDG.
The Contractor shall use the following scheme to identify
pesticide/Aroclor standards:
Name
EPA Sample Number
Individual Mix A (low point)
Individual Mix A (mid-point)
Individual Mix A (high point)
Individual Mix B (low point)
Individual Mix B (mid-point)
Individual Mix B (high point)
Resolution Check
Performance Evaluation Mixture
Toxaphene
Aroclor 1016
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260"
Aroclor 1016/1260 Mix
INDAL##
INDAM##
INDAH##
INDBL##
INDBM##
INDBH##
RESC##
PEMtt#
TOXAPH##
AR1016##
AR1221##
AR1232##
AR1242##
AR1248##
AR1254##
AR1260##
AR1660##
B-31
OLM04.2
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Exhibit B--Section 3
Forms Instructions
General Information
The Contractor shall replace the two-character terminator (##) of
the identifier with one or two characters or numbers, or a
combination of both, to create a unique EPA sample number within
an SDG.
3.3.7.7 If the standards are injected onto both GC columns on the same
instrument simultaneously, the same EPA sample number may be used
for reporting data for the standards for both columns. If
simultaneous injections are not made, then the same number shall
not be used.
3.3.7.8 The EPA sample number for GPC shall be GPC#########, where
######### is the GPC column ID. If the GPC column ID is more than
nine characters, truncate at the ninth character.
3.3.7.9 The EPA sample number for florisil shall be FLO#######tt#, where
######### is the florisil cartridge lot number. If the florisil
cartridge lot number is more than nine characters, truncate at the
ninth character.
3.3.8 Other Common Fields. Several other pieces of information are common
to many of the data reporting forms. These include matrix, sample
weight/volume, level, lab sample identifier, and lab file identifier.
In the "Matrix" field, enter SOIL for soil/sediment samples and
WATER for water samples.
NOTE: The matrix shall be spelled out. Abbreviations such as S
or W shall not be used.
In the "Sample wt/vol" field, enter the number of grams (for
soil) or milliliters (for water) of sample used in the first
blank. Enter the units, either G or ML, in the second blank.
The "Level" field is used for the volatile and semivolatile
fractions. Enter the determination of concentration level made
from the screening of soils. Enter as LOW or MED, not L or M.
All water samples shall be entered as LOW.
NOTE: There is no differentiation between low and medium soil
samples for the pesticide/Aroclor fraction, and no level is
entered on any of these forms.
The lab sample identifier is a unique laboratory-generated
internal identifier pertaining to a particular analysis. The
Contractor can enter up to 12 alpha-numeric characters in the
"Lab Sample ID" field. The Contractor may use the EPA sample
number as the lab sample identifier.
The lab file identifier is the unique laboratory-generated name
of the GC/MS data system file containing information pertaining
to a particular analysis. The Contractor can enter up to 14
alpha-numeric characters in the "Lab File ID" field.
B-32 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
3.3.8.1 The "Instrument ID" field is common to the forms containing
calibration data. The identifier used by the Contractor shall
include some indication of the manufacturer and/or model of the
instrument, and shall contain additional characters that
differentiate between all instruments of the same type in the
laboratory.
3.3.8.2 Forms II, IV, V, VIII, IX, and X contain a field labeled "page _
of _" in the bottom lefthand corner. If the number of entries
required on any of these forms exceeds the available space,
continue entries on another copy of the same fraction-specific
form, duplicating all header information. If a second page is
required, number the pages consecutively (i.e., "page 1 of 2" and
"page 2 of 2"). If a second page is not required, number the page
"page 1 of 1."
NOTE: These forms are fraction-specific, and often matrix-
specific within a fraction. For example, Form II VOA-1 and Form
II VOA-2 are for different data. Therefore, do not number the
pages of all six versions of Form II as "1 of 6," "2 of 6," etc.
Number only pages corresponding to the fraction-specific and
matrix-specific form.
3.3.9 Rounding Rule. For rounding off numbers to the appropriate level of
precision, the Contractor shall follow these rules. If the figure
following those to be retained is less than 5, drop it (round down).
If the figure is greater than or equal to 5, drop it and increase the
last digit to be retained by 1 (round up).
3.4 Organic Analysis Data Sheet (Form I, All Fractions)
3.4.1 Purpose. This form is used for tabulating and reporting sample
analysis, including blank, matrix spike, and matrix spike duplicate
results for target compounds. If all fractions are not requested for
analysis, only the pages for the fractions required shall be
submitted. For example, if only volatiles analysis is requested,
Form I, VOA-1, VOA-2 and Form I VOA-TIC shall be submitted. If only
the pesticide/Aroclor fraction is requested for analysis, Form I PEST
shall be submitted. Furthermore, pesticide instrument blanks
(PIBLKs) shall be reported on a per column/per analysis basis on Form
I PEST. Each PIBLK shall be named with a unique EPA sample number.
3.4.2 Instructions.. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions.
3.4.2.1 For soil samples analyzed-for volatiles, enter the non-decanted
percent moisture in the "% Moisture: not dec." field on Form I,
VOA-1, VOA-2. This is the only percent moisture determination
made for volatiles since the entire contents of the VOA vial are
considered as the sample. For water samples, leave this field
blank.
B-33 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
3.4.2.2 For soil samples analyzed for semivolatiles and
pesticides/Aroclors, enter the values for the percent moisture
determined during the analysis in the "% Moisture" field on Form I
SV-1, SV-2, or PEST. In the "decanted (Y/N)" field, enter Y if
the sample had standing water above the soil/sediment that was
decanted, or N if no water was decanted off the surface of the
sample. Report percent moisture (decanted or not decanted) to the
nearest whole percentage point (e.g., 5%, not 5.3%). For water
samples, method blanks, sulfur cleanup blanks, and instrument
blanks, leave these fields on Form I blank.
3.4.2.3 For volatiles, enter the GC column identifier in the "GC Column"
field on Form I, VOA-1, VOA-2, and the internal diameter in
millimeters (mm), to two decimal places, in the "ID" field. For
packed columns, convert the internal diameter from inches to
millimeters as necessary before entering in the "ID" field.
3.4.2.4 For semivolatiles and pesticides/Aroclors, enter the method of
extraction in the "Extraction" field on Form I SV-1, SV-2, SV-TIC,
and PEST as SEPF for separatory funnel, CONT for continuous
liquid-liquid extraction without hydrophobia membrane, CONH for
continuous liquid-liquid extraction with hydrophobic membrane,
SONG for sonication (soils only), SOXH for Automated Soxhlet
Extraction (soils only), or PFEX for Pressurized Fluid Extraction
(soils only) .
3.4.2.5 If gel permeation chromatography (GPC) was performed, enter Y in
the "GPC Cleanup" field on Form I SV-1, SV-2, or PEST. Enter N in
this field if GPC was not performed.
NOTE: GPC is required for all soil samples analyzed for
semivolatiles and pesticides/Aroclors; therefore, all forms for
soil samples will contain a Y in this field.
3.4.2.6 For soil samples only, enter the pH for semivolatiles and
pesticides/Aroclors, reported to 0.1 pH units, on Form I SV-1,
SV-2, or PEST.
3.4.2.7 Enter the date of sample receipt at the laboratory, as noted on
the Traffic Report (i.e., the VTSR), in the "Date Received" field.
The date shall be entered as MM/DD/YY.
3.4.2.8 Complete the "Date Extracted" and "Date Analyzed" fields in the
same format (MM/DD/YY). When continuous liquid-liquid extraction
procedures are used for water samples, enter the date that the
procedure was started in the "Date Extracted" field. If
separatory funnel (pesticides only), sonication, soxhlet, or
pressurized fluid procedures are used, enter the date that the
procedure was completed in the "Date Extracted" field. For
pesticide/Aroclor samples, enter the date of the first GC analysis
performed in the "Date Analyzed" field. The date of sample
receipt will be compared with the extraction and analysis dates of
each fraction to ensure that contract holding times were not
exceeded.
B-34 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
3.4.2.9 If a medium soil sample is analyzed for volatiles, enter total
volume of the methanol extract in microliters (uL) in the "Soil
Extract Volume" field on Form I, VOA-1, VOA-2. This volume
includes any methanol not collected from the filtration of the
extract through glass wool; the volume is typically 10,000 uL
(i.e., the 10 mL of methanol used for the extraction). If a
medium soil sample is analyzed,, enter the volume of the methanol
extract added to the reagent water in the purge tube and analyzed
in the "Soil Aliquot Volume" field. Enter this volume in
microliters (uL).
9
3.4.2.10 For semivolatiles and pesticides/Aroclors, enter the actual volume
of the most concentrated sample extract, in microliters (uL), in
the "Concentrated Extract Volume" field on Form I SV-1, SV-2 or
PEST. For semivolatiles, this volume will typically be 1,000 uL
(for water) or 500 uL (for water and soil) when GPC is performed.
For pesticides/Aroclors, the volume of the most concentrated
extract will typically be 10,000 uL (for water) or 5,000 uL (for
water and soil) when GPC is performed. For pesticides/Aroclors,
the volume of the most concentrated extract is not the volume
taken through the Florisil and sulfur cleanup steps. If a
dilution of the sample extract is made in a subsequent analysis,
this volume will remain the same, but the dilution factor will
change.
3.4.2.11 For semivolatiles and pesticides/Aroclors, enter the volume of the
sample extract injected into the GC in the "Injection Volume"
field on Form I SV-1, SV-2 or PEST. Report this volume in
microliters (uL) to one decimal place (e.g., 1.0 uL).
NOTE: A 2.0 microliter injection is required for semivolatile
analyses.
3.4.2.12 If pesticides/Aroclors are analyzed using two GC columns connected
to a single injection port, enter the amount of half the volume in
the syringe in the "Injection Volume" field (i.e., assume that the
extract injected is evenly divided between the two columns).
3.4.2.13 If a sample or sample extract has been diluted for analysis, enter
the dilution factor as a single number (e.g., enter 100.0 for a 1
to 100 dilution of the sample) in the "Dilution Factor" field.
The dilution factor shall not be entered as a fraction. If a
sample was not diluted, enter 1.0. Report dilution factors to one
decimal place.
3.4.2.14 If sulfur cleanup is employed, enter Y in the "Sulfur Cleanup"
field; if not, enter N on Form I PEST.
3.4.2.15 For positively identified target compounds, the Contractor shall
report the concentrations as uncorrected for blank contaminants.
3.4.2.16 For volatile and semivolatile results, report analytical results
to one significant figure if the value is less than 10, and two
B-35 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
significant figures if the value is 10 or above. Report all
pesticide/Aroclor results to two significant figures.
3.4.2.17 Enter the appropriate concentration units, ug/L or ug/Kg.
3.4.2.18 Under the column labeled "Q" for qualifier, flag each result with
the specific data reporting qualifiers listed below. When
reporting results to EPA, the Contractor shall use these contract-
'specific qualifiers. The Contractor shall not modify the
qualifiers. Up to five qualifiers may be reported on Form I for
each compound. The Contractor is encouraged to use additional
flags or footnotes (see the X qualifier).
The EPA-defined qualifiers to be used are:
U: This flag indicates the compound was analyzed for but not
detected. The CRQL shall be adjusted according to the
equation listed in Exhibit D. CRQLs are listed in Exhibit C.
J: This flag indicates an estimated value. This flag is used
(1) when estimating a concentration for tentatively
identified compounds where a 1:1 response is assumed, (2)
when the mass spectral and retention time data indicate the
presence of a compound that meets the volatile and
semivolatile GC/MS identification criteria, and the result is
less than the CRQL but greater than zero, and (3) when the
retention time data indicate the presence of a compound that
meets the pesticide/Aroclor identification criteria, and the
result is less than the CRQL but greater than zero. For
example, if the sample quantitation limit is 10 ug/L, but a
concentration of 3 ug/L is calculated, report it as 3J.
NOTE: The J flag is not used and the compound is not
reported as being identified for pesticide/Aroclor results
less than the CRQL if the pesticide residue analysis expert
determines that the peaks used for compound identification
resulted from instrument noise or other interferences (column
bleed, solvent contamination, etc.).
N: This flag indicates presumptive evidence of a compound. This
flag is only used for tentatively identified compounds
(TICs), where the identification is based on a mass spectral
library search. It is applied to all TIC results. For
generic characterization of a TIC, such as chlorinated
hydrocarbon, the N flag is not used.
P: This flag is used for a pesticide/Aroclor target analyte when
there is greater than 25% difference for detected
concentrations between the two GC columns (see Form X). The
lower of the two values is reported on Form I and flagged
with a P.
C: This flag applies* to pesticide results where the
identification has been confirmed by GC/MS. If GC/MS
B-36 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
confirmation was attempted but was unsuccessful, do not apply
this flag; use a laboratory-defined flag instead (see the X
qualifier).
B: This flag is used when the analyte is found in the associated
method blank as well as in the sample. It indicates probable
blank contamination and warns the data user to take
appropriate action. This flag shall be used for a
tentatively identified compound as well as for a positively
identified target compound.
The combination of flags BU or UB is expressly prohibited.
Blank contaminants are flagged B only when they are detected
in the sample.
E: This flag identifies compounds whose concentrations exceed
the upper level of the calibration range of the instrument
for that specific analysis. If one or more compounds have a
response greater than the upper level of the calibration
range, the sample or extract shall be diluted and reanalyzed.
according to the specifications in Exhibit D; exceptions are
also noted in Exhibit D. All such compounds with a response
greater than the upper level of the calibration range shall
have the concentration flagged with an E on Form I for the
original analysis.
NOTE: For total xylene, where three isomers are quantified
as two peaks, the calibration range of each peak shall be
considered separately. For example, a diluted analysis is
not required for total xylene unless the concentration of the
peak representing the single isomer exceeds 200 ug/L or the
peak representing the two co-eluting isomers on that GC
column exceeds 400 ug/L.
D: If a sample or extract is reanalyzed at a higher dilution
factor, for example when the concentration of an analyte
exceeds the upper calibration range, the DL suffix is
appended to the sample number on Form I for the more diluted
sample, and all reported concentrations on that Form I are
flagged with the D flag. This flag alerts data users that
any discrepancies between the reported concentrations may be
due to dilution of the sample or extract. NOTE 1: The D
flag is not applied to compounds which are not detected in
the sample analysis (i.e., compounds reported with the CRQL
and the U flag). NOTE 2: Separate Form Is are required for
reporting the original analysis (EPA Sample No. XXXXX) and
the more diluted sample analysis (EPA Sample No. XXXXXDL)
(i.e., the results from both analyses cannot be combined on a
single Form I).
A: This flag indicates that a tentatively identified.compound is
a-suspected aldol-condensation product.
B-37 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form I
X: Other specific flags may be required to properly define the
results.' If used, the flags shall be fully described, with
the description attached to the sample data summary package
and the SDG Narrative. Begin by using X. If more than one
flag is required, use Y and Z as needed. If more than five
qualifiers are required for a sample result, use the X flag
to represent a combination of several flags. For instance,
the X flag might combine the A, B, and D flags for some
samples. The laboratory-defined flags are limited to X, Y,
and Z.
3.5 Organic Analysis Data Sheet: Tentatively Identified Compounds (Form I
VOA-TIC and Form I SV-TIC)
3.5.1 Purpose. This form is used to report analysis results for non-target
compounds (e.g., compounds not listed in Exhibit C), excluding system
monitoring compounds, surrogates, and internal standards. See
Exhibit D for instructions on identification and quantitation. The
Contractor shall submit Form I VOA-TIC or SV-TIC for every analysis,
including required dilutions and reanalyses, even if no TICs are
found.
3.5.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions in addition to the instructions in
Section 3.4.
3.5.2.1 Report all TICs including CAS number (if applicable), compound
name, retention time, and the estimated concentration as
uncorrected for blank contaminants. If the analytical result is
less than 10, report to one significant figure. If the analytical
result is 10 or greater, report to two significant figures.-
(Criteria for reporting TICs are given in Exhibit D, Section 11).
Retention time shall be reported in minutes and decimal minutes,
not seconds or minutes:seconds. If, in the opinion of the mass
spectral interpretation specialist, no valid tentative
identification can be made, the compound shall be reported as
unknown.
3.5.2.2 Total the number of TICs found, including aldol-condensation
products (see Section 3.5.2.4), and enter this number in the
"Number TICs found" field. If no TICs were found, enter 0 (zero).
3.5.2.3 If the name of a compound exceeds the 28 spaces in the TIC column,
truncate the name to 28 characters. If the compound is an
unknown, restrict the description to ho more than 28 characters
(e.g., unknown hydrocarbon).
3.5.2.4 Peaks that are suspected to be aldol-condensation reaction
products (e.g., 4-methyl-4-hydroxy-2-pentanone and
4-methyl-3-pentene-2-one) shall be summarized on this form,
flagged A, and included in the "Number TICs found" field. .The
B-38 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form II
peaks shall be counted as part of the 30 most intense non-target
semivolatile compounds to be searched. .
3.6 System Monitoring Compound Recovery (Form II, VOA-1, VOA-2)
3.6.1 Purpose. For volatiles, Form II, VOA-1, VOA-2 is used to report the
recoveries of the system monitoring compounds added to each volatile
sample, including dilutions and reanalyses, blank, matrix spike, and
matrix spike duplicate. The system monitoring compounds are used to
monitor the performance of the purge and trap-gas chromatograph-mass
spectrometer system as a whole. Form II VOA is matrix-specific, so
that system monitoring compound recoveries for water samples are
reported on a different version of Form II than the recoveries for
soil samples. Soil sample recoveries are further differentiated by
concentration level.
3.6.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Complete one form for each level. Do
not mix low and medium level samples on one form. NOTE: For
volatile soil samples only, specify the level as LOW or MED.
Complete the remainder of the form using the following instructions.
3.6.2.1 For each system monitoring compound listed in Table 1, report the
percent recovery to the nearest whole percentage point, and to the
number of significant figures given by the QC limits at the bottom
of the form.
3.6.2.2 Flag each system monitoring compound recovery outside the QC
limits with an asterisk (*). The asterisk shall be placed in the
last space in each appropriate column, under the "#" symbol.
3.6.2.3 In the "TOT OUT" column, total the number of system monitoring
compound recoveries that were outside the QC limits for each
sample. If no system monitoring compounds were outside the
limits, enter 0 (zero).
3.6.2.4 Number all pages as described in Section 3.3.
Table 1
System Monitoring Compounds
Volatile System CAS Number
Monitoring Compounds
SMC 1: Toluene-d8 (TOL) 2037-26-5
SMC 2: Bromofluorobenzene (BFB) 460-00-4
SMC 3: l,2-Dichloroethane-d4 (DCE) 17060-07-0
3.7 Surrogate Recovery (Form II, SV-1, SV-2 and Form II, PEST-1, PEST-2)
3.7.1 Purpose. Form II, SV-1, SV-2 and Form II, PEST-1, PEST-2 are used to
report the recoveries of the surrogate compounds added to each
B-39 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form II
semivolatile and pesticide/Aroclor sample, blank, matrix spike, and
matrix spike duplicate. Form II SV and Form II PEST are
matrix-specific as well as fraction-specific, so surrogate recoveries
for semivolatile and pesticide water samples are reported on a
different version of Form II than surrogate recoveries for
semivolatile and pesticide soil samples.
3.7.2 Instructions. Complete the header information according to the
instructions in Section 3.3. NOTE: For semivolatile soil samples
only, specify the level as LOW or MED. Complete one form for each
level. Do not mix low and medium level samples on one form.
Complete the remainder of the form using the following instructions.
3.7.2.1 For each surrogate listed in Tables 2 and 3, report the percent
recovery to the nearest whole percentage point.
3.7.2.2 Flag each surrogate recovery outside the QC limits with an
asterisk (*). The asterisk shall be placed in the last space
in each appropriate column, under the "#" symbol.
3.7.2.3 In the "TOT OUT" column, total the number of surrogate
recoveries that were outside the QC limits for each sample. If
no surrogates were outside the limits, enter 0 (zero).
3.7.2.4 If the sample is diluted and the surrogates are outside the
acceptance window in any analysis, .enter the calculated
recovery, and flag the surrogate recoveries with a D in the
column under the "#" symbol. Do not include results flagged
with a D in the total number of recoveries for each sample
outside the QC limits.
3.7.2.5 The pesticide surrogate recoveries shall be reported from both
GC columns used for the analyses. Therefore, identify each GC
column at the top of Form II, PEST-1, PEST-2, entering the
stationary phase in the "GC Column" field, and the internal
diameter of the column in millimeters (mm) in the "ID" field.
3.7.2.6 The assignment of columns as "1" and "2" is left to the
discretion of the Contractor when the analyses are performed by
simultaneous injection into a GC containing two columns. If so
analyzed, the assignment of "GC Column 1" and "GC Column 2"
shall be consistent across all the reporting forms. If the
analysis is not performed by simultaneous injection, then the
assignment of GC column number shall be based on the
chronological order of the two analyses.
3.7.2.7 Although the pesticide surrogate recovery limits for samples,
matrix spike and matrix spike duplicates are only advisory, the
Contractor shall flag those recoveries that are outside the
advisory QC limits or are diluted out. The total number of
recoveries that are outside the QC limits shall include all
values from both of GC columns. In counting the total number
of recoveries that are outside the QC limits, do not include
the results flagged with a D.
B^40 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form III
3.7.2.8 Number all pages as described in Section 3.3.
Table 2
Semivolatile Surrogates
Semivolatile Surrogates
CAS Number
SI
S2
S3
S4
S5
S6
S7
S8
Nitrobenzene-d5 (NBZ) 4165-60-0
2-Fluorobiphenyl (FBP) 321-60-8
Terphenyl-dl4 (TPH) 98904-43-9
Phenol-d5 (PHL) 4165-62-2
2-Fluorophenol (2FP) 367-12-4
2,4,6-Tribromophenol (TBP) 118-79-6
2-Chlorophenol-d4 (2CP) 93951-73-6
l,2-Dichlorobenzene-d4 (DCS) 2199-69-1
Table 3
Pesticide Surrogates
Pesticide Surrogates
CAS Number
Decachlorobiphenyl (DCB)
Tetrachloro-m-xylene (TCX)
2051-24-3
877-09-8
3.8. Matrix Spike/Matrix Spike Duplicate Recovery (Form III, All Fractions)
3.8.1 Purpose. This form is used to report the results of the analyses of
matrix spikes and matrix spike duplicates (MS/MSD). The form is
matrix-specific for volatiles, semivolatiles, and pesticides.
3.8.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Include the EPA sample number for the
matrix spike, without the suffixes MS or MSD. Complete the remainder
of the form using the following instructions.
3.8.2.1 For volatile and Semivolatile soil samples, specify level as LOW
or MED on Form III, VOA-2, and SV-2. SDGs containing soil samples
at both levels require a MS/MSD at each level; therefore, for
soils, prepare one form for each level.
3.8.2.2 In the first table under the "SPIKE ADDED" column, enter the
calculated concentration in ug/L or ug/Kg (according to the
matrix) that results from dividing each spike compound amount
added to the aliquot weight/volume chosen for the matrix spike.
For instance, for base/neutral compounds in medium level soils, if
50 ug of spike are added to 1 g of soil, the resulting
concentration is 50,000 ug/Kg.
B-41
OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form IV
3.8.2.3 Enter the sample concentration in the next column, in similar
units, of each spike compound detected in the original sample. If
a spike compound was not detected during the analysis of the
original sample, enter the sample result as 0 (zero).
3.8.2.4 In the "MS CONCENTRATION" column, enter the actual concentration
of each spike compound detected in the matrix spike aliquot.
3.8.2.5 Calculate the percent recovery of each spike compound in the
matrix spike aliquot to the nearest whole percent, according to
Exhibit D. Enter the percent recovery in the "MS % REC" column.
3.8.2.6 Flag all percent recoveries outside the QC limits with an asterisk
(*). The asterisk shall be placed in the last space of the "MS %
REC" column, under the "#" symbol.
3.8.2.7 For pesticide/Aroclor matrix spikes and matrix spike duplicates,
the MS concentration and MSD concentration shall be the
concentration of the spiked analyte reported on Form I for those
analyses. Of the two concentrations calculated for each
pesticide/Aroclor target compound, one on each GC column, the
lower concentration shall be reported on Form I, and both
concentrations shall be reported on Form X.. The lower
concentration is also reported on Form III and used in the
calculation of spike recovery, even if that concentration yields a
recovery value that is outside the advisory QC limits.
3.8.2.8 Follow Sections 3.8.2.2 through 3.8.2.7 to complete the lower
table, using the results of the analysis of the MSD aliquot.
3.8.2.9 Calculate the relative percent difference (RPD) between the matrix
. spike recovery and the matrix spike duplicate recovery, and enter
this value in the "% RPD" column. Report the RPD to the nearest
whole percent.
3.8.2.10 Compare the RPDs to the QC limits given on the form, and flag each
RPD outside the QC limits with ah asterisk (*) in the last space
of the "% RPD" column, under the "#" symbol.
3.8.2.11 Summarize the values outside the QC limits at the bottom of the
page. No further action is required by the Contractor.
3.9 Method Blank Summary (Form IV, All Fractions)
3.9.1 Purpose. This form summarizes the samples associated with each
method blank analysis. The Contractor shall submit the appropriate
Form IV for each blank.
3.9.2 Instructions. Complete the header information according to the
instructions in Section 3.3. The EPA sample number entered in the
upper righthand corner shall be the same number entered on Form I for
the blank. Complete the remainder of the form using the following
instructions.
B-42 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form IV
3.9.2.1 Complete the following fields: "Instrument ,10, " "Date Analyzed,"
and "Time Analyzed." Dates shall be entered as MM/DD/YY. The
time shall be reported in military.time.
3.9.2.2 Pesticide/Aroclor .contaminants shall meet the identification
criteria requiring analysis of the blank on two different GC
columns (see Exhibit D PEST). Enter the date, time, and
instrument ID of both analyses of the blank on the pesticide
method blank summary (Form IV PEST). The information on the two
analyses is differentiated as Date Analyzed (1), Date Analyzed
(2), etc. If the analyses were run simultaneously, the order of
reporting is not important, but shall be consistent with the
information reported on all other pesticide forms. Otherwise,
Date Analyzed (1) shall indicate the analysis on column 1, and
Date Analyzed (2) shall indicate the analysis on column 2.
3.9.2.3 Identify the GC column and internal diameter in the appropriate
fields.
3.9.2.4 For volatiles, indicate the purging method by entering Y for
heated purge or N for ambient temperature purge in the "Heated
Purge: Y/N" field on Form IV VGA.
3.9.2.5 For pesticide/Aroclor blanks, enter the method of extraction as
SEPF for separatory funnel, CONH for continuous liquid-liquid
extraction with hydrophobia membrane, CONT for continuous
liquid-liquid extraction without hydrophobic membrane, SONC for
sonication, SOXH for automated soxhlet extraction or PFEX for
pressurized fluid extraction on Form IV PEST.
3.9.2.6 For semivolatile and pesticide/Aroclor method blanks, enter the
date of extraction of the blank on Form IV SV or PEST.
3.9.2.7 If the samples associated with pesticide/Aroclor blank are
subjected to sulfur cleanup, then the blank shall also be
subjected to sulfur cleanup. If sulfur cleanup is employed, enter
Y in the "Sulfur Cleanup" field; if not, enter N on Form IV PEST.
If only some of the samples associated with the method blank are
subjected to sulfur cleanup, a separate sulfur cleanup blank is
required (see Exhibit D PEST). If a separate sulfur cleanup blank
is prepared, complete one version of Form IV associating all the
samples with the method blank, and a second version of Form IV
listing only those samples associated with the separate sulfur
cleanup blank. NOTE: Subjecting all samples associated with a
method blank to sulfur cleanup avoids the need for two forms.
3.9.2.8 For all three fractions, as appropriate, summarize the samples
including storage and volatile instrument blanks, associated with
a given method blank in the table, entering the EPA sample number
and lab sample identifier. For volatiles, enter the lab file
identifier and the time of analysis of each sample. For
semivolatiles, enter lab file identifier and the date of analysis.
For pesticides/Aroclors, enter the dates of both analyses as Date
Analyzed (1) and Date Analyzed (2), as discussed previously.
B-43 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form V
3.9.2.9 For pesticide/Aroclor fraction, enter the lab file identifier only
if GC/MS confirmation was attempted. Otherwise, leave this field
blank.
3.9.2.10 Number all pages as described in Section 3.3.
3.10 GC/MS:Instrument Performance Check and Mass Calibration (Form V VGA and
Form V SV)
3.10.1 Purpose. This form is used to report the results of the GC/MS
instrument performance check for the volatile and semivolatile
fractions and to summarize the date and time of analyses of samples,
including dilutions, reanalyses, standards, blanks, matrix spikes,
and matrix spike duplicates associated with each analysis of the
instrument performance check solution.
3.10.-2 Instructions. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions.
3.10.2.1 Enter the date and time of injection of the instrument performance
check solution (BFB for volatiles--CAS Number 460004, DFTPP for
semivolatiles--CAS Number 5074715). The date shall be entered as
MM/DD/YY. The time shall be reported as military time.
3.10.2.2 For volatiles, identify the GC column and internal diameter on
Form V VGA.
3.10.2.3 For each ion listed on the form, enter the percent relative
abundance in the righthand column of the first table. Report
relative abundances to the number of significant figures given for
each ion in the ion abundance criteria column.
NOTE: For both BFB and DFTPP, one or more of the high mass ions
may exceed the abundance of the ion listed on the form as the
nominal base peak, m/z 95 for BFB and m/z 198 for DFTPP. Despite
this possibility, all ion abundances shall be normalized to the
nominal base peaks listed on Form V (see Exhibits D and E).
3.10.2.4 All relative abundances shall be reported as a number. If the
relative abundance is zero, enter 0, not a dash or other
non-numeric character. Where parentheses appear, compute the
percentage of the ion abundance of the mass given in the
appropriate footnote, and enter that value in the parentheses.
3.10.2.5 In the lower table, list all samples, including dilutions and
reanalyses, standards, blanks, matrix spikes, and matrix spike
duplicates analyzed under that instrument performance check in
chronological order, by time of analysis (in military time).
Refer to Section 3.3.7 for specific instructions for identifying
standards and blanks.
B-44 . OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form VI
3.10.2.6 Complete the following fields for all standards, samples,
including dilutions and reanalyses, blanks, matrix spikes, and
matrix spike duplicates: "EPA Sample No.," "Lab Sample ID," "Lab
File ID," "Date Analyzed," and "Time Analyzed."
3.10.2.7 Number all pages as described in Section 3.3.
3.11 GC/MS Initial Calibration Data (Form VI, VOA-1, VOA-2 and Form VI, SV-1,
SV-2)
3.11.1 Purpose. After a GC/MS system has undergone an initial five-point3
calibration at the specific concentration levels described in Exhibit
D, and after all initial calibration criteria have been met, the
Contractor shall complete and submit this form for each volatile or
semivolatile target compound initial calibration performed which is
relevant to the samples, including dilutions and reanalyses, blanks,
matrix spikes, or matrix spike duplicates in the SDG, regardless of
when that calibration was performed.
3.11.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Enter the Case number and SDG number
for the current data package, regardless of the original Case for
which the initial calibration was performed. Complete the remainder
of the form using the following instructions.
3.11.2.1 Enter the date(s) of the calibration. If the calendar date
..- changes, during the calibration procedure, the inclusive dates
shall be recorded. Dates shall be entered as MM/DD/YY.
3.11.2.2 Enter the injection times of the first and last of the standards
analyzed in the "Calibration Times" field. Times shall be
reported in military time.
3.11.2.3 For volatiles, complete the "GC Column" and "ID" fields. Indicate
the purging method by entering "Y" for heated purge or "N" for
ambient temperature purge in the "Heated Purge: (Y/N)" field.
3.11.2.4 Enter the lab file identifier for each of the five calibration
standards injected. Complete the response factor data for the
five calibration points, and then calculate and report the average
relative response factor (RRF) for all target compounds.
3.11.2.5 For volatiles, report the relative response factors for the system
monitoring compounds in the calibration standards., For
semivolatiles, report the response factors for all surrogate
3For semivolatiles, eight compounds (2,4-Dinitrophenol, 2,4,5-
Trichlorophenol, 2-Nitroaniline, 3-Nitroaniline, 4-Nitroaniline,
4-Nitrophenol, 4,6-Dinitro-2-Methylphenol, and Pentachlorophenol) will only
require a four-point initial calibration at 50, 80, 120, and 160 total
nanograms because detection at less than 50 ng per injection is difficult. If
a four-point calibration is performed for these compounds, leave the "RRF20"
column blank.
B-45 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form VI
compounds in the calibration standards. The Contractor shall
report the relative standard deviation (%RSD) for all compounds.
See Exhibit D for equations.
3.12 GC/EC Initial Calibration Data (Form VI, PEST-1, PEST-2)
3.12.1 Purpose. The initial calibration of pesticides/Aroclors involves the
determination of retention times, retention time windows, and
calibration factors. For single component pesticide target
compounds, these data are calculated from the analyses of the
Individual Standard Mixtures A and B at three different concentration
levels. For the multicomponent target compounds, these data are
calculated from a single point calibration.
3.12.2 Instructions. Complete one Form VI for each GC column used for the
three analyses of Individual Standard Mixture A (low point, mid-
point, and high point) and the three analyses of Individual Standard
Mixture B during an initial calibration. Complete the header
information according to the instructions in Section 3.3. Complete
the remainder of the form using the following instructions.
3.12.2.1 In the "Level (x low)" field, enter the concentration of the .low
point, mid-point, and high point calibration standards as a
multiplier of the low point. Therefore, for the low point, enter
"1.0." The concentration of the mid-point standard is specified
in Exhibit D as four times the low point; therefore, enter "4.0."
The high point standard shall be at least 16 times the low point,
but may be higher, if that value lies within the linear range of
the instrument, as specified in Exhibit D-. Therefore, enter the
appropriate multiplier to the high point standard concentration to
one decimal place.
3.12.2.2 Identify the GC column and internal diameter (in millimeters, mm)
in the appropriate fields.
3.12.2.3 Enter the dates of analysis of the first and last of the six
standards on each form in the "Date(s) Analyzed" field. Dates
shall be entered as MM/DD/YY.
3.12.2.4 For each standard analyzed, enter the retention time of each
applicable analyte in minutes and decimal minutes, under the
appropriate concentration level in the "RT OF STANDARDS" column on
Form VI PEST-1.
3.12.2.5 Calculate the mean retention time of each analyte from the three
individual mixtures, and report it in the "MEAN RT" column on Form
VI PEST-1.
3.12.2.6 Calculate the retention time window for each analyte using the
specifications in Exhibit D, and enter the lower limit of the
window in the "RT WINDOW" column under "FROM," and the upper limit
of the window under "TO" on Form VI PEST-1.' The retention times
of the surrogates are reported from the analyses of Individual
B-46 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Eorm VI
Mixture A and the windows are only required to be calculated for
Individual Mixture A. . ; .
3.12.2.7 For the six analyses of the Individual Standard Mixtures, the
Contractor shall also complete the calibration factor data on Form
VI PEST-2. Prepare one form for each instrument and GC column
used. Enter the calibration factor for each compound in each of
the standards. Calculate and enter a mean calibration factor and
a relative standard deviation (%RSD). As with surrogate retention
times, the surrogate calibration factors are only required from
Individual Mixture A analyses. .
3.12.2.8 For the multicomponent target compounds, the retention times,
.retention time windows, and calibration factors shall be reported
in a similar fashion for each single point calibration standard.
For each multicomponent compound, the Contractor shall select at
least three peaks from each analyte, according to the
specifications in Exhibit D. The retention time and calibration
factor data apply to each peak. Complete one version of Form VI
PEST-3 for each GC column, for each initial calibration that
applies to samples in the data package.
3.12.3 Form VI is also used to report the results of analysis of the
Resolution Check Standard that shall begin each pesticide/Aroclor
initial calibration sequence (Form VI PEST-4). The Contractor shall
submit one Form VI PEST-4 for both GC columns.
3.12.4 Complete the header information as described in Section 3.3. Using
the same assignment of first and second GC columns made for Form IV,
enter the GC column identifier, internal diameter, and date and time
of analysis(es). Enter the EPA sample number for the Resolution
Check Standard. If simultaneous injections on a single GC are used,
the EPA sample number may be the same for both Resolution Check
Standards. If simultaneous injections are not used, use different
suffixes to identify the standards. Complete the remainder of the
form using the following instructions.
3.12.4.1 List each analyte, in retention time order, including both
surrogate compounds. Thus, the order of analytes in the two
boxes on this form will be different due to the dissimilarity
of the stationary phases of the two GC columns used. Enter the
name of each target analyte in the Resolution Check Mixture as
it appears on Form I PEST. Spell out the names of the
surrogates as they appear on Form VII PEST-2.
3.12.4.2 Enter the 'retention time of each analyte from the analysis in
the "RT" column.
3.12.4.3 Calculate the resolution between each pair of analytes. Enter
the resolution between the first and second peaks on the line
for the first analyte listed in the box. Enter the resolution
between the second and third peaks on the line for the second
analyte, and so on, until the resolutions of all possible pairs
B-47 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form VII
of adjacent analytes have been entered. NOTE: Only eight of
the nine resolution fields will be filled.
3.12.4.4 Form VI (PEST-5, PEST-6 and PEST-7 for each pair of PEM, mid-
level initial calibration mixture A, and mid-level initial
calibration mixture B, respectively) shall be used to report
the percent resolution between each pair of analytes according
. to the definition in Exhibit D (Pesticides).
3.12.4.5 Complete the header information as described in Section 3.3.
Using the same assignment of first and second GC columns made
for Form IV, enter the GC column identifier,'internal diameter,
and date and time of analysis. Enter the EPA sample number for
the respective standards. If simultaneous injections are not
used, use different suffixes to identify the standards.
Complete the remainder of the form using the following
instructions.
3.12.4.5.1 List each analyte, in retention time order, including both
surrogate compounds. Thus, the order of analytes in the two
boxes on this form will be different due to the
dissimilarity of the stationary phases of the two GC columns
used. Enter the name of each target analyte in the standard
as it appears on Form I PEST. Spell out the names of the
surrogates as they appear on Form VII PEST-2.
3.12.4.5.2 Enter the retention time of each analyte from the analysis
in the "RT" column.
3.12.4.5.3 Calculate the resolution between each pair of analytes.
Enter the resolution between the first and second peaks on
the line for the first analyte listed in the box. Enter the
resolution between the second and third peaks on the line
for the second analyte, and so on, until the resolutions of
all possible pairs of adjacent analytes have been entered.
NOTE: The last resolution field will be left blank in each
table.
3.13 GC/MS Continuing Calibration Data (Form VII, VOA-1, VOA-2 and Form VII,
SV-1, SV-2)
3.13.1 Purpose. For volatiles and semivolatiles, this form is used to
report the calibration of the GC/MS system by the analysis of
specific calibration standards. Form VII is required for each 12-
hour time period for both volatile and semivolatile target compound
analyses. The Contractor shall analyze calibration standards and
meet all criteria outlined in Exhibit D for the minimum RRF and
maximum percent difference between initial and continuing
calibrations.
3.13.2 -Instructions. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions.
B-48 OLM04.2
-------
Exhibit B -- Section 3
Forms Instructions
Form VII
3.13.2.1 Enter the date and time of the continuing calibration and the
date(s) and time(s) of the initial calibration (give inclusive
dates if the initial calibration is performed over more than one
date). Dates shall be entered as MM/DD/YY. Times shall be
reported in military time.
3.13.2.2 For vblatiles, enter the purge method, GC column identifier, and
internal diameter. For semivolatiles, enter GC column identifier
and internal diameter.
3.13.2.3 Using the appropriate initial calibration (volatile or
semivolatile), enter the average relative response factor (KRF)
for each target compound, for each system monitoring compound for
volatiles, and for each surrogate for semivolatiles.
3.13.2.4 Report the relative response factor (RRF50) from the continuing
calibration standard analysis.
3.13.2.5 Calculate the percent difference (%D) for all compounds. See
Exhibit D for equation. If the %D is greater than 999.9, report
as 999.9. If the %D is less than -99.9, report as -99.9.
3.14 GC/EC Calibration Verification Summary (Form VII, PEST-1, PEST-2)
3.14.1 Purpose. Form VII is used to report the results of the Performance
Evaluation Mixtures (PEMs) and the mid-point concentrations of
Individual Standard Mixtures A and B that, along with the PEM,
bracket each 12-hour period of sample analyses. The Contractor shall
submit Form VII PEST-1 for each 12-hour sequence analyzed. Form VII
PEST-2 shall be completed each time the Individual Standard Mixtures
are analyzed, for each GC column used.
3.14.2 Instructions. Complete Form VII PEST-1 and PEST-2 for each standard
reported on Form VIII PEST. Complete the header information
according to the instructions in Section 3.3. Complete the remainder
of the form using the following instructions.
FORM VII PEST-1
3.14.2.1 Enter the date(s) of the initial calibration(s). Give inclusive
dates if the initial calibration is performed over more than one
day. Dates shall be entered as MM/DD/YY.
3.14.2.2 Identify the GC column and internal diameter in the appropriate
fields.
3.14.2.3 On Form VII PEST-1, enter the EPA sample number, lab sample
identifier, and date and time of analysis for the instrument blank
that preceded the 12-hour sequence (PIBLK). For the PEM that
initiated or terminated the 12-hour sequence (PEM), enter the EPA
sample number, lab sample identifier, and date and time of
analysis.
B-49 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form VIII
3.14.2.4 When reporting data for the PEM at the beginning of the initial
calibration sequence, leave the "EPA Sample No.," "Lab Sample ID,"
"Date Analyzed," and "Time Analyzed" fields blank for the
instrument blank (PIBLK), when no instrument blank is analyzed
before the PEM. When reporting all other PEM analyses, the
instrument blank fields shall be completed.
3.14.2.5 'In the table, report the retention time for each analyte in the
PEM as well as the retention time windows.
3.14.2.6 For each analyte in the PEM, enter the amount of the analyte found
in the PEM, in nanograms (ng) to three decimal places, in the
"CALC AMOUNT" column.
3.14.2.7 Enter the nominal amount of each analyte in the PEM in the "NOM
AMOUNT" column.
3.14.2.8 Calculate the percent difference between the calculated amount and
nominal amount for each analyte according to Exhibit D. Report
the values in the "%D" column. If the %D is greater than 999.9,
report as 999.9. If the %D is less than -99.9, report as -99.9.
3.14.2.9 Calculate the percent breakdown for endrin and 4,4'-DDT and the
combined percent breakdown in the PEM according to Exhibit D.
Enter the values for the breakdown of endrin and 4,4'-DDT in their
respective fields immediately under the table.
FORM VII PEST-2
3.14.2.10 The upper table on Form VII PEST-2 contains the retention time and
amount data for Individual Standard Mixture A compounds. The
lower table contains the data for Mixture B. Complete the form
using the instructions in.Sections 3.14.2.1 through 3.14.2.8 for
Form VII PEST-1.
3.15 Internal Standard Area.and RT Summary (Form VIII VGA and Form VIII,
SV-1, SV-2)
3.15.1 Purpose. This form is used to summarize the peak areas and retention
times of the internal standards added to all volatile and
semivolatile samples, including: dilutions, reanalyses, blanks,
matrix spikes, and matrix spike duplicates. The data are used to
determine when changes in internal standard responses will adversely
affect quantification of target compounds. This form shall be
completed each time a continuing calibration is performed, or when
samples are analyzed under the same GC/MS instrument performance
check as an initial calibration.
3.15.2 Instructions. Complete the header information according to Section
3.3. Complete the remainder of the form using the following
instructions. If samples 'are analyzed immediately following an
initial calibration, before another instrument performance check and
a continuing calibration, Form VIII shall be completed on the basis
of the internal standard areas of the 50 ug/L initial calibration
B-50 OLM04.2
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Exhibit B -- Section 3
Forms Instructions
Form VIII
standard for volatiles, and the 50 ng initial calibration standard
for semivolatiles. Use the date and time of analysis of this
standard and the lab file identifier and areas in place of those of a
continuing calibration standard.
3.15.2.1 Enter the date and time of analysis of the continuing calibration
standard. The date shall be entered as MM/DD/YY. The time shall
be reported as military time.
3.15.2.2 For volatiles, enter the purge method, GC column identifier, and
internal diameter. For semivolatiles, enter GC column identifier
and internal diameter.
3.15.2.3 From the results of the analysis of the continuing calibration
standard, enter the area measured for each internal standard and
its retention time (in decimal minutes) under the appropriate
column in the "12 HOUR STD" row.
3.15.2.4 For each internal standard listed in Tables 4 and 5, calculate the
upper limit of the area as the area of the particular standard
plus 100 percent of its area (i.e., two times the area in the "12
HOUR STD" field), and the lower limit of the area as the area of
the internal standard minus 50 percent of its area (i.e., one half
the area in the "12 HOUR STD" field). Report these values in the
"UPPER LIMIT" and "LOWER LIMIT" rows, respectively. Calculate the
upper limit of the retention time as the retention of the internal
standard, plus 0.50 minutes (30 seconds), and the lower limit of
the retention time as the retention time in the standard minus
0.50 minutes (30 seconds).
3.15.2.5 For.each sample,.including dilutions, reanalyses, blanks, matrix
spikes, and matrix spike duplicates, analyzed under a given
continuing calibration, enter the EPA sample number and the area
measured for each internal standard and its retention time. If
the internal standard area is outside the upper or lower limits
calculated in step 4, flag that area with an asterisk (*). The
asterisk shall be placed in the far righthand space of the box for
each internal standard area, directly under the "#" symbol.
Similarly, flag the retention time of any internal standard that
is outside the limits with an asterisk.
3.15.2.6 Number all pages as described in Section 3.3.
Table 4
Volatile Internal Standards
.Volatile Internal Standards CAS Number
IS1: Bromochloromethane (BCM) 74-97-5
IS2: 1,4-Difluorobenzene (DFB) 540-36-3
IS3: Chlorbbenzene-d5 (CBZ) 3114-55-4
B-51 OLM04.2
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Exhibit E -- Section 3
Forms Instructions
Form VIII
Table 5
Semivolatiie Internal Standards
Semivolatile Internal Standards CAS Number
IS1
IS2
IS3
IS4
IS5
IS6
l,4-Dichlorobenzene-d4 (DCB)
Naphthalene -d8 (NPT)
Acenaphthene-dlO (ANT)
Phenanthrene-dlO (PHN)
Chrysene-dl2 (CRY)
Perylene-dl2 (PRY)
3855-82-1
1146-65-2
15067-26-2
1517-22-2
1719-03-5
1520-96-3
3.16 Pesticide Analytical Sequence (Form VIII PEST)
3.16.1 Purpose. This form is used to report the analytical sequence for
pesticide analysis. At least one form is required for each GC column
used for pesticide/Aroclor analyses.
3.16.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions.
3.16.2.1 Enter the date(s) of the initial calibration. Give inclusive
dates if the initial calibration is performed over more than one
day. Dates shall be entered as MM/DD/YY.
3..16.2.2 Identify the GC column and internal diameter in the appropriate
fields.
3.16.2.3 At the top of the table, report the mean retention time for
tetrachloro-m-xylene (TCX) and decachlorobiphenyl (DCB) calculated
from the initial calibration sequence.
3.16.2.4 For every analysis associated with a particular analytical
sequence starting with the initial calibration, enter the EPA
sample number, lab sample identifier, and date and time of
analysis. Each sample analyzed as part of the sequence shall be
reported on Form VIII PEST even if it is not associated with the
SDG. The Contractor shall use ZZZZZ as the EPA sample number to
distinguish all samples that are not part of the SDG being
reported.
3.16.2.5 Report the retention time of .the surrogates for each analysis in
the "TCX RT" and "DCB RT" columns. All sample analyses shall be
bracketed by acceptable analyses of instrument blanks, a PEM, and
Individual Standard Mixtures A and B. Given the fact that the
initial calibration may remain valid for some time (see Exhibit
D), it is only necessary to report the data from 12-hour periods
when samples, dilutions, reanalyses, matrix spike, matrix spike
duplicate, blanks, or multicomponent analytes for the 72 hour
B-52 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form IX
confirmation requirement in an SDG were analyzed. All data
necessary to demonstrate compliance with the requirements
specified in Exhibit D-Pest Section 9.3 must be reported. The
Contractor shall submit Form VIII for the initial calibration
sequence and forms that include the PEMs and Individual Standard
Mixtures that bracket any and all samples in the SDG. While the
data for time periods between the initial calibration and samples
in the SDG are not a routine deliverable, the data shall be
available as requested (e.g., at on-site evaluations). Non-EPA
samples or samples from SDGs not being reported shall be numbered
ZZZZZ.
3.16.2.6 Flag all those values which do not meet the contract requirements
by entering an asterisk (*) in the "RT" column, under the "#"
symbol. If the retention time cannot be calculated due to
interfering peaks, leave the "RT" column blank for that surrogate,
enter an asterisk in the last column, and document the problem in
the SDG Narrative.
3.16.2.7 If more than a single copy of Form VIII PEST is required, enter
the same header information on all subsequent pages for that GC
column and instrument, and number each page as described in
Section 3.3.
3.17 Pesticide Cleanup Summary (Form IX, PEST-1, PEST-2)
3.17.1 Purpose. This form summarizes the results of the checks performed
for both cleanup procedures employed during the preparation of
pesticide extracts for analysis. Form IX PEST-1 is used to report
the results of the check of the Flori'sil cartridges used to process
all sample extracts and to associate the lot of cartridges with
particular sample results so that problems with a particular
cartridge lot may be tracked across all associated samples. Form IX
PEST-2 summarizes the results of the calibration verification of the
Gel Permeation Chromatography (GPC) device that shall be used to
process all soil sample extracts for pesticide/Aroclor analyses.
3.17.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Enter the Case number and SDG number
for the current data package, regardless of the original Case for
which the cartridge check was performed. Complete the remainder of
the form using the following instructions.
FORM IX PEST-1
3.17.2.1 Enter the Florisil cartridge lot number.
3.17.2.2 Enter the date the Florisil cartridge check solution was analyzed
in the "Date of Analysis" field. The date shall be entered as
MM/DD/YY.
3.17.2.3 Complete the "GC Column" and "ID" fields for the two GC columns
used to analyze the samples, including blanks, matrix spikes, and
B-53 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form X
matrix spike duplicates. Report all results from either GC column
1 or GC column 2.
3.17.2.4 In the first table, enter the amount of spike added and spike
recovered in nanograms (ng) for each analyte.
3.17.2.5 Calculate the percent recovery to the nearest whole percent, and
enter the number in the "% REC" field. Flag each spike recovery
outside the QC limits (shown on the form) with an asterisk (*) .
The asterisk shall be placed in the last space in the "% REC"
column, under the "#" symbol.
3.17.2.6 In the second table, complete the "EPA Sample No.," the "Lab
Sample ID," and "Date Analyzed" fields for each sample and blank
that were cleaned up using this lot of Florisil cartridges.
3.17.2.7 Number the pages as described in Section 3.3.
FORM IX PEST-2
3.17.2.8 On Form IX PEST-2, enter an identifier for the GPC column and the
analysis date of calibration verification in the appropriate
fields.
3.17.2.9 Complete the "GC Column" and "ID" fields as on Form IX PEST-1 for
florisil. Report all results from a single column.
3.17.2.10 For each of the pesticide matrix spike compounds listed in the
first table, enter the amount of the spike added to the GPC column
and the amount recovered, in nanograms (ng).
3.17.2.11 Calculate the percent recovery of each analyte, and enter these
values on the form, to the nearest percent. Compare the
recoveries to the QC limits shown on the form, and flag all those
values outside the limits with an asterisk (*) in the "% REC"
column under the "#" symbol.
3.17.2.12 For each sample in the data package that was subjected to GPC
under this calibration verification, enter the EPA sample number,
lab sample identifier, and the date of both analyses in the second
table.
3.17.2.13 If more than one copy of Form IX PEST-2 is required, number all
pages as described in Section 3.3.
3.18 Pesticide/Aroclor Identification (Form X, PEST-1, PEST-2)
3.18.1 Purpose. This form summarizes the quantitations of all target
pesticides/Aroclors detected in a given sample. It reports the
retention times of the compound on both columns on which it was
analyzed, as well as the retention time windows of the standard for
that compound on both of these columns. In addition, it is used to
report the concentration determined from each-GC column, and the
percent difference between the two quantitative results. Separate
B-54 OLM04.2
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Exhibit B--Section 3
Forms Instructions
Form X
forms are used for single component analytes and multicomponent
analytes.
Form X is required for each sample, including dilutions and
reanalyses, blank, matrix spike, and matrix spike duplicate in which
compounds listed in Exhibit C (Pesticides/Aroclors) are reported on
Form I. Do not generate a Form X for pesticide instrument blanks.
3.18.2 Instructions. Complete the header information according to the
instructions in Section 3.3. Complete the remainder of the form
using the following instructions.
3.18.2.1 Enter the date(s) of analysis. Dates shall be entered as
MM/DD/YY.
3.18.2.2 Enter the GC column and internal diameter for each of the two
columns.
3.18.2.3 For each single component pesticide positively identified,
enter the name of the compound in the "ANALYTE" column as it
appears on Form I.
3.18.2.4 Enter the retention times on each column of the compounds
detected in the sample next to the appropriate column
designation (1 or 2).
3.18.2.5 Enter the retention time windows on each column from the
initial calibration standard. . These data shall correspond with
those on Form VI and shall be entered in a similar manner. The
lower value is entered under the "FROM" column, the upper value
under the "TO" column.
3.18.2.6 Enter the concentration calculated from each GC column under
the "CONCENTRATION" column. Although the units are the same as
those used on Form I, ug/L for water samples and ug/Kg for soil
samples, do not enter any units on Form X.
3.18.2.7 Calculate the percent difference between the concentrations
entered on this form. See Exhibit D for equation, and report
to a tenth of a percent in the "%D" column. If the %D is
greater than 999.9, report it as 999.9.
3.18.2.8 The lower of the two concentrations is reported on Form I for
each pesticide compound. The lower concentration is used
because, if present, coeluting interferences are likely to
increase the calculated concentration of any target compound.
If the percent difference between the calculated concentrations
is greater than 25.0 percent, flag the concentration on Form I,
as described previously. This will alert the data user to the
potential problems in quantitating this analyte.
3.18.2.9 If more pesticide compounds are identified in an individual
sample than can be reported on one Form X, complete as many
additional copies of Form X as necessary, duplicating all
B-55 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form DC-1
header information and numbering the pages as described in
Section 3.3.
3.18.2.10 Report multicomponent analytes detected in samples on Form X
PEST-2. Complete the header information and GC column fields
as described above. For multicomponent analytes, it is
necessary to report the retention time and concentration of
each peak chosen for quantitation in the target analyte in a
fashion similar to that for single component pesticides. The
concentrations of all peaks quantitated (three are required, up
to five may be used) are averaged to determine the mean
concentration. Report the lower of the two mean concentrations
on Form I. Flag this value if the mean concentrations from the
two GC columns differ by more than 25 percent, as described
previously.
3.18.2.11 If more multicomponent compounds,are identified in an
individual sample than can be reported on one Form X, complete
as many additional copies of Form X. as necessary, duplicating
all header information and numbering the pages as described in
Section 3.3.
3.19 Sample Log-In Sheet (Form DC-1)
3.19.1 Purpose. This form is used to document the receipt and inspection of
sample containers and samples. One original of Form DC-1 is required
for each sample shipping container (only the hardcopy form is-
required). If the samples in a single sample shipping container are
assigned to more than one SDG, the original Form DC-1 shall be placed
with the deliverables for the SDG of the lowest alpha-numeric number,
and a copy of Form DC-1 shall be placed with the deliverables for the
other SDGs. The copies shall be identified as "copy(ies)", and the
location of the original shall be noted on the copies.
3.19.2 Instructions
3.19.2.1 Sign and date the airbill (if present).
3.19.2.2 Complete the header information on the form, including the log-in
date.
3.19.2.3 Examine the shipping container and record the presence/absence of
custody seals and their condition (e.g., intact, broken) in item
1.
3.19.2.4 Record the custody seal numbers in item 2.
3.19.2.5 Open the container, remove the enclosed sample documentation, and
record the presence/absence of chain-of-custody record(s), SMO
forms (e.g., Traffic Reports, Packing Lists), and airbills or
airbill stickers in items 3-5. Specify if there is an airbill
present or an airbill sticker in item 5. Record the airbill or
sticker number in item 6.
B-56 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form DC-2
3.19.2.6 Remove the samples from the shipping container(s), examine the
samples and the sample tags (if present), record the condition of
the sample bottles (e.g., intact, broken, leaking), and presence
| . or absence of sample tags in items 7 and 8.
| '3.19.2.7 Record the cooler temperature in item 9.
\ 3.19.2.8 Review the sample shipping documents and compare the information
recorded on all the documents and samples and circle the
| appropriate answer in item 10.
| 3.15.2.9 Record the date and time of cooler receipt at the laboratory in
| items 11 and 12.
| 3.19.2.10 If there are no problems observed during receipt, sign and date
(include the time) Form DC-1, the chain-of-custody record, the
Traffic Report, and write the sample numbers on Form DC-1 in the
"EPA Sample #" column.
| 3.19.2.11 Record the appropriate sample tags and assigned laboratory
numbers, if applicable.
| 3.19.2.12 Any comments should be made in the "Remarks" column.
| 3.19.2.13 Record the fraction designation (if appropriate) and the specific
area designation (e.g., refrigerator number) in the "Sample
Transfer" block. Sign and date the "Sample Transfer" block.
| 3.19.2.14 Cross out unused columns and spaces.
| 3.19.2.15 If there are problems observed during receipt or an answer marked
with an asterisk (e.g., "absent*") was circled, contact SMO and
document the contact as well as resolution of the problem on a CLP
Communication Log. Following resolution, sign and date the forms
and note, where appropriate, the resolution of the problem.
3.20 Document Inventory Sheet (Form DC-2)
3.20.1 Purpose. The Document Inventory Sheet (Form DC-2) is used to record
both the inventory of Complete SDG File (CSF) documents and the
number of documents in the original sample data package which is sent
to the EPA Region.
3.20.2 Instructions
3.20.2.1 Organize all EPA CSF documents as described in Exhibit B, Sections
II and III. Assemble the documents in the order specified on Form
DC-2 and Sections II and III, and stamp each page with a
consecutive number; however, do not number Form DC-2. Inventory
the CSF by reviewing the document numbers and recording page
number ranges in the columns provided on Form DC-2. The
Contractor shall verify and record in the "Comments" section on
Form DC-2 all intentional gaps in the page numbering sequence (for
example, "page numbers not used, XXXX - XXXX, XXXX - XXXX." If
B-57 OLM04.2
-------
Exhibit B--Section 3
Forms Instructions
Form DC-2
there are no documents for a specific document type, enter a "NA"
in the empty space.
3.20.2.2 Certain laboratory-specific documents related to the CSF may not
fit into a clearly defined category. The Contractor shall review
Form DC-2 to determine if it is most appropriate to place them
under categories 7, 8, 9, or 10. Category 10 should be used if
there is no appropriate previous category. These types of
documents should be described or listed in the blanks under each
appropriate category on Form DC-2.
3.20.2.3 If it is necessary to insert new or inadvertently omitted
documents, the Contractor shall identify the documents with unique
accountable numbers and record the unique accountable numbers and
the locations of the documents in the CSF (in the "Other Records",
section on Form DC-2).
B-58 OLM04.2
-------
Exhibit B -- Section 4
Data Reporting Forms
4.0 DATA REPORTING FORMS
The data reporting forms are shown on the following pages.
B-59 OLM04.2
-------
1A
VOLATILE ORGANICS ANALYSIS DATA SHEET
EPA SAMPLE NO.
Lab Name:
Lab Code:
Contract:
Matrix: (soil/water).
Sample wt/vol:
Case No.:
.(g/mL).
SAS No.:
SDG No.:
Level: (low/med).
% Moisture: not dec..
GC Column:
Soil Extract Volume:
ID:
(mm)
Lab Sample ID:
Lab File ID:
Date Received:
Date Analyzed:
Dilution Factor:
Soil Aliquot Volume:
.(uL)
CAS NO. COMPOUND
CONCENTRATION UNITS:
(ug/L or ug/Kg)
75-71-8
74-87-3
75-01-4
74-83-9
75-00-3
75-69-4
75-35-4
76-13-1
67-64-1
75-15-0
79-20-9
75-09-2
156-60-5
1634-04-4
75-34-3
156-59-2
78-93-3
67-66-3
71-55-6
110-82-7
56-23-5
71-43-2
107-06-2
Di chlorodi f luorome thane
Chloromethane
Vinyl Chloride
Bromomethane
Chloroethane
Trichlorof luoromethane
1, 1-Dichloroethene
1,1, 2-Trichloro-l, 2, 2-trif luoroethane
Acetone
Carbon Disulfide
Methyl Acetate
Methylene Chloride
trans-1, 2-Dichloroethene
Methyl tert-Butyl Ether
1 , 1-Dichloroethane
cis-1, 2-Dichloroethene
2-Butanone
Chloroform
1,1, 1-Trichloroethane
Cyclohexane
Carbon Tetrachloride
Benzene
1 , 2 -Dichloroethane
FORM I VOA-1
OLM04.2
-------
Lab Name:
Lab Code:
IB
VOLATILE ORGANICS ANALYSIS DATA SHEET
Contract:
Case No. : SAS No. :
EPA SAMPLE NO.
SDG No.:
Matrix: (soil/water)
Sample wt/vol: (g/mL).
Lab Sample ID:
Lab File ID:
Level: (low/med).
% Moisture: not dec..
GC Column:
Date Received:
Date Analyzed:
ID:
(mm)
Dilution Factor:
Soil Extract Volume:
CAS NO. COMPOUND
Soil Aliquot Volume:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
.(UL)
79-01-6
108-87-2
78-87-5
75-27-4
10061-01-5
108-10-1
108-88-3
10061-02-6
79-00-5
127-18-4
591-78-6
124-48-1
106-93-4
108-90-7
100-41-4
1330-20-7
100-42-5
75-25-2
98-82-8
79-34-5
541-73-1
106-46-7
95-50-1
96-12-8
120-82-1
Trichloroethene
Me thy 1 eye lohexane
1 , 2 -Dichlorbpropane
Bromodichloromethane
cis-1, 3-Dichloropropene
4 -Methyl - 2 -pentanone
Toluene
trans-1, 3-Dichloropropene
1,1, 2-Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1 , 2 - D ibromoe thane
Chlorobenzene
Ethylbenzene
Xylene (total)
Styrene
Bromoform
Isopropylbenzene
1 , 1 , 2 , 2 - Tetrachloroethane
1 , 3 -Dichlorobenzene
1,4-Dichlorobenzene
1 , 2 -Dichlorobenzene
1, 2-Dibromo-3-chloropropane
1,2, 4 -Trichlorobenzene
FORM I VOA-2
OLM04.2
-------
Lab Name:
Lab Code:
1C
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
Contract:
EPA SAMPLE NO.
Case No.:
SAS No.:
SDG No.
Matrix: (soil/water).
Sample wt/vol:
.(g/mL).
Lab Sample ID:
Lab File ID:
Level: (low/med)
% Moisture:
Decanted:(Y/N)
Concentrated Extract Volume: (uL)
Injection Volume: (uL)
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
GPC Cleanup: (Y/N).
PH:.
CAS NO. COMPOUND
Extraction: (Type).
CONCENTRATION UNITS:
(ug/L or ug/Kg)
100-52-7
108-95-2
111-44-4
95-57-8
95-48-7
108-60-1
98-86-2
106-44-5
621-64-7
67-72-1
98-95-3
78-59-1
88-75-5
105-67-9
111-91-1
120-83-2
91-20-3
106-47-8
87-68-3
105-60-2
59-50-7
91-57-6
77-47-4
88-06-2
95-95-4
92-52-4
91-58-7
88-74-4
131-11-3
606-20-2
208-96-8
99-09-2
83-32-9
Benzaldehyde
Phenol .
bis (2-Chloroethyl) ether
2-Chlorophenol
2 -Methylphenol
2,2' -oxybis (1-Chloropropane)
Acetophenone
4 -Methylphenol
N-Nitroso-di-n-propylamine
Hexachloroethane . .
Nitrobenzene
Isophorone
2-Nitrophenol
2 , 4 -Dimethylphenol
bis (2 -Chloroethoxy) methane
2 , 4 -Dichlorophenol
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
Caprolactam
4 -Chloro- 3 -methylphenol
2 -Methylnaphthalene
Hexachlorocyclopentadiene
2,4, 6 -Trichlorophenol
2,4 , 5-Trichlorophenol
1,1' -Biphenyl
2-Chloronaphthalene
2-Nitroaniline
Dimethylphthalate
2, 6-Dinitrotoluene
Acenaphthylene
3-Nitroaniline
Acenaphthene
,
.
FORM I SV-1
OLM04.2
-------
ID
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
EPA SAMPLE NO.
Lab Name:
Lab Code:
Contract:
Case No.:
SAS No.:
SDG NO.:
Matrix: (soil/water).
Sample 'wt/vol:
.(g/mL).
Leve1: (1ow/me d)
% Moisture:
Decanted: (Y/N).
Concentrated Extract Volume:
Injection Volume:
| GPC Cleanup: (Y/N).
pH:
.(uL)
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
CAS NO. COMPOUND
Extraction: (Type).
CONCENTRATION UNITS:
(ug/L or ug/Kg)
51-28-5
100-02-7
132-64-9
121-14-2
84-66-2
86-73-7
7005-72-3
100-01-6
534-52-1
86-30-6
101-55-3
118-74-1
1912-24-9
87-86-5
85-01-8
120-12-7
86-74-8
84-74-2
206-44-0
129-00-0
85-68-7
91-94-1
56-55-3
218-01-9
117-81-7
117-84-0
205-99-2
207-08-9
50-32-8
193-39-5
53-70-3
191-24-2
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran
2 , 4 -Dinitrotoluene
Diethylphthalate
Fluorene
4 -Chlorophenyl -phenylether
4-Nitroaniline
4, 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine (1)
4 -Bromophenyl-phenylether
Hexachlorobenzene
Atrazine
Pentachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene
Chrysene
bis ( 2 - Ethylhexyl ) phthalate
Di -n-octylphthalate
Benzo (b) f luoranthene
Benzo (k) f luoranthene
Benzo (a) pyrene
.Indeno (1,2, 3 -cd) pyrene
Dibenzo (a, h) anthracene
Benzo (q,h, i)perylene
'
(1) Cannot be separated from Diphenylamine
FORM I SV-2
OLM04.2
-------
Lab Name:
Lab Code:
IE
PESTICIDE ORGANICS ANALYSIS DATA SHEET
Contract:
EPA SAMPLE NO.
Case No. :
SAS No.:
SDG No.
Matrix: (soil/water)
Sample wt/vol: (g/mL)
% Moisture: Decanted: (Y/N).
Extraction: (Type)
Lab Sample ID:
Lab File ID:
Concentrated Extract Volume: _
Injection Volume: (uL)
GPC Cleanup: (Y/N) pH:
.(uL)
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
CAS NO. COMPOUND
Sulfur Cleanup: (Y/N)
CONCENTRATION UNITS:
(ug/L or ug/Kg)
Q
319-84-6
319-85-7
319-86-8
58-89-9
76-44-8
309-00-2
1024-57-3
959-98-8
60-57-1
72-55-9
72-20-8
33213-65-9
72-54-8
1031-07-8
50-29-3
72-43-5
53494-70-5
7421-93-4
5103-71-9
5103-74-2
8001-35-2
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
alpha -BHC
beta-BHC
delta-BHC
gamma -BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4, 4 '-DDE
Endrin
Endosulfan II
4/4 '-ODD
Endosulfan sulfate
4, 4 '-DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
alpha-Chlordane
gamma - Chlordane
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
,
FORM I -PEST
OLM04.2
-------
IF
VOLATILE ORGANICS ANALYSIS DATA SHEET
TENTATIVELY IDENTIFIED COMPOUNDS
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix: (soil/water).
Sample wt/vol:
.(g/mL).
Lab Sample ID:
Lab File ID:
Level: (low/med).
% Moisture: not dec.
GC Column: ID:
Soil Extract Volume:
Number TICs found:
Date Received:
Date Analyzed:
.(mm)
Dilution Factor:
Soil Aliquot Volume:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
.(uL)
CAS NUMBER
1.
2.
3.
4 .
5.
6.
7.
8.
9.
10.
11.
12.
13.
14 .
15.
16.
17.
18.
19.
20.
21.
22.
23.
24 .
25.
26.
27.
28.
29.
30'.
COMPOUND NAME
RT
EST . CONC .
Q
FORM I VOA-TIC
OLM04.2
-------
Lab Name:
Lab Code:
1G
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
TENTATIVELY IDENTIFIED COMPOUNDS
Contract: .
EPA SAMPLE NO.
Case No.:
SAS NO.:
SDG No.:
Matrix: (soil/water).
Sample wt/vol:
.(g/mL).
Lab Sample ID:
Lab File ID:
Level: (low/med).
% Moisture:
Decanted: (Y/N).
Concentrated Extract Volume:
Injection Volume: (pL)
| GPC Cleanup: (Y/N) pH:
Number TICS found:
.(uL)
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
Extraction: (Type).
CONCENTRATION UNITS:
(ug/L or ug/Kg)
CAS NUMBER
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
. 14'.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
COMPOUND NAME
-
RT
EST. CONC.
-
Q
'
'
FORM I SV-TIC
OLM04.2
-------
2A
WATER VOLATILE SYSTEM MONITORING COMPOUND RECOVERY
Lab Name:
Lab Code:
Case No.
Contract:
SAS No.:
SDG No.
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
2.1
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
'
.
^
SMC1
(TOL) #
SMC2
(BFB) #
SMC3
(DCE) #
OTHER
TOT
OUT
SMC1 (TOL) = Toluene-d8
SMC2 (BFB) = Bromofluorobenzene
SMC3 (DCE) = l,2-Dichloroethane-d4
# Column to be used to flag recovery values
* Values outside of contract required QC limits
QC LIMITS
(88-110)
(86-115)
(76-114)
page
of
FORM II VOA-1
OLM04.2
-------
2B
SOIL VOLATILE SYSTEM MONITORING COMPOUND RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Level: (low/med).
01
02
03
04
05
06
07
08 .
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
SMC1
(TOL) #
_, .
SMC2
(BFB) #
SMC3
(DCE) #
OTHER
TOT
OUT
QC LIMITS
SMC1 (TOL) = Toluene-d8 (84-138)
SMC2 (BFB) = Bromofluorobenzene (59-113)
SMC3 (DCE) = l,2-Dichloroethane-d4 (70-121)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
page
.of
FORM II VOA-2
OLM04.2
-------
Lab Name:
Lab Code:
- 2C
WATER SEMIVOLATILE SURROGATE RECOVERY
Contract:
SAS No.:
Case No.:
SDG No.:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
SI
(NBZ)#
S2
(FBP)#
S3
(TPH)#
S4
(PHL)#
S5
(2FP)#
S6
(TBP)#
S7
(2CP)#
S8
(DCB)#
-
TOT
OUT
page
QC LIMITS
SI (NBZ)
S2 (FBP)
S3 (TPH)
S4 (PHL)
S5 (2FP)
S6 (TBP)
S7 (2CP)
S8 (DCB)
# Column
* Values
= Nitrobenzene-d5
= 2 - Fluorobiphenyl
= Terphenyl-dl4
= Phenol -d5
= 2-Fluorophenol
= 2,4,6- Tr ibromophenol
= 2-Chlorophenol-d4
= 1, 2-Dichlorobenzene-d4
(35-114)
(43-116)
(33-141)
(10-110)
(21-110)
(10-123)
(33-110)
(16-110)
(advisory)
(advisory)
to be used to flag recovery values
outside of contract required QC
limits
D Surrogate diluted out
of
FORM II SV-1
OLM04.2
-------
Lab Name:
Lab Code:
2D
SOIL SEMIVOLATILS SURROGATE RECOVERY
Contract:
Case No.:
SAS No.
SDG No.:
Level: (low/med).
EPA
SAMPLE NO.
SI
(NBZ)#
S2
(FBP)#
S3
(TPH) #
S4
(PHL)#
S5
(2FP)#
S6
(TBP)#
S7
(2CP)#
S8
(DCB)#
TOT
OUT
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
SI (NBZ) = Nitrobenzene-d5
S2 (FBP) = 2-Fluorobiphenyl
S3 (TPH) = Terphenyl-dl4
S4 (PHL) = Phenol-d5
S5 (2FP) = 2-Fluorophenol
S6 (TBP) = 2,4,6-Tribromophenol
S7 (2CP) = 2-Chlorophenol-d4
S8 (DCB) = l,2-Dichlorobenzene-d4
QC LIMITS
(23-120)
(30-115)
(18-137)
(24-113)
(25-121)
(19-122)
(20-130)
(20-130)
(advisory)
(advisory)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogate diluted out
page
of
FORM II SV-2
OLM04.2
-------
2E
WATER PESTICIDE SURROGATE RECOVERY
Lab Name:
Contract:
Lab Code:
GC Column(1):
Case No.:
ID:
SAS No.:
SDG NO.:
(mm) GC Column (2) :
ID:
.(mm)
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
TCX 1
%REC #
TCX 2
%REC #
DCB 1
%REC #
DCB 2
%REC tt
OTHER
(1)
OTHER
(2)
TOT
OUT
TCX = Tetrachloro-m-xylene
DCB = Decachlorobiphenyl
QC LIMITS
(30-150)
(30-150)
# Column to be used to flag recovery values
* Values outside of QC limits
D Surrogate diluted out
page
of
FORM II.PEST-1
OLM04.2
-------
2F
SOIL PESTICIDE SURROGATE RECOVERY
Lab Name :
Lab Code:
GC Column (1) :
Case No. :
ID:
Contract :
SAS No . : SDG No . :
(mm) GC Column (2) : ID:
(mm)
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
TCX 1
%REC #
TCX 2
%REC #
DCB 1"
%REC #
DCB 2
%REC #
OTHER
(1)
OTHER
(2)
TOT
OUT
TCX = Tetrachloro-m-xylene
DCB = Decachlorobiphenyl
QC LIMITS
(30-150)
(30-150)
# Column to be used to flag recovery values
* Values outside of QC limits
D Surrogate diluted out
page
of
FORM II PEST-2
OLM04.2
-------
3A
WATER VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Matrix Spike - EPA Sample No.:
Contract:
SAS No.:
SDG No.:
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
' (ug/L)
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC
LIMITS
REC.
61-145
71-120
76-127
76-125
75-130
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
MSD
%
REC #
%
RPD #
QC
RPD
14
14
11
13
13
LIMITS
REC.
61-145
71-120
76-127
76-125
75-130
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD: out of outside limits
Spike Recovery: out of outside limits
COMMENTS:
FORM III VOA-1
OLM04.2
-------
3B
SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Matrix Spike - EPA Sample No.:
Contract:
SAS No.:
SDG No.:
Level:(low/med).
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/Kg)
SAMPLE
CONCENTRATION
(ug/Kg)
MS
CONCENTRATION
(ug/Kg)
MS
%
REC #
QC
LIMITS
REC.
59-172
62-137
66-142
59-139
60-133
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/Kg)
MSD
CONCENTRATION
(ug/Kg)
MSD
%
REC #
%
RPD #
QC
RPD
22
24
21
21
21
LIMITS
REC.
59-172 .
62-137
66-142
59-139
60-133
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of 'QC limits
RPD: out of
Spike Recovery:
COMMENTS:
outside limits
out of outside limits
FORM III VOA-2
OLM04.2
-------
3C
WATER SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike - EPA Sample No.:
COMPOUND
Phenol
2 - Chlorophenol
N-Nitroso-di-n-prop. (1)
4 -Chloro- 3 -methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4 -Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
(ug/L)
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC
LIMITS
REC.
12-110
27-123
41-116
23-97
46-118
10-80
24-96
9-103
26-127
COMPOUND
Phenol
2 -Chlorophenol
N-Nitroso-di-n-prop. (1)
4 - Chloro - 3 -methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4 -Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
MSD
%
REC #
%
RPD #
QC L]
RPD
42
40
38
42
31
' 50
38
50
31
EMITS
REC.
12-110
27-123
41-116
23-97
46-118
10-80
24-96
9-103
26-127
(1) N-Nitroso-di-n-propylamine
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
out of
RPD:
Spike Recovery:
COMMENTS:
outside limits
out of outside limits
FORM .III SV-1
OLM04.2
-------
3D
SOIL SEMIVOLATILE MATRIX SP.IKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Matrix Spike - EPA Sample No.:
Contract:
SAS No.:
SDG No.:
Level:(low/med)
COMPOUND
Phenol
2-Chlorophenol
N-Nitroso-di-n-prop. (1)
4-Chloro-3-methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4 -Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/Kg)
SAMPLE
CONCENTRATION
(ug/Kg)
MS
CONCENTRATION
(ug/Kg)
-
MS
%
REC #
QC
LIMITS
REC.
26-90
25-102
41-126
26-103
31-137
11-114
28-89
17-109
35-142
COMPOUND
Phenol
2 -Chlorophenol
N-Nitroso-di-n-prop. (1)
4-Chloro-3-methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4 -Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/Kg)
MSD
CONCENTRATION
(ug/Kg)
MSD
%
REC #
%
RPD #
QC L
PRO
35
50
38
33
19
50
47
47
36
IMITS
REC. '
26-90
25-102
41-126
26-103
31-137
11-114
28-89
17-109
35-142
(1) N-Nitroso-di-n-propylamine
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD: out of outside limits
Spike Recovery: out of outside limits
COMMENTS:
FORM III SV-2
OLM04.2
-------
3E
WATER PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No. -.
Matrix Spike - EPA Sample No.:
Contract:
SAS No.:
SDG No.
COMPOUND
gamma -BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4, 4 '-DDT
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
(ug/L)
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC
LIMITS
REC.
56-123
40-131
40-120
52-126
56-121
38-127
COMPOUND
gamma -BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4, 4 '-DDT
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
'N
MSD
%
REC #
%
RPD #
QC I
PRD
15
20
22
18
21
27
IMITS
REC.
56-123
40-131
40-120
52-126
56-121
38-127
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD: out of outside limits
Spike Recovery: out of outside limits
COMMENTS:
FORM III PEST-1
OLM04.2
-------
3F
SOIL PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Matrix Spike - EPA Sample No. :
Contract:
SAS No.:
SDG No.:
COMPOUND
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4 ' -DDT
SPIKE
ADDED
(ug/Kg)
SAMPLE
CONCENTRATION
(ug/Kg)
. ;.
MS
CONCENTRATION
(ug/Kg)
MS
%
REC #
QC
LIMITS
REC.
46-127
35-130
34-132
31-134
42-139
23-134
COMPOUND
gamma - BHC (Lindane ) "
Heptachlor
Aldrin
Dieldrin
Endrin
4,4 ' -DDT
SPIKE
ADDED
(ug/Kg)
MSD
CONCENTRATION
'. (ug/Kg)
MSD
%
REC #
%
RPD #
QC L
RPD
50
31
43
38
45
50
IMITS
REC.
46-127
35-130
34-132
31-134
42-139
23-134
# Column to.be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD: out of outside limits
Spike Recovery: out of outside limits
COMMENTS:
FORM III PEST-2
OLM04.2
-------
4A
VOLATILE METHOD BLANK SUMMARY
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Lab File ID:
Date Analyzed:
GC Column:
Lab Sample ID:
Time Analyzed:
ID:
.(mm) Heated Purge: (Y/N)
Instrument ID:
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS, AND MSD:
COMMENTS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
LAB
SAMPLE ID
LAB
FILE ID
TIME
ANALYZED
page
of
FORM IV VOA
OLM04.2
-------
4B
SEMIVOLATILE METHOD BLANK SUMMARY
EPA SAMPLE NO.
Lab Name -.
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Lab File ID:
Instrument ID:
Matrix: (soil/water)
Level: (low/med)
Lab Sample ID:
Date Extracted:
Date Analyzed:
Time Analyzed:
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS, AND MSD:
COMMENTS:
01
0-2
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
j
LAB
SAMPLE ID
..
LAB
FILE ID
DATE
ANALYZED
page
of
FORM IV SV
OLM04.2
-------
4C
PESTICIDE METHOD BLANK SUMMARY
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.: .
Lab Sample ID:
Lab File ID:
Matrix: (soil/water)
Sulfur Cleanup: (Y/N).
Date Analyzed (1) :
Time Analyzed (1) :
Instrument ID (1):
GC Column (1):
Extraction: (Type)
Date Extracted:
Date Analyzed (2):
Time Analyzed (2):
Instrument ID (2):
ID:
.(mm) GC Column (2):
ID:
(mm)
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS, AND MSD:
COMMENTS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
EPA
SAMPLE NO.
LAB
SAMPLE ID
DATE
ANALYZED 1
DATE
ANALYZED 2
page
of
FORM IV PEST
OLM04.2
-------
Lab Name:
Lab Code:
5A
VOLATILE ORGANIC INSTRUMENT PERFORMANCE CHECK
BROMOFLUOROBENZENE (BFB)
Contract:
SAS No.:
Case No.:
SDG No.:
Lab File ID:
Instrument ID:
GC Column:
BFB Injection Date:
BFB Injection Time:
ID:
(mm)
m/e
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA
8.0 - 40.0% of mass 95
30.0 - 66.0% of mass 95
Base peak, 100% relative abundance
5.0 - 9.0% of mass 95
Less than 2.0% of mass 174
50.0 - 120.0% of mass 95
4.0 - 9.0 % of mass 174
93.0 - 101.0% of mass 174
5.0 - 9.0% of mass 176
% RELATIVE
ABUNDANCE
( )1
( )1
( )1
( 12
1-Value is % mass 174
2-Value is % mass 176
THIS CHECK APPLIES TO THE FOLLOWING SAMPLES, MS, MSP, BLANKS,' AND STANDARDS:
01
02
03
04
05
06
.07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
EPA
SAMPLE NO.
LAB
SAMPLE ID
LAB
FILE ID
DATE
ANALYZED
TIME
ANALYZED
page
of
FORM V VGA
OLM04.2
-------
5B
SEMIVOLATILE ORGANIC INSTRUMENT PERFORMANCE CHECK
DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP)
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Lab File ID:
Instrument ID:
DFTPP Injection Date:
DFTPP Injection Time:
m/e
51
68
69
70
127
197
198
199
275
365
441
442
443
ION ABUNDANCE CRITERIA
30.0- 80.0% of mass 198
Less than 2.0% of mass 69
Mass 69 relative abundance
Less than 2.0% of mass 69
25.0 - 75.0% of mass 198
Less than 1.0% of mass 198
Base Peak, 100% relative abundance
5.0 to 9.0% of mass 198
10.0- 30.0% of mass 198
Greater than 0.75% of mass 198
Present, but less than mass 443
40.0 - 110.0% of mass 198
15.0 - 24.0% of mass 442
% RELATIVE
ABUNDANCE
( )1
( )1
( - )2
1-Value is % mass 69
2-Value is % mass 442
THIS CHECK APPLIES TO THE FOLLOWING SAMPLES, MS, MSP, BLANKS, AND STANDARDS;
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
EPA
SAMPLE NO.
LAB
SAMPLE ID
LAB
FILE ID
DATE
ANALYZED
TIME
ANALYZED
page
of
FORM V SV
OLM04.2
-------
6A
VOLATILE ORGANICS INITIAL CALIBRATION -DATA
Lab Name:
Lab Code:
Instrument ID:
Contract:
Case No.:
SAS No.:
Heated Purge: (Y/N)
GC Column:
ID:
Calibration Date(s):
Calibration Times:
(mm)
SDG No.
LAB FILE ID: RRF10 =
RRF50 - RRF100 -
COMPOUND ,
Dichlorodif luoromethane
Chlorome thane
Vinyl Chloride *
Bromomethane *
Chloroethane
Trichlorof luoromethane
1, 1-Dichloroethene *
1, 1, 2-Trichloro- '
1,2 , 2-trif luoroethane
Acetone
Carbon Disulfide
Methyl Acetate
*1ethylene Chloride
trans-1, 2-Dichloroethene
Methyl tert -Butyl Ether
1,1-Dichloroethane *
cis-1, 2-Dichloroethene
2-Butanone
Chloroform *
1, 1, 1-Trichloroethane *
Cyclohexane .
Carbon Tetrachloride *
Benzene *
1,2-Dichloroethane *
Trichloroethene *
Methyl eye lohexane
RRF10
RRF20
RRF50
RRF20
RRF200
RRF100
_
-
RRF200
RRF
%
RSD
*
*
*
*
*
*
*
*
*
it
*Compounds with required minimum RRF and maximum %RSD values.
All other compounds must meet a minimum RRF of 0.010.
page
of
FORM VI VOA-1
OLM04.2
-------
6B
VOLATILE ORGANICS INITIAL CALIBRATION DATA
Lab Name:
Lab Code:
Case No.:
Instrument ID:
Heated Purge: (Y/N)
GC Column: ID:
Contract:.
SAS No.:
Calibration Date(s):
Calibration Times:
(mm)
SDG No.
LAB FILE ID: RRF10 =
RRF50 - RRF100 -
COMPOUND
1 , 2 -Dichloropropane
Bromodichloromethane *
cis-1, 3-Dichloropropene *
4 -Methyl - 2 -pentanone
Toluene *
trans-1, 3-Dichloropropene *
1, 1, 2-Trichloroethane *
Tetrachloroethene *
2-Hexanone
Dibromochloromethane *
1, 2-Dibromoethane
Chlorobenzene *
Ethylbenzene *
Xylene (total) *
Styrene *
Bromoform *
Isopropylbenzene
1, 1, 2, 2-Tetrachloroethane *
1, 3-Dichlorobenzene *
1, 4-Dichlorobenzene *
1, 2-Dichlorobenzene *
1, 2-Dibromo-3-chloropropane
1,2,4-Trichlorobenzene *
Toluene -d8
Bromoflurobenzene *
1, 2-Dichloroethane-d4
RRF10
RRF20
_
RRF200 -
RRF20
RRF50
RRF100
RRF200
RRF
%
RSD
*
*
it
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*Compounds with required minimum RRF and maximum %RSD values.
All other compounds must meet a minimum RRF of 0.010.
FORM VI VGA-2
OLM04.2
-------
Lab Name:
Lab Code:
6C
SEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA
Contract:
Case No. : SAS No. : SDG No. :
Instrument ID:
Calibration Date(s):
Calibration Times:
LAB FILE ID: RRF20
RRF80 - RRF12
COMPOUND
Benzaldehyde
Phenol *
bis- (2-Chloroethyl) ether *
2-Chlorophenol *
2-Methylphenol *
2,2 ' -oxybis (1-Chloropropane)
Ac e t ophe none
4-Methylphenol *
N-Nitroso-di-n-propylamine *
Hexachloroethane *
Nitrobenzene *
Isophorone *
2-Nitrophenol *
2, 4-Dimethylphenol ' *
bis (2 -Chloroethoxy) methane *
2, 4-Dichlorophenol *
Naphthalene *
4-Chloroaniline
Hexachlorobutadiene
Caprolactam
4-Chloro-3-methylphenol *
2-Methylnaphthalene *
Hexachlorocyclopentadiene
2, 4, 6-Trichloropheriol *
2, 4, 5-Trichlorophenol *
1,1' -Biphenyl
2-Chloronaphthalene *
2 -Nitroaniline
Dimethylphthalate
2 , 6 -Dinitrotoluene *
Acenaphthylene' *
3 -Nitroaniline
Acenaphthene *
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran *
0 =
RRF20
RRF50
RRF80
RRF50
RRF160
RRF120
=
RRF160
"
RRF
""
%
RSD
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
*
* Compounds with required minimum RRF and maximum %RSD values.
All other compounds must meet a minimum RRF of 0.010.
FORM VI SV-1
OLM04.2
-------
Lab Name:
Lab Code:
6D
SEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA
Contract:
Case No. : SAS No. : SDG No. :
Instrument ID:
Calibration Date(s):
Calibration Times:
LAB FILE ID: RRF20
=
RRF80 - RRF120 -
COMPOUND
2,4-Dinitrotoluene *
Diethylphthalate
Fluorene *
4-Chlorophenyl-phenylether *
4 -Nitroaniline
4, 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine (1)
4-Bromophenyl-phenylether *
Hexachlorobenzene *
Atrazine
Pentachlorophe'nol' *
Phenanthrene *
Anthracene *
Carbazole
Di-n-butylphthalate
Fluoranthene *
Pyrene *
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene *
Chrysene *
bis(2-Ethylhexyl)phthalate
Di-n-octylphthalate
Benzo (b ) fluoranthene *
Benzo (k) fluoranthene *
Benzo (a)pyrene ' *
Indeno(l,2,3-cd)pyrene *
Dibenzo (a, h) anthracene *
Benzo (a,h, i)r>ervlene *
Nitrobenzene-d5 *
2-Fluorobiphenvl *
Terphenvl-dl4 *
Phenol -d5 *
2 - Fluorophenol *
2,4, 6-TribromoDhenol
2-Chlorot)henol-d4 *
1 . 2-Dichlorobpn7£?np-d4 *
RRF20
RRF50
RRF80
RRF50
=
RRF160 -
RRF120
RRF160
RRF
%
RSD
*
*
*
*
*
*
*
*
*
*
*
*
*
*
.*
it
*
*
*
*
*
*
*
*
*
(1) Cannot be separated from Diphenylamine
* Compounds with required minimum RRF and maximum %RSD values.
All other compounds must meet a minimum RRF of 0.010.
FORM VI SV-2
OLM04.2
-------
6E
PESTICIDE INITIAL CALIBRATION OF SINGLE COMPONENT ANALYTES
Lab Name:
Lab Code:
Instrument ID:
GC Column: ;
Case No.:
Contract:
SAS No.:
Level (x low): low
ID: (mm) Date(s) Analyzed:
SDG No.:
mid high
COMPOUND
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4,4' -DDE
Endrin
Endosulfan II
4,4' -ODD
Endosulfan sulfate
4,4' -DDT
Methbxychlor
Endrin ketone
Endrin aldehyde
alpha - Chlordane
gamma- Chlordane
Tetrachloro-m-xylene
Decachlorobiphenyl
RT
LOW
OF STANDA
MID
RDS
HIGH
MEAN
RT
RT W]
FROM
-
:NDOW
TO
* Surrogate retention times are measured from Standard Mix A analyses.
Retention time windows are ± 0.05 minutes for all compounds that elute before
Heptachlor expoxide, ± 0.07 minutes for all other compounds, except ± 0.10
minutes for Decachlorobiphenyl.
FORM VI PEST-1
OLM04.2
-------
Lab Name:
Lab Code:
6F
PESTICIDE INITIAL CALIBRATION OF SINGLE COMPONENT ANALYTES
Contract:
SAS No.:
Instrument ID:
GC Column:
Case No.:
Level (x low): low
ID: (mm) Date(s) Analyzed:
SDG No.:
mid high
COMPOUND
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4,4' -DDE
Endrin
Endosulfan II
4,4' -ODD
Endosulfan sulfate
4 ,4 ' -DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
alpha- Chlordane
gamma - Chlordane
Tetrachloro-m-xylene
Decachlorobiphenyl
LOW
CALIBRATIC
MID
)N FACTORS
HIGH
MEAN
%RSD
:
* Surrogate calibration factors are measured from Standard Mix A analyses.
FORM VI PEST-2
OLM04.2
-------
6G
PESTICIDE INITIAL CALIBRATION OF MULTICOMPONENT ANALYTES
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Instrument ID:
GC Column:
Date(s) Analyzed:
ID: (mm)
COMPOUND
Toxaphene
Aroclor 1016
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
AMOUNT
(ng)
PEAK1
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
. 5
1
2
3
4
5
RT
RT WI
FROM
NDOW
TO
CALIBRATION
FACTOR
lAt least 3 peaks for each column are required for identification of
multicomponent analytes.
FORM VI PEST-3
OLM04.2
-------
6H
PESTICIDE ANALYTE RESOLUTION SUMMARY
Lab Name:
Lab Code:
Case No.
Contract:
SAS No.:
SDG No.
GC Column (1):
ID:
EPA Sample No. (RESC##):
Date Analyzed (1) :
.(mm) Instrument ID (1):
Lab Sample ID (1):
Time Analyzed (1):
01
02
03
04
05
06
07
08
09
ANALYTE
RT
RESOLUTION
mn
pie
aly
01
02
03
04
05
06
07
08
09
(2) : ID: (mm) Instr
No. (RESC##) : Lab S
zed (2) : Time
ANALYTE
ument ID (2) :
ample ID (2) :
Analyzed (2) :
RT
RESOLUTION
(%)
FORM VI PEST-4
OLM04.2
-------
61
PERFORMANCE EVALUATION MIXTURE (PEM)
Lab Name:
Lab Code:
Case No.
Contract:
SAS No.:
SDG No.
GC Column (1) :
ID:
EPA Sample No. (PEM##):
Date Analyzed (1):
.(mm) Instrument ID (1) :
Lab Sample ID (1):
Time Analyzed (1):
01
02
03
04
05
06
07
08
ANALYTE
- -
RT
RESOLUTION
mn
iple
aly
01
02
03
04
05
06
07
08
(2) : . ID: (mm) Instl
No. (PEM##) : Lab £
zed (2) : Time
ANALYTE
-ument ID (2) :
.ample ID (2) :
Analyzed (2) :
RT
RESOLUTION
(%)
FORM VI PEST-5
OLM04.2
-------
6J
INDIVIDUAL STANDARD MIXTURE A
Lab Name:
Lab Code:
Case No.
Contract:
SAS No.:
SDG No.
GC Column (1) :
ID:
EPA Sample No. (INDAM##):
Date Analyzed (1):
.(mm) Instrument ID (1):
Lab Sample ID (1):
Time Analyzed (1) :
01
02
03
04
05
06
07
08
09
10
11
ANALYTE
.
RT
RESOLUTION
mn (2) : % ID: (mm) Instrument ID (2) :
pie
aly
01
02
03
04
05
06
07
08
09
10
11
No. (INDAMtttf) : Lab £
zed (2) : Time
ANALYTE
ample ID (2) :
Analyzed (2) :
RT
RESOLUTION
(%)
FORM VI PEST-6
OLM04.2
-------
Lab Name:
Lab Code:
6K
INDIVIDUAL STANDARD MIXTURE B
Contract:
Case No. : SAS No. :
SDG No.:
GC Column (1) :
ID:
EPA Sample No. (INDBMtftf):
Date Analyzed (1):
.(mm) Instrument ID (1):
Lab Sample ID (1):
Time Analyzed (1):
01
02
03
04
05
06
07
08
09
10
11
12
13
ANALYTE
RT
RESOLUTION
GC Column (2):
ID:
EPA Sample No, (INDBM##):
Date Analyzed (2):
.(mm) Instrument ID (2):
Lab Sample ID (2):
Time Analyzed (2):
01
02
03
04
05
06
07
08
09
10
11
12
13
ANALYTE
RT
RESOLUTION
FORM VI PEST-7
OLM04.2
-------
7A
VOLATILE CONTINUING CALIBRATION CHECK
Lab Name :
Lab Code :
Instrument ID:
Lab File ID:
Contract :
Case No.: SAS No.: SDG No.:
Calibration Date: Time:
Init. Calib. Date(s) :
EPA Sample No.(VSTD050##):
Heated Purge: (Y/N)
GC Column: ' ID:
Init. Calib. Times:
(mm)
COMPOUND
Dichlorodif luoromethane
Chlorome thane
Vinyl Chloride
Bromome thane
Chloroethane
Trichlorof luoromethane
1, 1-Dichloroethene
1,1, 2-Trichloro-l, 2, 2-trif luoroethane
Acetone
Carbon Disulfide
Methyl Acetate
Methylene Chloride
trans- 1, 2-Dichloroethene
Methyl tert -Butyl Ether
1, 1-Dichloroethane
cis-1, 2-Dichloroethene
2-Butanone
Chloroform
1,1, 1-Trichloroethane
Cyclohexane
Carbon Tetrachloride
Benzene
1 , 2 -Dichloroethane
Trichloroethene
Methylcyclohexane
RRF
RRF50
MIN
RRF
0.100
0.100
0.100
0.200
0.200
0.100
0.100
0.500
0.100
0.300
%D
MAX
%D
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
All other compounds must meet a minimum RRF of 0.010.
FORM VII VOA-1
OLM04.2
-------
Lab Name:
Lab Code:
Instrument ID:
Lab File ID:
7E
VOLATILE CONTINUING CALIBRATION CHECK
Contract:
SAS No.:
Case No.:
EPA Sample No.(VSTD050##):
Heated Purge: (Y/N) ;
GC Column: ID:
SDG No.:
Calibration Date:
Time:
Init. Calib. Date(s):
Init. Calib. Times:
.(mm)
COMPOUND
1,2-Dichloropropane
Bromodichloromethane
cis-1, 3-Dichloropropene
4'-Methyl - 2 -pentanone
Toluene
trans-1, 3-Dichloropropene
1, 1, 2-Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1 , 2 -Dibromoethane
Chlorobenzene
Ethylbenzene
Xylene (total)
Styrene
Bromof orm
Isopropylbenzene
1,1,2, 2-Tetrachloroethane
1 , 3 -Dichlorobenzene
1,4-Dichlorobenzene
1., 2 -Dichlorobenzene.
1, 2-Dibromo-3-chloropropane
1, 2,4-Trichlorpbenzene
Toluene -d8
Bromof lurobenzene
l,2-Dichloroethane-d4.
RRF
RRF50
MIN
RRF
0.200
0.200
0.400
0.100
0.100
0.200
0.100
0.500
0.100
0.300
0.300
0.100
0.300
0.600
0.500
0.400
0.200
0.200
%D
.
MAX
%D
.
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25:0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
All other compounds must meet a minimum RRF of 0.010.
FORM VII VOA-2
OLM04.2
-------
Lab Name:
Lab Code:
7C
SEMIVOLATILE CONTINUING CALIBRATION CHECK
Contract:
SAS No.:
Case No.:
SDG No.:
Instrument ID:
Lab File ID:
Calibration Date:
Time:
EPA Sample No.(SSTD050##):
GC Column: ID:
Init. Calib. Date(s) :.
Init. Calib. Times:
(mm)
COMPOUND
Benzaldehyde
Phenol
bis- (2-Chloroethyl) ether
2-Chlorophenol
2 -Methylphenol
2,2' -oxybis (1-Chloropropane)
Acetophenone
4 -Methylphenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Nit roberiz ene
Isophorone
2 -Nitrophenol
2 , 4 -Dimethylphenol
bis (2 -Chloroethoxy) methane
2 , 4 -Dichlorophenol
Naphthalene
4 - Chloroani 1 ine
Hexachlorobutadiene
Caprolactam
4 -Chloro- 3 -methylphenol
2 -Methylnaphthalene
Hexachlorocyclopentadiene
2,4, 6-Trichlorophenol
2,4, 5-Trichlorophenol
1,1' -Biphenyl
2-Chloronaphthalene
2 -Nitroaniline
Dimethylphthalate
2, 6-Dinitrotol'uene
Acenaphthylene
3 -Nitroaniline
Acenaphthene
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran
RRF
-
RRF50
MIN
RRF
0.800
0.700
0.800
0.700
0.600
0.500
0.300
0.200
0.400
0.100
0.200
0.300
0.200
"0.700
0.200
0.400
0.200
0.200
0.800
0.200
0.900
0.900
0.800
%D
MAX
%D
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
All other compounds must meet a minimum RRF of 0.010.
FORM VII SV-1
OLM04.2
-------
Lab Name:
Lab Code:
7D
SEMIVOLATILE CONTINUING CALIBRATION CHECK
Contract:
SAS No.:
Case No.:
Instrument ID:
Lab File ID:
Calibration Date:
SDG No.: _
Time:
EPA Sample No.(SSTD050##):
GC Column: ID:
Init. Calib. Date(s):
Init. Calib. Times:
(mm)
COMPOUND
2 , 4 -binitrotoluene
Diethylphthalate
Fluorene
4-Chlorophenyl-phenylether
4 -Nitroaniline
4, 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine (1)
4 -Brpmophenyl-phenylether
Hexachlorobenzene
Atrazine
Pentachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene
Chrysene
bis (2-Ethylhexyl)phthalate
Di-n-octylphthalate
Benzo (b) f luoranthene
Benzo (k) f luoranthene
Benzo (a) pyrene
Indeno ( 1 , 2 , 3 - cd) pyrene
Dibenzo (a, h) anthracene
Benzo (g, h, i) perylene
Nitrobenzene -d5
2-Fluorobiphenyl
Terphenyl-dl4
Phenol -d5
2-Fluorophenol .
2,4, 6 -Tribromophenol
2-Chlorophenol-d4
1, 2-Dichlorobenzene-d4
RRF
RRF50
MIN
RRF
0.200
0.900
0.400
0.100
0.100
0.050
0.700
0.700
0.600
0.600
0.800
0.700
0.700
0.700
0.700
0.500
0.400
0.500
0.200
0.700
0.500
0.800
0.600
0.800
0.400
%D
MAX
%D
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
(1) Cannot be separated from Diphenylamine
All other compounds must meet a minimum RRF of 0.010.
FORM VII SV-2
OLM04.2
-------
7E
PESTICIDE CALIBRATION VERIFICATION SUMMARY
Lab Name :
Lab Code :
GC Column:
Case No. :
ID:
Contract :
SAS No. : SDG No. :
(mm) Init . Calib. Date(s):
EPA Sample No. (PIBLK##):
Lab Sample ID (PIBLK):
EPA Sample No. (PEM##): _
Lab Sample ID (PEM):
Date Analyzed:
Time Analyzed:
Date Analyzed:
Time Analyzed:
PEM
COMPOUND
alpha -BHC
beta-BHC
gamma-BHC (Lindane)
Endrin
4, 4 '-DDT .
Methoxychlor
RT
RT Wl
FROM
NDOW
TO
CALC
AMOUNT
(ng)
NOM
AMOUNT
(ng)
%D
4,4'-DDT % Breakdown (1)
Combined % Breakdown (1)
Endrin % breakdown (1):.
FORM VII PEST-1
OLM04.2
-------
7F
PESTICIDE CALIBRATION VERIFICATION SUMMARY
Lab Name :
Lab Code :
GC Column:
Case No. :
ID:
Contract :
SAS No. :
(mm) Init. Calib.
SDG No . :
Date(s) :
EPA Sample No. (PIBLK##):
Lab Sample ID (PIBLK):
EPA Sample No. (INDAM##):
Lab Sample ID (INDA):
Date Analyzed:
Time Analyzed:
Date Analyzed:
Time Analyzed:
INDIVIDUAL MIX A
COMPOUND
alpna-BHC
gamma -BHC (Lindane)
Heptachlor
Endosulfan I
Dieldrin
Endrin
4,4' -ODD
4,4' -DDT
Methoxychlor
Tetrachloro-m-xylene
Decachlorobiphenyl
RT
RT W]
FROM
ENDOW
TO
CALC
AMOUNT
(ng)
NOM
AMOUNT
(ng)
%D
EPA Sample No. (INDBM##)
Lab Sample ID (INDB): _
Date Analyzed:
Time Analyzed:
INDIVIDUAL MIX B
COMPOUND
tieta-BHC
delta-BHC
Aldrih
Heptachlor epoxide
4, 4 '-DDE
Endosulfan II
Endosulfan sulfate
Endrin ketone
Endrin aldehyde
alpha- Chlordane
gamma- Chlordane
Tetrachloro-m-xylene
Decachlorobiphenyl
RT
RT W]
FROM
CNDOW
TO
CALC
AMOUNT
(ng)
NOM
AMOUNT
(ng)
%D
FORM VII PEST-2
OLM04.2
-------
Lab Name:
Lab Code:
8A
VOLATILE INTERNAL STANDARD AREA AND RT SUMMARY
Contract:
Case No. : SAS No. :
SDG No.:
EPA Sample No.(VSTD050##):
Lab File ID (Standard):
Instrument ID:
GC Column: ID:
Date Analyzed:
Time Analyzed:
Heated Purge: (Y/N).
.(mm)
12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
'
IS1 (BCM)
AREA #
RT #
IS2 (DFB)
AREA #
RT #
IS3 (CBZ)
AREA #
RT #
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
IS1 (BCM) = Bromochloromethane
IS2 (DFB) = 1,4-Difluorobenzene
IS3 (CBZ) = Chlorobenzene-d5
AREA UPPER LIMIT = + 100% of internal standard area
AREA LOWER LIMIT = - 50% of internal standard area
RT UPPER LIMIT = + 0.50 minutes of internal standard RT
RT LOWER LIMIT = - 0.50 minutes of internal standard RT
# Column used to flag values outside QC limits with an asterisk.
* Values outside of QC limits
page_
of
FORM VIII VOA
OLM04.2
-------
Lab Name:
Lab Code:
SB
SEMIVOLATILE INTERNAL STANDARD AREA AND RT SUMMARY
Contract:
SAS No.:
Case No.:
EPA Sample No. (SSTD050M) :
Lab File ID (Standard):
Instrument ID:
SDG No.:
Date Analyzed:
Time Analyzed:
GC Column:
ID:
(mm)
12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
NO.
T*
-."'
*
"
ISl (DCB)
AREA '#
RT #
IS2 (NPT)
AREA #
RT #
IS3 (ANT)
AREA #
RT #
-
o-
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
ISl (DCB) = l,4-Dichlorobenzene-d4
IS2 (NPT) = Naphthalene-d8
IS3 (ANT) = Acenaphthene-dlO
AREA UPPER LIMIT = + 100% of internal standard area
AREA LOWER LIMIT = - 50% of internal standard area
RT UPPER LIMIT = + 0.50 minutes of internal standard RT
RT LOWER LIMIT = - 0.50 minutes of internal standard RT
# Column used to flag values outside QC limits with an asterisk.
* Values outside of QC limits
page.
of
FORM VIII SV-1
OLM04.2
-------
Lab Name:
Lab Code:
8C
SEMIVOLATILE INTERNAL STANDARD AREA AND RT SUMMARY
' Contract:
Case No. : . SAS No. : SDG No. :
EPA Sample No.(SSTD050##):
Lab File ID (Standard):
Instrument ID:
Date Analyzed:
Time Analyzed:
GC Column:
ID:
.(mm)
12 HOUR STD
UPPER LIMIT -
LOWER LIMIT
EPA SAMPLE
NO.
IS4 (PHN)
AREA #
RT #
X
IS5 (CRY)
AREA #
RT #
IS6 (PRY)
AREA #
RT #
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
IS4 (PHN) = Phenanthrene-dlO
IS5 (CRY) = Chrysene-dl2
IS6 (PRY) = Perylene-dl2
AREA UPPER LIMIT = + 100% of internal standard area
AREA LOWER LIMIT = - 50% of internal standard area
RT UPPER LIMIT = + 0.50 minutes of internal standard RT
RT LOWER LIMIT = - 0.50 minutes of internal standard RT
# Column used to flag values outside QC limits with an asterisk.
* Values outside of QC limits
page_
of
FORM VIII SV-2
OLM04.2
-------
Lab Name:
Lab Code:
GC Column:
8D
PESTICIDE ANALYTICAL SEQUENCE
Contract:
SAS No.:
Case No. :
ID: (mm) Init. Calib. Date(s):
SDG No.:
Instrument ID:
THE ANALYTICAL SEQUENCE OF PERFORMANCE EVALUATION MIXTURES, BLANKS, SAMPLES,
AND STANDARDS IS GIVEN BELOW:
MEAN SURROGATE RT FROM INITIAL CALIBRATION
TCX : DCB :
EPA
SAMPLE NO .
LAB
SAMPLE ID
DATE
ANALYZED
TIME
ANALYZED
-
TCX
. RT #
DCB
RT #
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
TCX = Tetrachloro-m-xylene
DCB = Decachlorobiphenyl
QC LIMITS
(± 0.05 MINUTES)
(± 0.10 MINUTES)
# Column used to flag retention time values with 'an asterisk.
* Values outside of QC limits.
page
of
FORM VIII PEST
OLM04.2
-------
9A
PESTICIDE FLORISIL CARTRIDGE CHECK
Lab Name:
Lab Code:
Case No.:
Florisil Cartridge Lot Number:
GC Column (1) : ID: (mm)
Contract:
SAS No. : SDG No. :
Date of Analysis:
GC Column(2) : ID:
(mm)
COMPOUND
alpna-BHC
gamma-BHC (Lindane)
Heptachlor
Endosulfan I
Dieldrin
Endrin
4,4' -ODD
4,4 ' -DDT
Methoxychlor
Tetrachloro-m-xylene
Decachlorobiphenyl
2,4. 5-Trichloror>henol
SPIKE
ADDED
(ng)
SPIKE
RECOVERED
(ng)
%
REC #
QC
LIMITS
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
<5
# Column to be used to flag recovery with an asterisk.
* Values outside of QC limits.
THIS CARTRIDGE LOT APPLIES TO THE FOLLOWING SAMPLES, BLANKS, MS, AND MSD:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
EPA
SAMPLE NO.
LAB
SAMPLE ID
DATE
ANALYZED 1
DATE
ANALYZED 2
page
of
FORM IX PEST-1
OLM04.2
-------
9B
PESTICIDE GPC CALIBRATION VERIFICATION
Lab Name:
Lab Code:
GPC Column:
Case No.:
Contract:
SAS No.:
SDG No.:
GC Column(1):
ID:
Calibration Verification Date:
.(mm) GC Column(2) : ID: (mm)
COMPOUND
gamma-BHC (Liridane)
HeTDtachlor
Aldrin
Dieldrin
Endrin
4.4' -DDT
SPIKE
ADDED
(ng)
SPIKE
RECOVERED
(ng)
%
REC #
QC
LIMITS
80-110
80-110
80-110
80-110
80-110
80-110
# Column to be used to flag recovery with an asterisk.
* Values outside of QC limits.
THIS GPC CALIBRATION VERIFICATION APPLIES TO THE FOLLOWING SAMPLES, BLANKS,
MS, AND MSD:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
. EPA
SAMPLE NO.
LAB
SAMPLE ID
DATE
ANALYZED 1
DATE '
ANALYZED 2
page
of
FORM IX PEST-2
OLM04.2
-------
10A
PESTICIDE IDENTIFICATION SUMMARY
FOR SINGLE COMPONENT ANALYTES
Lab Name:
Lab Code:
Case No.:
Lab Sample ID:
Instrument ID (1):
GC Column:(1):
ID:
Contract:
SAS No.:
.(mm) GC Column:(2):
EPA SAMPLE NO.
SDG No.:
Date(s) Analyzed:
Instrument ID (2):
ID:
.(mm)
ANALYTE
COL
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
RT
RT WI
FROM
NDOW
TO
CONCENTRATION
%D
page
of
FORM X PEST-1
OLM04.2
-------
Lab Name:
Lab Code:
10B
PESTICIDE IDENTIFICATION SUMMARY
FOR MULTICOMPONENT ANALYTES
Contract:
SAS No.:
EPA SAMPLE NO.
Case No.:
SDG No.:
Lab Sample ID:
Instrument ID (1):
GC Column:(1):
Date(s) Analyzed:
Instrument ID (2):
ID:
.(mm) GC Column:(2):
ID:
(mm)
ANALYTE
COLUMN 1
COLUMN 2
COLUMN 1
COLUMN 2
COLUMN 1
COLUMN 2
PEAK
1
2
3
4
5 '
1.
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
1
2
3
4
5
RT
RT W]
FROM
.,
NDOW
TO
CONCENTRATION
J-
MEAN
CONCENTRATION
%D
At least 3 peaks for each column are required for identification of
multicomponent analytes.
page
of
FORM X PEST-2
OLM04.2
-------
SAMPLE LOG-IN SHEET
Lab Name
Received By (Print Name)
Page of 1
c
Log- in Date
Received By (Signature)
Case Number
Remarks :
1. Custody Seal(s)
2 . Custody Seal Nos .
3 . Chain of Custody
Records
4 . Traffic Reports
or Packing Lists
5. Airbill
6. Airbill No.
7 . Sample .Tags
Sample Tag
Numbers
8 . Sample Condition
9. Cooler
Temperature
10. Does information
on custody
records, traffic
reports, and
sample tags
agree?
11. Date Received at
Lab
12. Time Received
Present /Absent*
Intact /Broken
Present /Absent*
Present /Absent*
Airbill/Sticker
Present /Absent*
Present /Absent*
Listed/Not
Listed on Chain-
of -Custody
Intact/Broken* /
Leaking
Yes/No*
Sample Transfer
Fraction
Area #
By
On
Fraction
Area #
By
On
Sample Delivery Group No.
EPA Sample
#
Corresponding
Sample Tag
#
Assigned Lab #
SAS Number
Remarks :
Condition of
Sample
Shipment , etc .
I
* Contact SMO and attach record of resolution
Reviewed By
Date
Logbook No. f
Logbook Page No.
FORM DC-1
OLM04.2
-------
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET
LABORATORY NAME,
CITY/STATE
CASE NO. SDG NO. SDG NOS. TO FOLLOW_
SAS NO.
CONTRACT NO.
SOW NO.
All documents delivered in the Complete SDG File must be original documents where
possible.
PAGE NOs CHECK
FROM TO LAB EPA
1. Inventory Sheet (Form DC-2) (Do not Number)
2. SDG Case Narrative
3. SDG Cover Sheet/Traffic Report
4. Volatiles Data
a. QC Summary
System Monitoring Compound Summary (Form II .
Matrix Spike/Matrix Spike Duplicate Summary
(Form III VOA)
Method Blank Summary (Form IV VOA) '
GC/MS Instrument Performance Check (Form V VOA)
Internal Standard Area and RT Summary
(Form VIII VOA)
b. Sample Data
TCL Results - (Form I VOA-1, VOA-2)
Tentatively Identified Compounds (Form I VOA-
Reconstructed total ion chromatograms (RIC) for
each sample
For each sample:
Raw Spectra and background-subtracted mass
spectra of target compounds identified
Quantitation reports
Mass Spectra of all reported TICs with three
best library matches
c. Standards Data (All Instruments)
Initial Calibration Data (Form VI VOA-1, VOA-2)
RICs and Quan Reports for all Standards
Continuing Calibration Data
(Form VII VOA-1, VOA-2)
RICs and Quantitation Reports for all Standards
d. Raw QC Data
BFB
Blank Data
Martix Spike/Matrix Spike Duplicate Data
FORM DC-2-1 OLM04.2
-------
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (cont.)
CASE NO. SDG NO. SDG NOS. TO FOLLOW .
SAS NO. '
PAGE NOs CHECK
FROM TO LAB EPA
5. Semivolatlies Data
a. QC Summary
Surrogate Percent Recovery Summary (Form II SV)
MS/MSD Summary (Form III SV)
Method Blank Summary (Form IV SV)
GC/MS Instrument Performance Check (Form V SV)
Inte'rnal Standard Area and RT Summary
(Form VIII SV)
b. Sample Data
TCL Results - (Form I SV-1, SV-2)
Tentatively Identified Compounds (Form I SV-
Reconstructed total ion chromatograms (RIC) for
each sample
For each sample:
Raw Spectra and background-subtracted mass
spectra of target compounds
Quantitation reports
Mass Spectra of TICs with three best library
matches
GPC chromatograms (if GPC is required)
c. Standards Data (All Instruments)
Initial Calibration Data (Form VI SV-1, SV-2)
RICs and Quan Reports for all Standards
Continuing Calibration Data (Form VII SV-1, SV-
RICs and Quantitation Reports for all Standards
d. Raw QC Data
DFTPP
/
Blank Data
Matrix Spike/Matrix Spike Duplicate Data
e. Raw GPC Data
6. Pesticides Data
a. QC Summary
Surrogate Percent Recovery Summary (Form II
MS/MSD Duplicate Summary (Form III PEST)
Method Blank Summary (Form IV PEST)
FORM DC-2-2 OLM04 . 2
-------
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (cont.)
CASE NO. SDG NO. SDG NOS. TO FOLLOW .
SAS NO.
PAGE NOs CHECK
FROM TO LAB EPA
6. Pesticides Data (Cont.)
b. Sample Data
TCL Results - Organic Analysis Data Sheet
(Form I PEST)
Chromatograms (Primary Column)
Chromatograms from second GC column
GC Integration report or data system printout
Manual work sheets
For pesticides/Aroclors by GC/MS,
Copies of raw spectra and copies of
background-subtracted mass spectra of target
compounds (samples & standards)
c. Standards Data
Initial Calibration of Single Component
(Form VI PEST-1 and PEST-2)
Initial Calibration of Multicomponent Analytes
(Form VI PEST-3)
Analyte Resolution Summary (Form VI PEST-4)
Performance Evaluation Mixture (Form VI PEST-5)
Individual Standard Mixture A (FORM VI PEST-6)
Individual Standard Mixture B (FORM VI PEST-7)
Calibration Verification Summary
(Form VII PEST-1)
Calibration Verification Summary
(Form VII PEST-2)
Analytical Sequence (Form VIII PEST)
Florisil Cartridge Check (Form IX PEST-1)
Pesticide GPC Calibration (Form IX PEST-2)
Pesticide Identification Summary for Single
Component Analytes (Form X PEST-1)
Pesticide Identification Summary for
Multicomponent Analytes (Form X PEST-2)
Chromatograms and data system printouts
A printout of retention times and
corresponding peak areas or peak heights
d. Raw QC Data
Blank Data
Matrix Spke/Matrix Spike Duplicate Data
FORM DC-2-3 OLM04 . 2
-------
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (cont.)
CASE NO.
SDG NO.
SDG NOS. TO FOLLOW.
SAS NO.
6. Pesticides Data (Cont.)
e. Raw GPC Data
PAGE NOs
FROM TO
CHECK
LAB EPA
f. Raw Florisil Data
7. Miscellaneous Data
Original preparation and analysis forms or
of preparation and analysis logbook pages
Internal sample and sample extract transfer
chain-of-custody records
Screening records
All instrument output, including strip charts
from screening activities (describe or list)
8. EPA Shipping/Receiving Documents
Airbills (No. of shipments )
Chain-of-Custody Records
Sample Tags
Sample Log-in Sheet (Lab & DC1)
Miscellaneous Shipping/Receiving Records
(describe or list)
9. Internal Lab Sample Transfer Records and Tracking
Sheets (describe or list)
10. Other Records (describe or list)
Telephone Communication Log
11. Comments;
FORM DC-2-4
OLM04 . 2
-------
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (cont.)
CASE NO. SDG NO. SDG NOS. TO FOLLOW
SAS NO.
Completed by: _____^^^_^^_^^_^^_ _^^__^^^^^
(CLP Lab) (Signature)(Printed Name/Title) (Date)
Verified by: _^_^_^ ^_^_^_ ^_^.
(CLP Lab) (Signature) (Printed Name/Title) (Date)
Audited by:
(EPA) (Signature) (Printed Name/Title) (Date)
FORM DC-2-5 OLM04.2
-------
EXHIBIT C
TARGET COMPOUND LIST AND
CONTRACT REQUIRED QUANTITATION LIMITS
NOTE: Specific quantitation limits are highly matrix-dependent. The
guantitation limits listed herein are provided for guidance and may not
always be achievable.
All CRQLs are rounded to two significant figures.
The CRQL values listed on the following pages are based on the analysis
of samples according to the specifications given in Exhibit D.
For soil samples, the moisture content of the samples must be used to
adjust the CRQL values appropriately.
C-l OLM04.2
-------
Exhibit C - Target Compound List and Contract Required Quantitation Limits
Table of Contents
Section . Page
1.0 VOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION
LIMITS 3
2.0 SEMIVOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION
LIMITS , 5
3.0 PESTICIDES/AROCLORS TARGET COMPOUND LIST AND CONTRACT REQUIRED
QUANTITATION LIMITS 8
C-2 OLM04.2
-------
Exhibit C -- Section 1
Volatiles (VOA)
1.0 VOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION LIMITS
Ouantitation Limits
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
34.
35.
Volatiles
Di chl orodi fl uorome thane
Chlorome thane
Vinyl Chloride
Bromomethane
Chloroethane
Tri chl orofl uorome thane
1, 1-Dichloroethene
1, 1,2-Trichloro-
1,2,2-trifl uoroe thane
Acetone
Carbon Disulfide
Methyl Acetate
Methylene Chloride
trans-1, 2-Dichloroethene
Methyl tert -Butyl Ether
1 , 1-Dichloroe thane
cis- 1, 2-Dichloroethene
2-Butanone
Chloroform
1,1, 1-Trichloroethane
Cyclohexane
Carbon Tetrachloride
Benzene
1 , 2 -Dichloroethane
Trichloroethene
Me thyl cycl ohexane
1 , 2 -Dichloropropane
Bromodichloromethane
cis-1 , 3-Dichloropropene
4 -Methyl -2 -pentanone
Toluene
trans -1,3-
Dichloropropene
1,1, 2-Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
CAS Number
75-71-8
74-87-3
75-01-4
74-83-9
75-00-3
75-69-4
75-35-4
76-13-1
67-64-1
75-15-0
79-20-5
75-09-2
156-60-5
1634-04-4
75-34-3
156-59-2
78-93-3
67-66-3
71-55-6
110-82-7
56-23-5
71-43-2
107-06-2
79-01-6
108-87-2
78-87-5
75-27-4
10061-01-5
108-10-1
108-88-3
10061-02-6
79-00-5
127-18-4
591-78-6
124-48-1
Water
ua/L
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Low
Soil
uq/Kq
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Med.
Soil
uq/Kq
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1.200
1200
On
Column
(nq)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(5.0)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
C-3
OLM04.2
-------
Exhibit C -- Section 1
Volatiles (VGA)
1.0 VOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION LIMITS
(Con't)
Ouantitation Limits
36.
37.
38.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48.
Volatiles
1 , 2 -Dibromoethane
Chlorobenzene
Ethylbenzene
Xylenes (total)
Styrene
Bromoform
Isopropylbenzene
1,1,2,2-
Tetrachloroethane
1,3-Di chlorobenzene
1,4-Di chlorobenzene
1, 2-Dichlorobenzene
'. 1, 2-Dibromo-3-chloropropane
1,2,4- Trichlorobenzene
CAS Number
106-93-4
108-90-7
100-41-4
1330-20-7
100-42-5
75-25-2
98-82-8
79-34-5
541-73-1
106-46-7
95-50-1
96-12-8
120-82-1
Water
UQ/L
10
10
10
10
10
10
10
10
10
10
10
10
10
Low
Soil
uq/Kq
10
10
10
10
10
10
10
10
10
10
10
10
10
Med.
Soil
uq/Kq
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
1200
On
Column
(nq)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
C-4
OLM04.2
-------
2.0
Exhibit C -- Section 2
Semivolatiles .(SVGA)
SEMIVOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION
LIMITS
Ouantitation Limits
49.
' 50.
. 51.
52.
53.
54.
55.
56.
57.
58.
59.
60.
61.
62.
63.
64.
65.
66.
67.
68.
69.
70.
71.
72.
73.
Semivolatiles CAS
Benzaldehyde
Phenol
bis- (2-Chloroethyl)
ether
2 - Chi or opheno 1
2-Methylphenol
2,2 ' -oxybis (1-
Chloropropane ) 1
Acetophenone
4 -Methylphenol
N-Nitroso-di-n
propylatnine
Hexachloroethane
Nitrobenzene
Isophorone
2 -Nitrophenol
2 , 4 -Dimethylphenol
bis (2-Chloroethoxy)
methane
2 , 4 -Dichlorophenol
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
Caprolactam
4-Chloro-3-
methylphenol
2 -Methylnaphthalene
Hexachlorocyc lo -
pentadiene
2,4, 6 -Trichlorophenol
2 , 4 , 5-Trichlorophenol
Number
100-52-7
108-95-2
111-44-4
95-57-8
95-48-7
108-60-1
98-86-2
106-44-5
621-64-7
67-72-1
98-95-3
78-59-1
88-75-5
105-67-9
111-91-1
120-83-2
91-20-3
106-47-8
87-68-3
105-60-2
59-50-7
91-57-6
77-47-4
88-06-2
95-95-4
Water
UQ/-L
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
25
Low
Soil
uq/Kq
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
830
Med.
Soil
uq/Kq
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
25000
On
Column
(nq)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(50)
1 Previously known by the name bis(2-Chloroisopropyl)ether.
C-5
OLM04.2
-------
Exhibit C -- Section 2
Semivolatiles (SVGA)
2.0 SEMIVOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION
LIMITS (Con't)
Ouantitation Limit
74.
75.
76.
77.
78.
79.
80.
81.
82.
83 .
84.
85.
86.
87.
88.
89.
90.
91.
92.
93.
94.
95.
96.
97.
98.
99.
100.
101.
102.
103.
104.
105.
Semivolatiles
1,1' -Biphenyl
2-Chloronaphthalene
2 -Nitroaniline
Dimethylphthalate
2 , 6-Dinitrotoluene
Acenaphthylene
3 -Nitroaniline
Acenaphthene
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran
2 , 4-Dinitrotoluene
Diethylphthalate
Fluorene
4-Chlorophenyl-
phenyl ether
4 -Nitroaniline
4, 6-Dinitro-2-
methylphenol
N-Nitroso
diphenylamine
4 - Bromophenyl -
phenylether
Hexachlorobenzene
Atrazine
Pehtachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3'-
Dichlorobenz idine
Benzo (a) anthracene
Chrysene
CAS Number
92-52-4
91-58-7
88-74-4
131-11-3
606-20-2
208-96-8
99-09-2
83-32-9
51-28-5
100-02-7
132-64-9
121-14-2
84-66-2
86-73-7
7005-72-3
100-01-6
534-52-1
86-30-6
101-55-3
118-74-1
1912-24-9
87-86-5
85-01-8
120-12-7
86-74-8
84-74-2
206-44-0
129-00-0
85-68-7
91-94-1
56-55-3
218-01-9
Water
UQ/L
10
10
25
10
10
10
25
10
25
25
10
10
10
10
10
25
25
10
10
10
10
25
10
10
10
10
10
10
10
10
10
10
Low
Soil
ua/Ka
330
330
830
330
330
330
830
330
830
830
330
330
330
330
330
830
830
330
330
330
330
830
330
330
330
330
330
330
330
330
330
330
Med.
Soil
UQ/Kq
10000
10000
25000
10000
10000
10000
25000
10000
25000
25000
10000
10000
10000
10000
10000
25000
25000
10000
10000
10000 -
10000
25000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
On
Column
(net)
(20)
(20)
(50)
(20)
(20)
(20)
(50)
(20)
(50)
(50)
(20)
(20)
(20)
. (20)
(20)
(50)
(50)
(20)
(20)
(20)
(20)
(50)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
C-6
OLM04.2
-------
2.0
Exhibit C -- Section 2
Semivolatiles (SVOA)
SEMIVOLATILES TARGET COMPOUND LIST AND CONTRACT REQUIRED QUANTITATION
LIMITS (Con't)
Ouantitation Limits
Semivolatiles
Water
CAS Number uq/L
Low
Soil
uq/Kq
Med.
Soil
uq/Kq
On
Column
(nor)
106. bis(2-Ethylhexyl) 117-81-7 10 330 10000 (20)
phthalate
107. Di-n-octylphthalate 117-84-0 10 330 10000 (20)
108. Benzo(b)fluoranthene 205-99-2 10 330 10000 (20)
109. Benzo(k)fluoranthene 207-08-9 10 330 10000 (20)
110. Benzo(a)pyrene - 50-32-8 10 330 10000 (20)
111.. Indeno(l,2,3-cd)- 193-39-5 10 330 10000 (20)
pyrene
112. Dibenzo(a.h)- 53-70-3 10 330 10000 (20)
anthracene
113. Benzo(g,h,i)perylene 191-24-2 10 330 10000 (20)
C-7
OLM04.2
-------
EXHIBIT D
ANALYTICAL METHODS
FOR VOLATILES
D-l/VOA OLM04.2
-------
Exhibit C -- Section 3
Pesticides/Aroclors (PEST/ARO)
3.0 PESTICIDES/AROCLORS TARGET COMPOUND LIST AND CONTRACT REQUIRED
QUANTITATION LIMITS2
Ouantitation
Pesticides/Aroclors
114.
115.
116.
117.
118.
119.
120.
121.
122.
123.
124.
125.
126.
127.
128.
129.
130.
131.
132.
133.
134.
135.
136.
137.
138.
139.
140.
141.
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide3
Endosulfan I
Dieldrin
4,4' -DDE
Endrin
Endosulfan II
4,4' -ODD
Endosulfan sulfate
4,4' -DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
a Ipha - Chi or dane
gamma- Chlordane
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
CAS Number
319-84-6
319-85-7
319-86-8
58-89-9
76-44-8
309-00-2
1024-57-3
959-98-8
60-57-1
72-55-9
72-20-8
33213-65-9
72-54-8
1031-07-8
50-29-3
72-43-5
53494-70-5
7421-93-4
5103-71-9
5103-74-2
8001-35-2
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
Water
ua/L
0.050
0.050
0.050
0.050
0.050
0.050
0.050
0.050
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.50
0.10
0.10
0.050
0.050
5.0
1.0
2.0
1.0
1.0
1.0
1.0
1.0
Soil
UQ/Kq
1.7
1.7
1.7
1.7
1.7
1.7
1.7 -
1.7
3.3
3.3
3.3
3.3
3.3
3.3
3.3
17
3.3
3.3
1.7
1.7
170
33
67
33
33
33
33
33
Limits
On Column
(oa)
5
5
5
5
5
5
5
5
.10
10
10
10
10
10
10
50
10
10
5
5
500
100
200
100
100
100
100
100
2There is no differentiation between the preparation of low and medium
soil samples in this method for the analysis of pesticides/Aroclors.
3Only the exo-epoxy isomer (isomer B) of heptachlor epoxide is reported
on the data reporting forms (Exhibit B).
C-8 ' OLM04.2
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Exhibit D - Analytical Methods for Volatiles
Table of Contents
Section Page
1.0 SCOPE AND APPLICATION 4
2.0 SUMMARY OF METHOD 5
2.1 Water 5
2.2 Low Level Soil 5
2.3 Medium Level Soil 5
3.0 DEFINITIONS 5
4 . 0 INTERFERENCES 6
5.0 SAFETY 6
6.0 EQUIPMENT AND SUPPLIES 7
7.0 REAGENTS AND STANDARDS 13
7.1 Reagents 13
7.2 Standards 13
7.3 Storage of Standard Solutions 16
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 18
8.1 Sample Collection and Preservation 18
8.2 Procedure for Sample Storage 18
8.3 Contract Required Holding Times ... 19
9.0 CALIBRATION AND STANDARDIZATION 20
9.1 Instrument Operating Conditions ... 20
9.2 GC/MS Calibration (Tuning) and Ion Abundance 22
9.3 Initial Calibration 23
9.4 Continuing Calibration 26
10.0 PROCEDURE 29
10.1 Sample Preparation 29
10.2 pH Determination (Water Samples) 35
10.3 Percent Moisture Determination 35
11.0 DATA ANALYSIS AND CALCULATIONS 37
11.1 Qualitative Identification 37
11.2 Calculations 39
11.3 Technical Acceptance Criteria for Sample Analysis 44
11.4 Corrective Action for Sample Analysis 45
12.0 QUALITY CONTROL 48
12.1 Blank Analyses 48
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD) 51
13.0 METHOD PERFORMANCE 55
14.0 POLLUTION PREVENTION 55
D-2/VOA OLM04.2
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15.0 WASTE MANAGEMENT 55
16.0 REFERENCES . 55
17.0 TABLES/DIAGRAMS/FLOWCHARTS 56
APPENDIX A - SCREENING OF HEXADECANE EXTRACTS FOR VOLATILES 65
1.0 SCOPE AND APPLICATION 65
2.0 SUMMARY OF METHODS 65
3.0 INTERFERENCES 66
4.0 SAFETY 66
5.0 EQUIPMENT AND SUPPLIES 66
6.0 REAGENTS AND STANDARDS 67
7.0 QUALITY CONTROL 68
8.0 CALIBRATION AND STANDARDIZATION 69
9.0 PROCEDURE 69
APPENDIX B - MODIFIED SW-846 METHOD 5035 FOR VOLATILES IN LOW LEVEL SOILS . 72
1.0 SCOPE AND APPLICATION '. . . 72
2. 0 SUMMARY OF METHOD 72
3.0 INTERFERENCES 72
4.0 SAFETY , . 73
5.0 EQUIPMENT AND SUPPLIES 73
6. 0 REAGENTS AND STANDARDS ' 75
7.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 76
8.0 CALIBRATION AND STANDARDIZATION 77
9.0 PROCEDURE : 79
10.0 DATA ANALYSIS AND CALCULATIONS , . . 81
11.0. QUALITY CONTROL 81
D-3/VOA OLM04.2
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Exhibit D Volatiles -- Section 1
Scope and Application
1.0 SCOPE AND APPLICATION
1.1 In 1978, EPA Headquarters and Regional representatives designed
analytical methods for the analysis of volatiles in hazardous waste
samples. These methods were based on EPA Method 624, Purgeables. In
1980, these methods were adopted for use in the Contract Laboratory
Program (CLP). As the requirements of CERCLA evolved, the CLP methods,
as well as their precedent EPA 600 Series methods, established the basis
for other EPA methods to perform the analysis of volatiles contained in
hazardous waste samples (i.e., Stf-846) . The following CLP method has
continuously improved to incorporate technological advancements
promulgated by EPA, and has continued to set the standard for the
preparation, extraction, isolation, identification, and reporting of
volatiles at hazardous waste sites.
1.2 The analytical method that follows is designed to analyze water,
sediment, and soil from hazardous waste sites for the volatile organic
compounds on the Target Compounds List (TCL, see Exhibit C). The method
includes sample preparation, screening to determine the approximate
concentration of organic constituents in the sample, and the actual
analysis which is based on a purge and trap gas chromatograph/mass
spectrometer (GC/MS) method.
1.3 This analytical method includes the use of the Modified SW-846 Method
5035 for the preparation and analysis of low level soil/sediment samples.
A detailed description of the sample preparation, analysis, and quality
control procedures to be followed when this method option is requested
can be found in Appendix B.
1.4 Problems have been associated with the following compounds analyzed by
this method.
Chloromethane, vinyl chloride, bromomethane, and chloroethane can
display peak broadening if the compounds are not delivered to the GC
column in a tight band.
Acetone, hexanone, 2-butanone, and 4-methyl-2-pentanone have poor
purge efficiencies.
1,1,1-trichloroethane and all the dichloroethanes can
dehydrohalogenate during storage or analysis.
Chloromethane can be lost if the purge flow is too fast.
Bromoform is one of the compounds most likely to be adversely affected
by cold spots and/or active sites in the transfer lines. Response of
its quantitation ion (m/z 173) is directly affected by the tuning of
the GC/MS to meet the instrument performance criteria for 4-
bromofluorobenzene (BFB) at ions m/z 174/176. Increasing the m/z
174/176 ratio may improve bromoform response.
D-4/VOA OLM04.2
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Exhibit D Volatile -- Sections 2 & 3
Summary of Method/Definitions
2.0 SUMMARY OF METHOD
2.1 Water
An inert gas is bubbled through a.5 mL sample contained in a specifically
designed purging chamber at ambient temperature. The purgeable compounds
are efficiently transferred from the aqueous phase to the vapor phase.
The vapor is swept through-a sorbent column where the purgeables are
trapped. After purging is completed, the sorbent column is heated and
backflushed with the inert gas to desorb the purgeable compounds onto a
gas chromatographic column. The gas chromatograph is temperature-
programmed to separate the purgeable compounds which are then detected
with a mass spectrometer.
2.2 Low Level Soil
An inert gas is bubbled through a mixture of reagent water and 5 g of
sample contained in a specifically designed purging chamber that is held
at an elevated temperature. The purgeable compounds are efficiently
transferred from the aqueous phase to the vapor phase. The vapor is
swept through a sorbent column where the purgeables are trapped. After
purging is completed, the sorbent column is heated and backflushed with
the inert gas to desorb the purgeable compounds onto a gas
chromatographic column. The gas chromatograph is temperature-programmed
to separate the purgeable compounds which are then detected with a mass
spectrometer.
2.3 Medium Level Soil
A measured amount of soil is collected/extracted with methanol. A
portion of the methanol is diluted to 5 mL with reagent water. An inert
gas is bubbled through this solution in a specifically designed purging
chamber at ambient temperature. The purgeable compounds are effectively
transferred from the aqueous phase to the vapor phase. The vapor is
swept through a sorbent column where the purgeables are trapped. After
purging is completed, the sorbent column is heated and backflushed with
the inert gas to desorb the purgeable compounds onto a gas
chromatographic column. The gas chromatograph is temperature-programmed
to separate the purgeable compounds which are then detected with a mass
spectrometer.
3 . 0 DEFINITIONS
See Exhibit G for a complete list of definitions.
D-5/VOA
OLM04.2
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Exhibit D Volatiles -- Sections 4 & b
Interferences/Safety
4.0 INTERFERENCES
4.1 Method interference may be caused by impurities in the purge gas, organic
compounds out-gassing from the plumbing ahead of the trap, and solvent
vapors in the laboratory. The analytical system must be demonstrated to
be free from contamination under the conditions of the analysis by
running laboratory method and instrument blanks as described in Section
12. The use of non-Polytetrafluoroethylene (PTFE) tubing, non-PTFE
thread sealants, or flow controllers with rubber components in the
purging device should be avoided.
4.2 Samples can be contaminated by diffusion of volatile organics
(particularly fluorocarbons and methylene chloride) through the septum
seal into the sample during storage and handling.
4.3 Contamination by carryover can occur whenever high level and low level
samples are sequentially analyzed. To reduce carryover, the purging
'device and sampling syringe must be rinsed with reagent water between
sample analyses. For samples containing large amounts of water-soluble
materials, suspended solids, high-boiling compounds, or high purgeable
levels, it may be necessary to wash out the purging device with a
detergent solution between analyses, rinse it with distilled water, and
.then dry it in an oven at 105 °C. The trap and other parts of the system
are also subjected to contamination; therefore, frequent bakeout and
purging of the entire system may be required.
4.4 The laboratory where volatile analysis is performed should be completely
free of solvents. '
5.0 SAFETY
5.1 The toxicity or carcinogenicity of each reagent used in this method has
not been precisely defined; however, each chemical compound should be
treated as a potential health hazard. From this viewpoint, exposure to
these chemicals must be reduced to the lowest possible level by whatever
means available. The laboratory is responsible for maintaining a current
awareness file of OSHA regulations regarding the safe handling of the
chemicals specified in this method. A reference file of material data
handling sheets should also be made available to all personnel involved
in the chemical analysis.
5.2 The following analytes covered by this method have been tentatively
classified as known or suspected, human or mammalian carcinogens:
benzene, carbon tetrachloride, chloroform, and vinyl chloride. Primary
standards of these toxic compounds should be prepared in a hood. A
NIOSH/Mass approved toxic gas respirator should be worn when the analyst
handles high concentrations of these toxic compounds.
D-6/VOA OLM04.2
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Exhibit D Volatiles -- Section 6
Equipment and Supplies
6.0 EQUIPMENT AND SUPPLIES
Brand names, suppliers, and part numbers are for illustrative purposes
only.. No endorsement is implied. Equivalent performance may be achieved
using equipment and supplies other than those specified here, but
demonstration of equivalent performance meeting the requirements of this
SOW is the responsibility of the Contractor. The Contractor shall
document any use of alternate equipment or supplies in the SDG Narrative.
6.1 Glassware
6.1.1 Syringes - 5 mL, gas-tight with shut-off valve. Micro syringes - 25
uL and larger, 0.006 inch ID needle.
6.1.2 Syringe Valve - two-way, with Luer ends (three each), if applicable to
the purging device.
6.1.3 Pasteur Pipets - disposable.
6.1.4 Vials and Caps - 2 mL for GC.
6.1.5 Volumetric Flasks.
6.1.6 Bottle - 15 mL, screw-cap, with Teflon cap liner. '
6.2 pH Paper - wide range
6.3 Balances - analytical, capable of accurately weighing ± 0.0001 g, and a
top-loading balance capable of weighing 100 g ± 0.01 g. The balances
must be calibrated with class S weights or known reference weights once
per each 12-hour work shift. The balances must be calibrated with class
S weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
6.4 Purge and Trap Device - consists of three separate pieces of equipment:
the sample purge chamber, trap, and the desorber. Several complete
devices are now commercially available.
6.4.1 The sample purge chamber must be designed to accept 5 mL samples with
a water column at least 3 cm deep. The gaseous head space between the
water column and the trap must have a total volume of less than 15 mL.
The purge gas must pass through the water column as finely divided
bubbles, each with a diameter of less than 3 mm at the origin. The
purge gas must be introduced no more than 5 mm from the base of the
water column.
6.4.2 The trap must be at least 25 cm long and have an inside diameter of at
least 0.105 inch. The trap must be packed to contain the following
minimum lengths of absorbents: (starting from inlet) 0.5 cm silanized
glass wool, 1 cm methyl silicone, 8 cm of 2,6-diphenylene oxide
polymer (Tenax-GC, 60/80 mesh), 8 cm of silica gel (Davison Chemical,
35/60 mesh, grade 15 or equivalent), 7 cm of coconut charcoal (prepare
from Barnebey Cheney, CA-580-26, or equivalent, by crushing through 26
mesh screen), and 0.5 cm silanized glass wool. A description of the
trap used for analysis shall be provided in the SDG Narrative.
D-7/VOA OLM04.2
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Exhibit D Volatiles -- Section 6
Equipment and Supplies
6.4.3 The desorber should be capable of rapidly heating the trap to 180 °C.
The polymer section of the trap should not be heated higher than
180 °C and the remaining sections should not exceed 220 °C during
bakeout mode.
6.4.4 Trap Packing
6.4.4.1 2,6-Diphenylene oxide polymer, 60/80 mesh chromatographic grade
(Tenax GC or equivalent).
6.4.4.2 Methyl silicone packing, 3.0 percent OV-1 on Chromasorb W, 60/80
mesh (or equivalent).
6.4.4.3 Silica gel, 35/60 mesh, Davison, grade 15 (or equivalent)-.
6.4.4.4 Coconut charcoal (prepare from Barnebey Cheney, CA-580-26, or
equivalent, by crushing through 26 mesh screen).
6.4.4.5 Alternate sorbent traps may be used if:
The trap packing materials do not introduce contaminants which
interfere with identification and quantitation of the'compounds
listed in Exhibit C (Volatiles).
The analytical results generated using the trap meet the initial
and continuing calibration technical acceptance criteria listed
in the SOW,and the CRQLs listed in Exhibit C (Volatiles).
The trap can accept up to 1000 ng of each compound listed in
Exhibit C (Volatiles) without becoming, overloaded.
6.4.4.5.1 The alternate trap must be designed to optimize performance.
Follow manufacturer's instructions for the use of its
product. Before use of any trap, other than the one
specified in Section 6.4.2, the Contractor must first meet
the criteria listed in Section 6.4.4.5. Once this has been
demonstrated, the Contractor must document its use in each
SDG Narrative by specifying .the trap composition (packing
material/brand name, amount of packing material). Other
sorbent traps include, but are not limited to, Tenax/Silica
Gel/Carbon Trap from EPA Method 524.2, Tenax - GC/Graphpac-D
Trap (Alltech) or~equivalent, and Vocarb 4000 Trap (Supelco)
or equivalent.
6.4.4.5.2 The Contractor must maintain documentation that the
alternate trap meets the criteria listed in Section 6.4.4.5.
The minimum documentation requirements are as follows:
6.4.4.5.2.1 Manufacturer provided information concerning the
performance characteristics of the trap.
6.4.4.5.2.2 Reconstructed ion chromatograms and data system reports
generated on the Contractor's GC/MS used for CLP
analyses:
D-8/VOA OLM04.2
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Exhibit D Volatiles -- Section 6
Equipment and Supplies
From instrument blank analyses which demonstrate that
there are no contaminants which interfere with the
volatile analysis when using the alternate trap;
From initial and continuing calibration standards
analyzed using the trap specified in Section 6.4.4.
| 6.4.4.5.2.3 Based on Contractor generated data described above, the
Contractor must complete a written comparison/review,
which has been signed by the Laboratory Manager,
certifying that:
The alternate trap performance meets the technical
acceptance criteria listed in Sections 9.3.5 and
9.4.5;
The low point initial calibration standard analysis
has adequate sensitivity to meet the volatile CRQLs;
The high point initial calibration standard analysis
was not overloaded;
The alternate trap materials do not introduce
contaminants which interfere with the identification
and/or quantitation of the compounds listed in Exhibit
C (Volatiles).
| 6.4.4.5.2.4 The documentation must be made available to the Agency
during on-site laboratory evaluations or sent to the
Agency upon request of the Technical Project Officer or
the Administrative Project Officer.
6.4.5 The purge and trap apparatus may be assembled as a separate unit or be
an integral unit coupled with a gas chromatograph.
6.5 A heater or heated bath capable of maintaining the purge chamber at 40 °C
(± 1 °C) is to be used for low level soil/sediment analysis, but not for
water or medium level soil/sediment analyses.
6.6 Gas Chromatography/Mass Spectrometer (GC/MS) System
6.6.1 Gas Chromatograph - the gas chromatograph (GC) system must be capable
of temperature programming and have a flow controller that maintains a
constant column flow rate throughout desorption and temperature
program operations. The system must include or be interfaced to a
purge and trap system as specified in Section 6.4 and have all
required accessories including syringes, analytical columns, and
gases. All GC carrier gas lines must be constructed from stainless
steel or copper tubing. Non-PTFE thread sealants, or flow controllers
with rubber components are not to be used.
6.6.2 Gas Chromatography Columns - a description of the column used for
analysis shall be provided in the SDG Narrative.
6.6.2.1 Packed columns - 6 ft. long x 0.1 inch ID glass, packed with 1.0
..D-9/VOA OLM04.2
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Exhibit D Voiatiles -- Section 6
Equipment and Supplies
percent SP-1000 on Carbopack B (60/80) mesh or equivalent.
6.6.2.2 Capillary Columns
6.6.2.2.1 Minimum length 30 m x 0.53 mm ID VOCOL (Supelco) or equivalent
. fused silica widebore capillary column with 3 um film thickness.
6.6.2.2.2 Minimum length 30 m x 0.53 mm ID DB-624 (J & W Scientific) or
equivalent fused silica widebore capillary column with 3 pm film
thickness.'
6.6.2.2.3 Minimum length 30 m x 0.53 mm ID AT-624 (Alltech) or equivalent
fused silica widebore capillary column with 3 um film thickness.
6.6.2.2.4 Minimum length 30 m x 0.53 mm ID HP-624 (Hewlett-Packard) or
equivalent fused silica widebore capillary column with 3 um film
thickness.
6.6.2.2.5 Minimum length 30 m x 0.53 mm ID RTx-624 (Restek) or equivalent
fused silica widebore capillary column with 3 um film thickness.
6.6.2.2.6 Minimum length 30 m x 0.53 mm ID BPX-624 (SGE) or equivalent
fused silica widebore capillary column with 3 um film thickness.
->
6.6.2.2.7 Minimum length 30 m x 0.53 mm ID CP-Sil 13CB (Chrompack) or
equivalent fused silica widebore capillary column with 3 pm film
thickness.
6.6.2.3 A capillary column is considered equivalent if:
The column does not introduce contaminants which interfere with
the identification and quantitation of the compounds listed in
Exhibit C (Voiatiles).
The analytical results generated using the column meet the
initial and continuing calibration technical acceptance criteria
listed in the SOW, and the CRQLs listed in Exhibit C
(Voiatiles).
The column can accept up to 1000 ng of each compound listed in
Exhibit C (Voiatiles) without becoming overloaded.
The column provides equal or better resolution of the compounds
listed in Exhibit C (Voiatiles) than the columns listed in
Section 6.6.2.2.
6.6.2.4 As applicable, follow the manufacturer's instructions for use of its
product.
6.6.2.5 The Contractor must maintain documentation that the column met the
criteria in Section 6.6.2.3. The minimum documentation is as
follows:
6.6.2.5.1 Manufacturer provided information concerning the performance
characteristics of the column.
D-10/VOA OLM04.2
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Exhibit D Volatiles -- Section 6
Equipment and Supplies
6.6.2.5.2 Reconstructed ion chromatograms and data system reports
generated on the GC/MS used for the CLP analyses:
From instrument blanks which demonstrate that there are no
contaminants which interfere with the volatile analysis when
using the alternate column,-
From initial and continuing calibration standards analyzed
using the alternate column.
6.6.2.5.3 Based on the Contractor-generated data described above, the
' Contractor shall complete a written review, signed by the
Laboratory Manager, certifying that:
The column performance meets the technical acceptance
criteria in Sections 9.3:5 and 9.4.5;
The low point initial calibration standard analysis has
adequate sensitivity to meet the volatile CRQLs;
The high point initial calibration standard analysis was not
overloaded;
The column does not introduce contaminants which interfere
with the identification and/or quantitation of compounds
listed in Exhibit C (Volatiles).
6.6.2.5.4 The documentation must be made available to the Agency during
on-site laboratory evaluations or sent to the Agency upon
request of the Technical Project Officer or Administrative
Project Officer.
6.6.3 Mass Spectrometer - must be capable of scanning from 35 to 300 amu
every 1 second or less to every 2 seconds or less utilizing 70 volts
(nominal) electron energy in the electron impact ionization mode, and
producing a mass spectrum which meets all the instrument performance
acceptance criteria when 50 ng of BFB is injected through the gas
chromatograph inlet. The instrument conditions required for the
acquisition of the BFB mass spectrum are given in Section 9.
6.6.3.1 NOTE: The MS scan rate should allow acquisition of at least five
spectra while a sample compound elutes from the GC. The purge and
trap GC/MS system must be in a room whose atmosphere is demonstrated
to be free of all potential contaminants which will interfere with
the analysis. The instrument must be vented to the outside of the
facility or to a trapping system which prevents the release of
contaminants into the instrument room.
6.6.4 GC/MS interface - any gas chromatograph to mass spectrometer interface
that gives acceptable calibration points at 50 ng or less per
injection for each of the parameters of interest, and achieves all
acceptance criteria, may be used. Gas chromatograph to mass
spectrometer interfaces constructed of all-glass or glass-lined
materials are recommended. Glass can be deactivated by silanizing
with dichlorodimethylsilane.
D-ll/VOA OLM04.2
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Exhibit D Volatilss -- Section 6
Equipment and Supplies
6.6.5 Data system - a computer system interfaced to the mass spectrometer
that allows the continuous acquisition and storage, on machine-
readable media, of all mass spectra obtained throughout the duration
of the chromatographic program. The computer must have software that
allows searching any GC/MS data file for ions of a specified mass and
plotting such ion abundances versus time or scan number. This type of
plot is defined as an Extracted Ion Current Profile (EICP). Software
must also be available that allows integrating the abundance in any
EICP between specified time or scan number limits. Also, for the non-
target compounds, software must be available that allows for the
comparison of sample spectra against reference library spectra. The
NIST/EPA/NIH (May 1992 release or later) and/or Wiley (1991 release or
later), or equivalent mass spectral library shall be used as the
reference library. The data system must be capable of flagging all
data files that have been edited manually by laboratory personnel.
6.6.6 Magnetic tape storage device - capable of recording data and must be
suitable for long-term, off-line storage.
D-12/VOA OLM04.2
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Exhibit D Volatiles -- Section 7
Reagents and Standards
7.0 REAGENTS AND STANDARDS
7.1 Reagents
7.1.1 Reagent water - defined as water in which an interferant is not
observed at or above the CRQL of the analytes of interest. Reagent
water may be generated by passing tap water through a carbon filter
bed containing about 453 g (1 Ib) of activated carbon (Calgon Corp.,
Filtrasorb-300 or equivalent).
7.1.1.1 A water purification system (Millipore Super-Q or equivalent) may be
used to generate reagent water.
7.1.1.2 Reagent water may also be prepared by boiling water for 15 minutes.
Subsequently, while maintaining the temperature at 90 °C, bubble a
contaminant-free inert gas through the water for one hour. While
still hot, transfer the water to a narrow-mouth screw-cap bottle and
seal with a Teflon-lined septum and cap.
7.1.2 Methanol - pesticide quality or equivalent
7.2 Standards
7.2.1 Introduction
The Contractor must provide all standards to be used with this
contract. These standards may be used only after they have been
certified according to the procedure in Exhibit E. The Contractor
must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must b.e retained by the
Contractor and presented upon request.
7.2.2 Stock Standard Solutions
7.2.2.1 Stock standard solutions may be purchased or may be prepared in
tnethanol from pure standard materials.
7.2.2.2 Prepare stock standard solutions by placing about 9.8 mL of methanol
into a 10 mL ground-glass stoppered volumetric flask. Allow the
flask to stand, unstoppered, for about 10 minutes, or until all .
alcohol-wetted surfaces have dried. Weigh the flask to the nearest
0.1 mg.
7.2.2.3 Add the assayed reference material as described below. .
7.2.2.3.1 If the compound is a liquid, using a 100 uL syringe, immediately
add two or more drops of assayed reference material to the
flask, then reweigh. The liquid must fall directly into the
alcohol without contacting the neck of the flask.
7.2.2.3.2 If the compound is a gas at room temperature, fill a 5 mL valved
gas-tight syringe with the reference standard to the 5 mL mark.
Lower the needle to 5 mm above the methanol meniscus. Slowly
introduce the reference standard above the surface of the
liquid. The gas will rapidly dissolve in the methanol.
D-13/VOA
OLM04.2
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Exhibit D Volatiles -- Section 7
Reagents and Standards
7.2.2.3.3 The procedure in Section 7.2.2.3.2 may also be accomplished by
. . using a lecture bottle equipped with a Hamilton Lecture Bottle
Septum (#86600). Attach Teflon tubing to the side-arm relief
valve and direct a gentle"stream"of the reference standard"into
the methanol meniscus.
7.2.2.3.4 Reweigh, dilute to volume, stopper, then mix by inverting the
flask several times. For non-gaseous compounds, calculate the
concentration in micrograms per microliter from the net gain in
weight. When compound purity is assayed to be 97.0 percent or
greater, the weight may be used without correction to calculate
the concentration of the stock standard. If the compound purity
is assayed to be less than 97.0 percent, the weight must be
corrected when calculating the concentration of the stock
solution. See Exhibit E (Analytical Standards Requirements).
For gaseous -compounds, calculate the concentration in micrograms
per microliter, using the Ideal Gas Law; taking into account the
temperature and pressure conditions within the laboratory.
7.2.2.3.5 Prepare fresh stock standards every two months for gases or for
reactive compounds such as styrene. All other stock standards
for non-gases/non-reactive purgeable compounds must be replaced
after six months, or sooner if the standard has degraded or
evaporated.
7.2.3- Secondary Dilution Standards
7.2.3.1 Using stock standard solutions, prepare secondary dilution standards
" in methanol that contain the compounds of interest, either singly or
- mixed together. Secondary dilution standard solutions should be
prepared at concentrations that can be easily diluted to prepare
working standard solutions.
7.2.3.2 Prepare fresh secondary dilution standards for gases and for
reactive compounds such as styrene every month, or sooner, if
standard has degraded or evaporated. Secondary dilution standards
for the other purgeable compounds must be replaced after six months,
or sooner, if standard has degraded or evaporated.
7.2.4 Working Standards
7.2.4.1 System Monitoring Compound (SMC) Spiking Solution
Prepare a system monitoring compound spiking solution containing
toluene-d8, 4-bromofluorobenzene (BFB), and 1,2-dichloroethane-d4 in
methanol at a concentration of 25 ug/mL. Add 10 uL of this spiking
solution into 5 mL of sample, sample extract or calibration standard
for -a concentration of 50 ug/L. Prepare fresh spiking solution
weekly, or sooner, if the solution has degraded or evaporated.
7.2.4.2 Matrix Spiking Solution
Prepare a spiking solution in methanolthat contains the following
compounds at a concentration of 25 ug/mL: 1,1-dichloroethene,
trichloroethene, chlorobenzene, toluene, and benzene. Prepare fresh
D-14/VOA OLM04.2
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Exhibit D Volatiles -- Section 7
Reagents and Standards
spiking solution weekly, or sooner, if the solution has degraded or
evaporated.
7.2.4.3 Internal Standard Spiking Solution
Prepare an internal standard spiking solution containing
bromochloromethane, chlorobenzene-d5, and 1,4-difluorobenzene in
methanol at a concentration of 25 ug/mL for each internal standard.
Add 10 uL of this spiking solution into 5 mL of sample or
calibration standard for a concentration of 50 ug/L. Prepare fresh
spiking solution weekly, or sooner, if the solution has degraded or
evaporated.
7.2.4.4 Instrument Performance Check Solution - 4-Bromofluorobenzene (BFB)
Prepare a 25 ng/uL solution of BFB in methanol. Prepare fresh BFB
solution every six months, or sooner, if the solution has degraded
or evaporated. NOTE: The 25 ng/uL concentration is used with a 2
uL injection volume. The laboratory may prepare a 50 ng/uL solution
of BFB if a 1 uL injection volume" is used.
7.2.4.5 Calibration Standard.Solution
Prepare a calibration standard solution containing all of the
purgeable target compounds in methanol. The recommended
concentration of the target compounds is 100 ug/mL. Prepare fresh
calibration standard solutions weekly, or sooner, if solutions have
degraded or evaporated.
7.2.4.6 Initial and Continuing Calibration Standards
7.2.4.6.1 Prepare five aqueous initial calibration standard solutions
containing all of the purgeable target compounds and system
monitoring compounds at 10, 20, 50, 100, and 200 ug/L levels.
It is required that all three xylene isomers (o-, m-, and p-
xylene) be present in the calibration standards at
concentrations of each isomer equal to that of the other target
compounds.(i.e., 10, 20, 50, 100, and 200 ug/L). Similarly, the
cis and trans isomers of 1,2-dichloroethene must both be present
in the standards at concentrations of each isomer equal to that
of the other target compounds.
7.2.4.6.2 Aqueous calibration standards may be prepared in a volumetric
flask or in the syringe used to inject the standard into the
purging device.
7.2.4.6.2.1 Volumetric flask - add an appropriate volume of the 100
ug/mL calibration standard solution (Section 7-2.4.5) to an
aliquot of reagent water in a volumetric flask. Use a
microsyringe and rapidly inject the alcohol standard into
the expanded area of the filled volumetric flask. Remove
the needle as quickly as possible after injection. Bring.to
volume. Mix by inverting the flask three times only.
Discard the contents contained in the head of the flask.
D-15/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 7
Reagents and Standards
7.2.4.6.2.2 Syringe - remove the plunger from a 5 mL "Luerlock" syringe.
Pour reagent water into the syringe barrel to just short of
overflowing. Replace the syringe plunger and compress the
water. Invert the syringe, open the syringe valve and vent
any residual air. Adjust the water volume to 5 mL minus the
amount of calibration standard to be added. Withdraw the
plunger slightly and add an appropriate volume of working
calibration standard through the valve bore of the syringe.
Close the valve and invert three times.
7.2.4.6.2.3 The 50 ug/L aqueous calibration standard solution is the
continuing calibration standard.
7.2.4.6.3 The methanol contained in each of the aqueous calibration
standards must not exceed 1.0 percent by volume.
7.2.5 Ampulated Standard Extracts
Standard solutions purchased from a chemical supply house as ampulated
extracts in glass vials may be retained and used until the expiration
date provided by the manufacturer. If no manufacturer's expiration
.date is provided, the standard solutions as ampulated extracts may be
retained and used for 2 years from the preparation date. Standard
-r- solutions, prepared by the Contractor which are immediately ampulated
- in glass vials, may be retained for 2 years from the preparation date.
/; Upon breaking the glass seal, the expiration times listed in Sections
7.2.2 through 7.3 will apply. The Contractor is responsible for
' assuring that the integrity of the standards has not degraded (see
Section 7.3.5).
7.3 Storage of Standard Solutions
7.3.1 Store the stock standards in Teflon-sealed screw-cap bottles with zero
headspace at -10 °C to -20 °C, and protect the standards from light.
Once one of the bottles containing the stock standard solution has
been opened, it may be used for no longer than one week.
7.3.2 Store secondary dilution standards in Teflon-sealed screw-cap bottles
with minimal headspace at -10 °C to -20 °C, and protect the standards
from light. The secondary dilution standards must be checked
frequently for signs of degradation or evaporation, especially just
prior to preparing working standards from them.
7.3.3 Aqueous standards may be stored for up to 24 hours if held in
Teflon-sealed screw-cap vials with zero headspace at 4 °C (±2 °C) .
Protect the standards from light. If not so stored, they must be
discarded after one hour unless they are set up to be purged by an
autosampler. When using an autosampler the standards may be kept for
up to 12 hours in purge tubes connected via the autosampler to the
purge and trap device. All other working standards may be stored at
-10 °C to -20 °C.
7.3.4 Purgeable standards must be stored separately from other standards.
D-16/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 7
Reagents and Standards
7.3.5 The Contractor is responsible for maintaining the integrity of
standard solutions and verifying prior to use. This means that
standards must be brought to room temperature prior to use, checked
for losses, and checked that all components have remained in the
solution.
D-17/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 8
Sample Collection, Preservation, and Storage
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 Sample Collection and Preservation
8.1.1 Water samples may be collected in glass containers having a total
volume of at least 40 mL with a Teflon-lined septum and an open top
screw-cap. Soil samples may be collected in glass containers or
closed end tubes (e.g., brass sleeves) in sufficient quantity to
perform the analysis. Headspace should be avoided. Soil samples for
medium level analysis may also be collected in pre-weighed vials
containing 10 ml of methanol. The specific requirements for site
sample collection are outlined by the Region.
8.1.2 For collection of water samples, the containers must be. filled in such
a manner that no air bubbles pass through the sample as the container
is being filled. Seal the vial so that no air bubbles are entrapped
in it.
8.1.3 Water samples are preserved to a pH of 2 at the time of collection.
8.1.4 For collection of medium level soil samples with methanol, the sample
vial, with 10 ml of methanol and all labeling, is weighed to the
nearest 0.1 g prior to the addition of sample. Approximately 5 g of
sample is added to the vial. The sample vial with sample is weighed
to the nearest 0.1 g. The initial weight, final weight and sample
weight will be recorded and provided to the laboratory.
8.1.5 All samples must be iced or refrigerated at 4 °C (±2 °C) from the time
of collection until analysis.
8.2 Procedure for Sample Storage
8.2.1 The samples must be protected from light and refrigerated at 4 °C
(±2 °C) from the time of receipt until 60 days after delivery of a
reconciled, complete sample data package to the Agency. After 60
days, the samples may be disposed of in a manner that complies with
all applicable regulations.
8.2.2 The samples must be stored in an atmosphere demonstrated to be free of
all potential contaminants and in a refrigerator used only for storage
of volatile samples.
8.2.3 All volatile samples in an SDG'must be stored together in the same
refrigerator.
8.2.4 Storage blanks shall be stored with samples until all samples are
analyzed.
8.2.5 Samples, sample extracts, and standards must be stored separately.
8.2.6 Volatile standards must be stored separately from semivolatile and
pesticide/Aroclor standards.
D-18/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 8
Sample Collection, Preservation, and Storage
8.3 Contract Required Holding Times
Analysis of water and soil/sediment samples must be completed within 10
days of Validated Time of Sample Receipt (VTSR). As part of the Agency's
QA program, the Agency may provide Performance Evaluation (PE) samples as
standard extracts which the Contractor is required to prepare per the
instructions provided by the Agency. PE samples must be prepared and
analyzed concurrently with the samples in the SDG. The contract required
10 day holding time does not apply to PE samples received as standard
extracts.
D-19/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and Standardization
Instrument Operating Conditions
9.0 CALIBRATION AND STANDARDIZATION
9.1 Instrument Operating Conditions
9.1.1 Purge and Trap
9.1.1.1 The following are the recommended purge and trap analytical
conditions. The conditions are recommended unless otherwise noted.
Purge conditions
Purge Gas: Helium or Nitrogen
Purge Time: 11.0 ± 0.1 minute
Purge Flow Rate: 25-40 mL/minute
Purge Temperature: Ambient temperature for water or
medium level soil/sediment samples
(required); 40 °C low level
soil/sediment samples (required)
Desorb Conditions
Desorb Temperature: 180 °C
Desorb Flow Rate: 15 mL/minute
Desorb Time: 4 . 0 ± 0 .1 minute
Trap Reconditioning Conditions
Reconditioning Temperature: 180 °C
Reconditioning Time: 7.0 ± 0.1 minute (minimum). A
longer time may be required to bake
contamination or water from the
system.
9.1.1.2 Before initial use, condition the trap overnight at 180 °C by
backflushing with at least 20 mL/minute flow of inert gas. Do not
vent the trap effluent onto the analytical column. Prior to daily
use, condition the trap by heating at 180 °C for 10 minutes while
backflushing. The trap may be vented to the analytical column
during daily conditioning; however, the column must be run through
the temperature program prior to the analysis of samples.
9.1.1.3 Optimize purge and trap conditions for sensitivity and to minimize
cross-contamination between samples. Once optimized, the same purge
and trap conditions must be used for the analysis of all standards,
samples, and blanks.
9.1.1.4 A moisture reduction/water management system may be used to improve
the chromatographic performance by controlling moisture or water if:
The system does not introduce contaminants which interfere with
identification and quantitation of compounds listed in Exhibit C
(Volatiles),
The analytical results generated when using the moisture
D-20/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and Standardization
Instrument Operating Conditions
reduction/water management system meet the initial and
continuing calibration technical acceptance criteria listed in
the SOW and the CRQLs listed in Exhibit C (Volatiles),
All calibration standards and samples, including blanks and
MS/MSDs, are analyzed under the same conditions,
The Contractor performs acceptably on the Performance Evaluation
samples using this system.
9.1.2 Gas Chromatograph
9.1.2.1 The following are the recommended GC analytical conditions. These
conditions are recommended unless otherwise noted.
Packed columns
Carrier Gas: Helium
Flow Rate: 30 mL/minute
Initial Temperature: 45 °C
Initial Hold Time: 3 minutes
Ramp Rate: 8 °C/minute
Final Temperature: 220 °C
Final Hold Time: Until three minutes after all
compounds listed in Exhibit C
(Volatiles) elute (required)
Transfer Line Temperature: 250-300 °C
Capillary Columns
Carrier Gas: ' Helium
Flow Rate: 15 mL/minute
Initial Temperature: 10 °C
Initial Hold Time: 1,0 - 5.0 (± 0.1) minutes
Ramp Rate: 6 °C/minute
Final Temperature: 160 °C
Final Hold Time: Until three minutes after all
compounds listed in Exhibit C
(Volatiles) elute (required)
9.1.2.2 Optimize GC conditions for analyte separation and sensitivity. Once
optimized, the same GC conditions must be used for the analysis of
.all standards, samples, blanks, matrix spikes, and matrix spike
duplicates.
9.1.2.3 For capillary columns, if the gaseous compounds chloromethane,
bromomethane, vinyl chloride, and chloroethane fail to exhibit
narrow, symmetrical peak shape, are not separated from the solvent
front, or are not resolved greater than 90.0 percent from each
other, then a subambient oven controller must be used, and the
initial temperature must be less .than or equal to 10 °C.
D-21/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and Standardization
GC/MS Calibration and Ion Abundance
9.1.3 Mass Spectrometer
The following are the required mass spectrometer analytical
conditions:
Electron Energy: 70 volts (nominal)
Mass Range: 35-300 amu
Scan Time: To give at least 5 scans per peak, not to exceed
2 seconds per scan for capillary column.
To give at least 5 scans per peak, not to exceed
3 seconds per scan for packed column.
9.2 GC/MS Calibration (Tuning) and Ion Abundance
9.2.1 Summary of GC/MS Performance Check
9.2.1.1 The GC/MS system must be tuned to meet the manufacturer's
specifications, using a suitable calibrant such as perfluoro-tri-n-
butylamine (FC-43) or perfluorokerosene (PFK). The mass calibration
and resolution of the GC/MS system are verified by the analysis of
the instrument performance check solution (Section 7.2.4.4).
9.2.1.2 Prior to the analysis of any samples, including MS/MSDs, blanks, or
calibration standards, the Contractor must establish that the GC/MS
system meets the' mass spectral ion abundance criteria for the
instrument performance check solution containing BFB.
9.2.2 Frequency of GC/MS Performance Check
The instrument performance check solution must be injected once at the
beginning of each 12-hour period, during which samples or standards
are to be analyzed. The twelve (12) hour time period for GC/MS
instrument performance check (BFB), standards calibration (initial or
continuing calibration criteria), blank and sample analysis begins at
the moment of injection of the BFB analysis that the laboratory
submits as documentation of a compliant instrument performance check.
The time period ends after twelve (12) hours have elapsed according to
the system clock.
9.2.3 Procedure for GC/MS Performance Check
9.2.3.1 The analysis of the instrument performance check solution may be
performed as follows:
As an injection of up to 50 ng of BFB into the GC/MS.
By adding 50 ng of BFB to 5 mL of reagent water and analyzing
the resulting solution as if it were an environmental sample
(See Section 10).
9.2.3.2 The instrument performance check solution must be analyzed alone
without calibration standards. NOTE: The calibration standards
contain BFB as a system monitoring compound (SMC).
D-22/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 9 .
Calibration and Standardization
Initial Calibration
9.2.4 Technical Acceptance Criteria for GC/MS Performance Check
9.2.4.1 The mass spectrum of BFB must be acquired in the following manner.
Three scans (the peak apex scan and the scans immediately preceding
and following the apex) are acquired and averaged. Background
subtraction is required, and must be accomplished using a single
scan no more than 20 scans prior to the elution of BFB. Do not
background subtract part of the BFB peak.
9.2.4.2 NOTE: All subsequent standards, samples, MS/MSD, and blanks
associated with a BFB analysis must use identical mass spectrometer
instrument conditions.
9.2.4.3 The analysis of the instrument performance check solution must meet
the ion abundance criteria given in Table 1.
9.2.5 Corrective Action for GC/MS Performance Check
9.2.5.1 If the technical acceptance criteria are not met, retune the GC/MS
system. It may also be necessary to clean the ion source, clean the
quadrupole rods, or take other corrective actions td achieve the
technical acceptance criteria.
9.2.5.2 BFB technical acceptance criteria must be met before any standards,
samples, including MS/MSDs or required blanks are analyzed. Any
samples or required blanks analyzed when tuning technical acceptance
criteria have not been met will require reanalysis at no additional
cost to the Agency.
9.3 Initial Calibration
9.3.1 Summary of Initial Calibration
Prior to the analysis of samples and required blanks, and after the
instrument performance check solution criteria have been met, each
GC/MS system must be calibrated at five concentrations to determine
instrument sensitivity and the linearity of GC/MS response for the
purgeable target compounds.
9.3.2 Frequency of Initial Calibration
9.3.2.1 Each GC/MS system must be calibrated upon award of the contract,
whenever the Contractor takes corrective action which may change or
affect the initial calibration criteria (e.g., ion source cleaning
or repair, column replacement, etc.), or if the continuing
calibration acceptance criteria have not been met.
9.3.2.2 If time remains in the 12-hour time period after meeting the
technical acceptance criteria for the initial calibration, samples
may be analyzed. It is not necessary to analyze a continuing
calibration standard if the initial calibration standard that is the
same concentration as the continuing calibration standard meets the
continuing calibration technical acceptance criteria. A method
blank is required. Quantify all sample and quality control sample
D-23/VGA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and -Standardization
Initial Calibration
results, such as internal standard area response change and
retention time shift, against the initial calibration standard that
is the same concentration as the continuing calibration standard.
9.3.3 Procedure for Initial Calibration
9.3.3.1 Assemble a purge and trap device that meets the specifications in
Section 6.4. Condition the device as described in Section 9.1.1.
9.3.3.2 Connect the purge and trap device to the gas chromatograph. The
gas chromatograph must be operated using temperature and flow rate
parameters equivalent to those in Section 9.1.2.
9.3.3.3 Add 10 uL of the internal standard solution (Section 7.2.4.3) to
each of the five aqueous calibration standard solutions containing
the system monitoring compounds (Section 7.2.4.6) for a
concentration of 50 pg/L at time of purge. Analyze each calibration
standard according to Section 10.
9.3.3.4 Separate initial and continuing calibrations must be performed for
water samples and low level soil/sediment samples (unheated purge
vs. heated purge). Extracts of medium level soil/sediment samples
may be analyzed using the calibrations of water samples.
The laboratory may run different matrices in the same 12-hour time
period under the same tune, as long as separate calibrations are
performed for each matrix within that 12-hour period.
9.3.4 Calculations for Initial Calibration
9.3.4.1 Calculate the relative response factor (RRF) for each volatile
target and system monitoring compound using Equation 1. The primary
characteristic ions used for quantitation are listed in Table 2 and
Table 4. Assign the target compounds and system monitoring compound
to an internal standard according to Table 3. If an interference
prevents the use of a primary ion for a given internal standard, use
a secondary ion listed in Table 4. NOTE: Unless otherwise stated,
the area response of the primary characteristic ion is the
quantitation ion.
EQ.
RRF = X
Ais CX
Where,
AX = Area of the characteristic ion (EICP) for the compound to be
measured (see Table 2)
AiS = Area of the characteristic ion (EICP) for the specific
internal standard (see Tables 3 and 4)
Cis = Concentration of the internal standard
Cx = Concentration of the compound to be measured
D-24/VGA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and Standardization
Initial Calibration
9.3.4.2 Calculating the relative response factor of the xylenes and the bis
and trans isomers of 1,2-dichloroethene requires special attention.
On packed columns, o- and p-xylene isomers co-elute. On capillary
columns, the m- and p-xylene isomers co-elute. Therefore, when
calculating the relative response factor in the equation above, use
the area response (Ax) and concentration (Cx) of the peak that
represents the single isomer on the GC column used for analysis.
9.3.4.3 The mean relative response factor (~RR~F~) must be calculated for all
compounds.
9.3.4.4 Calculate the % Relative Standard Deviation (%RSD) of the RRF values
over the working range of the curve.
EQ. 2
Standard Deviation
%RSD =
Mean
Where,
Standard Deviation =
£ (x, -x):
i 1
(n-1)
X± = each individual value used to calculate the mean
X = the mean of n values
n = the total number of values
9.3.5 Technical Acceptance Criteria' for Initial Calibration
9.3.5.1 All initial calibration standards must be analyzed at the
concentration levels described in Section 7.2.4.6.1, and at the
frequency described in Section 9.3.2 on a GC/MS system meeting the
BFB technical acceptance criteria.
9.3.5.2 The relative response factor (RRF) at each calibration concentration
for each purgeable target and system monitoring compound must be
greater than or equal to the compound's minimum acceptable response
factor listed in Table 5.
9.3.5.3 The %RSD for each target or system monitoring compound listed in
Table 5 must be less than or equal to that value listed.
9.3.5.4 Up to two compounds may fail the criteria listed in Sections 9.3.5.2
and 9.3.5.3 and still meet the minimum response factor and %RSD
requirements. However, these compounds must have a minimum RRF
greater than or equal to 0.010, and the %RSD must be less than or
D-25/VOA OLM04.2
-------
Exhibit L) Voiatiies -- section 9
Calibration and Standardization
Continuing Calibration
equal to 40.0 percent.
9.3.5.5 Excluding those ions in the solvent front, and the combined xylenes
in the 200 ug/L standard, no quantitation ion may saturate the
detector. Follow the manufacturer's instrument operating manual to
determine how saturation is indicated for your instrument.
9.3.6 Corrective Action for Initial Calibration
9.3.6.1 If the initial calibration technical acceptance criteria are not
met, inspect the system for problems. It may be necessary to clean
the ion source, change the column, service the purge and trap
device, or take other corrective actions to achieve the technical
acceptance criteria.
9.3.6.2 Initial calibration technical acceptance criteria must be met before
any samples or required blanks are analyzed. Any samples including
MS/MSD or required blanks analyzed when initial calibration
technical acceptance criteria have not been met will require
reanalysis at no additional cost to the Agency.
9.4 Continuing Calibration
9.4.1 Summary of Continuing Calibration
Prior to the analysis of samples and required' blanks and after BFB and
initial calibration acceptance criteria have been met, each GC/MS
system must be routinely checked by analyzing a continuing calibration
standard containing all the purgeable target and system monitoring
compounds to ensure that the instrument continues to meet the
instrument sensitivity and linearity requirements of the SOW.
9.4.2 Frequency of Continuing Calibration
9.4.2.1 A check of the calibration curve must be performed once every 12
hours (see Section 9.2.2 for the definition of the 12-hour time
period). If time remains in the 12-hour time period after meeting
the technical acceptance criteria for the initial calibration,
samples may be analyzed. It is not necessary to analyze a
continuing calibration standard if the initial calibration 'standard
that is the same concentration as the continuing calibration
standard meets the continuing calibration technical acceptance
criteria. A method blank is required. Quantify all sample results
against the initial calibration standard that is the same
concentration as the continuing calibration standard (50 ug/L).
9.4.2.2 If time does not remain in the 12-hour period beginning with the
injection of the instrument performance check solution, a new
injection of the instrument performance check solution must be made.
If the new injection meets the ion abundance criteria for BFB, then
a continuing calibration standard may be injected.
9.4.3 Procedure for Continuing Calibration
D-26/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 9
Calibration and Standardization
Continuing Calibration
9.4.3.1 Set up the purge and trap GC/MS system per the requirements in
Section 9.1.1.
9.4.3.2 Add 10 uL of internal standard solution (Section 7.2.4.3) to the 5
mL syringe or volumetric flask containing the continuing calibration
standard (Section 7.2.4.6). Analyze the continuing calibration
standard according to Section 10.
9.4.4 Calculations for Continuing Calibration
9.4.4.1 Calculate a relative response factor (RRF) for each target and
system monitoring compound using Equation 1.
9.4.4.2 Calculate the percent difference between the continuing calibration
relative response factor and the most recent initial calibration
mean relative response factor for each purgeable target and system
monitoring compound-using Equation 3.
EQ. 3
RRF_ - RRF.
%Difference = == x 100
RRF±
Where,
RRFC = Relative response factor from continuing calibration
standard
RKF± = Mean relative, response factor from the most recent
initial calibration meeting technical acceptance criteria
9.4.5 Technical Acceptance Criteria for Continuing Calibration
9.4.5.1 The continuing calibration standard must be analyzed at the
frequency described in Section 9.4.2 on a GC/MS system meeting the
BFB and initial calibration technical acceptance criteria.
9.4.5.2 The relative response factor (RRF) for each purgeable target and
system monitoring compound listed in Table 5 must be greater than or
equal to the compound's minimum acceptable response factor listed in
« Table 5.
9.4.5.3 The relative response factor percent difference for each purgeable
target and system monitoring compound listed in Table 5 must be less
than or equal to the value listed.
9.4.5.4 Up to two compounds may fail the requirements listed in Sections
9.4.5.2 and 9.4.5.3 and still meet the minimum relative response
factor criteria and percent difference criteria. However, these
compounds must have a minimum relative response factor greater than
or equal to 0.010 and the percent difference must be within the
inclusive range of ±40.0 percent.
9.4.5.5 Excluding those ions in the solvent front, no quantitation ion may
D-27/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 3
Calibration and Standardization
Continuing Calibration
saturate the detector. Consult the manufacturer's instrument
operating manual to determine how saturation is indicated for your
instrument.
9.4.6 Corrective Action for Continuing Calibration
9.4.6.1 If the continuing calibration technical acceptance criteria are not
met, recalibrate the GC/MS instrument according to Section 9.3.3.
It may be necessary to clean the ion source, change the column, or
take other corrective actions to achieve the continuing calibration
technical acceptance criteria.
9.4.6.2 Continuing calibration technical acceptance criteria must be met
before any samples, which include MS/MSD samples, or required blanks
are analyzed. Any samples or required blanks analyzed when
continuing calibration technical acceptance criteria have not been
met will require reanalysis at no additional cost to the Agency.
D-28/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
Sample Preparation
10.0 PROCEDURE
10.1 Sample Preparation
10.1.1 If insufficient sample amount (less than 90%, of the required amount)
is received to perform the analyses, the Contractor shall contact SMO
to apprise them of the problem. SMO will contact the Region for
instructions. The Region will either require that no sample analyses
be performed or will require that a reduced volume be used for the
sample analysis. No other changes in the analyses will be permitted.
The Contractor shall document the Region's decision in the SDG
Narrative.
10.1.2 If multiphase samples (e.g., two-phase liquid sample, oily
sludge/sandy soil sample) are received by the Contractor, the
Contractor shall contact SMO to apprise them of the type of sample
received. SMO will contact the Region. If all phases of the sample
are amenable to analysis, the Region may require the Contractor to do
any of the following:
Mix the sample and analyze an aliquot from the homogenized sample.
Separate the phases of the sample and analyze each phase
separately. SMO will provide EPA sample numbers for the
additional phases, if required.
Separate the phases, and analyze one or more of the phases, but
not all of the phases. SMO will provide EPA sample numbers for
the additional phases, if required.
Do not analyze the sample.
10.1.2.1 If all of the phases are not amenable to analysis (i.e., outside
scope), the Region may require the Contractor to do any of the
following:
Separate the phases and analyze the phase(s) that is amenable to'
analysis. SMO will provide EPA sample numbers for the
additional phases, if required.
Do not analyze the sample.
10.1.2.2 No other changes in the analyses will be permitted. The
Contractor shall document the Region's decision in the SDG
Narrative.
10.1.3 Water Samples
10.1.3.1 All water samples must be allowed to warm to ambient temperature
before analysis.
10.1.3.2 Prior to the analysis of samples, establish the appropriate purge
and trap GC/MS operating conditions, as outlined in Section 9.1,
analyze the instrument performance check solution (Section 9.2),
D-29/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
Sample Preparation
and calibrate the GC/MS system according to Sections 9.3 through
9.4.6.
10.1.3.3 If time remains in the 12-hour period (as described in Section
9.3.2), samples may be analyzed without analysis of a continuing
calibration standard.
10.1.3.4 If time does not remain in the 12-hour period since the injection
of the instrument performance check solution, both the instrument
performance check solution and the continuing calibration standard
must be analyzed before sample analysis may begin (see Section
9.4.2).
10.1.3.5 Adjust the purge gas (helium) flow rate to 25-40 mL/minute.
Variations from this flow rate may be necessary to achieve better
purging and collection efficiencies for some compounds,
particularly chloromethane and bromoform.
10.1.3.6 Remove the plunger from a 5 mL syringe and attach a closed syringe
valve. Open the sample or standard bottle which has been allowed
to come to ambient temperature, and carefully pour the sample into
the syringe barrel to just short of overflowing. Replace the
syringe plunger and compress the sample. Open the syringe valve
and vent any residual air while adjusting the sample volume to 5
mL. This process of taking ari aliquot destroys the validity of
the sample for future analysis so, if there is only one VOA vial,
the analyst must fill a second syringe at this time to protect
against possible loss of sample integrity. This second sample is
maintained only until such time-as the analyst has determined that
the first sample has been analyzed properly. Filling one 5 mL
syringe would allow the use of only one syringe. If an analysis
is needed from the second 5 mL syringe, it must be performed
within 24 hours. Care must also be taken to prevent air from
leaking into the syringe.
10.1.3.7 Add 10 uL of the system monitoring compound spiking solution
(Section.7.2.4.1) and 10 uL of the internal standard spiking
solution (Section 7.2.4.3) through the valve bore of the syringe,
then close the valve. The system monitoring compounds and
internal standards may be mixed and added as a single spiking
solution. The addition of 10 uL of the system monitoring compound
spiking solution to 5 mL of sample is equivalent to a
concentration of 50 ug/L of each system monitoring compound.
10.1.3.8
Attach the syringe-syringe valve assembly to the syringe valve on
the purging device. Open the syringe valves and inject the sample
into the purging chamber.
10.1.3.9 Close both valves and purge the sample for 11.0 (±0.1) minutes at
ambient temperature.
10.1.3.10 At the conclusion of the purge time, attach the trap to the
chromatograph, adjust the device to the desorb mode, and begin the
gas chromatographic temperature program. -Concurrently, introduce
D-30/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
Sample Preparation
the trapped materials to the gas chromatographic column by rapidly
heating the trap to 180 °C while backflushing the trap with an
inert gas between 20 and 60 mL/minute for four minutes.
10.1.3.11 While the trap is being desorbed into the gas chromatograph, empty
the purging chamber. Wash the chamber with a minimum of two 5 mL
flushes of reagent water to avoid carryover of target compounds.
For samples containing large amounts of water-soluble materials,
suspended solids, high-boiling compounds, or high purgeable
levels, it- may be necessary to wash out the purging device with a
detergent solution between analyses, rinse it with distilled
water, and then dry it in an oven at 105 °C.
10.1.3.12 After desorbing the sample for four minutes, recondition the trap
by returning the purge and trap device to the purge mode. Wait 15
seconds, then close the syringe valve on the purging device to
begin gas flow through the trap. The trap temperature should be
maintained at 180 °C. Trap temperatures up to 220 °C may be
employed. However, the higher temperature will shorten the useful
life of the trap. After approximately seven minutes, turn off the
trap heater and open the syringe valve to stop the gas flow
through the trap. When cool, the trap is ready for the next
sample.
10.1.4 Low Level Soil/Sediment Samples
10.1.4.1 The Contractor must determine whether a soil/sediment sample
should be analyzed by the low or medium method. It is the
responsibility of the Contractor to analyze the sample at the
correct level.
10.1.4.2 Three approaches may be taken to determine whether'the low level
or medium level method must be followed.
Assume the sample is low level and analyze a 5 g sample.
Use the X factor calculated from the hexadecane screen (Appendix
A) to determine the appropriate method for analysis.
Use other EPA approved screening procedures, or an in-house
laboratory screening procedure. The procedure must be
documented and available for review during on-site, laboratory
evaluation or when requested by the Technical Project Officer or
Administrative Project Officer.
10.1.4.3 If the on column concentration of any target compound exceeds the
initial calibration range from the analysis of'5 g sample, a
smaller sample size must be analyzed. However, the smallest
sample size permitted is 0.5 g. If smaller than 0.5 g sample size
is needed to prevent the on column concentration of target
compounds from exceeding the initial calibration range, the medium
level method must be used.
10.1.4.4 The low level soil/sediment method is based on a heated purge of a
D-31/VOA OLM04.2
-------
Exhibit D Volatiies -- Section 10
Procedure
Sample Preparation
soil/sediment sample mixed-with reagent water containing the
system monitoring compounds and the internal standards. Analyze
all matrix spike/matrix spike duplicate samples, blanks, and
standards under the same condition as the samples.
10.1.4.5 The procedure described below is to be utilized for volatile low
level soil samples unless the Modified SW-846 Method 5035 is
specified at the time of sample scheduling. If the Modified SW-
846 Method 5035 is to be utilized for low level soil samples, use
the procedure outlined in Appendix B and follow the equipment
manufacturer's instructions. Note: The requirements of this SOW
must be met at all times. If the above method is specified at the
time of sample scheduling, but the Contractor believes that the
samples cannot be processed by this method, the Contractor shall
immediately contact SMO. SMO will contact the Region for
instructions.
10.1.4.6 Use 5 grams of sample, or use the X Factor (Appendix A) or your
in-house screening procedure to determine the sample size for
purging.
10.1.4.7 Prior to the analysis of samples, establish the appropriate purge
and trap GC/MS operating conditions, as outlined in Section 9.1,
analyze the instrument performance check solution (Section 9.2),
and calibrate the GC/MS system according to Sections 9.3 through
9.4.6. This should be done prior to the preparation of the sample
to .avoid lose of volatiles from standards and sample. A heated
purge calibration curve must be prepared and used for the
quantitation of all samples analyzed with the low level method.
Follow the initial and daily calibration instructions (Sections
9.3.3 and 9.4.3), but increase the purge temperature to 40 °C.
10.1.4.8 To prepare the reagent water containing the system monitoring
compounds and the internal standards, remove the plunger from a 5
mL "Luerlok" type syringe equipped with a syringe valve and fill
until overflowing with reagent water. Replace the plunger and
compress the water to vent trapped air. Adjust the volume to 5
mL. Add 10 uL of the.system monitoring compound spiking solution
and 10 uL of the internal standard solution to the syringe through
the valve. NOTE: Up to 10 mL of reagent water may be added to a
soil sample to increase purge gas/sample interaction. All soil
samples including MS and HSD, standards, and blanks within an SDG
must have the same amount of reagent water added. Do not
increase/change the amount of system monitoring compound and
internal standard solution added.
10.1.4-. 9 The sample (for volatile organics) is'defined as the entire
contents of the sample container. Do not discard any supernatant
liquids. Mix the contents of the sample container with a narrow
metal spatula. Weigh 5 g or the amount determined in using the
screening procedure in Appendix A or an in-house screening
procedure into a tared purge device. Use a top loading balance.
Note and record the actual weight to the nearest 0.1 g.
D-32/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
Sample Preparation
10.1.4-.10 Add the spiked reagent water to the purge device and connect the
device to the purge and trap system. .
10.1.4.11 NOTE: Prior to the attachment of the purge device, the steps in
Sections 10.1.4.8 and 10.1.4.10 above must be performed rapidly to
avoid loss of volatile organics. These steps must be performed in
a laboratory free of solvent fumes.
10.1.4.12 Heat the sample to 40 °C (± 1 °C) and purge the sample for 11.0 (±
0.1) minutes.
10.1.4.13 Proceed with the analysis as outlined in Sections 10.1.3.9 through
10.1.3.12.
10.1.5 Medium Level Soil/Sediment Samples
10.1.5.1 The medium level soil/sediment method is based on extracting the
soil/sediment sample with methanol. An aliquot of the methanol
extract is .added to reagent water containing the system monitoring
compounds and the internal standards. The reagent water
containing the methanol extract is purged at ambient temperature.
When using the screening method in Appendix A, all samples with an
X Factor > 1.0 should be analyzed by the medium level method.
10.1.5.2 Prior to the analysis of samples, establish the appropriate purge
and trap GC/MS operating conditions, as outlined in Section 9.1,
analyze the instrument performance check solution (Section 9.2),
and calibrate the GC/MS system according to Sections 9.3 through
9.4.6. This should be done prior to the addition of the methanol
extract to reagent water. Because the methanol extract and
reagent water mixture is purged at ambient temperature, the
instrument performance check, initial calibration, and continuing
calibration for water samples may be used for analyses of medium
level soil/sediment sample extracts.
10.1.5.3 The sample (for volatile organics) is defined as the entire
contents of the sample container. Do not discard any supernatant
liquids. Mix the contents of the sample container with a narrow
metal spatula. Weigh 4 g (wet weight) into a tared 15 mL vial.
Use a top loading balance. Record the actual weight to the
nearest 0.1 g.
NOTE: If methanol preserved sample is to be analyzed, weigh sample
vial and contents to the nearest 0.1 g and record the weight.
Record any discrepancies between laboratory determined weight and
sampler determined weight in the SDG Narrative and utilize the
sampler determined weight in any calculations. Proceed to Section
10.1.5.6.
10.1.5.4 Quickly add 10 mL of methanol to the vial. Cap and shake for 2
minutes.
10..1.5.5 NOTE: The steps in Sections 10.1.5.3 and 10.1.5.4 must be
performed rapidly to avoid loss of volatile organics. These steps
D-33/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
Sample Preparation
must be performed in a laboratory free of solvent fumes.
10.1.5.6 Let the solution settle. Then, using a disposable pipette,
transfer approximately 1 mL of extract into a GC vial for storage.
The remainder may be discarded. The 1 mL extract may be stored in
the dark at 4 °C (±2 °C) prior to the analysis.
10.1.5.7 Table 6 can be used to determine the volume of methanol extract to
add to the 5 mL of reagent water for analysis. If the hexadecane
screen procedure (Appendix A) was followed, use the estimated
concentration (Option A) or the X Factor (Option B) to determine
the appropriate volume. Otherwise, estimate the concentration
range of the sample from the low level analysis or from the in-
house screening procedure to determine the appropriate volume.
10.1.5.8 Remove the plunger from a 5 mL "Luerlok" type syringe equipped
with a syringe valve and fill until overflowing with reagent
water. Replace the plunger and compress the water to vent trapped
air. Adjust the volume to 4.9 mL. Pull the plunger back to 5 mL
to allow volume for the addition of sample and standards. Add 10
uL of system monitoring compound and 10 uL of the internal
standard solution. Also add the volume of methanol extract
determined in Section 10.1.5.7 and a volume of clean methanol to
total 100 uL (excluding methanol in system monitoring/internal
standard solutions).
10.1.5.9 Attach the syringe-syringe valve assembly to the syringe valve on
the purge device. Open the syringe valve and inject the
water/methanol sample into the purging chamber.
10.1.5.10 Proceed with the analysis as outlined in Section 10.1.3.9 through
10.1.3.12.
10.1.6 Sample Dilutions
10.1.6.1 If the on-column concentration of any target compound in any
sample exceeds the initial calibration range, a new aliquot of
that sample must be diluted and purged. Guidance in performing
dilutions and exceptions to this requirement are given in Sections
10.1.6.2 through 10.1.6.10.
10.1.6.2 Use the results of the original analysis to determine.the
approximate dilution factor required to get the largest analyte
peak within the initial calibration range.
10.1.6.3 The dilution factor chosen should keep the response of the largest
analyte peak for a target compound in the upper half of the
initial calibration range of the instrument.
10.1.6.4 For medium level soil/sediment analyses, the purgeable organics
screening procedure (Appendix A), if used, will show the
approximate concentrations of major sample components. If a
dilution of the sample was -indicated, this dilution shall be made
D-34/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
pH Determination/Percent Moisture
just prior to GC/MS analysis of the sample. All steps in the
dilution procedure must be performed without delays until the
point at which the diluted sample is in a gas tight syringe.
10.1.6.5 For water samples, all dilutions are made in volumetric flasks (10
mL to 100 mL). Select the volumetric flask that will allow for
the necessary dilution. Intermediate dilutions may be necessary
for extremely large dilutions. Calculate the approximate volume
of reagent water which will be added to the volumetric flask
selected and add slightly less than this quantity of reagent water
to the flask.
10.1.6.6 . For water samples, inject the proper aliquot from the syringe
prepared in Section 10.1.3.6 into the volumetric flask. Only
aliquots of 1 mL increments are permitted. Dilute the aliquot to
the mark on the flask with reagent water. Cap the flask, invert,
and shake three times.
10.1.6.7 Fill a 5 mL syringe with the diluted sample as in Section
10.1.3.6.
10.1.6.8 If this is an intermediate dilution, use it and repeat the above
procedure to achieve larger dilutions.
10.1.6.9 Do not submit data for more than two analyses, i.e., from the
original sample and one dilution, or, if the volatile screening
procedure was employed, from the most concentrated dilution
analyzed.and one further dilution.
10.1.6.10 For total xylenes, where three isomers are quantified as two
peaks, the calibration of each peak should be considered
separately, i.e., a diluted analysis is not required for total
xylenes unless the concentration of the peak representing the
single isomer exceeds 200 ug/L (ug/kg for soils/sediment) or the
peak representing the two co-eluting isomers on the GC column
exceeds 400 ug/L (ug/kg for soils/sediment).
10.2 pH Determination (Water Samples)
Once the sample aliquots have been taken from the VOA vial, the pH of
the water sample must be determined. The purpose of the pH
determination is to ensure that all VOA samples were acidified in the
field. Test the pH by placing one or two drops of sample on the pH
paper (do not add pH paper to the vial). Record the pH of each sample,
and report these data in the SDG Narrative, following the instructions
in Exhibit B. No pH adjustment is to be performed by the Contractor.
10.3 Percent Moisture Determination
Immediately after weighing the sample for analysis, weigh 5-10 g of the
soil/sediment into a tared crucible. Determine the percent moisture by
drying overnight at 105 °C. Allow to cool in a desiccator before
weighing. Concentrations of individual analytes will be reported
relative to the dry weight of soil/sediment.
D-35/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 10
Procedure
pH Determination/Percent Moisture
EQ.
grams of wet sample - grams of dry sample
%Moisture = x 100
grams of wet sample
D-36/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.0 DATA ANALYSIS AND CALCULATIONS
11.1 Qualitative Identification
11.1.1 Identif icati'on of Target Compounds
11.1.1.1 The compounds listed in the Target Compound List (TCL) in Exhibit C
(Volatiles) shall be identified by. an analyst competent in the
interpretation of mass spectra (see Exhibit A, Section 4.3.1) by
comparison of the sample mass spectrum to the mass spectrum of a
standard of the suspected compound. Two criteria must be satisfied
to verify the identifications: (1) elution, of the sample component
at the same GC relative retention time as the standard component,
and (2) correspondence of the sample component and standard
component mass spectra.
11.1.1.2 For establishing correspondence of the GC relative retention time
(RRT), the sample component RRT must compare within ±0.06 RRT units
of the RRT of the standard component. For reference, the standard
must be run in the same 12-hour time period as the sample. If
samples are analyzed during the same 12-hour time period as the
initial calibration standards, use the RRT values from the 50 ug/L
standard. If co-elution of interfering components prohibits
accurate assignment of the sample component RRT from the total ion
chromatogram, the RRT should be assigned by using extracted ion
current profiles for ions unique to the component of interest.
11.1.1.3 For comparison of standard and sample component mass spectra, mass
spectra obtained on the Contractor's GC/MS are required. Once
obtained, these standard spectra may be used for identification
purposes, only if the Contractor's GC/MS meets the daily instrument
performance requirements for BFB. These standard spectra may be
obtained from the run used to obtain reference RRTs.
11.1.1.4 The requirements for qualitative verification by comparison of mass
spectra are as follows:
All ions present in the standard mass spectra at a relative
intensity greater than 10.0 percent (most abundant ion in the
spectrum equals 100.0 percent) must be present in the sample
spectrum.
The relative intensities of ions specified above must agree
within ± 20.0 percent between the standard and sample spectra.
(Example: For an ion with an abundance of 50.0 percent in the
standard spectra, the corresponding sample abundance must be
between 30.0 and 70.0 percent).
Ions greater than 10.0 percent in the sample spectrum but not
present in the standard spectrum must be considered and
accounted for by the analyst making the comparison. In Exhibit
A, Task II, the verification process should favor false
positives. All compounds meeting the identification criteria
must be reported with their spectra. For all compounds below
the CRQL, report the actual value followed by a "J", e.g., "3J".
D-37/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.1.1.5 If a compound cannot be verified by all of the criteria in Section
11.1.1.4, but in the technical judgment of the mass spectral
interpretation specialist, the identification is correct, then the
Contractor shall report that identification and proceed with
guantitation in Section 11.2.
11.1.2 Identification of Non-Target Compounds
11.1.2.1 A library search shall be executed for non-target sample components
for the purpose of tentative identification. For this purpose, the
NIST/EPA/NIH (May 1992 release or later) and/or Wiley. (1991 release
or later), or equivalent mass spectral library, shall be used.
11.1.2.2. Up to 30 organic compounds of greatest apparent concentration not
listed in Exhibit C for the volatile and semivolatile organic
fraction, excluding the system monitoring compounds and internal
standard compounds, shall be tentatively identified via a forward
search of the NIST/EPA/NIH (May 1992 release or later) and/or Wiley
(1991 release or later), or equivalent mass spectral library. The
following are not to be reported: 1) Substances with responses less
than 10' percent' of the internal standard (as determined by
inspection of the peak areas or height), 2) Substances which elute
earlier than 30 seconds before the first purgeable compound listed
in Exhibit C (Volatiles) or three minutes after the last purgeable
compound listed in Exhibit C (Volatiles) has eluted are not required
to be searched in this fashion, 3) Carbon dioxide, and 4)
Semivolatile TCL compounds listed in Exhibit C. Only after visual
comparison of sample spectra with the nearest library searches will
the mass spectral interpretation specialist assign a tentative
identification. NOTE: Computer generated library search routines
must not use normalizations which would misrepresent the library or
unknown spectra when compared to each other. . -
11.1.2.3 Up to 20 peaks of greatest apparent concentration (as determined by-
inspection of peak areas or heicjhts) that are suspected to be
straight-chain, branched, or cyclic alkanes, alone or part of an
alkane series shall be library searched. Documentation for the
tentative identification must be supplied. Alkanes are not counted
as part of the 30 organic compounds described in Section 11.1.2.2.
11.1.2.4 Guidelines for making tentative identification:
Relative intensities of major ions in the reference spectrum
(ions greater than 10.0 percent of the most abundant ion) should
be present in the sample spectrum.
The relative intensities of the major ions should agree within
±20.0 percent. Example: For an ion with an abundance of 50.0
percent of the standard spectra, the corresponding sample ion
abundance must be between 30.0 and 70.0 percent.
Molecular ions present in reference spectrum should be present
in sample spectrum.
Ions present in the sample spectrum but not in the reference
D-3 8/VGA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Calculations
spectrum should be reviewed for possible background
contamination or presence of co-eluting compounds.
Ions present in the reference spectrum but not in the sample
spectrum should be reviewed for possible subtraction from the
sample spectrum because of background contamination or co-
eluting compounds. Data system library reduction programs can
sometimes create these discrepancies.
11.1.2.5 If, after careful review and in the technical judgement of the mass
spectral interpretation specialist, no valid identification can be
made, the compound should be reported as follows:
If the library search produces a match at or above 85%, 'report
that compound.
If the library search produces more ;than one compound at or
above 85%, report the first compound (highest).
Tf the library search produces no matches at or above 85%, the
compound should be reported as unknown. The mass spectral
specialist should give additional classification of the unknown
compound, if possible (i.e. unknown aromatic, unknown
hydrocarbon, unknown acid type, unknown chlorinated compound).
If probable molecular weights can be distinguished, include
them.
11.1.2.6 Straight-chain, branched, or cyclic alkanes are not to be reported
as tentatively identified compounds on FORM I VOA-TIC. When the
above alkanes are tentatively identified, the concentration (s) are
to be estimated as described in Section 11.2.2 and reported in the
SPG Narrative as alkanes, by class (i.e., straight-chain, branched,
or cyclic; as a series; as applicable).
11.2 Calculations
11.2.1 Target Compounds
11.2.1.1 Target compounds identified shall be quantified by the internal
standard method using the equations below. The internal standard
used shall be that which is assigned in Table 3. The relative
response factor (RRF) from the continuing calibration standard is
used to calculate the concentration in the sample.
11.2.1.2 Water
EQ.'.5
(AJ (I) (Df)
Concentration (ug/L) =
(A.s) (RRF) (Vo)
Where,
D-39/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Calculations
A^ = Area of the characteristic ion (EICP) for the compound to
be measured (see Table 2)
Ais = Area of the characteristic ion (EICP) for the specific
internal standard (see Tables 3 and 4)
Ia = Amount of internal standard added in nanograms (ng)
RRF = Relative response factor from the ambient temperature
purge of the calibration standard.
V0 = Volume of water purged in milliliters (mL)
Df = Dilution factor. The dilution factor for analysis of
water samples for volatiles by this method is defined as
the ratio of the number of milliliters (mL) of water
purged (i.e., V0 above) to the number of mL of the
original water sample used for purging. For example, if
2.0 mL of sample is diluted to 5 mL with reagent water
and purged, Df = 5 mL/2.0 mL = 2.5.
If no dilution is performed, Df = 1.
| 11.2.1.3 Low Level Soil/Sediment
EQ. 6
Concentration (ug/Kg). (dry weight basis) =
(Ais) (RRF) (W8) (D)
Where,
Ax, Is, Ais are as given for water, Equation 5.
RRF = Relative response factor from the heated purge of the
calibration standard.
100 - %moisture
D = '
Ws = Weight of sample added to the purge tube, in grams (g).
| 11.2.1.4 Medium Level Soil/Sediment
EQ. 7
(A ) (I ) (V )(1000) (Df)
Concentration ug/Kg (dry weight basis) =
(Ais) (RRF) (Va) (Ws) (D)
Where,
Ax, Is, Als are as given for water, Equation 5.
RRF = Relative response factor from the ambient temperature purge
of the calibration standard.
Vc = Total volume of the methanol extract in milliliters (mL).
NOTE: This volume is typically 10 mL, even though only 1 mL
is transferred to the vial in Section 10.1.5.6.
Va = Volume of the aliquot of the sample methanol extract (i.e.,
sample extract not including the methanol added to equal 100
uL) in microliters (uL) added to reagent water for purging.
Ws = Weight of soil/sediment extracted, in grams (g).
D-40/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Calculations
100 - %moisture
D = 100
Df = Dilution factor. The dilution factor for analysis of
soil/sediment samples for volatiles by the medium level
method is defined as:
uL most cone, extract used to make dilution + uL clean solvent
uL most cone, extract used to make dilution
11.2.1.5 For water, low level and medium level soil/sediment samples, xylenes
(o-,m-, and p-isomers) are to be reported as xylenes (total).
Because the o- and p-xylene isomers co-elute on packed columns, and
the m- and p-xylene isomers co-elute on capillary columns, special
attention must be given to the quantitation of the xylenes. The
relative response factor (RRF) determined in Section 9.4.4 is based
on the peak that represents the single isomer on the GC column used
(m-xylene on packed columns, o-xylene on capillary columns). In
quantitating sample concentrations, use the areas on both peaks and
the RRF from Section 9.4.4. The areas of the two peaks may be
summed, and the concentration determined, or the concentration
represented by each of the two peaks may be determined separately,
and then summed. It is required that all three xylene isomers be
present in the initial and continuing calibration standards.
11.2.1.6 The cis and trans stereo isomers of 1,2-dichloroethene are to be
reported separately.
11.2.1.7 Secondary ion quantitation is allowed only when there are sample
matrix interferences with the primary ion. If secondary ion
quantitation is performed, document the reasons in the SDG
Narrative. A secondary ion cannot be used unless a relative
response factor is calculated using the secondary ion.
11.2.1.8 The requirements listed in Sections 11.2.1.9 and 11.2.1.10 apply to
all standards, samples including MS/MSDs, and blanks.
11.2.1.9 It is expected that situations will arise where the automated
quantitation procedures in the GC/MS software provide inappropriate
quantitations. This normally occurs when there is compound co-
elution, baseline noise, or matrix interferences. In these
circumstances the Contractor must perform a manual quantitation.
Manual quantitations are performed by integrating the area of the
quantitation ion of the compound. This integration shall only
include the area attributable to the specific TCL compound. The
area integrated shall not include baseline background noise. The
area integrated shall not extend past the point where the sides of
the peak intersect with the baseline noise. Manual integration is
not to be used solely to meet QC criteria, nor is it to be used as a
D-41/VGA OLM04.2
-------
Exhibit D Volatiles -- Section Ii
Data Analysis and Calculations
Calculations
substitute for corrective action on the chromatographic system. Any
instances of manual integration must be documented in the SDG
Narrative.
11.2.1.10 In all instances where the data system report has been edited,
or where manual integration or quantitation has been performed,
the GC/MS operator must identify such edits or manual procedures
by initialing and dating the changes made to the report, and
shall include the integration scan range. In addition, a
hardcopy printout of the EICP of the quantitation ion displaying
the manual integration shall be included in the raw data. This
applies to all compounds listed in Exhibit C (Volatiles),
internal standards, and system monitoring compounds.
11.2.2 Non-Target Compounds
11.2.2.1 An estimated concentration for non-target compounds tentatively
identified shall be determined by the internal standard method. For
quantitation, the nearest internal standard free of interferences
shall be used.
11.2.2.2 The formulas for calculating concentrations are the same as in
Sections 11.2.1.2, 11.2.1.3, and 11.2.1.4. Total area counts (or
peak heights) from the total ion chromatograms are to be used for
both the compound to be measured and the internal standard. A
relative response factor (RRF) of one (1) is to be assumed. The
resulting concentration shall be qualified as "J" (estimated, due to
lack of a compound-specific response factor), and "N" (presumptive
evidence of presence), indicating the quantitative and qualitative
uncertainties associated with this non-target component. An
estimated concentration must be calculated for all tentatively
identified compounds as well as those identified as unknowns.
11.2.3 CRQL Calculations
NOTE: If the adjusted CRQL is less than the CRQL listed in Exhibit C
(Volatiles), report the CRQL listed in Exhibit C (Volatiles).
11.2.3.1 Water
EQ. 8
Vx
Adjusted CRQL = Contract CRQL x - x Df
Where,
V0 and Df are as given in Equation 5
Vx = Contract Sample Volume (5 mL)
D-42/VOA ' OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Calculations
11.2.3.2 Low Level Soil/Sediment
EQ. 9
(Wx)
Adjusted CRQL = Contract CRQL x
(WJ (D)
Where,
Ws and D are as given in Equation 6
Wx = Contract Sample Weight (5 g)
11.2.3.3 Medium Level Soil/Sediment
EQ. 10
Adjusted CRQL = Contract CRQL x
(Wx) (Ve) (Vy) (1000) (Df)
(W.) (V) (V.) (D)
Where,
Vt, Df, Ws, Va and D are as given in Equation 7
Wx = Contract Sample Weight (4 g)
Vy = Contract Soil Aliquot Volume from soil methanol extract
(100 uL) -
Contract Soil Methanol Extract Volume (10,000 uL)
11.2.4 System Monitoring Compound Recoveries
11.2.4.1 Calculate the recovery of each system monitoring compound in all
samples, blanks, matrix spikes, and matrix spike duplicates.
Determine if the recovery is within limits (see Table 7), and report
on the appropriate form.
11.2.4.2 Calculate the concentrations of the system monitoring compounds
using the same equations as used for target compounds.
11.2.4.3 Calculate the recovery of each system monitoring compound as
follows:
EQ. 11
._ Concentration (amount) found
%Recovery = x 100
Concentration (amount) spiked
11.2.5 Internal Standard Responses and Retention Times
Internal standard responses and retention times in all samples must be
evaluated during or immediately after data acquisition. Compare the
sample internal standard responses and retention times to the
continuing calibration internal standard response and retention times.
D-43/VOA OLM04.2
-------
Exhibit D Volatiles -- Section II
Data Analysis and Calculations
.Technical Acceptance Criteria for Sample Analysis
For samples analyzed during the same 12-hour time period as the
initial calibration standards, compare the internal standard responses
and retention times against the 50 ug/L calibration standard. The
extracted ion current profile'(EICP) of the internal standards must be
monitored and evaluated for each sample, blank, matrix spike, and
matrix spike duplicate.
11.3 Technical Acceptance Criteria for Sample Analysis
11.3.1 The samples must be analyzed on a GC/MS system meeting the BFB,
initial calibration, continuing calibration, and blank technical
acceptance criteria.
11.3.2 The sample must be analyzed within the contract holding time.
11.3.3 The sample must have an associated method blank meeting the blank
technical acceptance criteria.
11.3.4 The percent recovery of each of the system monitoring compounds in the
sample must be within the acceptance windows in Table 7.
11.3.5 The EICP area for each of the internal standards must be within the
inclusive range of -50.0 percent and +100.0 percent of the response of
the internal standards in the most recent continuing calibration
analysis.
11.3.6 The retention time shift for each of the internal standards must be
within ± 0.50 minutes (30 seconds) between the sample and the most
recent continuing calibration standard analysis.
11.3.7 The relative retention time (RRT) of the system monitoring compound in
a sample must be within ±0.06 (RRT) units of its relative retention
time in the continuing calibration standard.
11.3.8 Excluding those ions in the solvent front, no ion may saturate the
detector. No target compound concentration may exceed the upper limit
of the initial calibration range unless a more diluted aliquot of the
sample is also analyzed according to the procedures in Section 10.1.6.
11.3.9 The Contractor must demonstrate that there is no carryover from a
contaminated sample before data from subsequent analyses may be
submitted. After a sample that contains a target compound at a level
exceeding the initial calibration range, the Contractor must either:
Analyze an instrument blank immediately after the contaminated
sample. If an autosampler is used, an instrument blank must
also be analyzed using the same purge inlet that was used for
the contaminated sample. The instrument blanks must meet the
technical acceptance criteria for blank analysis (see Section
12.1.4), or
Monitor the sample analyzed immediately after the contaminated
sample for all compounds that were in the contaminated sample
and that exceeded the calibration range. The maximum
contamination criteria are as follows: the sample must not
D-44/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Corrective Action for Sample Analysis
contain a concentration above the CRQL for the target compounds
that exceeded the limits in the contaminated sample. If an auto
sampler is used, the next sample analyzed using the same purge
inlet that was used for the contaminated sample must also meet
the maximum contamination criteria. If the maximum criteria
were exceeded, then all samples affected by the carryover must
be reanalyzed at no additional cost to the Agency.
11.4 Corrective Action for Sample Analysis
11.4.1 Sample technical acceptance criteria must be met before data are
reported. Samples contaminated from laboratory sources or sample
results which failed to meet the sample technical acceptance criteria
require reanalysis at no additional cost to the Agency.
11.4.2 Corrective actions for failure to.meet instrument performance checks,
initial and continuing calibration, and method blanks must be
completed before the analysis of samples.
11.4.3 Corrective action for system monitoring compounds and internal
standard compounds that fail to meet acceptance criteria.
11.4.3.1 If any of the system monitoring compounds and internal standard
compounds fail to meet acceptance criteria:
Check all calculations, instrument logs, the system monitoring
compound and internal standard compound spiking solutions, and
the instrument operation. If the calculations were incorrect.,
correct the calculations and verify that the system monitoring.
compound recoveries and internal standard compound responses
meet acceptance criteria.
If the instrument logs indicate that the incorrect amount of
system monitoring compound or internal standard compound spiking
solution was added, then reanalyze the sample after adding the
correct amount of system monitoring compound and internal
standard spiking solutions.
If the system monitoring compound spiking solution or internal
standard compound spiking solution was improperly prepared,
concentrated, or degraded, re-prepare the solutions and
reanalyze the samples.
If the instrument malfunctioned, correct the instrument problem
and reanalyze the sample. If the instrument malfunction
affected the calibration, recalibrate the instrument before
reanalyzing the sample. Verify that the system monitoring
compound recoveries meet acceptance criteria.
11.4.3.2 If the above actions do not correct the problem, then the problem
may be due to a sample matrix effect. To determine if there was a
matrix effect, take the following corrective action steps:
Reanalyze the sample. EXCEPTION: If system monitoring compound
recoveries or internal standard compound response in a sample
D-45/VOA OLM04.2
-------
Exhibit D Voiatiies -- Section II
Data Analysis and Calculations
Corrective Action for Sample Analysis
used for a matrix spike or matrix spike duplicate were outside
the acceptance criteria, then it should be reanalyzed only if
system monitoring compound recoveries and internal standard
compound response met acceptance criteria in both the matrix
spike and matrix spike duplicate analyses.
If the system monitoring compound recoveries and the internal
standard compound responses meet the acceptance criteria in the
reanalyzed sample, then the problem was within the Contractor's
control. Therefore, submit data only from the reanalysis.
If the system monitoring compound recoveries and/or the internal
standard compound responses fail to meet the acceptance windows
in the reanalysis, then submit data from both analyses.
Distinguish between the initial analysis and the reanalysis on
all deliverables using the suffixes on Exhibit B.
11.4.4 Corrective action for system monitoring compounds relative retention
times/internal standard compounds retention times outside acceptance
criteria.
11.4.4.1 If the system monitoring compounds relative retention times .or
internal standard compounds retention times are not within their
acceptance criteria, check the instrument for malfunctions. If the
instrument malfunctioned, correct the instrument problem and
reanalyze the sample. If the instrument malfunction affected the
calibration, recalibrate the instrument before reanalyzing the
samples.
11.4.4.2 If the above actions do not correct the problem, then the problem
may be due to a sample matrix effect. To determine if there was a
matrix effect, take the following corrective action steps:
Reanalyze the sample. EXCEPTION: If the system monitoring
compounds relative retention times or internal standard
compounds retention times in a sample used for a matrix spike or
matrix spike duplicate were outside the acceptance criteria,
then it should be reanalyzed only if the system monitoring
compounds and internal standard compounds retention times were
within the acceptance criteria in both the matrix spike and
matrix spike duplicate analyses.
If the system monitoring compounds relative retention times and
internal standard compounds retention times are within the
acceptance criteria, then the problem was within the
Contractor's control. Therefore, submit only data from the
reanalysis when the system monitoring compounds relative
retention times and the internal standard compounds retention
times are within the acceptance limits.
D-46/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 11
Data Analysis and Calculations
Corrective Action for Sample Analysis
If the system monitoring compounds relative retention times or
the internal standard compounds retention times are outside the
acceptance criteria in the reanalysis, then submit data from
both analyses. Distinguish between the initial analysis and the
reanalysis on all deliverables, using the suffixes in Exhibit B.
D-47/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
Quality Control
Blank Analyses
12.0 QUALITY CONTROL
12.1 Blank Analyses
12.1.1 Summary -- There are three different types of blanks required by this
method.
12.1.1.1 METHOD BLANK - a volume of a clean reference matrix (reagent water
for water samples or a purified solid matrix for soil/sediment
samples) that is carried through the entire analytical procedure.
The volume or weight of the reference matrix must be approximately
equal to the volume or weight of samples associated with the blank.
The purpose of a method blank is to determine the levels of
contamination associated with the processing and analysis of
samples.
12.1.1.2 STORAGE BLANK - upon receipt of the first samples in an SDG, two
40.0 mL screw-cap volatile vials with a PTFE-faced silicone septum
are filled with reagent water (80 mL total). The vials are stored
with the samples in the SDG under the same conditions. After all
samples in the SDG have been analyzed, the storage blank is
analyzed. The storage blank indicates whether contamination may
have occurred during storage of samples.
12.1.1.3 INSTRUMENT BLANK - a 5.0 mL aliquot of reagent water that is
carried through the entire analytical procedure. Instrument blanks
are analyzed after a sample/dilution which contains a target
compound exceeding the initial calibration range1: The results from
the instrument blank analysis indicate whether there is
contamination from a previous sample.
12.1.2 Frequency of Blank Analyses
12.1.2.1 The method blank must be analyzed at least once during every 12-
hour time period on each GC/MS system used for volatile analysis
(see Section 9.2.2 for the definition of the 12-hour time period).
12.1.2.2 The method blank must be analyzed after the continuing calibration
and before any samples, including matrix spike/matrix spike
duplicates, dilutions, or storage blanks are analyzed. The method
blank must be analyzed after the initial calibration sequence if
samples are analyzed before the 12-hour period expires. A method
blank must be analyzed in each 12-hour time period in which samples,
including dilutions, matrix spikes/matrix spike duplicates, and
storage blanks are analyzed.
12.1.2.3 A minimum of one storage blank must be analyzed per SDG after all
samples for that SDG have been analyzed.
12.1.2.4 The Contractor must demonstrate that there is no carryover from
contaminated samples before data from subsequent analyses may be
used. Samples/dilutions may contain target compounds at levels
exceeding the initial calibration range. An instrument blank must
be analyzed after the sample that exceeds the calibration range
(also in the same purge inlet if an autosampler is used) or a sample
. D-48/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
Quality Control
Blank Analyses
that meets the maximum contamination criteria in Section 11.3.8 must
be analyzed. For these purposes, if the instrument blank meets the
technical acceptance criteria for blank analyses or the sample meets
the maximum contamination criteria, the system is considered to be
uncontaminated. If the instrument blank or sample does not meet the
criteria (i.e., contaminated), the system must be decontaminated.
Until an instrument blank meets the blank technical acceptance
criteria or a sample meets the maximum contamination criteria in
Section 11.3.8; any samples analyzed since the original contaminated
sample will require reanalysis at no additional cost to the Agency.
NOTE: Only the instrument blank which demonstrates that there was
no carryover from the previous sample or the instrument blank that
demonstrates that the system is clean (Section 12.1.4) needs to be
reported. Instrument blanks analyzed during the instrument
decontamination process which exceed the requirements listed in
Section 12.1.4 do not need to be reported.
12.1.3 Procedure for Blank Analyses
12.1.3.1 For water samples, a volatile method blank consists of a 5 mL volume
of reagent water (Section 7.1.1) spiked with 10 uL of the system
monitoring compound spiking solution (Section 7.2.4.1) and 10 uL of
the internal standard spiking solution (Section 7.2.4.3) and carried
through the analytical procedure.
12.1.3.2 For low level soil/sediment samples, a volatile method blank
consists of 5 g of a purified solid matrix added to 5 mL of reagent
water that has been spiked with 10 uL each of the system monitoring
compound spiking solution and the internal standard spiking
solution. This method blank is then carried through the analytical
procedure.
12.1.3.3 For medium level soil/sediment samples, a volatile method blank
consists of 4 g of a purified solid matrix added to 10 mL of
methanol and extracted for two minutes. A 100 uL aliquot of the
methanol is added to reagent water and spiked with 10 uL of the
internal standard spiking solution and 10 uL of the system
monitoring compound spiking solution and taken through the
analytical procedure.
12.1.3.4 Storage/instrument blanks consist of a 5 mL volume of reagent water -
(Section 7.1.1) spiked with 10 uL of the system monitoring compound
spiking solution (Section 7.2.4.1) and 10 uL.of the internal
standard spiking solution (Section 7.2.4.3) and carried through the
analytical procedure.
12.1.3.5 A storage blank shall be analyzed and reported as a water sample
unless the SDG contains only soil samples. If an SDG contains only
soil samples, the storage blank may be analyzed and reported as a
soil sample.
12.1.3.6 Identify and quantitate analytes'according to Section 11.0.
12.1.4 Technical Acceptance Criteria for Blank Analyses
D-49/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
Quality Control
Blank Analyses
12.1.4.1 All blanks must be analyzed on a GC/MS system meeting the BFB,
initial calibration and continuing calibration technical acceptance
criteria and at the frequency" described in Section 12.1.2.
12.1.4.2 A storage blank shall be analyzed and reported as a water sample
unless the SDG contains only soil samples. If an SDG contains only
soil samples, the storage blank may be analyzed and reported as a
soil sample.
12.1.4.3 The percent recovery of each of the system monitoring compounds in a
blank must be within the acceptance windows in Table 7.
12.1.4.4 The EICP area for each of the internal standards in a blank must be
within the inclusive range of -50.0 percent and +100.0 percent of
the response of the internal standards in the most recent continuing
calibration analysis.
12.1.4.5 The retention time shift for each of the internal standards in a
blank must be within ±0.50 minutes (30 seconds) of its retention
time in the most recent continuing calibration standard analysis.
12.1.4.6 The concentration of each target compound found in the blank must be
less than its .CRQL listed in Exhibit C (Volatiles), except for
methylene chloride and cyclohexane which must be less than 2.5 times
their respective CRQLs, and acetone and 2-butanone, which must be
less than 5 times their respective CRQLs.
12.1.5 Corrective Action for Blank Analyses
12.1.5.1 It is the Contractor's responsibility to ensure that method
interferences caused by the contaminants in solvent, reagents,
glassware, laboratory air, and other sample storage and processing
hardware that lead to discrete artifacts and/or elevated baselines
in gas chromatograms, be eliminated. If a Contractor's blanks
exceed the criteria in Section 12.1.4.6, the Contractor must
consider the analytical system to be out of control. The source of
the contamination must be investigated and appropriate corrective
measures must be taken and documented before further analysis
proceeds.
12.1.5.2 Any method blank or instrument blank that fails to meet the
technical acceptance criteria for blank analyses must be reanalyzed
at no additional cost to the Agency. Furthermore, all samples,
including MS/MSD samples, processed within the 12-hour period with a
method blank or instrument blank that does not meet the technical
acceptance criteria for blanks will require reanalysis at no
additional cost to the Agency.
12.1.5.3 If the storage blank does not meet the technical acceptance criteria
for blank analyses in Sections 12.1.4.1 through 12.1.4.5, correct
system problems and reanalyze the storage blank. If the storage
blank does not meet the criteria in Section 12.1.4.6, reanalyze the
storage blank to determine whether the contamination occurred during
storage or during the analysis. If, upon reanalysis, the storage
blank meets the criteria in Section 12.1.4.6, the problem occurred
D-50/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
during the analysis and the reanalyzed storage blank results must be
reported. If upon reanalysis, the storage blank did not meet the
criteria in Section 12.1.4.6, the problem occurred during storage.
The laboratory manager or his/her designee must address the problem
in the SDG Narrative and discuss the corrective actions implemented
to prevent future occurrences. .NOTE: A copy of the storage blank
data must also be retained by the Contractor and be made available
for inspection during on-site laboratory evaluations.
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.1 Summary of MS/MSD
In order to evaluate the effects of the sample matrix on the methods
used for volatile analyses, the Agency has prescribed a mixture of
volatile target compounds to be spiked into two aliquots of a sample,
and analyzed in accordance with the appropriate method.
12.2.2 Frequency of MS/MSD
12.2.2.1 A matrix spike and matrix spike duplicate must be performed for each
group of samples of a similar matrix for the following, whichever is
most frequent:
Each SDG, or
Each matrix within an SDG, or
Each group of samples of a similar concentration level (soils
only).
MS/MSD samples shall be analyzed unless otherwise specified on the
Traffic Report (TR). If no MS/MSD samples are specified on the TR,
the Contractor shall contact SMO to confirm that MS/MSD analyses are
not required.
12.2.2.2 As a part of the Agency's QA/QC program, water rinsate samples
and/or field/trip blanks (field QC) may accompany soil/sediment
samples and/or water samples that are delivered to a laboratory for
analysis. The Contractor shall not perform MS/MSD analysis on any
of the field QC samples.
12.2.2.3 If the EPA Region designates a sample to be used as an MS/MSD, then
that sample must be used. If there is insufficient sample, less
than the required amount, remaining to perform an MS/MSD, then the
Contractor shall choose another sample to perform an MS/MSD
analysis. At the time the selection is made, the Contractor shall
notify the Region (through SMO) that insufficient sample was
received and identify the EPA sample selected for the MS/MSD
analysis. The rationale for the choice of a sample other than the
one designated by the Region shall be documented in the SDG
Narrative.
12.2.2.4 If there is insufficient sample remaining in any of the samples in
an SDG to perform an MS/MSD, then the Contractor shall immediately
D-51/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
contact SMO to inform them of the problem. SMO will contact the
Region for instructions. The Region will either approve that no
MS/MSD is required, or require that a reduced sample aliquot be used
for the MS/MSD analysis. SMO will notify the Contractor of the
resolution. The Contractor shall document the decision in the SDG
Narrative.
12.2.2.5 If it appears that the Region has requested MS/MSD analysis at a
greater frequency than required by the contract, the Contractor
shall contact SMO. SMO will contact the Region to determine which
samples should have an MS/MSD performed on them. SMO will notify
the Contractor of the Region's decision. The Contractor shall
document the decision in the SDG Narrative. If this procedure is
not followed, the Contractor will not be paid for MS/MSD analysis
performed at a greater frequency than required by the contract.
12.2.2.6 When a Contractor receives only a Performance Evaluation (PE)
sample(s), no MS/MSD shall be performed within that SDG.
12.2.2.7 When>a Contractor receives a PE sample as part of a larger SDG, a
sample other than the PE sample must be chosen for the MS/MSD when
the Region did not designate samples to be used for this purpose.
If the PE sample is received as an ampulated standard extract, the
ampulated PE sample is not considered to be another matrix type.
12 . 2 . 3 Procedure for. Preparing MS/MSD
12.2.3.1 Water
To prepare a matrix spike and matrix spike duplicate for water
samples, add 10 uL of the matrix spike solution (Section 7.2.4.2) to
each of the 5 mL aliquots of the sample chosen for spiking. Process
samples according to Sections 10.1.3.7 through 10.1.3.12.
Disregarding any dilution's, this is equivalent to a concentration of
50 ug/L of each matrix spike compound.
12.2.3.2 Soil - Low Level
To prepare a matrix spike and matrix spike duplicate for low level
soil/sediment samples, add 10 uL of the matrix spike solution to the
5 mL of spiked reagent water added to each of the two aliquots of
the soil/sediment from the sample chosen for spiking. Process
samples according to Sections 10.1.4.8 through 10.1.4.13. The
concentration for a 5 g sample should be equivalent to 50 ug/kg of
each matrix spike compound.
12.2.3.3 Soil - Medium Level
12.2.3.3.1 To prepare a matrix spike and matrix spike duplicate for medium
level soil/sediment samples, add 9 mL of methanol and 1 mL of
matrix spike solution to each of the two aliquots of the
soil/sediment sample chosen for spiking. Process samples
according to Sections 10.1.5.6 through 10.1.5.10. This results
in a 6,200 ug/kg concentration of each matrix spike compound
when added to a 4 g sample. Add a 100 uL aliquot of this
D-52/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 12
. Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
extract to 5 mL of water for purging (as per Sections 10.1.5.8
through 10.1.5.9).
12.2.3.3.2 NOTE: Before performing an MS/MSD analysis, analyze the sample
used for MS/MSD. If the sample analysis required dilution, the
aliquots for the MS/MSD shall be prepared at the same dilution
as the least diluted analysis for which the sample results will
be reported to the Agency. Sample dilutions must be performed
in accordance with Section 10.1.6. Do not further dilute MS/MSD
samples to get either spiked or non-spiked analytes within
calibration range.
12.2.4 Calculations for MS/MSD
12.2.4.1 Calculate the concentrations of the matrix spike compounds using the
same equations as used for target compounds (Equations 5, 6, and 7).
Calculate the recovery of each matrix spike compound as follows:
EQ. 12
SSR ~ SR
Matrix Spike Recovery = x 100
SA
Where,
SSR = Spiked sample result
SR = Sample result
SA = Spike added
12.2.4.2 Calculate the relative percent difference (RPD) of the recoveries of
each compound in the matrix spike and matrix spike duplicate as
follows:
EQ. 13
RPD = IMSR-MSDRI x 100
(MSR + MSDR )
2
Where,
MSR = Matrix spike recovery
MSDR = Matrix spike duplicate recovery
The vertical bars in the formula above indicate the absolute value
of the difference, hence RPD is always expressed as a positive
value.
12.2.5 Technical Acceptance Criteria for MS/MSD
12.2.5.1 All MS/MSDs must be analyzed on a GC/MS system meeting the BFB,
initial calibration and continuing calibration technical acceptance
.- D-53/VOA OLM04 . 2
-------
Exhibit D Voiatiies -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
criteria, the blank technical acceptance criteria, and at the
frequency described in Section 12.2.2.
12.2.5.2 The MS/MSD must be analyzed within the contract holding time.
12.2.5.3 The retention time shift for each of the internal standards in the
MS/MSD must be within ±0.50 minutes (30 seconds) of its retention
time and the most recent continuing calibration standard analysis.
12.2.5.4 The limits for matrix spike compound recovery and RPD are given in
Table 8. As these limits are only advisory, no further action by
the laboratory is required. However, frequent failures to meet the
limits for recovery or RPD warrant investigation by the laboratory,
and may result in questions- from the Agency.
12.2.6 Corrective Action for MS/MSD
Any MS/MSD that does not meet the technical acceptance criteria for
MS/MSD must be reanalyzed at no additional cost to the Agency.
D-54/VOA OLM04.2
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Exhibit D Volatiles -- Sections 13-16
Method Performance/Pollution Prevention/Waste Management/References
13.0 METHOD PERFORMANCE
Not applicable.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or
eliminates the quantity or toxicity of waste at the point of generation.
Numerous opportunities for pollution prevention exist in laboratory
operation. The EPA has established a preferred hierarchy of
environmental management techniques that places pollution prevention as
the management option of first choice. Whenever feasible, laboratory
personnel should use pollution prevention techniques to address their
waste generation. When wastes cannot be feasibly reduced at the source,
the Agency recommends recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to
laboratories and research institutions consult "Less is Better:
Laboratory Chemical Management for Waste Reduction," available from the
American Chemical Society's Department of Government Relations and
Science Policy, 1155 16th Street, N.W., Washington D.C., 20036, (202)
872-4477.
15.0 WASTE MANAGEMENT
The Environmental Protection Agency requires that laboratory waste
management practices be conducted consistent with all applicable rules
and regulations. The Agency urges laboratories to protect the air,
water, and land by minimizing and controlling all releases from hoods
and bench operations, complying with the letter and spirit of any sewer
discharge permits and regulations, and by complying with all solid and
hazardous waste regulations, particularly the hazardous waste
identification rules and land disposal restrictions. For further
information on waste management consult "The Waste Management Manual for
Laboratory Personnel," available from the American Chemical Society at
the address listed in Section 14.2.
16.0 REFERENCES
Not applicable.
.D-55/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
17.0 TABLES/DIAGRAMS/FLOWCHARTS
Table 1
BFB Key Ions and Ion Abundance Criteria
Mass Ion Abundance Criteria
50 8.0-40.0 percent of mass 95
75 30.0-66.0 percent of mass 95
95 base peak, 100 percent relative abundance
96 5.0-9.0 percent of mass 95 (see note)
173 less than 2.0 percent of mass 174
174 50.0-120.0 percent of mass 95
175 4.0-9.0 percent of mass 174
176 93.0-101.0 percent of mass 174
177 5.0-9.0 percent of mass 176
NOTE: All ion abundances must be normalized to m/z 95, the nominal
base peak, even though the ion abundance of m/z 174 may be up to 120.0
percent that of m/z 95.
D-56/VOA OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 2
Characteristic Ions for Volatile Target Compounds
Primary
Quantitation
Analvte Ion Secondary Ion(s)
Di chlorodi fl uoromethane
Chloromethane
Vinyl chloride
B romome thane
Chloroethane
Tri chl orofluoromethane
1, 1-Dichloroethene
1, l,2-Trichloro-l,2,2-trifluoroethane
Acetone
Carbon disulfide
Methyl Acetate
Methylene chloride
trans-1, 2-Dichloroethene
Methyl tert -Butyl Ether
1, 1-Dichloroethane
cis-1, 2-Dichloroethene
2-Butanone
Chloroform
1,1, 1-Trichloroethane
Cyclohexane
Carbon Tetrachloride
Benzene
1, 2-Dichloroethane
Trichloroethene
Me thyl cycl ohexane
1, 2-Dichloropropane
Bromodichloromethane
cis-1, 3-Dichloropropene .
4 -Methyl -2 -pentanone
Toluene
trans-1, 3-Dichloropropene
1,1, 2 -Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1 , 2 -Dibromoethane
Chlorobenzene
Ethylbenzene
Xylene (total)
Styrene
Bromoform
85
50
62
94
64
101
96
101
43
76
43
84
96
73
63
96
43*
83
97
56
117
78
62
130
83
63
83
75
43
91
75
97
164
43
129
107
112
106
106
104
173
87
52
64
96
66
103
61, 98
85, 151
58
78
74
49, 51, 86
61, 98
43, 57
65, 83, 85, 98, 100
61, 98
57
85
99, 117, 119
69, 84
119, 121
-
64, 100, 98
95, 97, 132
55, 98
65, 114
85
77
58, 100
92
77
83, 85, 99, 132, 134
129, 131, 166
58, 57, 100
208, 206
109
114
91
91
78, 103
171, 175, 250, 252, 254,
256
*m/z 43 is used for quantitation of 2-Butanone, but m/z 72 must be
present for positive identification.
D-57/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 2 (Con't)
Characteristic Ions for Volatile Target Compounds
Analvte
Primary
Quantitation
Ion
Secondary Ion(s)
Isopropylbenzene
1,1,2,2-Tetrachloroethane
1, 3-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
1,2-Dibromo-3-Chioropropane
1,2,4-Trichlorobenzene
105
83
146
146
146
75
180
120, 77
85, 131, 133, 166
111, 75
111, 75
111, 75
157, 155
182, 145
D-58/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 3
Volatile Internal Standards with Corresponding Target Compounds
and System Monitoring Compounds Assigned for Quantitation
Bromochloromethane
Dichlorodifluoromethane
Chloromethane |
Vinyl Chloride
Bromome thane
Chloroethane
Trichlorofluoromethane \
1,1-Dichloroethene
1,1,2-Trichloro-l, 2,2-
trifluoroethane
Acetone
Carbon Disulfide
Methyl Acetate
Methylene Chloride
trans-1,2-
Dichloroethene
Methyl tert-Butyl Ether
1,1-Dichloroethane
cis-l,2-Dichloroethene
2-Butanone
Chloroform
1,2-Dichloroethane
1, 2-D,ichloroethane-d4
(SMC)
1,4 -Pi fluorobenzene
1,1,1-Trichloroethane
Cyclohexane
Carbon Tetrachloride
Benzene
Trichloroethene |
Me thylcyclohexane
1,2-Dichloropropane
Bromodichloromethane
cis-1,3-Dichloropropene
trans-1,3- |
Dichloropropene
1,1,2-Trichloroethane
Dibromochloromethane
Bromoform
Chlorobenzene-d5
4-Methyl-2-pentanone
Toluene
Tetrachloroethene
2-Hexanone
1,2-Dibromoethane
Chlorobenzene
Ethylbenzene
Xylene (total)
Styrene
Isopropylbenzene
1,1,2,2-
Tetrachloroethane
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
l,2-Dibromo-3-
ch1oropropane
1,2,4-Trichlorobenzene
Toluene-d8 (SMC)
4-Bromofluorobenzene
(SMC)
(SMC) = system monitoring compound
D-59/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 4
Characteristic Ions for System Monitoring Compounds and
Internal Standards for Volatile Organic Compounds with CAS Numbers
Compound
Primary
Quantitation
Ion
Secondary
lon(s)
CAS Number
4-Bromofluorobenzene
1,2-Dichloroethane-d4
Toluene-d8
SYSTEM MONITORING COMPOUNDS
95 174, 176 460-00-4
65 102 17060-07-0
98 70, 100 2037-26-5
Bromochloromethane
1,4-Difluorobenzene
Chlorobenzene-d5
INTERNAL STANDARDS
128 49, 130, 51 74-97-5
114 . 63, 88 540-36-3
117 82, 119 3114-55-4
D-60/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 5
Relative Response Factor Criteria for Initial and Continuing
Calibration of Volatile Organic Compounds
Volatile
Compound
Di chlorodi fl uorome thane
Chloromethane
Vinyl chloride
Bromome thane
Chi oroe thane
Tri chl orofl uorome thane
1, 1-Dichloroethene
1, l,2-Trichloro-l,2,2-trifluoroethane
Acetone
Carbon disulfide
Methyl Acetate
Methylene chloride
trans-l,2-Dichloroethene
Methyl tert -Butyl Ether
1, 1-Dichloroethane
cis-l,2-Dichloroethene
2-Butanone
Chloroform
1,1, 1-Trichloroethane
Cyclohexane
Carbon tetrachloride
Benzene
1 , 2 -Dichloroethane
Trichloroethene
Me thyl cycl ohexane
1 , 2 -Dichloropropane
Bromodichloromethane
cis- 1 , 3 -Dichloropropene
4 -Methyl -2 -pentanone
Toluene
trans- 1, 3 -Dichloropropene
1,1, 2 -Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1, 2-Dibromoe thane
Chlorobenzene
Ethylbenzene
Xylene (total)
Styrene
Bromoform
Minimum
RRF
0.010
0.010
0.100
0.100
0.010
0.010
0.100
0.010
0.010
0.010
0.010
0.010
0.010
0. 010
0.200
0.010
0.010
0.200
0.100
0.010
0.100
0.500
0.100
0.300
0.010
0.010
0.200
0.200
0.010
0.400
0.100
0.100
0.200
0.010
0.100
0.010
0.500
0.100
0.300
0.300
0.100
Maximum
%RSD
none
none
20.5
20.5
none
none
20.5
none
none
none
none
none
none
none
20.5
none
none
20.5
20.5
none
20.5
20.5 .
20.5
20 .5
none
none
20.5
20.5
none
20.5
20 .5
20.5
20.5
none
20.5
none
20.5
20.5
20.5
20.5
20.5
Maximum
%Diff
none
none
±25.0
±25.0
none
none
±25.0
none
none
none
none
none
none
none
±25.0
none
none
±25.0
±25.0
none
±25.0
±25.0
±25.0
±25.0
none
none
±25.0
±25.0
none
±25.0
±25.0
±25.0
±25.0
none
±25.0
none
±25.0
±25.0
±25.0
±25.0
±25.0
D-61/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Talile 5 (Con't)
Relative Response Factor Criteria for Initial and Continuing
Calibration of Volatile Organic Compounds
Volatile
Compound
Minimum Maximum Maximum
RRF %RSD %Diff
Isopropylbenzene
1,1,2,2-Tetrachloroethane
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
1, 2-Dibromo-3-chloropropane
1,2,4-Trichlorobenzene
SYSTEM MONITORING COMPOUNDS
Bromofluorobenzene
Toluene-d8
1,2-Dichloroethane-d4
0.010
0.300
0.600
0.500
0.400
0. 010
0.200
none
20.5
20.5
20.5
20.5
none
20.5
none
±25.0
±25.0
±25. 0
±25.0
none
±25.0
0.200
0.010
0.010
20.5
none
none
±25.0
none
none
D-62/VOA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 6
The "X" Factor Table
X Factor
Estimated
Concentration Range1
(ug/kg)
Take This Volume of
Methanol Extract2 (uL)
0.25
0.5 -
2.5 -
12.5
- 5.0
10.0
50.0
- 250
500 - 10,000
1000 - 20,000
5000 - 100,000
25,000 - 500,000
100
50
10
100 of
1/50 dilution3
Calculate appropriate dilution factor for concentrations exceeding
those in the table.
Actual concentration ranges could be 10 to 20 times higher than this
if the compounds are halogenated and the estimates are from GC/FID.
The volume of methanol added to the 5 mL of water being purged should
be kept constant. Therefore, add to the 5 mL syringe whatever volume
of methanol is necessary to maintain a volume of 100 uL added to the
syringe.
Dilute an aliquot of the methanol extract and then take 100 uL for
analysis.
D-63/VGA
OLM04.2
-------
Exhibit D Volatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 7
System Monitoring Compound Recovery Limits
Compound % Recovery Water % Recovery Soil
Toluene-d8 88-110 84-138
Bromofluorobenzene 86-115 59-113
l,2-Dichloroethane-d4 76-114 70-121
Table 8
Matrix Spike Recovery and
Relative Percent Difference Limits
% Recovery RPD % Recovery RPD
Compound Water Water Soil Soil
1,1-Dichloroethene 61-145 14 59-172 22
Trichloroethene 71-120 14 62-137 24
Benzene 76-127 11 66-142 21
Toluene 76-125 13 59-139 21
Chlorobenzene 75-130 13 60-133 21
D-64/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
APPENDIX A - SCREENING OF HEXADECANE EXTRACTS FOR VOLATILES
1.0 SCOPE AND APPLICATION
1.1 The hexadecane extraction and screening methods for purgeables described '
in this section are designed to aid the analyst in deciding whether.a
soil sample is low or medium level in order to prevent saturation of the
purge and trap system and/or the GC/MS system. These or other screening
methods should be used, particularly if there is some doubt about the
level of organics in a sample. This is especially true in soil/sediment
analysis. Water samples may also be screened to determine an
appropriate dilution factor for analysis.
1.2 These extractions and preparation procedures were developed for rapid
screening of water and soil/sediment samples from hazardous waste sites.
The design of the methods thus does not stress efficient recoveries or
low limits of quantitation. Rather, the procedures were designed to
screen at moderate recovery and sufficient sensitivity for a broad
spectrum of organic chemicals. The results of the analyses thus may
reflect only a minimum of the amount actually present in some samples.
This is especially true if water soluble solvents are present.
2.0 SUMMARY OF METHODS
2.1 Sample Preparation
2.1.1 Water
A 40 mL aliquot of sample is extracted with 2 mL of hexadecane. This
provides a minimum quantitation limit (MQL) as follows:
Compounds MQL (uq/L)
non-halogenated aromatics 40-50
halogenated methanes - 80-1000
halogenated ethanes 400-500
2.1.2 Soil/Sediment
40 mL of reagent water are added to 10 g (wet weight) of
soil/sediment and shaken. The water phase is in turn extracted with
2 mL of hexadecane. This provides a minimum quantitation limit of
approximately four times higher than those listed for water.
2.2 GC/FID Screening
The hexadecane extracts of water and soil/sediment are screened on a gas
chromatograph/flame ionization detector (GC/FID). The results of the
screen will determine if volatile organics are to be analyzed by low or
medium level GC/MS procedures if the sample is a soil/sediment, or to
determine the appropriate dilution factor if the sample is water. Note:
The flame ionization detector varies considerably in sensitivity when
comparing aromatics and halogenated methanes and ethanes. Halomethanes
are approximately 2Ox less sensitive than aromatics and haloethanes are
D-65/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
approximately lOx less sensitive than aromatics. Low molecular weight,
water soluble solvents (e.g., alcohols and ketones) will not be
extracted from the water, and therefore will not be detected by the
GC/FID.
3.0 INTERFERENCES
Method interferences may be caused by contaminants in solvents,
reagents, glassware, and other sample processing hardware that lead to
discrete artifacts and/or elevated baselines in the total ion current
profiles. All of these materials must be routinely demonstrated to be
free from interferences under the conditions of the analysis by running
laboratory reagent blanks. Matrix interferences may be caused by
contaminants that are coextracted from the sample. The extent of matrix
interferences will vary considerably from source to source depending
upon the nature and diversity of the site being sampled.
4.0 SAFETY
The toxicity or carcinogenicity of each reagent used in this method has
not been precisely determined; however, each chemical should be treated
as a potential health hazard. Exposure to these reagents should be
reduced to the lowest possible level. The laboratory is responsible for
maintaining a current awareness file of OSHA regulations regarding the
safe handling of the chemicals specified in this method. A reference
file of data handling sheets should be made available to all personnel
involved in these analyses. Use all reagents in fume hoods whenever
possible. Always wear safety glasses or a shield for eye protection,
protective clothing, and observe proper mixing when working with these
reagents.
5.0 EQUIPMENT AND SUPPLIES
Brand names, suppliers, catalog and part numbers are for illustrative
purposes only. No endorsement is implied. Equivalent performance may
be achieved using equipment and supplies other than those specified
here, but demonstration of equivalent performance meeting the
requirements of this SOW is the responsibility of the Contractor.
5.1 Glassware
5.1.1 Syringes - 0.5 mL
5.1.2 Vials and Caps - 2 mL capacity for GC autosampler
5.1.3 Pasteur Pipets - disposable
5.1.4 Centrifuge Tube - 50 mL with ground glass stopper or Teflon-lined
screw cap.
5.1.5 Volumetric Flask - 50 mL with ground glass stopper.
5.2 Balance - analytical, capable of accurately weighing ±0.0001 g.
5.3 Pyrex Glass Wool
D-66/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
5.4 Balances - analytical, capable of accurately weighing ±0.0001 g, and a
top-loading balance capable of weighing 100 g ±0.01 g. The balances
must be calibrated with class S weights or known reference weights once
per each 12-hour work shift. The balances must be calibrated with class
S weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
5.5 Centrifuge
5.6 Gas Chromatograph/Mass Spectrometer (GC/MS) System
5.6.1 Gas Chromatograph - an analytical system complete with a temperature
programmable gas chromatograph suitable for on-column injection and
all required accessories including syringes, analytical columns,
gases, detector, and strip-chart recorder. A data system is
recommended for measuring peak areas.
5.6.2 Gas Chromatography Column - 30 m (or longer) x 2 mm ID glass column
packed with 10% OV-101 on 100-120 mesh chromosorb W-HP (or
equivalent). The column temperature should be programmed from 80 °C
to 280 °C at 16 C°/min and held at 280 °C for 10 minutes.
5.6.3 Flame lonization Detector
6.0 REAGENTS AND STANDARDS
6.1 Reagents
6.1.1 Reagent Water - defined as water in which'an interferant is not
observed at the CRQL of each analyte of interest.
6.1.2 Hexadecane and Methanol - pesticide residue analysis grade or
equivalent.
6.2 Standards
6.2.1 Introduction
The Contractor must provide all standard solutions to be used with
this contract. These standards may be used only after they have been
certified according to the procedure in Exhibit E. The Contractor
must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must be retained by the
contractor and presented upon request.
6.2.2 Stock Standard Solutions
6.2.2.1 Stock standard solutions (1 ug/uL) can be prepared from pure
standard materials or purchased as certified solutions.
D-67/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
6.2.2.2 Prepare stock standard solutions by accurately weighing about 0.01
g of pure material. Dissolve the material in methanol and dilute
to volume in a 10 mL volumetric flask. Larger volumes can be used
at the convenience of the analyst. If compound purity is
certified at 97% or greater, the weight can be used without
correction to calculate the concentration of the stock standard.
6.2.3 Working Standard Solutions
6.2.3.1 Standard Mixture #1
Prepare a working standard mixture containing benzene, toluene,
ethylbenzene, and xylene at 100 ng/uL of each compound in
methanol.
6.2.3.2 Standard Mixture #2
Prepare a working standard mixture containing n-nonane. And n-
dodecane at 100 ng/uL of each compound in methanol.
6.2.4 Storage of Standards
Transfer all standard solutions into multiple Teflon-sealed screw-cap
vials. Store, with no head-apace, at -10 °C to -20 °C, and protect
from light. Stock standard solutions should be.checked frequently
for signs of degradation or evaporation, especially just prior to
preparing calibration standards from them. These solutions must be
replaced after six months, or sooner, if comparison with quality
control check samples indicates a problem. Standards prepared from
gasses or reactive compounds such as styrene must be replaced after
two months, or sooner, if comparison with quality control check
samples indicates a problem.
7.0 QUALITY CONTROL
7.1 Method Blank
7.1.1 Summary
A method blank is a volume of clean reagent water taken through the
extraction and screening procedure. The volume of reagent water -used
must be approximately equal to the volume of associated samples. The
purpose of a method blank is to determine the levels of contamination
associated with the processing and analysis of samples.
7.1.2 Frequency
One method blank must be extracted and analyzed on each GC/FID system
used to screen samples for the following, whichever is most frequent.
Each SDG, or
D-68/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
Each 20 samples.in an SDG, excluding matrix spikes/matrix spike
duplicates, or
When samples are extracted.
7.1.3 Procedure
For screening of volatile organics, a method blank consists of a 40
mL volume of reagent water extracted with 2 mL of hexadecane. The
hexadecane extract is then screened on a GC/FID system.
8.0 CALIBRATION AND STANDARDIZATION
8.1 GC/FID Operating Conditions
Refer to Section 5.5.2 for recommended column temperature program.
8.2 GC Calibration
8.2.1 Summary
Prior to sample analysis each GC/FID system must be standardized for
half scale response.
8.2.2 Frequency
Each GC/FID system must be calibrated at the beginning of each 12-
hour shift.
8.2.3 Procedure
8.2.3.1 Add 200 uL of each of working standard mixtures #1 and #2 (Section
6.2.3) to separate 40 mL portions of reagent water in 50 mL
volumetric flasks. Immediately add 2 mL of hexadecane, cap the
flask, and shake vigorously for 1 minute. Let phases separate.
Open the flask and add sufficient reagent water to bring the
hexadecane layer into the neck of the flask. Transfer
approximately 1 mL of the hexadecane layer to a 2 mL GC vial.
8.2.3.2 Inject 1-2 uL of the extracts that contain approximately 10 ng/uL
each of standard mixture #1 and standard mixture #2 compounds.
9.0 PROCEDURE
9.1 Sample Preparation
9.1.1 Water
9.1.1.1 Allow.the contents of the 40 mL sample vial to come to room
temperature.' Quickly transfer the contents of the 40 mL sample
vial to a 50 mL volumetric flask. Immediately add 2 mL of
hexadecane, cap the flask, and shake vigorously for 1 minute. Let
phases separate. Open the flask and add sufficient reagent water
to bring the hexadecane layer into the neck of the flask.
D-69/VOA OLM04.2
-------
Exhibit D -- Volatiies Appendix-A
Screening of Hexadecane Extracts for Volatiies
9.1.1.2 Transfer approximately 1 mL of the hexadecane layer to a 2 mL GC
vial. If an emulsion is present after shaking the sample, break
it by doing the following:
Pulling the emulsion through a small plug of Pyrex glass
wool packed in a pipet, or
Transferring the emulsion to a centrifuge tube and
centrifuging for several minutes.
9.1.2 Soil/Sediment
Add approximately 10 g.of soil/sediment (wet weight) to 40 mL of
reagent water in a 50 mL centrifuge tube with a ground glass stopper
or Teflon-lined cap. Cap and shake vigorously for 1 minute.
Centrifuge the capped flask briefly. Quickly transfer supernatant
water to a 50 mL volumetric flask equipped with a ground-glass
stopper. Follow Section 9.1.1 starting with the addition of 2 mL of
hexadecane.
9.2 GC/FID Analysis
Inject the same volume of sample hexadecane extract as the extracted
standard mixture in Section 8.2.3.
9.2.1 GC/FID Chromatogram Interpretation -- Following are two options for
interpreting the GC/FID Chromatograms.
9.2.1.1 Option A is to use standard mixture #1 containing the aromatics to
calculate an approximate concentration of the aromatics in the
sample. Use this information to determine the proper dilution for
purge and trap if the sample is water, or whether to use the low
or medium level GC/MS purge and trap methods if the sample is
soil/sediment (see Table 1, Section 9.3 for guidance). This
should be the best approach; however, the aromatics may be absent
or obscured by higher concentrations of other purgeables. In
these cases, Option B may be the best approach.
9.2.1.2 Option B is to use standard mixture #2 containing n-nonane and n-
dodecane to calculate a factor. Use the factor.to calculate a
dilution for purge and trap of a water sample or to determine
whether to use the low or medium level GC/MS purge and trap
methods for soil/sediment samples (see Table 1, Section 9.3 for
guidance). All purgeables of interest have retention times less
than the n-dodecane.
9.3 Analytical Decision Point
9.3.1 Water
9.3.1.1 Compare the chromatograms of the hexadecane extract of the sample
with those of the reagent blank and extract of the standard.
9.3.1.2 If no peaks are noted, other than those also in the reagent blank,
analyze a 5 mL water sample by purge and trap GC/MS.
D-70/VOA " OLM04.2
-------
Exhibit D -- Volatiles Appendix A
Screening of Hexadecane Extracts for Volatiles
9.3.1.3 If peaks are present prior to the n-dodecane and the aromatics are
distinguishable, follow Option A (Section 9.2.1).
9.3.1.4 If peaks are present prior to the n-dodecane but the aromatics are
absent or indistinguishable, use option B as follows: if all
peaks are <3% of the n-nonane, analyze a 5 mL water sample by
purge and trap GC/MS. If any peaks are 23%of the n-nonane,
measure the peak height or area of the major peak and calculate
the dilution factor as follows:
., , _ Peak area of sample major peak
Dilution Factor = x 50
Peak area of n-nonane
The water sample will be diluted using the calculated factor just
prior to purge and trap GC/MS analysis.
9.3.2 Soil/Sediment
9.3.2.1 Compare the chromatograms of the hexadecane extract of the sample
with those of the reagent blank and extract of the standard.
9.3.2.2 If no peaks are noted, other than those also in the reagent blank,
analyze a 5 g sample by low level GC/MS.
9.3.2.3 If peaks are present prior to the n-dodecane and the aromatics are
distinguishable, follow Option A (Section 9.2.1) and the
concentration information in Table 1, to determine whether to
analyze by low or medium level method.
9.3.2.4 If peaks are present prior to the n-nonane but the aromatics are
absent or indistinguishable, and using Option B as follows,
calculate a factor using the following formula:
_ Peak area of sample major peak
Peak area of n-nonane
Table 1
Determination of GC/MS Purge and Trap Method
Approximate Concentration
X Factor Analyze by Range* (ug/Kg)
0-1.0 low level method 0-1,200
> 1.0 medium level method >1,200
* This concentration range is based on the response of aromatics to
GC/FID. When comparing GC/FID responses, the concentration for
halomethanes is 20 times higher, and that for haloethanes is 10 times
higher.
D-71/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix 3
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
APPENDIX B - MODIFIED SW-846 METHOD 5035 FOR VOLATILES IN LOW LEVEL SOILS
1.0 SCOPE AND APPLICATION
1.1 The analytical method that follows is designed to analyze low level
sediment and soil samples from hazardous waste sites for the volatile
organic compounds on the Target Compound List (TCL, see Exhibit C) . The
method includes sample preparation, screening to determine the
approximate concentration of organic constituents in the sample, and the
actual analysis which is based on a closed-system purge and trap gas
chromatograph/mass spectrometer (GC/MS) method.
2.0 SUMMARY OF METHOD
2.1 Low level volatile organic compounds are determined by analyzing
approximately 5 g of sample, in a pre-weighed vial with a septum-sealed
screw-cap (see Section 5.0) that already contains a stirring bar and a
sodium bisulfate preservative solution. Note: The sodium bisulfate
preservative and the stirring bar may be omitted under certain
circumstances (see Sections 9.3.2 and 9.3.8). The entire vial is placed
into the instrument carousel. Immediately before analysis, organic-free
reagent water, surrogates, and internal standards are 'automatically
added without opening the sample vial. The vial containing the sample
is heated to 40 "C and the volatiles purged through a sorbent trap using
an inert gas combined with agitation of the sample. When purging is
complete, the' trap is heated and backflushed with helium to desorb the
purgeable compounds onto a gas chromatograph column. The gas
chromatograph is temperature-programmed to separate the purgeable
compounds which are then detected with a mass spectrometer.
2.2 The sample introduction technique in Section 2.1 is not applicable to
all samples. If sample screening indicates that the soil/sediment
sample should be analyzed as a medium level .sample, the Contractor shall
follow the procedure described in Exhibit D-VOA Section 10.1.5 for
medium level soil/sediment samples.
3. 0 INTERFERENCES
3.1 Method interference may be caused by impurities in the purge gas,
organic compounds out-gassing from the plumbing ahead of the trap, and
solvent vapors in the laboratory. The analytical system must be
demonstrated to be free from contamination under the conditions of the
analysis by running laboratory method and instrument blanks as described
in Exhibit D-VOA Section 12. The use of non-Polytetrafluoroethylene
(PTFE) tubing, non-PTFE thread sealants, or flow controllers with rubber
components in the purging device should be avoided.
3.2 Samples can be contaminated by diffusion of volatile organics
(particularly fluorocarbons and methylene chloride) through the septum
seal into the sample during storage and handling.
3.3 Contamination by carryover can occur whenever medium level and low level
samples are sequentially analyzed. For samples containing large amounts
of water-soluble materials, suspended solids, high-boiling compounds, or
high purgeable levels, it may be necessary to wash out the purging
device. The trap and other parts of the system are also subjected to
: D-72/VOA OLM04 .2
-------
Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
contamination; therefore, frequent bakeout and purging of the entire
system may be required.
3.4 The laboratory where volatile analysis is performed should be completely
free of solvents. Special precautions must be taken, to determine
methylene chloride. The analytical and sample storage area should be
isolated from all atmospheric sources of methylene chloride, otherwise
random background levels will result. Since methylene chloride will
permeate through PTFE tubing, all GC carrier gas lines and purge gas
plumbing should be constructed of stainless steel or copper tubing.
Laboratory workers' clothing previously exposed to methylene chloride
fumes during common liquid/liquid extraction procedures can contribute
to sample contamination. The presence of other organic solvents in the
laboratory where volatile organics are analyzed will also lead to random
background levels and the same precautions must be taken.
4 . 0 SAFETY
4.1 The toxicity or carcinogenicity of each reagent used in this method has
not been precisely defined; however, each chemical compound should be
treated as a potential health hazard. From this viewpoint, exposure to
these chemicals must be reduced to the lowest possible level by whatever
means available. The laboratory is responsible for maintaining a
current awareness file of OSHA regulations regarding the safe handling
of the chemicals specified in this method. A reference file of material
data handling sheets should also be made available to all personnel
involved in the chemical analysis.
4.2 The following analytes covered by this method have been tentatively
classified as known or suspected, human or mammalian carcinogens:
benzene, carbon tetrachloride, chloroform, and vinyl chloride. Primary
standards of these toxic compounds should be prepared in a hood. A
NIOSH/Mass approved toxic gas respirator should be worn when the analyst
handles high concentrations of these toxic compounds.
5.0 EQUIPMENT AND SUPPLIES
Brand .names, suppliers, and part numbers are for illustrative purposes
only. No endorsement is implied. Equivalent performance may be
achieved using equipment and supplies other than those specified here,
but demonstration of equivalent performance meeting the requirements of
this SOW is the responsibility of the Contractor. The Contractor shall
document any use of alternate equipment or supplies in the SDG
Narrative.
5.1 Sample Containers
The specific sample containers required will depend on the purge-and-
trap system to be employed. Several systems are commercially available.
Some systems employ 40-mL clear vials with a special frit and equipped
with two PTFE-faced silicone septa. Other systems permit the use of any
good quality glass vial that is large enough to contain at least 5 g of
soil or solid material and at least 10 mL of water, and that can be
sealed with a screw-cap containing a PTFE-faced silicone septum. The
Contractor shall consult the purge-and-trap system manufacturer's
D-73/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
instructions regarding the suitable specific vials, septa, caps, and
mechanical agitation devices.
5.2 Glassware
5.2.1 Syringes - 25 mL glass hypodermic syringes with Luer-Lok (or
equivalent) tip (other sizes are acceptable depending on sample
volume used). 5.0, 1.0, and 0.5 mL syringes gas-tight with shut-off
valve.
5.2.2 Syringe valve - 2-way with Luer ends.
5.2.3 Micro syringes - 25 /uL with a 2 inch x 0.006 inch ID,' 22° bevel
needle (Hamilton '#702N or equivalent) . 10 and 100 x/L-
5.2.4 60-mL, septum-sealed glass vials to collect samples for screening,
dry weight determination.
5.2.5 40-mL, screw-cap, PTFE lined, septum-sealed glass vials. Examine
each vial prior to use to ensure that the vial has a flat, uniform
sealing surface.
5.2:6 Volumetric flasks - Class A, 10-mL and 100-mL, with ground glass
stoppers.
5.2.7 Disposable Pasteur pipettes.
5.3 Magnetic stirring bars - PTFE- or glass-coated, of the appropriate size
to fit the sample vials. Consult manufacturer's recommendation for
specific stirring bars. Stirring bars may be reused, provided that they
are thoroughly cleaned between uses. Consult the manufacturers of the
purging device and the stirring bars for suggested cleaning procedures.
5.4 Balances - analytical, capable of accurately weighing ± 0.0001 g, and a
top-loading balance capable of weighing 100 g ± 0.01 g. The balances
must be calibrated with class S weights or known reference weights once
per each 12-hour work shift. The balances must be calibrated with class
S weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
5.5 Purge and Trap Device - consists of a unit that automatically adds
water, SMCs, and internal standards to a hermetically sealed vial
containing the sample, purges the volatile compounds using an inert gas
stream while agitating the contents of the vial, and also traps the
released volatile compounds for subsequent desorption into the gas
chromatograph. Such systems are commercially available from several
sources and shall meet the following specifications.
5.5.1 The purging device should be capable of accepting a vial sufficiently
large to contain a 5 g soil/sediment sample plus a magnetic stirring
bar and 10 mL of water. The device must be capable of heating a soil
vial to 40°C and holding it at that temperature while the inert purge
gas is allowed to pass through the sample. The device should also be
capable of introducing at least 5 mL of organic-free reagent water
into the sample vial while trapping the displaced headspace vapors.
It must also be capable of agitating the sealed sample during
D-74/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SN-846 Method 5035 for Volatiles in Low Level Soils
purging, (e.g., using a magnetic stirring bar, sonication, or other
means). The analytes being purged must be quantitatively transferred
to an absorber trap. The trap must be capable of transferring the
absorbed volatile compounds to the gas chromatograph.
5.5.2 The trap must be at least 25 cm long and have an inside diameter of
at least 0.105 inch. Starting from the inlet, the trap must contain
equal amounts of the absorbents listed below. It is recommended that
1.0 cm of methyl silicone-coated packing (35/60) mesh (Davison, grade
15 or equivalent) be inserted at the inlet to extend the life of the
trap.
2,6-Diphenylene oxide polymer - 60/80 mesh, chromatographic grade
(Tenax GC or equivalent)
Methyl silicone packing - OV-1 (3%) on Chromosorb-W, 60/80 mesh or
equivalent
Coconut charcoal - Prepare from Barnebey Cheney, CA-580-26, or
equivalent, by crushing through 26 mesh screen
Trapping materials other than those listed above may also be used,
provided that they meet the specifications listed in Exhibit D-VOA
Sections 6.4.2 and 6.4.4.
5.5.3 The desorber for the trap must be capable of rapidly heating the trap
to 180 "C. The polymer section of the trap should not be heated
higher than 180 °C and the remaining sections should not exceed 220
"C during bakeout mode.
5.6 Gas Chromatograph/Mass Spectrometer (GC/MS) System
5.6.1 Gas chromatograph/mass spectrometer system specifications and
requirements are described in Exhibit D-VOA Section 6.6.
6.0 REAGENTS AND STANDARDS
6.1 Reagents
6.1.1 Reagent water - defined as water in which an interferant is not
observed at or above the CRQL of .the analytes of interest. Reagent
water may be generated by passing tap water through a'carbon filter
bed containing about 453 g (1 Ib) of activated carbon (Calgon Corp.,
Filtrasorb-300 or equivalent; .
6.1.1.1 A water purification system (Millipore Super-Q or equivalent) may
be used to generate reagent water.
6.1.1.2 Reagent water may also be prepared by boiling water for 15
minutes. Subsequently, while maintaining the temperature at 90
°C, bubble a contaminant-free inert gas through the water for one
hour. While still hot, transfer the water to a narrow-mouth
screw-cap bottle and seal with a Teflon-lined septum and cap.
6.1.2 Methanol - pesticide quality or equivalent.
D-75/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
6.1.3 Sodium bisulfate - ACS reagent grade or equivalent.
6.2 Standards
6.2.1 The Contractor must provide all standards to be used with this
contract. These standards may be used only after they have been
certified according to the procedure in Exhibit E. The Contractor
must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must be retained by the
Contractor and presented upon request.
6.2.2 The Contractor shall follow the procedures described in Exhibit D-VOA
Section 7.2 for preparing stock standards, secondary dilutions, and
all working standard solutions.
6.3 Storage of Standard Solutions
6.3.1 The Contractor shall follow the procedures described in Exhibit D-VOA
Section 7.3 for storage of all standard solutions.
6.3.2 The Contractor is responsible for maintaining the integrity of
standard solutions and verifying prior to use. This means that
standards must be brought to room temperature prior to use, checked
for losses, and checked that all components have remained in the
solution.
7.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
7.1 Sample Collection and Preservation
7.1.1 Soil/sediment samples should be collected in field core
sampling/storage containers (i.e., EnCore or equivalent) and 60 mL
septum-sealed glass vials in sufficient quantity to perform the
analysis. The field core sampling/storage containers should contain
approximately 5 g of sample each. The Contractor shall transfer the
contents of the field core sampling container immediately upon
receipt into the closed-system sample vial prepared as described in
Section 9.3 below and record the date and time of transfer. The
specific requirements for site sample collection are outlined by the
Region. If soil/sediment samples are received in pre-prepared
closed-system purge-and-trap sample vials as described in Section
9.3, then the Contractor shall proceed to Section 9.3.9 and determine
final sample weight.
7.1.2 All samples must be iced or refrigerated at 4 °C (±2 °C) from the
time of collection until analysis.
7.2 Procedure for Sample Storage
7.2.1 The samples must be protected from light and refrigerated at 4 °C
(±2 °C) from the time of receipt until 60 days after delivery of a
reconciled, complete sample data package to the Agency. After 60
days,, the samples may be disposed of in a manner that complies with
all applicable regulations.
D-76/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
7.2.2 The samples must be stored in an atmosphere demonstrated to be free
of all potential contaminants and in a refrigerator used only for
storage of volatile samples.
7.2.3 All volatile samples in an SDG must be stored together in the same
refrigerator.
7.2.4 Storage blanks shall be stored with samples until all samples are
analyzed.
7.2.5 Samples, sample extracts, and standards must be stored separately.
7.2.6 Volatile standards must be stored separately from semivolatile and
pesticide/Aroclor standards.
7.3 Contract Required Holding Times
Analysis of soil/sediment samples must be completed within 10 days of
Validated Time of Sample Receipt (VTSR). As part of the Agency's QA
program, the Agency may provide Performance Evaluation (PE) samples as
standard extracts which the Contractor is required to prepare per the
instructions provided by the Agency. PE samples must be prepared and
analyzed concurrently with the samples in the SDG. The contract
required 10 day holding time does not apply to PE samples received as
standard extracts.
8.0 CALIBRATION AND STANDARDIZATION
8.1 Purge and Trap
8.1.1 Assemble a purge-and-trap device that meets the specification in
Section 5.5 and that is connected to a gas chromatograph/mass
spectrometer system.
8.1.2 Before initial use, condition the trap overnight at 180°C by
backflushing with an inert gas flow of at least 20 mL/min, or
according to the manufacturer's recommendations. Vent the trap
effluent to the hood, not to the analytical column. Prior to daily
use, condition the trap for 10 min at 180°C while backflushing. The
trap may be vented to the analytical column during daily
conditioning; however, the column must be run through thetemperature
program prior to analysis of samples.
8.1.3 Establish the purge-and-trap instrument operating conditions. Adjust
the instrument to inject 5 mL of reagent water, to heat the sample to
40°C, and to hold the sample at 40°C for 1.5 minutes before
commencing the purge process, or as recommended by the instrument
manufacturer. Once established, the same purge and trap conditions
must be used for the analysis of all standards, samples, and blanks.
8.2 Gas Chromatograph/Mass Spectrometer
The Contractor shall follow the instrument conditions described in
Exhibit D-VOA Sections 9.1.2 and 9.1.3.
D-77/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
8.3 GC/MS Calibration (Tuning) and Ion Abundance
The Contractor shall follow the procedure described in Exhibit D-VOA
Section 9.2. All technical acceptance criteria for the GC/MS
performance check shall be met before any standards or samples,
including MS/MSDs or required blanks, are analyzed. Any samples or
required blanks analyzed when tuning technical acceptance criteria have
not been met will require reanalysis at no additional cost to the
Agency.
8.4 Initial Calibration
The Contractor shall follow the procedure described in Exhibit D-VOA
Section 9.3. However, the volume of reagent water used for calibration
must be the same volume used for sample analysis (normally 5 mL added to
the vial before sample addition plus the reagent water added by the
instrument). The calibration standards should also contain
approximately the same amount of the sodium bisulfate preservative as
the sample (e.g., approximately 1 g), as the presence of the
preservative will affect the purging efficiencies of the analytes. The
internal standard solution must be added automatically, by the
instrument, in the same fashion as used for the samples. Place the soil
vial containing the solution in the instrument carousel. In order to
calibrate the system monitoring compounds (SMCs) using standards at five
concentrations, it may be necessary to disable the automatic addition of
SMCs to each vial containing a calibration standard (consult the
manufacturer's instructions). Prior to purging, heat the sample vial to
40 "C for 1.5 minutes, or as recommended by the manufacturer.
All technical acceptance criteria for GC/MS initial calibration
specified in Exhibit D-VOA Section 9.3.5 shall be met prior to the
analysis of any samples, including MS/MSDs or required blanks. Any
samples or required blanks analyzed when initial calibration technical
acceptance criteria have not been met will require reanalysis at no
additional cost to the Agency.
8.5 Continuing Calibration
The Contractor shall follow the procedure for continuing calibration
described in Exhibit D-VOA Section 9.4. However, the continuing
calibration standard shall be prepared in the same manner as the initial
calibration standard of the same concentration as specified in Section
8.4 above (i.e., addition of the sodium bisulfate preservative).
All technical acceptance criteria for continuing calibration specified
in Exhibit D-VOA Section 9.4.5 shall be met prior to the analysis of any
samples, including MS/MSDs or required blanks. Any samples or required
blanks analyzed when continuing calibration technical acceptance
criteria have not been met will require reanalysis at no additional cost
to the Agency.
D-78/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix B
Modified SN-846 Method 5035 for Volatiles in Low Level Soils
9.0 PROCEDURE
9.1 The Contractor must determine whether a soil/sediment sample should be
analyzed by the low or medium method. Samples may contain higher than
expected quantities of purgeable organics that will contaminate the
purge-and-trap system thereby requiring extensive cleanup and instrument
maintenance. The Contractor may follow one of the screening procedures
identified in Exhibit D-VOA Section 10.1.4.2. The screening data are
used to determine which is the appropriate sample preparation procedure
for the particular sample. If, based on the screening results, medium
level analysis is required, the Contractor shall follow the procedure in
Exhibit D-VOA Section 10.1.5. If the Contractor received a pre-weighed
sample preserved in methanol (see Section 7.1.1), this sample shall be
utilized for the medium level analysis. It is the responsibility of the
Contractor to analyze the sample at the correct level.
9.2 If insufficient sample amount (less than 90% of the required amount) is
received to perform the analyses, the Contractor shall contact SMO to
notify them of the problem. SMO will contact the Region for
instructions. The Region will either require that no sample analyses be
performed or will require that a reduced volume be used for the sample
analysis.
9.3 Sample Preparation
9.3.1 The following steps apply to the preparation of vials used for the
analysis of low level soil/sediment samples by the closed-system
purge-and-trap equipment described in this method.
9.3.2 Add a clean magnetic stirring bar to each clean vial. If the purge-
and-trap device employs a means of stirring the sample other than a
magnetic stirrer (e.g., sonication or other mechanical means), then
the stir bar is omitted.
9.3.3 Add approximately 1 g of sodium bisulfate preservative to each vial.
If samples significantly smaller or larger than 5 g are to be used,
adjust the amount of preservative added to correspond to
approximately 0.2 g of preservative for-each 1 g of sample. Enough
sodium bisulfate should be present to ensure a sample pH of <2.
9.3.4 Add 5 ml/ of reagent water to each vial. The water and the
preservative will form an acid solution that will reduce or eliminate
the majority of the biological activity in the sample, thereby
preventing biodegradation of the volatile target compounds.
9.3.5 Seal the vial with the screw-cap and septum seal. If the double-
ended, fritted vials are used, seal both ends as recommended by the
manufacturer.
^
9.3.6 Affix a label to each vial and weigh the prepared vial to the nearest
0.01 g. Record the tare weight.
9.3.7 Because volatile organics will partition into the headspace of the
vial from the aqueous solution and will be lost when the vial is
opened, system monitoring compounds, matrix spikes and internal
standards should only be added to the vials after the sample has been
D-79/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
added to the vial. The standards should be introduced either
manually by puncturing the septum with a small-gauge needle or
automatically by the purge-and-trap system just prior to analysis.
9.3.8 Using the sample collection device, transfer the contents
(approximately 5 g) into the sample vial containing the preservative
solution. This sample transfer must be performed rapidly to minimize
loss of volatile compounds. Quickly brush any soil off the vial and
immediately seal the vial with the septum and screw-cap. The soil
vial is hermetically sealed and must remain so in order to guarantee
the. integrity of the sample. Gloves must be worn when handling the
sample vial since the vial has been tared. Record the date and time
of sample transfer onto the pre-prepared vials and submit with the
data package.
NOTE: Soil samples that contain carbonate minerals may effervesce
upon contact with the acidic preservative solution in the sample
vial. Therefore, if samples are known or suspected to contain high
levels of carbonates, a test sample (from the 60 mL glass vial)
should be added to a clean vial and checked for effervescence. If a
rapid or vigorous reaction occurs, the Contractor may discard the
test sample and proceed with sample preparation by transferring the
contents of the field core sampling/storage container into a clean
vial that does not contain the preservative.
9.3.9 Weigh the vial and contents to the nearest 0.01 g and record this
weight. Sample weight is determined by subtracting the sample vial
tared weight determined above from this final weight.
9.4 Sample Purge-and-Trap
5.4.1 Prior to sample purge, all soil/sediment samples must be allowed to
warm to ambient temperature. Shake the vial gently, to ensure that
the contents move freely and that stirring will be effective. Place
the sample vial in the instrument carousel according to the
manufacturer's instruction.
9.4.2 Without disturbing the hermetic seal on the sample vial, add 5 mL of
reagent water, .10 uL of the internal standard spiking solution
(Exhibit D-VOA Section 7.2.4.3), and 10 uL of the system monitoring
compound .spiking solution (Exhibit D-VOA Section 7.2.4.1). All
samples, including MS and USD, standards, and blanks, within an SDG
must have the same amount of reagent water added. Do not
increase/change the amount of system monitoring compound and internal
standard solution added. Prior to purging, heat the sample vial to
40 °C for 1.5 minutes, or as described by the manufacturer.
9.4.3 Purge the sample with helium or another inert gas at a flow rate of
20 to 40 mL/minute for 11 minutes while the sample is being agitated
with the magnetic stirring bar or other mechanical means. The purged
analytes are allowed to flow out of the vial through a glass-lined
transfer line to a trap packed with suitable sorbent materials.
9.4.4 If a non-cryogenic interface is to be utilized, place the purge-and-
trap system in the desorb mode after -the 11-minute purge, and preheat
the trap to 180 °C without a flow of desorption gas. Start the flow
D-80/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
of desorption gas at 10 mL/minute for about four minutes. Begin the
temperature program of the gas chromatograph and start data
acquisition.
9.4.5 If a cryogenic interface is to be utilized, place the purge-and-trap
system in the desorb mode after the 11-minute purge, making sure that
the cryogenic interface is at -150 °C or lower, and rapidly heat the
trap to 180 °C while backflushing with an inert gas at 4 mL/minute
for about 5 minutes. At the end of the 5-minute desorption cycle,
rapidly heat the cryogenic trap to 250 °C. Begin the temperature
program of the gas chromatograph and start the data acquisition.
9.4.6 After desorbing the sample for 4 to 5 minutes, recondition the trap
by returning the purge-and-trap system to the purge mode.. Maintain
the trap temperature at 180 °C. After approximately 10 minutes, turn
off the trap heater and halt the purge flow through the trap. When
the trap is cool, the next sample can be analyzed.
9.5 Sample Dilutions
If the on column concentration of any target compound exceeds the
initial calibration range from the analysis of 5 g sample, a smaller
sample size must be analyzed utilizing the procedure and methodology
described in Exhibit D-VOA. Guidance in performing dilutions and
exceptions to this requirement are given in Sections 10.1.6.2 through
10.1.6.10 of Exhibit D-VOA.
9.6 Percent Moisture Determination
It is highly recommended that the percent moisture determination only be
made after the analyst has determined that no sample aliquots will be
taken from the 60 mL vial for further analysis. This is to minimize
loss of volatiles and to avoid sample contamination from the laboratory
atmosphere. The Contractor shall follow the procedure described in
Exhibit D-VOA Section 10.3 for determining percent moisture of samples.
10.0 DATA ANALYSIS AND CALCULATIONS
The Contractor shall perform qualitative and quantitative analysis for
the target and non-target compounds following the procedures described
in Exhibit D-VOA Section 11.0. All technical acceptance criteria for
sample analysis described in Exhibit D-VOA Section 11.3 shall be met or
the corrective action for sample analysis described in Section 11.4 of
Exhibit D-VOA shall be followed.
11.0 QUALITY CONTROL
11.1 Blank Analyses
11.1.1 Summary -- There are three different types of blanks required by this
method.
11.1.1.1 METHOD BLANK - a volume of purified solid matrix (prepared as
described in Sections 9.3.2 through 9.3.5) and carried through the
entire analytical procedure. If any samples are prepared without
the sodium bisulfate preservative, a method blank will be prepared
D-81/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
in the same manner and run in the same 12 hour sequence as the
unpreserved samples. The weight of the purified solid matrix must
be approximately equal to the weight of samples associated with
the blank. The purpose of a method blank is to determine the
levels of contamination associated with the processing and
analysis of samples.
11.1.1.2 STORAGE BLANK - upon receipt of the first samples in an SDG, two
of the sample vials to be used for the closed-system purge-and-
trap analysis (prepared as described in Sections 9.3.2 through
9.3.5) are filled with reagent water. The vials are stored with
the samples in the SDG under the same conditions. After all
samples in the SDG have been analyzed, the storage blank is
analyzed. The storage blank indicates whether contamination may
have occurred during storage of samples.
11.1.1.3 INSTRUMENT BLANK - a 5.0 mL aliquot of reagent water that is
added to the sample vial (prepared as described in Sections 9.3.2
through 9.3.5) and carried through the entire analytical
procedure. Instrument blanks are analyzed after a sample which
contains a target compound exceeding the initial calibration
range. The results from the instrument blank analysis indicate
whether there is contamination from a previous sample.
11.1.2 Frequency of Blank Analyses
11.1.2.1 The method blank must be analyzed at least once during every
12-hour time period on each GC/MS system used for volatile
analysis (see Section 9.2.2 of Exhibit D-VOA for the definition of
the 12-hour time period).
11.1.2.2 The method blank must be analyzed after the continuing calibration
and before any samples, including matrix spike/matrix spike
duplicates, or storage blanks are analyzed. The method blank must
be analyzed after the initial calibration sequence if samples are
analyzed before the 12-hour period expires. A method blank must
be analyzed in each 12-hour time period in which samples,
including matrix spikes/matrix spike duplicates, and storage
blanks are analyzed.
11.1.2.3 A minimum of one storage blank must be analyzed per SDG after all
samples for that SDG have been analyzed.
11.1.2.4 The Contractor must demonstrate that there is no carryover from
contaminated samples before data from subsequent, analyses may be
used. Samples may contain target compounds at levels exceeding
the initial calibration range. An instrument blank must be
analyzed after the sample that exceeds the calibration range (also
in the same purge inlet if an autosampler is used) or a sample
that meets the maximum contamination criteria in Section 11.3.8 of
Exhibit D-VOA must be analyzed. For these purposes, if the
instrument blank meets the technical acceptance criteria for blank
analyses or the sample meets the maximum contamination criteria,
the system is considered to be uncontaminated. If the instrument
blank or sample does not meet the criteria (i.e., contaminated),
the system must be decontaminated. Until an instrument blank
D-82/VOA OLM04.2
-------
Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
meets the blank technical acceptance criteria or a sample meets
the maximum contamination criteria in Section 11.3.8 of Exhibit D-
VOA, any samples analyzed since the original contaminated sample
will require reanalysis at no additional cost to the Agency.
NOTE: Only the instrument blank which demonstrates that there was no
carryover from the previous sample or the instrument blank that
demonstrates that the system is clean (Section 12.1.4 Exhibit D-VOA)
needs to be reported. Instrument blanks analyzed during the
instrument decontamination process which exceed the requirements
listed in Exhibit D-VOA Section 12.1.4 do not need to be reported.
11.1.3 Procedure for Blank Analyses
11.1.3.1 Method blanks shall be analyzed in the same manner as the
associated samples, following the procedure described in Section
9.4.
11.1.3.2 Storage/instrument blanks shall be analyzed in the same manner as
the associated samples following the procedure outlined in section
9.4.
11.1.3.3 A storage blank may be analyzed and reported as a soil sample if
the SDG contains only soil samples.
11.1.3.4 Identify and quantitate analytes according to Section 11.0 of
Exhibit D-VOA.
11.1.4 Technical Acceptance Criteria for Blank Analyses
11.1.4.1 All technical acceptance criteria for blank analyses described in
Exhibit D-VOA Section 12.1.4 shall be met or corrective action for
blank analyses described in Exhibit D-VOA Section 12.1.5 shall be
followed.
11.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
11.2.1 Summary of MS/MSD
In order to evaluate the effects of the sample matrix on the methods
used for volatile analyses, the Agency has prescribed a mixture of
volatile target compounds to be spiked into two aliquots of a sample,
and analyzed in accordance with the appropriate method.
11.2.2 Frequency of MS/MSD
11.2.2.1 A matrix spike and matrix spike duplicate must be performed for
each group of samples of a similar matrix for the following,
whichever is most frequent:
Each SDG, or
Each matrix within an SDG, or
Each group of samples of a similar concentration level
(soils only) ..
D-83/VGA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
MS/MSD samples shall be analyzed unless otherwise specified on the
Traffic Report (TR) . If no MS/MSD samples are specified on the
TR, the Contractor shall contact SMO to confirm that MS/MSD
analyses are not required.
11.2.2.2 As a part of the Agency's QA/QC program, water rinsate samples
and/or field/trip blanks (field QC) may accompany soil/sediment
samples that are delivered to a laboratory for analysis. The
Contractor shall not perform MS/MSD analysis on any of the field
QC samples.
11.2.2.3 If the EPA Region designates a sample to be used as an MS/MSD,
then that sample must be used. If there is insufficient sample,
less than the required amount, remaining to perform an MS/MSD,
then the Contractor shall choose another sample to perform an
MS/MSD analysis. At the time the selection is made, the
Contractor shall notify the Region (through SMO) that insufficient
sample was received and identify the EPA sample selected for the
MS/MSD analysis. The rationale for the choice of a sample other
than the one designated by the Region shall be documented in the
SDG Narrative.
11.2.2.4 If there is insufficient sample remaining for any of the samples
in an SDG to perform an MS/MSD, then the Contractor shall
immediately contact SMO to inform them of the problem. SMO will
contact the Region for instructions. The Region will either
approve that no MS/MSD is required, or specify an alternative
means of performing the MS/MSD analysis. SMO will notify the
Contractor of the resolution. The Contractor shall document the
decision in the SDG Narrative.
11.2.2.5 If it appears that the Region has requested MS/MSD analysis at a
greater frequency than required by the contract, the Contractor
shall contact SMO. SMO will contact the Region to determine which
samples should have an MS/MSD performed on them. SMO will notify
the Contractor of the Region's decision. The Contractor shall
document the decision in the SDG Narrative. If this procedure is
not followed, the Contractor will not be paid for the MS/MSD
analysis performed at a greater frequency than required by the
contract.
11.2.2.6 When a Contractor receives only a Performance Evaluation (PE)
sample (s), no MS/MSD shall be performed within that SDG.
. 11.2.2.7 When a Contractor receives a PE sample as part of a larger SDG, a
sample other than the PE sample must be chosen for the MS/MSD when
the Region did not designate samples to be used for this purpose.
11.2.3 Procedure for Preparing MS/MSD
11.2.3.1 To prepare a matrix spike and matrix spike duplicate for low level
soil/sediment samples, follow the procedure outlined in Section
9.3. Add 10 uL of the matrix spike solution (Exhibit D-VOA
Section 7.2.4.2) either manually by puncturing the septum with a
small-gauge needle or automatically by the purge-and-trap system
just prior to analysis. Analyze the matrix spike and matrix spike
D-84/VOA OLM04.2
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Exhibit D -- Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
duplicate samples by the procedure described in Section 9.4. Do
not further dilute MS/MSD samples to get either spiked or non-
spiked analytes within calibration range.
11.2.4 Calculations for MS/MSD
The Contractor shall calculate the concentrations of the matrix spike
compounds in the matrix spike and matrix spike duplicate samples
using the same equation as used for target compounds (Equation 6)
Exhibit D-VOA Section 11.2.1.3. The recovery of each matrix spike
compound in the matrix spike and matrix spike duplicate samples and
the relative percent difference (RPD) of the recoveries shall be
calculated as specified in Exhibit D-VOA Section 12.2.4.
11.2.5 Technical Acceptance Criteria for MS/MSD
All technical acceptance criteria for MS/MSD specified in Exhibit D-
VOA Section 12.2.5 must be met or corrective action for MS/MSD in
Exhibit D-VOA Section 12.2.6 shall be followed.
D-85/VOA OLM04.2
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EXHIBIT D
ANALYTICAL METHODS
FOR SEMIVOLATILES
D-l/SVOA OLM04.2
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Exhibit D - Analytical Methods for SEMIVOLATILES
Table of Contents
Section Page
1..0 SCOPE AND APPLICATION 4
2.0 SUMMARY OF METHOD . . 5
2.1 Water ........ 5
2.2 Low Level Soil/Sediment ^ 5
2.3 Medium Level Soil/Sediment 5
3.0 DEFINITIONS 5
4.0 INTERFERENCES 6
5.0 SAFETY 6
6.0 EQUIPMENT AND SUPPLIES 7
7.0 REAGENTS AND STANDARDS 13
7.1 . Reagents , 13
7.2 Standards 13
7.3 Storage of Standard Solutions 16
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 18
8.1 Sample Collection and Preservation ' 18
8.2 Procedure for Sample Storage 18
8.3 Procedure for Sample Extract Storage 18
8.4 Contract Required Holding Times 18
9.0 CALIBRATION AND STANDARDIZATION 19
9.1 Instrument Operating Conditions 19
9.2 GC/MS Mass Calibration (Tuning) and Ion Abundance 19
9.3 Initial Calibration 21
9.4 Continuing Calibration . 23
10.0 PROCEDURE .27
10.1 Sample Preparation 27
10.2 Concentrating the Extract 33
10.3 Sample Cleanup by GPC 35
10.4 Sample Extract Cleanup by GPC 40
10.5 Final Concentration 42
10.6 Sample Analysis by GC/MS 42
11.0 DATA ANALYSIS AND CALCULATIONS 44
11.1 Qualitative Identification 44
11.2 Calculations 47
11.3 Technical Acceptance Criteria for Sample Analysis 51
11.4 Corrective Action 52
12.0 QUALITY CONTROL 55
12.1 Method Blanks 55
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD) 56
D-2/SVOA OLM04.2
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13.0 METHOD PERFORMANCE 61
14.0 POLLUTION PREVENTION 61
15-. 0 -WASTE MANAGEMENT .- . -.-;.-..- 61
16.0 REFERENCES 61
17.0 TABLES/DIAGRAMS/FLOWCHARTS . . . 62
APPENDIX A - SCREENING OF SEMIVOLATILE ORGANIC EXTRACTS 71
1.0 SCOPE AND APPLICATION 71
2.0 SUMMARY OF METHOD 71
3.0 INTERFERENCES 72
4.0 SAFETY 72
5.0 EQUIPMENT AND SUPPLIES 73
6.0 REAGENTS AND STANDARDS 75
7.0 QUALITY CONTROL 76
8.0 CALIBRATION AND STANDARDIZATION 77
9.0 PROCEDURE 78
D-3/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 1
Scope and Application
1.0 SCOPE AND APPLICATION
1.1 In 1978, EPA Headquarters and Regional representatives designed
analytical methods for the analysis of semivolatiles in hazardous waste
samples. These methods were based on EPA Method 625, Base/Neutral and
Acids. In 1980, these methods were adopted for use in the Contract
Laboratory Program (CLP). As the requirements of CERCLA evolved, the
CLP methods, as well as their precedent EPA 600 Series methods,
established the basis for other EPA methods to perform the analysis of
semivolatiles contained in hazardous waste samples (i.e., SW-846). The
following CLP method has continuously improved to incorporate
technological advancements promulgated by EPA, and has continued to set
the standard for the preparation, extraction, isolation, identification,
and reporting of semivolatiles at hazardous waste sites.
1.2 The analytical method that follows is designed to analyze water, soil
and sediment from hazardous waste sites for the semivolatile organic
compounds on the Target Compound List (TCL) (see Exhibit C). It covers
the determination of a number of organic compounds that are partitioned
into an organic solvent and are amenable to gas chromatography. The
method involves solvent extraction of the matrix sample,
characterization to determine the appropriate analytical protocol to be
used, followed by appropriate cleanup procedure and GC/MS analysis to
determine the semivolatile organic compounds present in the sample.
1.3 This analytical method provides the use of SH-846 Methods 3541
(Revision 0, September 1994) and 3545 (Revision 0, December 1996) for
the extraction of soil/sediment samples. However, prior to using either
one of these alternate extraction procedures, the Contractor must first
demonstrate that these procedures are equivalent to the existing
procedures, and obtain approval for use of these alternative extraction.
procedures from the EPA CLP National Program Manager. The process for
determining and documenting equivalency can be found in Exhibit E,
Section 6.0.
1.4 Problems have been associated with the following compounds analyzed by
this method.
1.4.1 Dichlorobenzidihe and 4-chloroaniline can be subject to oxidative
losses during solvent concentration.
1.4.2 Hexachlorocyclopentadiene is subject to thermal decomposition in the
inlet of the gas chromatograph, chemical reactions in acetone
solution, and photochemical decomposition.
1.4.3 N-nitrosodiphenylamine decomposes in the gas chromatograph inlet
forming diphenylamine and, consequently, may be detected as
diphenylamine.
D-4/SVOA OLM04.2
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2.0
Exhibit D Semivolatiles -- Sections 2 & 3
Summary of Method/Definitions
SUMMARY OF METHOD
2.1 Water
A one liter aliquot of sample is acidified to pH 2.0 and extracted with
methylene chloride using a continuous liquid-liquid extractor.
Separatory funnel extraction is NOT permitted. The methylene chloride
extract is dried with sodium sulfate, concentrated, subjected to GPC
(GPC is required when higher molecular weight compounds are present that
interfere with the analyses of target compounds; GPC is optional for all
other circumstances), and analyzed by GC/MS for extractable organics.
2.2 Low Level Soil/Sediment
A thirty (30) gram portion of soil/sediment is mixed with anhydrous
powdered sodium sulfate and extracted with 1:1 methylene
chloride/acetone solution using an ultrasonic probe or an alternate
extraction method that has been previously accepted by the Agency for
use by the Contractor. If the low level screen (Appendix A) is used, a
portion of this dilute extract is concentrated fivefold and screened by
GC/FID or GC/MS. If peaks are present at greater than 10,000 ug/Kg,
discard the extract and prepare the sample by the medium level method.
If no peaks are present at greater than 10,000 ug/Kg, the entire extract
is concentrated, subjected to GPC cleanup, and analyzed by GC/MS for
extractable organics.
2.3 Medium Level Soil/Sediment
Approximately one gram portion of soil/sediment is mixed with anhydrous
powdered sodium sulfate in a vial and extracted with methylene chloride.
The methylene chloride extract can be screened for extractable organics
using the procedure described in Appendix A, other EPA approved
screening procedures or an in-house laboratory screening procedure. If
organic compounds are detected by the screen, the methylene chloride
extract is subjected to GPC cleanup and analyzed by GC/MS for
extractable organics. If no organic compounds are detected by the
medium level screen, then a low level sample preparation is required.
3.0 DEFINITIONS
See Exhibit G for a complete list of definitions.
D-5/SVOA
OLM04.2
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Exhibit D Semivolatiles -- Sections 4 & 5
Interferences/Safety
4.0 INTERFERENCES
Contaminants in solvents, reagents, glassware, and other sample
processing hardware may cause method interferences such as discrete
artifacts and/or elevated baselines in the extracted ion current
profiles (EICPs). All of the materials routinely must be demonstrated
to be free from interferences under the conditions of the analysis by
running laboratory method blanks. Matrix interferences may be caused by
contaminants that are coextracted from the sample. The extent of matrix
interferences will vary considerably from source to source.
5.0 SAFETY
The toxicity or carcinogenicity of each reagent used in this method has
not been precisely determined; however, each chemical should be treated
as a potential health hazard. Exposure to these reagents should be
reduced to the lowest possible level. The laboratory is responsible for
maintaining a current awareness file of OSHA regulations regarding the
safe handling of the chemicals specified in this method. A reference
. file of data handling sheets should be made available to all personnel
involved in these analyses. Specifically, concentrated sulfuric acid
presents, some hazards and is moderately toxic and extremely irritating
to skin and mucous membranes. Use these reagents in a fume hood
whenever possible and if eye or skin contact occurs flush with large
volumes of water. Always wear safety glasses or a shield for eye
protection, protective clothing, and observe proper mixing when working
with these reagents.
D-6/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 6
Equipment and Supplies
6.0 EQUIPMENT AND SUPPLIES
Brand names, suppliers, catalog and part numbers are for illustrative
purposes only. No endorsement is implied. Equivalent performance may
be achieved using equipment and supplies other than those specified
here, but demonstration of equivalent performance meeting the
requirements of this Statement of Work is the responsibility of the
Contractor. The Contractor shall document any use of alternate
equipment or supplies in the SDG Narrative.
6.1 Glassware
6.1.1 Continuous Liquid-Liquid Extractors - equipped with Teflon or glass
connecting joints and stopcocks requiring no lubrication (Hershberg-
Wolf extractor, Ace Glass Company, Vineland, NJ P/N 6841-10 or
equivalent) or Hydrophobic Membrane-based Extractor (Accelerated One
Step Extractor, Corning series 3195 or equivalent).
6.1.2 Beakers - 400 mL
6.1.3 Syringes - 2 uL, 10 uL, 0.2 mL, 0.5 mL, and 10 mL with Luerlok
fitting.
6.1.4 Glass Scintillation Vials - at least 20 mL with screw-cap and Teflon
or aluminum foil liner.
6.1.5 Pasteur Pipets - 1 mL glass, disposable.
6.1.6 Vial and Caps - Amber glass, 2 mL capacity with Teflon-lined screw
cap, 2 mL capacity for GC auto sampler.
6.1.7 Drying Column - 19 mm ID chromatographic column with coarse frit
(substitution of a small pad of Pyrex glass wool for the frit will.
help prevent cross contamination of sample extracts).
6.2 Kuderna-Danish (K-D) Apparatus.
6.2.1 Concentrator Tubes - 15 mL and 10 mL graduated (Kontes K-570050-1025
or K-570040-1025 or equivalent). Calibration must be checked at the
volumes employed in the test. Ground-glass stoppers are used to
prevent evaporation of extracts.
6.2.2 Evaporative Flasks - 500 mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
6.2.3 Snyder Column - three-ball macro (Kontes K-503000-0121 or
equivalent).
6.2.4 Snyder Column - two-ball micro (Kontes K-569001-0219 or equivalent).
6.3 Spatula - stainless steel or Teflon.
6.4 Balances - analytical, capable' of accurately weighing ± 0.0001 g, and
one capable of weighing 100 g to ± 0.01 g. The balances must be
calibrated with class S weights or known reference weights once per each
D-7/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 6
Equipment and Supplies
12-hour work shift. The balances must be calibrated with class S
weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
6.5 Ultrasonic Cell Disrupters - Heat Systems, Ultrasonics Inc., Model W-385
Sonicator (475 watt with pulsing capability, No.200, M inch tapped
disrupter horn, No. 419, 1/8 inch standard tapered Microtip probe, and .
No. 305, 3/4 inch tapped high gain "Q" disruptor horn, or No. 208 3/4
inch standard solid disruptor horn), or equivalent devices with a
minimum of 375 watt output capability. NOTE: In order to ensure that
sufficient energy is transferred to the sample during extraction, the
Microtip probe or horn shall be replaced if the tip begins to erode.
Erosion of the tip is evidenced by a rough surface. .
6.6 Sonabox Acoustic Enclosure (or equivalent) - for use with disruptor to
decrease noise level.
6.7 Vacuum Filtration Apparatus.
6.7.1 Buchner Funnel. '
6.7.2 Filter Paper - Whatman No. 41 or equivalent.
6J8 Pyrex Glass Wool - rinsed with methylene chloride.
6.9 Test Tube Rack.
6.10 Silicon Carbide Boiling Chips - approximately 10/40 mesh. Heat to 400
°C for 30 minutes or Soxhlet extract with methylene chloride. Teflon
Boiling chips solvent rinsed prior to use are acceptable.
6.11 Water Bath - heated, with concentric ring cover, capable of temperature
control (±2 °C). The bath should be used in a hood.
6.12 Oven - drying.
6.13 Desiccator.
6.14 Crucibles - porcelain.
6.15 Nitrogen Evaporation Device - equipped with a water bath that can be
maintained at 35-40 °C. (N-Evap by Organomation Associates, Inc., South
Berlin, MA, or equivalent). To prevent the release of solvent fumes
into the laboratory, the nitrogen evaporator device must be used in a
hood.
6.16 pH Paper - including narrow range capable of measuring a pH of 2.0.
6.17 pH Meter - with a combination glass electrode, calibrate according to
manufacturer's instructions. The pH meter shall be calibrated prior to
each use.
D-8/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 6
Equipment and Supplies
6.18 GPC Cleanup System
6.18.1 Gel Permeation Chromatography System - GPC Autoprep Model 1002 A or
B, Analytical Biochemical Laboratories, Inc., or equivalent. Systems
that perform satisfactorily have been assembled from the following
components - an HPLC pump, an auto sampler or a valving system with
sample loops, and a fraction collector. All systems, whether
automated or manual, must meet the calibration requirements of
Section 10.3.3.
6.18.2 NOTE: GPC cleanup is required for all soil/sediment extracts, and
for water extracts containing higher molecular weight contaminants
that interfere with the analyses of the target compounds.
6.18.3 Chromatographic Column - 700 mm x 25 mm ID glass column. Flow is
upward. To simplify switching from the UV detector during
calibration to the GPC collection device during extract cleanup, an
optional double 3-way valve (Rheodyne Type 50 Teflon Rotary Valve
#10-262 or equivalent) may be attached so that the column exit flow
can be shunted either to the UV flow-through cell or to the GPC
collection device.
6.18.4 Guard Column (optional) - 5 cm, with appropriate fittings to connect
the inlet side of the analytical column (Supelco 5-8319 or
equivalent) ^
6.18.5 Bio Beads (SX-3) - 200-400 mesh, 70 g (Bio-Rad Laboratories,
Richmond, CA, Catalog 152-2750 or equivalent). An additional 5 g of
Bio Beads are required if the optional guard column is employed. The
quality of Bio Beads may vary from lot to lot because of excessive
fines in some lots. In addition to fines having a detrimental effect
on Chromatography, they can also pass through the column screens and
damage the valve.
6.18.6 Ultraviolet Detector - fixed wavelength (254 nm) with a semi-prep
flow-through cell.
6.18.7 Strip chart recorder, recording integrator, or laboratory data
system.
6.18.8 Syringe Filter Assembly disposable - Bio-Rad "Prep Disc" sample
filter assembly #343-0005, 25 mm, and 5 micron filter discs or
equivalent. Note: Some instrument manufacturers recommend a smaller
micron size filter disc. Consult the instrument operation manual to
determine the proper filter disc to use in the system. Check each
batch for contaminants. Rinse each filter assembly (prior to use)
with methylene chloride if necessary.
6.19 Gas Chromatograph/Mass Spectrometer (GC/MS) System
6.19.1 Gas Chromatograph - The-gas chromatograph (GC) system must be capable
of temperature programming and have a flow controller that maintains
a constant column flow rate throughout the temperature program
operations. The system must be suitable for splitless injection and
have all required accessories including syringes, analytical columns,
D-9/SVOA
OLM04.2
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Exhibit D Semivolatiles -- Section 6
Equipment and Supplies
and gases. All GC carrier gas lines must be constructed from
stainless steel or copper tubing. Non-polytetrafluoroethylene (PTFE)
thread sealants or flow controllers with rubber components are not to
be used.
6.19.2 Gas Chromatography Column - Minimum length 30 m x 0.25 mm ID (or 0.32
mm) bonded-phase silicon coated fused silica capillary column DB-5
(J&W Scientific); RTX-5 (Restek); SPB-5 (Supelco); AT-5 (Alltech);
HP-5 (Hewlett-Packard); CP-Sil 8CB (Chrompack); 007-2 (Quadrexj ; BP-5
(SGE); or equivalent. Note that this is a minimum requirement for
column length. Longer columns may be used. Although a film
thickness of 1.0 micron is recommended because of its larger
capacity, a film thickness of 0.25 micron may be used. A description
of the GC column used for analysis shall be provided in the SDG
Narrative.
6.19.2.1 A capillary column is considered equivalent if:
The column does not introduce contaminants which interfere
with the identification and quantification of the compounds
listed in Exhibit C (Semivolatiles).
The analytical results generated using the column meet the
initial and continuing calibration technical acceptance
criteria listed in the SOW, and the CRQLs listed in Exhibit
C (Semivolatiles) .
The column can accept up to 160 ng of each compound listed
in Exhibit C (Semivolatiles) without becoming overloaded.
The column provides equal or better resolution of the
compounds listed in Exhibit C (Semivolatiles) than columns
listed in Section 6.19.2.
6.19.2.2 As applicable, follow manufacturer's instructions for use of
its product.
6.19.2.3 The Contractor must maintain documentation that the column met
the criteria in Section 6.19.2.1. The minimum documentation is
as follows:
6.19.2.3.1 Manufacturer provided information concerning the performance
characteristics of the column.
6.19.2.3.2 Reconstructed ion chromatograms and data system reports
generated on the GC/MS used for CLP analyses:
From blanks which demonstrate that there are no contaminants
which interfere with the semivolatile analysis when using
the column;
For initial calibration standards.analyzed using the column;
For continuing calibration standards analyzed using the
column.
D-10/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 6
Equipment and Supplies
6.19.2.3.3 Based on the Contractor generated data described in Section
6.19.2.3.2, the Contractor must complete a written review,
signed by the Laboratory Manager certifying that:
The column performance meets the technical acceptance
criteria in Sections 9.3.5 and 9.4.5.
The low point initial calibration standard analysis has
adequate sensitivity to meet the semivolatile CRQLs.
The high point initial calibration standard analysis was not
overloaded.
The column does not introduce contaminants which interfere
with the identification and/or quantitation of compounds
listed in Exhibit C (Semivolatiles).
6.19.2.4 The documentation must be made available to the Agency during
on-site laboratory evaluations or sent to the Agency upon
request of the Technical Project Officer or the Administrative
Project Officer.
6.19.2.5 Packed columns cannot be used.
6.19.3 Mass Spectrometer - must be capable of scanning from 35 to 500 amu
every 1 second or less, utilizing 70 volts (nominal) electron energy
in the electron impact ionization mode, and producing a mass spectrum
which meets the tuning acceptance criteria when 50 ng of
decafluorotriphenylphosphine (DFTPP) is injected through the GC
inlet. The instrument must be vented to the outside of the facility
or to a trapping system which prevents the release of contaminants
into the instrument room.
6.19.4 GC/MS interface - any gas chromatograph to mass spectrometer
interface which provides acceptable sensitivity at contract required
quantitation limits. Gas chromatograph to mass spectrometer
interfaces constructed of all-glass or glass-lined materials are
recommended. Glass can be deactivated by silanizing with
dichlorodimethylsilane.
6.19.5 Data system - a computer system interfaced to the mass spectrometer
that allows the continuous acquisition and storage on machine-
readable media of all mass spectra obtained throughout the duration
of the chromatographic program. The computer must have
software that allows searching any GC/MS data file for ions of a
specified mass and plotting such ion abundance versus time or scan
number. This type of plot is defined as an Extracted Ion Current
Profile (EICP). Software must also be available that allows
integrating the abundance in any EICP between specified time or scan
number limits. Also, for the non-target compounds, software must be
available that allows for the comparison of sample spectra against
reference library spectra. The NIST/EPA/NIH (May 1992 release or
later)and/or Wiley (1991 release or later) or equivalent mass
spectral library shall be used as the reference library. The
operational data system must be able to flag the data files that have
D-11/SVOA OLM04.2
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Exhibit D Semivblatiles -- Section 6
Equipment and Supplies
been edited manually by laboratory personnel.
6.19.6 Magnetic tape storage device - must be capable of recording data and
suitable for long-term, off-line storage of GC/MS data.
D-12/SVOA OLM04.2
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7.0
Exhibit D Semivolatiles -- Section 7
Reagents and Standards
REAGENTS AND STANDARDS
7.1 Reagents
7.1.1 Reagent Water - defined as water in which an interferant is not
observed at or above the CRQL for each analyte of interest. Reagent
water may be generated by passing tap water through a carbon filter
bed containing about 453 g of activated carbon (Calgon Corp.,
Filtrasorb - 300 or equivalent).
7.1.2 Sodium Thiosulfate - (ACS) granular.
7.1.3 Sulfuric Acid Solution (H2SO4) - (1+1) slowly add 50 mL of
concentrated H2S04 (sp. gr. 1.84; 18 N) to 50 mL of reagent water.
7.1.4 Acetone, methanol, methylene chloride, iso-octane, 2-propanol, and
toluene - pesticide residue analysis grade or equivalent.
7.1.5 Sodium Sulfate - powdered or granular anhydrous reagent grade, heated
at 400 °C for four hours in a shallow tray, cooled in a desiccator,
and stored in a glass bottle (Baker anhydrous powder; catalog #73898;
Baker anhydrous granulated, catalog #3375; or equivalent). Caution:
An open container of sodium sulfate may become contaminated during
storage in the laboratory.
7.1.6 Sodium Sulfite - reagent grade.
7.2 Standards
7.2.1
Introduction
7.2.2
The Contractor must provide all standards to be used with this
contract. These standards may be used only after they have been
certified according to the procedure in Exhibit E. The Contractor
must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must be retained by the
Contractor and presented upon request.
Stock Standard Solutions
7.2.2.1 Stock standard solution may be purchased or prepared using the
following procedure.
7.2.2.1.1 Prepare stock standard solutions by accurately weighing about
0.0100 g of pure material. Dissolve the material in methylene
chloride or another suitable solvent and dilute to volume in a
10 mL volumetric flask. Larger volumes may be used at the
convenience of the analyst.
7.2.2.1.2 When compound purity is assayed to be 97.0 percent or greater,
the weight may be used without correction to calculate the
concentration of the stock solution. If the compound purity is
assayed to be less than 97.0 percent, the weight must be
corrected when calculating the concentration of the stock
solution. See Exhibit E (Analytical Standards Requirements).
D-13/SVGA
OLM04.2
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Exhibit D Semivolatiles -- Section 7
Reagents and Standards
7.2.2.1.3 Fresh stock standards must be prepared once every twelve
months, or sooner if standards have degraded or concentrated.
Stock standards must be checked for signs of degradation or
concentration just prior to preparing secondary dilution and
working standards from them.
7.2.3 Secondary Dilution Standards
(
7.2.3.1 Using stock standards, prepare secondary dilution standards in
methylene chloride that contain the compounds of interest either
singly or mixed together.
7.2.3.2 Fresh secondary dilution standards must be prepared once every
twelve months, .or sooner if standards have degraded or
concentrated. Secondary dilution standards must be checked for
signs of degradation or concentration just prior to preparing
working standards from them.
7.2.4 Working Standards
7.2.4.1 Surrogate Standard Spiking Solution
Prepare a surrogate standard spiking solution that contains
nitrobenzene-d5, terphenyl-d!4, 2-fluorobiphenyl, and 1,2-
dichlorobenzene-d4 at a concentration of 100 ug/mL; phenol-d5,
2,4, 6-tribromophenol, 2-fluorophenol, and 2-chlorophenol-d4 at a
concentration of 150 ug/mL. Surrogate standards are added to all
samples and calibration solutions. Additional surrogates may be
added at the laboratory's discretion.
7.2.4.2 Matrix Spiking Solution
7.2.4.2.1 The matrix spiking solution consists of the following:
Bases/Neutrals Acids
Acenaphthene Pentachlorophenol
2,4-Dinitrotoluene Phenol
Pyrene 2-Chlorophenol
N-Nitroso-di-n-propylamine 4-Chloro-3-methylphenol
4-Nitrophenoi
7.2.4.2.2 Prepare a spiking solution that contains each of the
base/neutral compounds above at 100 ug/mL in methanol and the
acid compounds at 150 pg/mL in methanol.
7.2.4.3 GPC Calibration and GPC Continuing Calibration Verification
Solution
D-14/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 7
Reagents and Standards
7.2.4.3.1 Prepare a calibration solution in methylene chloride containing
the following analytes at the minimum concentration listed (in
elution order):
Compound Concentration (mg/mL)
Corn oil 25.0
bis(2-ethylhexyl)phthalate O.5
Methoxychlor 0.1
Perylene 0.02
Sulfur 0.08
7.2.4.3.2 NOTE: Sulfur is not very soluble in methylene chloride, but it
is soluble in warm corn oil. Therefore, one approach is to
weigh out the corn oil, warm it, and transfer the weighed
amount of sulfur into the warm corn oil. Mix it and then
transfer into a volumetric flask with methylene chloride, along
with the other calibration compounds.
7.2.4.4 Instrument Performance Check Solution
Prepare a solution of decafluorotriphenylphosphine (DFTPP),
such that a 2 uL injection will contain 50 ng of DFTPP. The
DFTPP may also be included in the calibration standards at this
level.
7.2.4.5 Initial and Continuing Calibration Solutions
7.2.4.5.1 Prepare calibration standards at a minimum of five
concentration levels (20, 50, 80, 120, and 160 total ng per 2
uL). Each calibration standard should contain each compound of
interest and each surrogate. Eight compounds (2,4-
Dinitrophenol, 2,4,5-Trichlorophenol, 2-Nitroaniline, 3-
Nitroaniline, 4-Nitroaniline, 4-Nitrophenol, 4,6-Dinitro-2-
methylphenol, and Pentachlorophenol) will require only a four-
point initial calibration at 50, 80, 120, and 160 total ng per
2 uL since detection at less than 50 ng per injection is
difficult.
7.2.4.5.2 In order to facilitate the confirmation of single component
pesticides from the semivolatile library search data (see
Exhibit D (Pesticides/Aroclors), Section 12.1.2), the
laboratory may include the single component pesticide target
compounds listed in Exhibit C in the semivolatile continuing
calibration standard. The laboratory may add any or all of
these compounds to the semivolatile continuing calibration
standard, but at a concentration of 10 ng/uL or less. Do not
include the Aroclors or toxaphene mixtures in the semivolatile
initial and continuing calibration standards. If added to this
GC/MS standard, these additional analytes are not reported on
the semivolatile calibration form (Form VII), but must be
included in the quantitation report for the continuing
calibration standard. As only a single point calibration would
be performed, no %RSD or percent difference criteria would
apply to these additional analytes.
.D-15/SVOA OLM04.2
-------
Exhibit D Semiyolatiles -- Section 7
Reagents and Standards
7.2.4.5.3 The 50 ng/2 uL calibration standard is the continuing
calibration standard.
7.2.4.6 Internal Standard Solution
An internal standard solution can be prepared by dissolving 100 mg
of each of the following compounds in 15 mL of methylene chloride:
1,4-dichlorobenzene-d4, naphthalene-d8, acenaphthene-dlO,
phenanthrene-dlO, chrysene-d!2 and perylene-d!2. It may be
necessary to use 5.0 to 10.0 percent toluene in this solution and
a few minutes of ultrasonic mixing in order to dissolve all the
constituents. The resulting solution will contain each standard
at a concentration of 2000 ng/uL. A 10 uL portion of this
solution should be added to each 1 mL of sample extract just prior
to analysis by GC/MS. This will result in 40 ng of each internal
standard in the 2 uL volume of extract injected into the GC/MS.
NOTE: For automated systems using an injection volume of less
than 10 uL, the internal standard solution may need to be prepared
at a different concentration. Prepare the internal standard
solution such that the aliquot used by the system maintains the
required 40 ng of each internal standard in the 2 uL volume of
extract injected into the GC/MS.
7.2.5 Ampulated Standard Extracts
Standard solutions purchased from a chemical supply house as
ampulated extracts in glass vials may be retained and used until the
expiration date provided by the manufacturer. If no manufacturer's
expiration date is provided, the standard solutions as ampulated
extracts may be retained and used for 2 years from the preparation
date. Standard solutions prepared by the Contractor which are
immediately ampulated in glass vials may be retained for 2 years from
the preparation date. Upon breaking the glass seal, the expiration
times listed in Sections 7.2.2.1.3, 7.2.3.2, and 7.3.3 will apply.
The Contractor is responsible for assuring that the integrity of the
standards have not degraded (see Section 7.3.5).
7.3 Storage of Standard Solutions
7.3.1 Store the stock and secondary dilution standard solutions at
| 4°C (± 2°C) in Teflon-lined screw-cap amber bottles. Fresh standards
should be prepared every twelve months at a minimum.
| 7.3.2 Store the working standards at 4°C (± 2°C) in Teflon-sealed
containers. The solution should be checked frequently for stability.
These solutions must be replaced after twelve months, or sooner if ,
comparison with quality control check samples indicates a problem.
7.3.3 The continuing calibration standard (50 ng) should be prepared weekly
| and stored at 4 °C (± 2°C). Refrigeration of the GPC calibration
solution may cause the corn oil to precipitate. Before use, allow
the solution to stand at room temperature until the corn oil
dissolves. Replace this calibration solution every six months, or
more frequently if necessary.
. D-16/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 7
Reagents and Standards
7.3.4 Protect all standards from light. Samples, sample extracts, and
standards must be stored separately.
7.3.5 The Contractor is responsible for maintaining the integrity of
standard solutions and verifying prior to use. Storage of standard
solutions in the freezer may cause some compounds to precipitate.
This means, at a minimum, the standards must be brought to room
temperature prior to use, checked for losses, and checked that all
components have remained in solution. Additional steps may be
necessary to ensure all components are in solution.
D-17/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 8
Sample Collection, Preservation, and Storage
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 Sample.Collection and Preservation
8.1.1 Water samples may be collected in 1 L (or 1 quart) amber glass
containers, fitted with screw-caps lined with Teflon. If amber
containers are not available, the samples should be protected from
light. Soil samples may be collected in glass containers or closed
end tubes (e.g., brass sleeves) in sufficient quantity to perform the
analysis. The specific requirements for site.sample collection are
outlined by the Region.
8.1.2 All samples must be iced or refrigerated at 4 °C (±2 °C) from the
time of collection until extraction.
8.2 Procedure for Sample Storage
8.2.1 The samples must be protected from light and refrigerated at
4 °C (±2 °C) from the time of receipt until 60 days after delivery of
a complete, reconciled data package to the Agency. After 60 days the
samples may be disposed of in a manner that complies with all
applicable regulations.
8.2.2 The samples must be stored in an atmosphere demonstrated to be free
of all potential contaminants.
8.3 Procedure for Sample Extract Storage
| 8.3.1 Sample extracts must be protected from light and stored at 4°C
| (± 2°C) until 365 days after delivery of a reconciled, complete data
package to the Agency.
8.3.2 Samples, sample extracts, and standards must be stored separately.
8.4 Contract Required Holding Times
8.4.1 Extraction of water-samples by continuous liquid-liquid procedures
shall be started within 5 days of Validated Time of Sample Receipt
(VTSR). Extraction of soil/sediment samples by sonication procedures
shall be completed within 10 days of VTSR. NOTE: Separatory funnel
extraction procedures are not permitted.
8.4.2 As part of the Agency's QA program, the Agency may provide
Performance Evaluation (PE) samples as standard extracts which the
Contractor is required to prepare per the instructions provided by
| the Agency. PE samples must be prepared and analyzed concurrently
| with the samples in the SDG. The extraction holding time (5 days
after VTSR for water and 10 days after VTSR for soil/sediment) does
not apply to PE samples received as standard extracts.
8.4.3 Extracts of water and soil/sediment samples must be analyzed within
40 days following extraction.
D-18/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
Instrument Operating Conditions/GC/MS Calibration and Ion Abundance
9.0 CALIBRATION AND STANDARDIZATION
9.1 Instrument Operating Conditions
9.1.1 Gas Chromatograph
9.1.1.1 The following are the gas chromatographic analytical condition.
The conditions are recommended unless otherwise noted.
Initial Column Temperature Hold 40 °C for 4 minutes
Column Temperature Program 40-270 °C at 10 °C/min.
Final Column Temperature Hold 270 °C;
Hold Required: 3 minutes
after all compounds listed
in Exhibit C (SVOA). have
eluted
Injector Temperature 250-300 °C
Transfer Line Temperature 250-300 °C
Source Temperature According to manufacturer's
specifications
Injector Grob-type, splitless
Sample Volume 2 uL
Carrier Gas Helium at 30 cm/sec
9.1.1.2 Optimize GC conditions for analyte separation and sensitivity.
Once optimized, the same GC conditions must be used for the
analysis of all standards, samples, blanks, matrix spikes, and
matrix spike duplicates.
9.1.2 Mass Spectrometer
The following are the required mass spectrometer analytical
conditions:
Electron Energy 70 volts (nominal)
Mass Range 35 to 500 emu
Scan Time Not to exceed 1 second per
scan
9.2 GC/MS Mass Calibration (Tuning) and Ion Abundance
9.2.1 Summary of GC/MS Instrument Performance Check
The GC/MS system must be tuned to meet the manufacturer's
specifications, using a suitable calibration such as perfluoro-tri-n-
butylamine (FC-43) or perfluorokerosene (PFK). The mass calibration
and resolution of the GC/MS system are verified by the analysis of
the instrument performance check solution (Section 7.2.4.4). Prior
to the analysis of any samples, including matrix spike/matrix spike
duplicates, blanks, or calibration standards, the Contractor must
establish that the GC/MS system meets the mass spectral ion abundance
criteria for the instrument performance check solution containing
decafluorotriphenylphosphine (DFTPP).
D-19/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
GC/MS Calibration and Ion Abundance
9.2.2 Frequency of GC/MS Instrument Performance Check
9.2.2.1 The instrument performance check solution must be analyzed once at
the beginning of each 12-hour period during which samples or
standards are analyzed.
9.2.2.2 The 12-hour time period for a GC/MS system instrument performance
check and standards calibration (initial or continuing calibration
criteria) begins at the moment of injection of the DFTPP analysis
that the laboratory submits as documentation of a compliant
instrument performance check. The time period ends after 12 hours
have elapsed according to the system clock.
9.2.3 Procedure for GC/MS Instrument Performance Check
The analysis of the instrument performance check solution may be
performed as an injection of up to 50 ng of DFTPP into the GC/MS or
by adding 50 ng of DFTPP to the calibration standards (Section
7.2.4.5) and analyzing the calibration standard.
9.2.4 Technical Acceptance Criteria for GC/MS Instrument Performance Check
9.2.4.1 The GC/MS system must be tuned at the frequency described in
Section 9.2.2.
9.2.4.2 The abundance criteria listed in Table 1 must be met for a 50 ng
injection of DFTPP. The mass spectrum of DFTPP must be acquired
in the following manner: Three scans (the peak apex scan and the
scans immediately preceding and following the apex) are acquired
and averaged. Background subtraction is required, and must be
accomplished using a single scan acquired no more than 20 scans
prior to the elution of DFTPP. Do not subtract part of the DFTPP'
peak. NOTE: All subsequent standards, samples, MS/MSD, and
blanks associated with a DFTPP analysis must use the identical
mass spectrometer instrument conditions.
9.2.5 Corrective Action for GC/MS Instrument Performance Check
9.2.5.1 If the DFTPP acceptance criteria are not met, re-tune the GC/MS
system. It may be necessary to clean the ion source, clean
quadrupoles, or take other actions to achieve the technical
acceptance criteria.
9.2.5.2 DFTPP acceptance criteria MUST be met before any standards,
samples, including MS/MSD, or required blanks are analyzed. Any
standards, samples, or required blanks analyzed when tuning
technical acceptance criteria have not been met will require
reanalysis at no additional cost to the Agency.
D-20/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
Initial Calibration
9.3 Initial Calibration
9.3.1 Summary of Initial Calibration ., _. . __..._.
Prior to the analysis of samples and required blanks, and after the
instrument performance check solution criteria have been met, each
GC/MS system must be calibrated at a minimum of five concentrations
(Section 7.2.4.5) to determine instrument sensitivity and the
linearity of GC/MS response for the semivolatile target and surrogate
compounds.
9.3.2 Frequency of Initial Calibration
9.3.2.1 Each GC/MS system must be initially calibrated>upon award of the
contract, whenever the Contractor takes corrective action which
may change or affect the initial calibration criteria (e.g., ion
source cleaning or repairs, column replacement, etc.), or if the
continuing calibration technical acceptance criteria have not been
met.
9.3.2.2 If time still remains in the 12-hour time period after meeting the
technical acceptance criteria for the initial calibration, samples
may be analyzed. It is not necessary to analyze a continuing
calibration standard within this 12-hour time period, if the
initial calibration standard that is the same concentration as the
continuing calibration standard meets the continuing calibration
technical acceptance criteria. Quantitate all sample and quality
control sample results and quality control criteria results, such
as internal standard area response change and retention time
shift, against the initial calibration standard that is the same
concentration as the continuing calibration standard (50 ng/2 uL).
9.3.3 Procedure for Initial Calibration
9.3.3.1 All standard/spiking solutions and blanks must be allowed to warm
to ambient temperature (approximately 1 hour) before preparation
or analysis.
9.3.3.2 Prepare five calibration standards containing all the semivolatile
target and surrogate compounds at the concentrations described in
Section 7.2.4.5.
9.3.3.3 Add a 10 uL aliquot of internal standard solution (Section
7.2.4.6) to 1 tnL aliquot of calibration standards to result in 40
ng of internal standard in the 2 uL volume of calibration standard
injected onto the GC/MS. The internal standards specified in
Section 7.2.4.6 should permit most of the semivolatile target
compounds to have relative retention times of 0.80 to 1.20, using
the assignments of internal standards to target compounds given in
Table 2.
9.3.3.4 Analyze each calibration standard by injecting 2.0 uL of standard.
D-21/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 9 -^
Calibration and Standardization
Initial Calibration
9.3.4 Calculations for Initial Calibration
9.3.4.1 Calculate the relative response factors (RRF) for each
semivolatile target and surrogate compound using Equation 1 and
the primary characteristic ions found in Table 3 (Internal
Standards) and Table 4 (Target Compounds and Surrogates). Assign
the target compounds and surrogate to the internal standard
according to Table 2. For internal standards, use the primary ion
listed in Table 3 unless interferences are present. If
interferences prevent the use of the primary ion for a given
internal standards, use the secondary ion(s) listed in Table 3;
NOTE: Unless otherwise stated the area response of the primary
characteristic ion is the quantitation ion.
EQ.
RRF = x !
A. C
Where,
Ax = Area of the characteristic ion for the compound to be
measured (see Table 4) .
Ais = Area of the characteristic ion for specific internal
standard (see Table 3) .
Cis = Amount of the internal standard injected (ng).
Cx = Amount of the compound to be measured injected (ng).
9.3.4.2 The mean relative response factor (RRF) must be calculated for all
compounds. Calculate the % Relative Standard Deviation (%RSD) of
the RRF values for the initial calibration using the following
equation:
EQ. 2
Standard Deviation
%RSD =
Mean
Where,
£ (x/-x):
Standard Deviation =
Xt = each individual value used to calculate the mean.
x = the mean of n values.
n = the total number of values.
D-22/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
Continuing Calibration
9.3.5 Technical Acceptance Criteria for Initial Calibration
9.3.5.1 All initial calibration standards must be analyzed at the
concentration levels described in Section 7.2.4.5 and at the
frequency described in Section 9.3.2 on a GC/MS system meeting the
DFTPP technical acceptance criteria.
9.3.5.2 The relative response factor (RRF) at each calibration
concentration for each semivolatile target and surrogate compound
must be greater than or equal to the compound's minimum acceptable
relative response factor listed in Table 5.
9.3.5.3 The %RSD over the initial calibration range for relative response
factor for each semivolatile and surrogate compound that has a
required %RSD must be less than or equal to the %RSD listed in
Table 5.
9.3.5.4 Up to four compounds may fail to meet the criteria listed in Table
5. However, these four compounds must meet a minimum RRF
criterion of 0.010 and have a %RSD less than or equal to 40.0
percent.
9.3.5.5 Excluding those ions in the solvent front, no quantitation ion may
saturate the detector, with the exception of quantitation ions in
up to 3 compounds (including internal standards and surrogates)
from the high standard (160 ng/2 pL). Consult the manufacturer's
instrument manual to determine how saturation is indicated for
your instrument.
9.3.6 Corrective Action for Initial Calibration
9.3.6.1 If any technical acceptance criteria for initial calibration are
not met, inspect the system for problems. It may be necessary to
clean the ion source, change the column, or take other corrective
actions to achieve the acceptance criteria.
9.3.6.2 Initial calibration technical acceptance criteria must be met
before any samples, including matrix spike/matrix spike duplicates
or required blanks, are analyzed. Any samples, including matrix
spike/matrix spike duplicates or required blanks, analyzed when
initial calibration technical acceptance criteria have not been
met will require reanalysis at no additional cost to the Agency.
9.4 Continuing Calibration
9.4.1 Summary of Continuing Calibration
Prior to the analysis of samples, including MS/MSD and required
blanks, and after tuning criteria and initial calibration criteria
have been met, each GC/MS system must be routinely checked by
analyzing a continuing calibration standard to ensure that the
instrument continues to meet the instrument sensitivity and linearity
requirements of the SOW. The continuing calibration standard
contains all the semivolatile target and surrogate compounds and
- - D-23/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
Continuing Calibration
internal standards.
9.4.2 Frequency of Continuing Calibration
9.4.2.1 Each GC/MS used for analysis must be calibrated once every 12-hour
time period of operation. The 12-hour time period begins with the
injection of DFTPP.
9.4.2.2 If time still remains in the 12-hour time period after meeting the
technical acceptance criteria for the initial calibration, samples
may be analyzed. It is not necessary to analyze a continuing
calibration standard within this 12-hour time period if the
initial calibration standard that is the same concentration as the
continuing calibration standard meets the continuing calibration
technical acceptance criteria. Quantitate all sample results
against the initial calibration standard that is the same
concentration as the continuing calibration standard (50 ng/2 uL).
9.4.3 Procedure for Continuing Calibration
9.4.3.1 All standard/spiking solutions and blanks must be allowed to warm
to ambient temperature (approximately 1 hour) before preparation
or analysis.
9.4.3.2 Add a 10 uL aliquot of internal standard solution (Section
7.2.4.6) to 1 mL aliquot of continuing calibration standard to
result in 40 ng of internal standard in the 2 uL volume of
calibration standard injected onto the GC/MS. The internal
standards specified in. Section 7.2.4.6 should permit most of the
semivolatile target compounds to have relative retention times of
0.80 to 1.20, using the assignments of internal standards to
target compounds given in Table 2.
9.4.3.3 Analyze the continuing calibration standard by injecting 2.0 uL of
standard.
9.4.4 Calculations for Continuing Calibration
9.4.4.1 Calculate a relative response factor (RRF) for each semivolatile
target and surrogate compound using Equation 1 and the primary
characteristic ions found in Table 3 (Internal Standards) and
Table 4 (Target Compounds and Surrogates). For internal
standards, use the primary ions listed in Table 3 unless
interferences are present. If interferences prevent the use of
the primary ion for a given internal standard, use the secondary
ion(s) listed in Table 3.
D-24/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 9
Calibration and Standardization
Continuing Calibration
9.4.4.2 Calculate the percent difference between the mean relative
response factor from the most recent initial calibration and the
continuing calibration relative response .factor for each
semivolatile target and surrogate compound using Equation 3.
EQ. 3.
RRF - RRF.
% Difference,. = ----- x 100
*** RRF.
.
Where,
RRF. = Mean relative response factor from the most recent
initial calibration meeting technical acceptance
criteria.
RRFC = Relative response factor from continuing calibration
standard.
9.4.5 Technical Acceptance Criteria for Continuing Calibration
9.4.5.1 The continuing calibration standard must be analyzed at the 50
ng/2 uL concentration level at the frequency described in Section
9.4.2, on a GC/MS system meeting the DFTPP tuning and the initial
calibration technical acceptance criteria.
9.4.5.2 The relative response factor (RRF) for each semivolatile target
and surrogate compound must be greater than or equal to the
compound's minimum acceptable relative response factor listed in
Table 5.
9.4.5.3 The relative response factor percent difference for each
semivolatile target and surrogate compound that has a percent
difference criteria must be within the inclusive range listed in
Table 5.
9.4.5.4 Up to four semivolatile target compounds may fail to meet the
minimum RRF or maximum percent difference criteria listed in Table
5, but the RRFs of those four compounds must be greater than or
equal to 0.010, and the percent differences must be within the
inclusive range of ± 40.0 percent.
9.4.5.5 Excluding those ions in the solvent front, no quantitation ion may
saturate the detector. Consult the manufacturer's instrument
operating manual to determine how saturation is indicated for your
instrument.
9.4.6 Corrective Action for Continuing Calibration
9.4'.6.1 If any continuing calibration technical acceptance criteria are
1 not met, recalibrate the GC/MS instrument according to Section
9.3.3. It may be necessary to clean the ion source, change the
column, or take other corrective actions to achieve the continuing
calibration technical acceptance criteria.
D-25/SVOA OLM04.2
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Exhibit D Seraivolatiles -- Section 9
Calibration and Standardization
Continuing Calibration
9.4.6.2 Continuing calibration technical acceptance criteria MUST be met
before any samples, including MS/MSD or required blanks, are
analyzed. Any samples, including MS/MSD or required blanks,
analyzed when continuing calibration criteria have not been met
will require reanalysis at no additional cost to the Agency.
D-26/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 10
Procedure
Sample Preparation
10.0 PROCEDURE.
10.1 Sample Preparation
10.1.1 If sufficient sample amount (less than 90% of the required amount) is
received to perform the analyses, the Contractor shall contact SMO to
apprise them of the problem. SMO will contact the Region for
instructions. The Region will either require that no sample analyses
be performed, or will require that a reduced volume be used for the
sample analysis. No other changes in the analyses will be permitted.
The Contractor shall document the Region's decision in the SDG
Narrative.
10.1.2 If multiphase samples (e.g., a two-phase liquid sample, oily
sludge/sandy soil sample) are received by the Contractor, the
Contractor shall contact SMO to apprise them of the type of sample
received. SMO will contact the Region. If all phases of the sample
are amenable to analysis, the Region may require the Contractor to do
any of the following:
Mix the sample and analyze an aliquot from the homogenized sample.
Separate the phases of the sample and analyze each phase
separately. SMO will provide EPA sample numbers for the
additional phases.
Separate the phases and analyze one or more of the phases, but not
all of the phases. SMO will provide EPA sample numbers for the
additional phases, if required.
Do not analyze the sample.
10.1.2.1 If all of the phases are not amenable to analysis (i.e.,
outside scope), the Region may require the Contractor to do any
of the following:
Separate the phase(s) and analyze the phase(s) that is
amenable to analysis. SMO will provide EPA sample numbers
for the additional phases, if required.
Do not analyze the sample.
10:1.2.2 No other change in the analyses will be permitted. The
Contractor shall document the Region's decision in the SDG
Narrative.
10.1.3 Water Sample
10.1.3.1 Continuous liquid-liquid extraction is used to extract the
samples. Separatory funnel extraction or other manual
extraction techniques cannot be used.
10.1.3.2 Continuous Liquid-Liquid Extraction Without Hydrophobic
Membrane
D-27/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 10
Procedure
Sample Preparation
10.1.3.2.1 Follow manufacturer's instructions for set-up.
10.1.3.2.2 Add methylene chloride to the bottom of the extractor and
fill it to a depth of at least one inch above the bottom
sidearm.
10.1.3.2.3 Measure out a 1 L sample aliquot in a separate, clean
graduated cylinder; transfer the aliquot to the continuous
extractor. Measure and record the initial pH of the sample
with a pH meter or narrow range pH paper. Adjust the pH to
2.0 with 1:1 H2SO4 and record the final pH. NOTE: With
some samples, it may be necessary to place a layer of glass
wool between the methylene chloride and the water layer in
the extractor, to prevent precipitation of suspended solids
into the methylene chloride during extraction.
10.1.3.2.4 Using a syringe or volumetric pipet, add 0.5 mL of the
surrogate standard spiking solution (Section 7.2.4.1) into
the sample and mix well.
10.1.3.2.5 Rinse the graduated cylinder with 50 mL of methylene '
chloride and transfer the rinsate to the continuous
extractor. If the sample was received in a 1 L container,
rinse the empty container with 50 mL of methylene chloride
and add rinsate to the continuous extractor.
10.1.3.2.6 Add sufficient methylene chloride to the continuous
extractor to ensure proper solvent cycling during operation.
Adjust the drip rate to 5 to 15 mL/minute (recommended);
optimize the extraction drip rate. Extract for a minimum of
18 hours. NOTE: When a minimum drip rate of 10-15 mL/min
is maintained throughout the extraction, the extraction time
may be reduced to a minimum of 12 hours. Allow to cool then
detach the distillation flask. Proceed to Section 10.2.
10.1.3.2.7 NOTE: Some continuous liquid-liquid extractors are also
capable of concentrating the extract within the extraction
set-up. Follow the manufacturer's instructions for
concentration when using this type of extractor.
10.1.3.3 Continuous Liquid-Liquid Extraction With Hydrophobic Membrane
10.1.3.3.1 Follow the manufacturer's instructions for set-up.
10.1.3.3.2 Measure out each 1 L sample aliquot in a separate, clean
graduated cylinder. If the sample was received in a 1 L
container, rinse the empty container with 50 mL of methylene
chloride and add the rinsate to the continuous extractor.
If the sample was not received in a 1 L container, add 50 mL
of methylene chloride to the continuous extractor. Slowly
transfer the aliquot to the continuous extractor. Measure
and record the initial pH of the sample with a pH meter or
narrow range pH paper. Adjust the pH to 2.0 with 1:1 H 2SO4
D-28/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 10
Procedure
Sample Preparation
and record the final pH.
10 .-1.3.3.3 Using a syringe or volumetric pipet, add 0.5 mL of the
surrogate standard spiking solution (Section 7.2.4.1) into
the sample and mix well.
10.1.3.3.4 Rinse the graduated cylinder with 50 mL of methylene
chloride and transfer the rinsate to the continuous
extractor.
10.1.3.3.5 Add sufficient methylene chloride to the continuous
extractor to ensure proper solvent cycling during operation.
Adjust the drip rate to 15 mL/minute (recommended); optimize
the extraction drip rate. Extract for a minimum of 6 hours.
(NOTE: Due to the smaller volume of solvent used during the
extraction process, some sample matrices (e.g., oily
samples, samples containing a high concentration of
surfactants) may create an emulsion which will consume the
solvent volume, preventing the efficient extraction of the
sample. When this occurs, add additional solvent to assure
efficient extraction of the sample and extend the extraction
time for a minimum of 6 hours. If the sample matrix
prevents the free flow of solvent through the membrane, then
the non-hydrophobic membrane continuous liquid-liquid type
extractor must be used.) Allow to cool, then detach the
distillation flask. Proceed to Section 10.2.
10.1.3.3.6 NOTE: Some continuous liquid-liquid extractors are also
capable of concentrating the extract within the extraction
set-up. Follow the manufacturer's instructions for
concentration when using this type of extractor. Using the
hydrophobic membrane type extractor, it may not be necessary
to dry the extract with sodium sulfate.
10.1.3.4 NOTE: If low surrogate recoveries occur, assure: 1) the
apparatus was properly assembled to prevent leaks; 2) the drip
rate/solvent cycling was optimized; and 3) there was proper
cooling for condensation of solvent.
10.1.3.5 NOTE: Alternate continuous liquid-liquid extractor types that
meet the requirements of the SOW may also be used. If using
alternate extractors or design types follow the manufacturer's
instruction for set-up.
10.1.4 Soil/Sediment Samples
Decant and discard any water layer on a sediment sample. Mix samples
thoroughly, especially composited samples. Discard any foreign
objects such as sticks, leaves, and rocks.
D-29/SVOA OLM04.2
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Exhibit D Semivolatiles --. Section 10
Procedure
Sample Preparation
10.1.4.1 pH Determination
Transfer 50 g of soil/sediment to a 100 mL beaker. Add 50 mL
of water and stir for 1 hour. Determine pH of sample with a pH
meter while stirring. Report pH value on appropriate data
sheets. If the pH of the soil/sediment is greater than 11 or
less than 5, document this in the SDG Narrative. Discard this
portion of sample. NOTE: If limited sample volume is
received, use'a smaller 1:1 ratio of grams of soil/sediment
sample to mLs of water for the pH determination. Note this in
the SDG Narrative.
10.1.4.2 Percent Moisture
Immediately after weighing the sample for extraction, weigh 5-
10 g of the soil/sediment into a tared crucible. Determine the
percent moisture by drying overnight at 105 °C. Allow to cool
in a desiccator before weighing. Concentrations of individual
analytes will be reported relative to the dry weight of
soil/sediment.
EQ.4
grams of wi
n Ht-iiTf» =
grams of wet sample
. . grams of wet sample - grams of dry sample
% Moisture = x 100
10.1.4.3 Mandatory Determination of Concentration Level
The Contractor must determine whether a soil/sediment sample
should be analyzed by the low or medium level soil/sediment
method. It is the responsibility of the Contractor to analyze
the sample at the correct level. Three approaches may be taken
to determine whether the low level or medium level method must
be followed.
Assume the sample is low level and analyze a 30 g sample.
Use the screening method in Appendix A to determine the
appropriate method for analysis.
Use other EPA screening procedures or an in-house laboratory
screening procedure. The procedure must be documented and
available for review during on-site laboratory evaluation or
when requested by the Technical Project Officer or
Administrative Project Officer.
10.1.4.4 Low Level Soil/Sediment Samples
The procedure described below is for the extraction of
soil/sediment samples by sonication. The Contractor may also
use Automated Soxhlet Extraction (SW-846 Method 3541
Revision 0, September 1994) or Pressurized Fluid Extraction
{SW-846 Method 3545 Revision 0, December 1996) techniques for
. D-30/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Preparation
soil/sediment samples. The above SN-846 methods are provided
as reference only and the laboratory supplied Standard
Operating Procedures (SOP) -must be-accepted-by the Agency
before the laboratory can utilize these me'thods (See Exhibit E
for required IPR studies). The requirements of this SOW must
be met at all times (i.e., original sample weight). As
applicable, follow manufacturer's instructions for the use of
all extraction equipment. If one of the above alternative
extraction procedures is used, the Contractor must maintain
documentation of the procedure utilized, and document its
equivalence to the sonication procedure described below. If
the sample weight must be adjusted to utilize one of the
alternative extraction procedures, the Contractor shall
immediately contact SMO to inform them of the problem. SMO
will contact the Region for instructions.
NOTE: All soil/sediment samples in a Case must Jbe extracted by
the same procedure.
10.1.4.4.1 The following steps should be performed rapidly to avoid
loss of the more volatile extractables. Weigh approximately
30 g of sample, to the nearest 0.1 g, into a 400 mL beaker
and add 60 g of anhydrous powdered or granulated sodium
sulfate. Mix well. The sample should have a sandy texture
at this point. Add 0.5 mL of the surrogate standard spiking
solution (Section 7.2.4.1) to the sample, then immediately
add 100 mL of 1:1 methylene chloride-acetone.
10.1.4.4.2 Place the bottom surface of the tip of the 3/4 inch tapered
disrupter horn about M inch below the surface of the
solvent, but above the sediment layer.
10.1.4.4.3 Sonicate for 3 minutes using a 3/4 inch disrupter horn at
full power (output control knob at 10) with pulse on and
percent duty cycle knob setat 50.0 percent. Do not use a
microtip. NOTE: These settings refer to the Model W-385.
When using a sonicator other than Model W-385, refer to the ,
instructions provided by the manufacturer for appropriate
output settings. Decant and filter extracts through Whatman
#41 filter paper using vacuum filtration or centrifuge and
'decant extraction solvent.
10.1.4.4.4 Repeat the extraction two more times with 2 additional 100
mL portions of 1:1 methylene chloride-acetone. Before each
extraction, make certain that the sodium sulfate is free-
flowing and not a consolidated mass. As required, break up
large lumps with a clean spatula, or, very carefully, with
the tip of the unenergized probe. Decant the extraction
solvent after each sonication. On the final sonication,
pour the entire sample into the Buchner funnel and rinse
with 1:1 methylene chloride-acetone.
10.1.4.4.5 If the sample is to be screened following the low level
preparation method prior to GPC, refer to Appendix A,
D-31/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Preparation
"Screening of Seraivolatile Organic Extracts."
10.1.4.4.6 After screening, transfer the remainder of the 1 mL back to
the total extract. CAUTION: To minimize sample loss,
autosamplers which pre-flush samples through the syringe,
should not be used.
10.1.4.5 Medium Level Soil/Sediment Samples
The procedure described below is for the extraction of
soil/sediment samples by sonication. The Contractor may also
use Automated Soxhlet Extraction (SH-846 Method 3541
Revision 0, September 1994) or Pressurized Fluid Extraction
(SN-846 Method 3545 Revision 0, December 1996) techniques for
soil/sediment samples. The above SN-846 methods are provided
as reference only and the laboratory supplied Standard
Operating Procedures (SOP) must be accepted by the Agency
before the laboratory can utilize these methods (See Exhibit E
for required IPR studies). The requirements of this SOW must
be met at all times (i.e., original sample weight). As
applicable, follow manufacturer's instructions for the use of
all extraction equipment. If one of the above alternative
extraction procedures is used, the Contractor must maintain
documentation of the procedure utilized, and document its
equivalence to the sonication procedure described below. If
the sample weight must be adjusted to utilize one of the
alternative extraction procedures, the Contractor shall
immediately contact SMO to inform them of the problem. SMO
will contact the Region for instructions.
NOTE: All soils/sediment samples in a Ca.se must be extracted by
the same procedure.
10.1.4.5.1 Transfer approximately 1 g (record weight to the nearest
0.1 g) of sample to a 20 mL vial. Wipe the mouth of the
vial with a tissue to remove any sample material. Record
the exact weight of sample taken. Cap the vial before
proceeding with the next sample to avoid any cross-
contamination.
10.1.4.5.2 Add 2.0 g of anhydrous powdered or granulated sodium sulfate
to the sample in the 20 mL vial and mix well.
10.1.4.5.3 Surrogates are added to all samples, spikes, and blanks.
Add 0.5 mL of surrogate spiking solution (Section 7.2.4.1)
to the sample mixture.
10.1.4.5.4 Immediately add 9.5 mL of methylene chloride to the sample
and disrupt the sample with the 1/8 inch tapered Microtip
ultrasonic probe for 2 minutes at output control setting 5,
in continuous mode (if using a sonicator other than Models
W-375 or W-385, contact the instrument manufacturer for
appropriate output settings). Before extraction, make
certain that the sodium sulfate is free-flowing and not a
. . . D-32/SVOA OLM04.2
-------
Exhibit D Semivolatilss -- Section 10
Procedure
Sample Concentration
consolidated mass. Decant and filter extract through
Whatman #41 filter paper using vacuum filtration or
centrifuge-and decant extraction solvent.-
10.2 Concentrating the Extract
NOTE: Low level soil/sediment samples prepared by the procedure
described in Section 10.1.4.4 will result in extracts containing a
mixture of acetone and methylene chloride. Because all soil/sediment
sample extracts MUST be subjected to GPC cleanup prior to analysis, the
majority of the acetone must be removed from the extract, otherwise, it
will have adverse effects on the GPC column. To remove the acetone from
the soil/sediment sample extract, follow the steps in Section 10.2.1
then concentrate to 1 mL using the nitrogen evaporation technique in
Section 10.2.2.2.
10.2.1 Concentration by K-D
10.2.1.1 Assemble a Kuderna-Danish (K-D) apparatus by attaching a 10 mL
concentrator tube to a 500 mL evaporative flask. Other
concentration devices or techniques may be used in place of the
K-D, if equivalency is demonstrated for all the semivolatile
target compounds listed in Exhibit C.
10.2.1.2 For water samples, transfer the extract to a Kuderna-Danish (K-
D) concentrator by pouring the extract through a drying column
containing about 10 cm of anhydrous granular sodium sulfate.
10.2.1.2.1 For soil/sediment samples, directly transfer the extract to
the K-D concentrator.
10.2.1.2.2 Rinse the Erlenmeyer flasks (for both water and
soil/sediment samples) and the column (for water samples)
with 20-30 mL of methylene chloride to complete the
quantitative transfer.
10.2.1.3 Add one or two clean boiling chips to the evaporative flask and
attach a three-ball Snyder column. Pre-wet the Snyder column
by adding about 1 mL methylene chloride to the top of the
column. Place the K-D apparatus in a hot water bath (60 °C to
70 °C recommended) so that.the concentrator tube is partially
immersed in the hot water and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust the vertical
position of the apparatus and the water temperature as required
to complete the concentration in 10 to 15 Minutes. At the
proper rate of distillation, the balls of the column will
chatter actively, but the chambers will not flood with
condensed solvent. When the apparent volume of liquid reaches
1 mL, remove the K-D apparatus from the water bath and allow it
to drain and cool for at least 10 minutes. DO NOT ALLOW THE
EVAPORATOR TO GO DRY. Remove the Snyder column and rinse the
flask and its lower joint into the concentrator tube with 1 or
2 mL of methylene chloride. A 5-mL syringe is recommended for
this operation.
b-33/SVOA OLM04.2
-------
Exhibit D Semivolatiles. -- Section 10
Procedure
Sample Concentration
10.2.1.4 For water samples which do not require GPC cleanup, proceed to
final concentration of extract (Section 10.2.2). Oily water
samples require GPC.
10.2.1.5 For water samples which require GPC, adjust the volume of the
extract to 10.0 mL with methylene chloride and proceed with GPC
cleanup (Section 10.3).
10.2.1.6 For soil/sediment samples, adjust the volume of the extract to
10.0 mL with methylene chloride, and proceed with GPC cleanup
(Section 10.3).
10.2.1.7 For water samples or soil/sediment samples which have undergone
GPC, proceed to final concentration of extract (Section
10.2.2) .
10.2.2 Final Concentration of Extract
Two different concentration techniques are permitted to obtain the
final extract volume, Micro Snyder column and Nitrogen Evaporation
Techniques:
10.2.2.1 Micro Snyder Column Technique
Add another one or two clean boiling chips to the concentrator
tube and attach a two-ball micro Snyder column. Pre-wet the
Snyder column by adding about 0.5 mL of methylene chloride to
the top of the column. Place the K-D apparatus on a hot water
bath (60 °C to 70 "C recommended) so that the concentrator tube
is partially immersed in the hot water. Adjust the vertical
position of the apparatus and the water temperature as required
to complete the concentration in 5 to 10 minutes. At the
proper rate of distillation, the balls of the column will
chatter actively, but the chambers will not flood with
condensed solvent. When the apparent volume of liquid reaches
about 0.5 mL (0.4 mL for soil/sediment samples or water samples
that have undergone GPC), remove the K-D apparatus from the
water bath and allow it to drain for at least 10 minutes while
cooling. Remove the Snyder column and rinse the evaporative
flask and its lower joint into the concentrator tube with 0.2
mL (O.I mL for soil/sediment samples and water samples that
have undergone GPC) of methylene chloride.- Adjust the final
volume to 1.0 mL (0.5 mL for soil/sediment samples and water
samples that have undergone GPC) with methylene chloride.
Transfer the extract to the Teflon-sealed screw-cap bottle,
label the bottle, and store at 4°C (± 2°C).
10.2.2.2 Nitrogen Evaporation Technique (Taken from ASTM Method D3086)
The following method may be used for final concentration of the
semivolatile extract instead of the procedure in Section
10.2.2.1, Place the concentrator tube in a warm water bath
(30 °C to 35 °C recommended) and evaporate the solvent volume
D-34/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Cleanup.(GPC)
to just below 1 mL (below 0.5 mL for soil/sediment samples and
water samples that have undergone GPC) by blowing a gentle
stream of clean, dry nitrogen (filtered through a column of
activated carbon) above the extract. CAUTION: Gas lines from
the gas source to the evaporation apparatus must be stainless
steal, copper, or Teflon tubing. New plastic tubing must not
be used between the carbon trap and the sample, since it may
introduce interferences. The internal wall of the concentrator
tube must be rinsed down several times with methylene chloride
during the operation. During evaporation, the tube solvent
level must be kept below the water level of the bath. The
extract must never be allowed to become dry.
10.2.2.3 Final Extract Volumes
10.2.2.3.1 Water
For water samples that did not undergo GPC, the extract must
be brought to a final volume of 1.0 mL with methylene
chloride. For water samples that underwent GPC, the extract
must be brought to a final volume of 0.5 mL with methylene
chloride (concentrating the extract to 0.5 mL will result in
no loss of sensitivity despite the volume of extract (5 mL)
not recovered after GPC).
10.2.2.3.2 Soil/Sediment
Adjust the final volume to 0.5 mL with methylene chloride
(concentrating the extract to 0.5 mL will result in no loss
of sensitivity despite the volume of extract (5 mL) not
recovered after GPC).
10.2.2.3.3 Transfer the extract to a Teflon-sealed screw-cap bottle,
label the bottle, and store at 4°C (± 2"C).
10.3 Sample Cleanup by GPC
10.3.1 Introduction
10.3.1.1 Gel Permeation Chromatography (GPC) is a size exclusion cleanup
procedure using organic solvents and hydrophobic gels in the
separation of natural macromolecules. The packing gel is
porous and is characterized by the range or uniformity
(exclusion range) of that pore size. In the choice of gels,
the exclusion range must be larger than the molecular size of
the molecules to be separated.
10.3.1.2 GPC must be performed for all soil/sediment extracts. GPC must
be performed for water extracts that contain higher molecular
weight contaminants that interfere with the analysis of the
target analytes.
D-35/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Cleanup (GPC)
10.3.2 GPC Column Preparation
The instructions listed below for GPC column preparation are for Bio
Beads. Alternative column packings may be used if 1) the column
packings have equivalent or better performance than the Bio Beads and
meet the technical acceptance criteria for GPC calibration and GPC
continuing calibration verification ,2) the column packings do not
introduce contaminants/artifacts into the sample which interfere with
the analysis of the semivolatile compounds. Follow the
manufacturer's instructions for preparation of the GPC column
packing.
10.3.2.1 Weigh out 70 g of Bio Beads (SX-3). Transfer them to a quart
bottle with a Teflon-lined cap or a 500 mL separatory funnel
with a large bore stopcock, and add approximately 300 mL of
methylene chloride. Swirl the container to ensure the wetting
of all beads. Allow the beads to swell for a minimum of 2
hours. Maintain enough solvent to cover the beads sufficiently
at all times. If a guard column is to be used, repeat the
above with 5 g of Bio Beads in a 125 mL bottle or a beaker
using 25 mL of the methylene chloride.
10.3.2.2 Turn the column upside down from its normal position and remove
the inlet bed support plunger (the inlet plunger is longer than
the outlet plunger). Position and tighten the outlet bed
support plunger as near the end as possible, but no closer than
5 cm (measured from the gel packing to the collar).
10.3.2.3 Raise the end of the outlet tube to keep the solvent in the GPC
column, or close the column outlet stopcock. Place a small
amount of solvent in the column to minimize the formation of
air bubbles at the base of poured column packing.
10.3.2.4 Swirl the bead/solvent slurry to get a homogeneous mixture and,
if the wetting was done in a quart bottle, quickly transfer it
to a 500 mL separatory funnel with a large bore stopcock.
Drain the excess methylene chloride directly into the waste
beaker, and start draining the slurry into the column by
placing the separatory funnel tip against the column wall.
This will help to minimize bubble formation. Swirl
occasionally to keep the slurry homogeneous. Drain enough to
fill the column. Place the tubing from .the column outlet into
a waste beaker below the column, open the stopcock (if
attached), and allow the excess solvent to drain. Raise the
tube to stop the flow, and close the stopcock when the top of
the gel begins to look dry. Add additional methylene chloride
to just rewet the gel.
10.3.2.5 .. Wipe any remaining beads and solvent from the inner walls of
the top of the column with a laboratory tissue. Loosen the
seal slightly on the other plunger assembly (long plunger) and
insert it into the column. Make the seal just tight enough so
that any beads on the glass surface will be pushed forward, but
loose enough so that the plunger can be pushed forward.
D-36/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Cleanup (GPC)
CAUTION: Do not tighten the seal if beads are between the seal
and the glass surface because, this can damage the seal and
cause--leakage. ._..... ... _ .
10.3.2.6 Compress the column as much as possible without applying
excessive force. Loosen the seal and gradually pull out the
plunger. Rinse and wipe off the plunger. Slurry any remaining
beads and transfer them into the column. Repeat the step in
Section 10.3.2.5 and reinsert the plunger. If the plunger
cannot be inserted and pushed in without allowing beads to
escape around the seal, continue compression of the beads
without tightening the seal, and loosen and remove the plunger
as described. Repeat this procedure until the plunger is
inserted successfully.
10.3.2.7 Push the plunger until it meets the gel, then compress the
column bed about four centimeters.
10.3.2.8 Pack the optional 5 cm column with approximately 5 g of pre-
swelled beads (different guard columns may require different
amounts). Connect, the guard column to the inlet of the
analytical column.
10.3.2.9 Connect the column inlet to the solvent reservoir (reservoir
should be placed higher than the top of the column) and place
the column outlet tube in a waste container. Placing a
restrictor in the outlet tube will force air out of the column
more quickly. A restrictor can be made from a piece of
capillary stainless steel tubing of 1/16" OD x O.010" ID x 2".
Pump methylene chloride through the column at a rate of 5
mL/min for one hour.
10.3.2.10 After washing the column for at least one hour, connect the
column outlet tube, without the restrictor, to the inlet side
of the UV detector. Connect the system outlet to the outlet
side of the UV detector. A restrictor (same size as the one in
Section 10.3.2.9) in the outlet tube from the UV detector will
prevent bubble- formation which causes a noisy UV baseline.
10.3.2.11 The restrictor will not affect flow rate. After pumping
methylene chloride through the column for an additional 1-2
hours, adjust the inlet bed support plunger until approximately
6-10 psi backpressure is achieved. Push the plunger in to
increase pressure or slowly pull outward to reduce pressure.
10.3.2.12 ' When the GPC column is not to be used for several days, connect
the column outlet line to the column inlet to prevent column
drying and/or channeling. If channeling occurs, the"gel must
be removed from the column, re-swelled', and re-poured as
described above. If drying occurs, methylene chloride should
be pumped through the column until the observed column pressure
is constant and the column appears wet. Always recalibrate
after column drying has occurred to verify retention volumes
have not changed.
D-37/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Cleanup (GPC)
10.3.3 Calibration of GPC
10.3.3.1 Summary of GPC Calibration and GPC Continuing Calibration
Veri ficat ion (CCV)
The GPC calibration procedure and GPC CCV procedure are based
on monitoring the elution of standards with a UV detector
connected to the GPC column.
10.3.3.2 Frequency of GPC Calibration and GPC CCV
Each GPC system must be. calibrated upon award of a contract,
when the column is changed, when channeling occurs, and once
every seven days CGPC Continuing. Calibration Verification,) when
samples, including matrix spikes, matrix spike duplicates, and
blanks, are cleaned up using GPC.
10.3.3.3 Procedure for GPC Calibration and GPC CCV
Follow the manufacturer's instructions for operating the GPC
system. Changes in pressure, solvent flow rate, and
temperature conditions can affect analyte retention times and
must be monitored.
10.3.3.3.1 Using a 10 mL syringe, load the calibration solution
(Section 7.2.4.3) onto the GPC. Establish appropriate
collect and dump time periods to ensure collection of all
target analytes. Initiate column eluate collection just
before elution of bis (2-ethylhexyl) phthalate and after the
elution of corn oil. Stop eluate collection shortly after
the elution of perylene. Collection should be stopped
before sulfur elutes. Use a "wash" time of 10 minutes after
the elution of sulfur. Each laboratory is required to
.establish its specific time sequences.
10.3.3.3.2 Reinject the calibration solution after appropriate collect
and dump cycles have been set, and the solvent flow and
column pressure have been established.
10.3.3.3.3 Measure and record the volume of collected GPC eluate in a
graduated cylinder. The volume of GPC eluate collected for
each sample extract processed may be used to indicate
problems with the system during sample processing.
10.3.3.3.4 Analyze a GPC blank of methylene chloride after each GPC
calibration or each GPC CCV . Concentrate the methylene
chloride that passes through the system during the collect
cycle using a Kuderna-Danish (K-D) evaporator. Add internal
standards at the appropriate concentration and analyze the
concentrate by GC/MS.
D-38/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Cleanup (GPC)
| 10.3.4 Technical Acceptance Criteria for GPC Calibration and GPC CCV
| 10.3.4.1 The GPC system must be calibrated and verified at the frequency
described in Section 10.3.3.2. The UV trace must meet the
following requirements:
Peaks must be observed and should be symmetrical for all
compounds in the calibration solution.
Corn oil and the phthalate peaks must exhibit > 85.0 percent
resolution.
The phthalate and methoxychlor peaks must exhibit > 85.0
percent resolution.
Methoxychlor and perylene peaks must exhibit > 85.0 percent
resolution.
Perylene and sulfur peaks must not be saturated and must
exhibit > 90.0 percent baseline resolution.
10.3.4.2 The solvent flow rate and column pressure must be within the
| manufacturer's specified ranges .
10.3.4.3 If the retention time shift is > 5.0 percent between
calibrations take corrective action. Excessive retention time
shifts are caused by the following:
Poor laboratory temperature control or system leaks.
An unstabilized column that requires pumping methylene
chloride through it for several more hours or overnight.
Excessive laboratory temperatures causing outgassing of the
methylene chloride.
| 10.3.4.4 A copy of the two most recent UV traces of the calibration
solution must be submitted with the data for the associated
samples.
| 10.3.4.5 The analyte concentrations in the GPC blank must be less than
the CRQL for all target compounds in Exhibit C (Semivolatiles),
| except phthalate esters, which must be less than 5 times the
CRQL.
| 10.3.5 Corrective Action for GPC Calibration and GPC CCV
10.3.5.1 If the requirements in Section 10.3.4 cannot be met, the column
may be cleaned by processing several 5 mL volumes of
butylchloride through the system. Butylchloride removes the
discoloration and particles that may have precipitated out of
the methylene chloride extracts. If a guard column is being
used, replace it with a new one. This may correct the problem.
If column maintenance does not restore the performance of the
D-39/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Extract Cleanup (GPC)
column, the column must be repacked with new packing and
recalibrated. It may be necessary to obtain a new lot of Bio
Beads if the column fails all criteria.
10.3.5.2 If the GPC blank exceeds the requirements in Section 10.3.4.5,
pump additional methylene chloride through the system for 1-2
hours. Analyze another GPC blank to ensure the system is
sufficiently clean. Repeat the methylene chloride pumping if
necessary.
10.4 Sample Extract Cleanup by GPC
10.4.1 It is very important to have constant laboratory temperatures during
an entire GPC run, which could be 24 hours or more. If temperatures
are not constant, retention times will shift, and the dump and
collect times determined by the calibration standard no longer will
be appropriate. The ideal laboratory temperature to prevent
outgassing of the methylene chloride is 22 °C.
10.4.2 In order to prevent overloading of the GPC column, highly viscous
sample extracts must be diluted prior to cleanup. Any sample extract
with a viscosity greater than that of a 1:1 glycerol:water solution
must be diluted and loaded into several loops. Similarly, extracts
containing more than 40 mg/mL of non-volatile residue must be diluted
and loaded into several loops. The non-volatile residue may be
determined by evaporating' a 100 uL aliquot of the extract to dryness
in a tared aluminum weighing pan, or other suitable container.
Systems using automated injection devices to load the sample on the
column must be carefully monitored to assure that the required amount
is being injected on the column. Viscous extracts or extracts
containing a large amount of non-volatile residue will cause problems
with an automated injection system's ability to inject the proper
amount of sample extract on a column. After the sample extract has
been processed, the remaining sample extract in the injection vial
must be checked before proceeding with extract cleanup to assure that
the proper amount was injected on the column. If the proper amount
of extract was not injected, the sample must be re-prepared at no
additional cost to the Agency, and the sample extract must either be
diluted and loaded into several loops, or the sample extract must be
injected manually.
NOTE: When multiple loops/runs are necessary for an individual
sample, be sure to combine all of the sample eluates collected from
each run.
10.4.3 Frequency of GPC Sample Cleanup
GPC cleanup must be performed once for each soil/sediment extract and
for water extracts that contain high molecular weight contaminants
that interfere with the analysis of the target analytes. In
addition, GPC must be performed for all associated blanks, matrix
spikes, and matrix spike duplicates. If cleanup procedure is
inadequate, contact SMO.
D-40/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Extract Cleanup (GPC)
10.4.4 Procedure for GPC Sample Cleanup
10.4.4.1 - --Particles greater-than 5-microns may scratch-the valve, which
may result in a system leak and cross contamination of sample
extracts in the sample loops. To avoid such problems, filter
the extract through a 5 micron filter disc by attaching a
syringe filter assembly containing the filter disc to a 10 mL
syringe. Draw the sample extract through the filter assembly
and into the 10 mL syringe. Disconnect the filter assembly
before transferring the sample extract into a small glass
container, e.g., a 15 mL culture tube with a Teflon-lined screw
cap. Alternatively, draw the extract into the syringe without
the filter assembly. Attach the filter assembly and force the
extract through the filter and into the glass container. Draw
a minimum of 8 mL of extract' into a 10 mL syringe.
NOTE: Some GPC instrument manufacturers recommend using a
smaller micron size filter. Follow the manufacturer's
recommended operating instructions.
10.4.4.2 Introduction of particulates or glass wool into the GPC
switching valves may require factory repair of the apparatus.
10.4.4.3 Follow the manufacturer's instructions for operation of the GPC
system being utilized. A 2 mL injection loop may be used in
place of a 5 mL injection loop. If a 2 mL injection loop is
used, concentrate the sample extract to 4 mL instead of 10 mL
and inject 2 mL instead of 5 mL.
10.4.4.4 If the sample is difficult to load, part of the system may be
blocked. Take appropriate corrective action following
manufacturer's recommendations. The problem must be resolved
prior to loading sample extracts.
10.4.4.5 After loading each sample loop, wash the loading port with
methylene chloride to minimize cross-contamination. Inject
approximately 10 mL of methylene chloride to rinse the common
tubes.
10.4.4.6 After loading all the sample loops, process each sample using
the collect and dump cycle time established in Section
10.3.3.3.1.
10.4.4.7 Collect each sample in a 250 mL Erlenmeyer flask, covered with
aluminum foil to reduce solvent evaporation, or directly into a
Kuderna-Danish (K-D) evaporator. Monitor sample volumes
collected. Changes in sample volumes collected may indicate
one or more of the following problems.
Change in solvent flow rate, caused by channeling in the
column or changes in column pressure.
Increase in column operating pressure due to the absorption
of particles or gel fines onto either the guard column or
D-41/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Final Concentration/Sample Analysis by GC/MS
the analytical column gel, if a guard column is not used.
Leaks in" the system or significant variances in room
temperature.
10.4.4.8 Any samples that were loaded into two or more loops must be
recombined before proceeding with concentration.
10.5 Final Concentration
Concentrate the extract as per Section 10.2.2. Final volumes should be
brought to the volumes stated in Section 10.2.2.3.
10.6 Sample Analysis by GC/MS
10.6.1 Sample extracts shall be analyzed only after the GC/MS system has met
the instrument performance check, initial calibration, and continuing
calibration requirements. The same instrument conditions must be
employed for the analysis of samples as were used for calibration.
10.6.2 Internal standard solution is added to each sample extract. Add 10
uL of internal standard solution to each accurately measured 1.0 mL
of water sample extract. For soil/sediment samples and water samples
subjected to GPC, add 5 uL of internal standard solution to each
accurately measured 0.5 mL of sample extract. This will result in a
concentration of 20 ng/uL of each internal standard.
NOTE: An alternate amount of internal standard solution may be
added; however, the internal standards must be added to maintain the
required 20 ng/uL of each internal standard in the sample extract.
10.6.3 Prior to the addition of internal standards, make any extract
dilution indicated by characterization step. Add internal standards
after dilution. Internal standards must be added to maintain the
required 20 ng/uL of each internal standard in the extract volume.
10.6.4 Inject 2 uL of the sample extract into the GC/MS. This 2 uL volume
must contain 40 ng of each internal standard.
10.6.5 Sample Dilutions
10.6.5.1 If the on-column concentration of any target compound in any sample
exceeds the initial calibration range, that sample extract must be
diluted, the internal standard concentration must be readjusted, and
sample extract must be reanalyzed. Guidance in performing dilution
and exceptions to this requirement are given below.
10.6.5.2 Use the results of the original analysis to determine the
approximate dilution factor required to get the largest analyte
peak within the initial calibration range.
D-42/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 10
Procedure
Sample Analysis by GC/MS
10.6.5.3 The dilution factor chosen should keep the response of the
largest peak for a target compound in the upper half of the
calibration range of the instrument-.- - _
10.6.5.4 The maximum dilution factor permitted for low level soils is
30. If a low level soil sample requires a dilution factor
greater than 30, to bring target compounds within the
calibration range, then the medium level method shall be
utilized.
10.6.5.5 Do not submit data for more than two analyses, i.e., from the
original sample extract and one dilution, or if the
semivolatile screening procedure was employed, from the most
concentrated dilution analyzed and one further dilution.
D-43/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.0 DATA ANALYSIS AND CALCULATIONS
11.1 Qualitative Identification
11.1.1 Identification of Target Compounds
11.1.1.1 The compounds listed in the Target Compound List (TCL), Exhibit
C (Semivolatile), shall be identified by an analyst competent
in the interpretation of mass spectra (see Exhibit A, Section
4.3.1) by comparison of the sample mass spectrum to the mass
spectrum of the standard of the suspected compound. Two
criteria must be satisfied to verify the identifications.
Elution of the sample analyte within GC relative retention
time unit window established from the 12-hour calibration
standard.
Correspondence of the sample analyte and calibration
standard component mass spectra.
11.1.1.2 For establishing correspondence of the GC relative retention
time (RRT), the sample component RRT must compare within ±0.06
RRT units of the RRT of the standard component. For samples
analyzed during the same 12-hour time period as the initial
calibration standards, compare the analyte retention times to
those from the 50 ng calibration standard. For reference, the
standard must be run on the same shift as the sample. If co-
elution of interfering components prohibits accurate assignment
of the sample component RRT from the total ion chromatogram,
the RRT should be assigned by using extracted ion current
profiles for ions unique to the component of interest.
11.1.1.3 For comparison of standard and sample component mass spectra,
mass spectra obtained from a calibration standard on the
Contractor's GC/MS meeting the daily instrument performance
requirements for DFTPP are required. Once obtained, these
standard spectra may be used for identification purposes only
if the contractor's GC/MS meets the DFTPP daily instrument
performance requirements.
11.1.1.4 The requirement for qualitative verification by comparison of
mass spectra are as follows:
All ions present in the standard mass spectrum at a relative
intensity greater than 10.0 percent (most abundant ion in
the spectrum equals 100.0 percent) must be present in the
sample spectrum.
The relative intensities of ions specified in the paragraph
above must agree within ±20.0 percent between the standard
and sample spectrum, (Example: For an ion with an abundance
of 50.0 percent in the standard spectrum, the corresponding
sample ion abundance must be between 30.0 and 70.0 percent).
D-44/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Qualitative Identification
Ions greater than 10.0 percent in the sample spectrum, but
not present in the standard spectrum, must be considered and
accounted for by the analyst making the comparison. In Task
II (Exhibit A), the verification process should favor false
positives. All compounds meeting the identification
criteria must be reported with their spectra. When target
compounds are below contract required quantitation limits
(CRQL) but the spectrum meets the identification criteria,
report the concentration with a "J". For example, if the
CRQL is 10 ug/L and concentration of 3 ug/L is calculated,
report as "3J".
11.1.1.5 If a compound cannot be verified by all of the criteria in
Section 11.1.1 (11.1.1.1. through 11.1.1.4), but in the
technical judgement of the mass spectra interpretation
specialist, the identification is correct, then the contractor
shall report the identification and proceed with quantitation.
11.1.2 Identification of Non-Target Compounds
11.1.2.1 A 'library search shall be executed for non-target sample
components for the purpose of tentative identification. For
this purpose, the NIST/EPA/NIH (May 1992 release or later)
and/or Wiley (1991 release or later), or equivalent mass
spectral library shall be used.
11.1.2.2 Up to 30 organic compounds of greatest apparent concentration
not listed in Exhibit C for the volatile and semivolatile
fraction, excluding the surrogate and internal standard
compounds, shall be identified tentatively via a forward search
of the NIST/EPA/NIH (May 1992 release or later) and/or Wiley
(1991 release or later), or equivalent mass spectral library. ..
The- following are not to be reported : 1) Substances with
responses less than 10 percent of the internal standard (as
determined by inspection of the peak areas or heights); 2)
substances which elute earlier than 30 seconds before the first
semivolatile compound listed in Exhibit C (Semivolatiles), or
three minutes after the last semivolatile compound listed in
Exhibit C has eluted; and 3) volatile compounds listed in
Exhibit C. Only after visual comparison of sample spectra to
spectra resulting from the library search(es) will the mass
spectral interpretation specialist assign a tentative
identification. NOTE: Computer generated library search
routines must not use normalization routines that would
misrepresent the library or unknown spectra when compared to
each other.
11.1.2.3 Up to 20 peaks of greatest apparent concentration (as
determined by inspection of peak areas or heights) that are
suspected to be straight-chain, branched, or cyclic alkanes,
alone or part of an al.ka.ne series shall be library searched.
Documentation for the tentative identification must be
supplied. Alkanes-are not counted as part of the 30 organic
compounds described in Section 11.1.2.2.
D-45/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.1.2.4 Peaks that are suspected to be aldol-condensation reaction
products (i.e., 4-methyl-4-hydroxy-2-pentanone and 4-methyl-3-
pentene-2-one) shall be searched, reported, and counted as part
of the 30 most intense non-target semivolatile compounds, and
qualified with an "A" flag on. Form I TIC.
11.1.2.5 Guidelines for Making Tentative Identifications
11.1.2.5.1 Major ions in the reference spectrum (ions greater than 10
percent of the most abundant ion, should be present in the
sample spectrum.
11.1.2.5.2 The relative intensities of the major ions should agree
within ±20 percent (Example: For an ion with an abundance
of 50 percent in the standard spectrum, the corresponding
sample ion abundance must be between 30 and 70 percent).
11.1.2.5.3 Molecular ions present in the reference spectrum should be
present in the sample spectrum..
11.1.2.5.4 Ions present in the sample spectrum, but not in the
reference spectrum, should be reviewed for possible
background contamination or presence of co-eluting
compounds.
11.1.2:5.5 Ions present in the reference spectrum, but not in the
sample spectrum, should be reviewed for possible subtraction
from the_ sample spectrum because of background contamination
or co-eluting compounds. NOTE: Data system library
reduction programs .sometimes can create these discrepancies.
11.1.2.5.6 If, after careful review and in the technical judgement of
the mass spectral interpretation specialist, no valid
tentative identification can be made, the compound should be
reported as follows:
9 If the library search produces a match at or above 85%,
report that compound.
If the library search produces more than one compound at
or above 85%, report the first compound (highest).
If the library search produces no matches at or above
85%, the compound should be reported as unknown. The
mass spectral specialist should give additional
classification of the unknown compound, if possible
(i.e., unknown aromatic, unknown hydrocarbon, unknown
acid type, unknown chlorinated compound). If probable
molecular weights can be distinguished, include them .
11.1.2.5.7 The Contractor shall report pesticide target compounds
listed in Exhibit C (Pesticides) that appear as semivolatile
tentatively identified compounds.
D-46/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Calculations
11.1.2.5.8 Straight-chain, branched, or cyclic alkanes are not to be
reported as tentatively identified compounds on FORM I SV-
- - - TIC.- When the above-alkanes are- tentatively--identified, the
concentration(s) are to be estimated as described in Section
11.2.2 and reported in the SPG Narrative as alkanes. bv
class (i.e., straight-chain, branched, or cyclic; as a "
series; as applicable).
11.2 Calculations
11.2.1 Target Compounds
11.2.1.1 Target compounds identified shall be quantitated by the
internal standard method. The internal standard used shall be
the one assigned to that analyte for quantitation (see Table
2). The EICP area of primary characteristic ions of analytes
listed in Tables 3 and 4 are used for quantitation.
11.2.1.2 It is expected that situations will arise when the automated
quantitation procedures in the GC/MS software provide
inappropriate quantitations. This normally occurs when there
is compound co-elution, baseline noise, or matrix
interferences. In these circumstances, the Contractor must
perform a manual quantitation. Manual quantitations are
performed by integrating the area of the quantitation ion of
the compound. This integration shall only include the area
attributable to the specific TCL compound. The area integrated
shall not include baseline background noise. The area
integrated shall not extend past the point where the sides of
the peak intersect with the baseline noise. Manual integration
is not to be used solely to meet QC criteria, nor is it to be
used as a substitute for corrective action on the
chromatographic system. Any instance of manual integration
must be documented in the SDG Narrative.
11.2.1.3 In all instances where the data system report has been edited
or where manual integration or quantitation has been performed,
the GC/MS operator must identify such edits or manual
procedures by initialing and dating the changes made to the
report, and shall include the integration scan range. In
addition, a hardcopy printout of the EICP of the quantitation
ion displaying the manual integration shall be included in the
raw data. This applies to all compounds listed in Exhibit C
(Semivolatiles) , internal standards, and surrogates.
11.2.1.4 The requirements listed in Sections 11.2.1.2 and 11.2.1.3 apply
to all standards, samples including MS/MSD, and blanks.
11.2.1.5 The relative response factor (RRF) from the continuing
calibration analysis is used to calculate the concentration in
the sample. For samples analyzed during the same 12-hour time
period as the initial calibration standards, use the RRF values
from the 50 ng calibration standard. Secondary ion
quantitation is allowed ONLY when there are sample
D-47/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Calculations
interferences with the primary ion. If secondary ion
quantitation is performed, document the reason in the SDG
Narrative. The area of a secondary ion cannot be used for the
area of a primary ion unless a relative response factor is
calculated using the secondary ion.
11.2.1.6 Calculate the concentration in the sample using the relative
response factor (RRF) and the following equations.
11.2.1.6.1 Water
EQ. 5
(A ) (I ) (V ) (Df) (GPC)
Concentration ug/L = ;:
^ (Ais) (RRF) (Vo) (V±)
Where,
~AX = Area of the characteristic ion for the compound to
be measured.'
Als = Area of the characteristic ion for the internal
standard.
IB = Amount of internal standard injected in nanograms
(ng) .
V0 = Volume of water extracted in milliliters (mL).
Vt = Volume of extract injected in microliters (uL).
Vt = Volume of the concentrated extract in microliters
(uL) (Vt = 1,000 uL if sample was not subjected to
GPC; Vt = 500 uL if sample was subjected to GPC).
RRF = Relative response factor determined from the 12-
hour calibration standard.
GPC = GPC factor.
GPC = 1.0 if water sample was not subjected to GPC;
GPC = 2.0 if water sample was subjected to GPC.
Df = Dilution factor. The dilution factor for analysis
of water samples for semivolatiles by this method
is defined as follows:
, _ uL most cone, extract used to make dilution + uL clean solvent
uL most cone, extract used to make dilution
If no dilution is performed, Df = 1.0.
D-48/SVOA OLM04.2
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11.2.1.6.2
Exhibit D Semivoiatiies -- Section 11
Data Analysis and Calculations
Calculations
Soil/Sediment
EQ. 6
Concentration ug/Kg (Dry weight basis) =
(Ax)
(Vt) (Df) (GPC)
(A.s) (RRF) (V.) (WJ (D)
Where,
**x' ^s
vt
Vi
D
GPC
RRF
Df
and Ais, are as given for water, above.
Volume of the concentrated extract in microliters
(uL) (Vt = 500 uL).
Volume of the extract injected in microliters (uL)
100 - % Moisture
100
Weight of sample extracted in grams (g)
GPC factor (GPC = 2.0 to account for GPC cleanup).
Relative response factor determined from the 12-
hour calibration standard.
Dilution factor. The dilution factor for analysis
of soil/sediment samples for semivolatiles by this
method is defined as follows:
_ _ uL most cone, extract used to make dilution + uL clean solvent
uL most cone. extract used to make dilution
If no dilution is performed, Df = 1.0.
The factor of 2.0 in the numerator is used to account for
the amount of extract that is not recovered from the
mandatory use of GPC cleanup. Concentrating the extract
collected after GPC to O.5 mL maintains the sensitivity of
the soil/sediment method.
11.2.2 Non-Target Compound
An estimated concentration for non-target compounds tentatively
identified shall be quantitated by the internal standard method. For
quantitation, the nearest internal standard free of interferences
shall be used. The equations for calculating concentration are the
same as Equations 5 and 6. Total area counts (or peak heights) from
the total ion chromatograms are to be used for both the compounds to
be measured and the internal standard. A relative response factor
(RRF) of one (1) is to be assumed. The resulting concentration shall
be qualified as "J" (estimated, due to lack of a compound specific
response factor), and "N" (presumptive evidence of presence),
indicating the quantitative and qualitative uncertainties associated
with this non-target component. An estimated concentration should be
calculated for all tentatively identified compounds as well as those
identified as unknowns.
D-49/SVOA . OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Calculations
11.2.3 CRQL Calculations
If the CRQL is less than the CRQL in Exhibit C (Seraivolatiles),
report the CRQL listed in Exhibit C (Semivolatiles).
11.2.3.1 Water Samples
EQ. 7
Adjusted _ Contract (Vx) (Vt) (Vy) (Df )
CRQL CRQL X (V) (V) (V)
Where,
Vc, Df, V0, and V\ are as given in Equation 6.
Vx = Contract sample volume (1,000 mL).
Vy = Contract injection volume (2 uL).
Vc = Contract concentrated extract volume (1,000 uL if GPC is
not performed, and 500 uL if GPC was performed.
11.2.3.2 Soil/Sediment Samples
EQ. 8
Adjusted _ Contract (Wx) (Ve) (Vy) (Df)
CRQL CRQL (W(j) (vj (V± ) (D)
Where,
Vc, Df, Ws, Vi( and D are as given in Equation 6.
Wx = Contract sample weight (30 g for low level and 1 g for
medium level soil/sediment samples).
Vy = Contract injection volume (2 uL).
Vc = Contract concentrated extract volume (500 uL, GPC is
required).
11.2.4 Surrogate Recoveries
11.2.4.1 Calculate surrogate standard recovery on all samples, blanks,
matrix spikes, and matrix spike duplicates. Determine if
recovery is within limits (see Table 7) and report on
appropriate form.
D-50/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Calculations
11.2.4.2 Calculate the concentrations of the surrogate compounds using
the same equations as used for the target compounds. Calculate
the recovery of each surrogate-using, the following- equation:
EQ. 10
. _ Concentration (or amount) found ,
% Recovery = : x 100
Concentration (or amount) spiked
11.3 Technical Acceptance Criteria' for Sample Analysis
11.3.1 The samples must be analyzed on a GC/MS system meeting the DFTPP
initial calibration, continuing calibration, and blank technical
acceptance criteria. the sample must undergo cleanup procedures,
when required, on a GPC meeting the technical acceptance criteria for
GPC calibration.
11.3.2 The sample must be extracted-and analyzed within the contract holding
times.
11.3.3 The sample must have an associated method blank meeting the blank
technical acceptance criteria.
11.3.4 The sample must have an acceptable surrogate recovery. The sample
surrogate recovery will be considered unacceptable if the following
occurs.
Any surrogate has a recovery less than 10.0 percent.
More than one base neutral surrogate or more than one acid
surrogate is outside the surrogate acceptance windows listed in
Table 7.
NOTE: These requirements do not apply to surrogates with advisory
windows and to dilutions of samples.
11.3.5 The relative retention time of each surrogate must be within ±0.06
RRT units of its relative retention time in the continuing
calibration standard.
11.3.6 The instrumental response (ElCP.area) for each of the internal
standards must be within the inclusive range of -50.0 percent and
+100.0 percent ofthe response of the internal standards in the most
recent continuing calibration analysis.
11.3.7 The retention time shift for each of the internal standards must be
within ± 0.50 minutes (30 seconds) between the sample and the most
recent continuing calibration standard analysis.
11.3.8 Excluding those ions in the solvent front, no ion may saturate the
detector. No target compound concentration may exceed the upper
' '. D-51/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Corrective Action
limit of the 12-hour standard calibration range unless a more dilute
aliquot of the sample extract is also analyzed according to the
procedures in Section 10.6.5.
11.4 Corrective Action
11.4.1 Corrective Action for Sample Analysis
The sample technical acceptance criteria must be met before data are
reported. Samples contaminated from laboratory sources, or sample
results submitted not meeting the sample technical acceptance
criteria, will require re-extraction and/or reanalysis at no
additional, cost to the Agency.
11.4.2 Corrective Action for Surrogate Recoveries which Fail to Meet Their
Acceptance Criteria (Section 11.3.4, Table 7).
11.4.2.1 If the surrogate compounds fail to meet their recovery
acceptance criteria, check calculations, sample preparation
logs, surrogate compound spiking solutions, and the instrument
operation. If the calculations were incorrect, correct the
calculations and verify that the surrogate compound recoveries
meet their acceptance criteria. If the sample preparation logs
indicate that the incorrect amount of surrogate compound
spiking solution was added, then re-extract/reanalyze the
sample after adding the correct amount of surrogate spiking
solution. If the surrogate compound spiking solution was
improperly prepared, concentrated, or degraded, re-prepare
solutions and re-extract/reanalyze samples. If the surrogate
recoveries were outside the lower surrogate acceptance limit
and the extract from the sample was cleaned up on a GPC using
an automated injection system, the Contractor shall verify that
the proper amount was injected on the GPC column. If
insufficient sample volume was injected on the GPC, the sample
must be reprepared and reanalyzed at no additional cost to the
Agency. If the instrument malfunctioned, correct the
instrument problem and reanalyze the sample extract. Verify
that the surrogate recoveries meet their acceptance criteria.
If the instrument malfunction affected the calibrations,
recalibrate the instrument before reanalyzing the sample
extract.
11.4.2.2 If the above actions do not correct the problem, then the
problem may be due to a sample matrix effect. To determine if
there was matrix effect, take the following corrective action
steps.
11.4.2.2.1 Re-extract and reanalyze the sample. EXCEPTION: If
surrogate compound recoveries in a sample used for a matrix
spike and/or matrix spike duplicate were considered
unacceptable, then it should be re-extracted/reanalyzed only
if surrogate compound recoveries met the surrogate
acceptance criteria in both the matrix spike and matrix
spike duplicate analyses.
D-52/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Corrective Action
11.4.2.2.2 If the surrogate compound recoveries meet acceptance
criteria in the re-extracted/reanalyzed sample, then the
. problem-was-within -the Contractor's-control. Therefore,
submit only data from the re-extraction/reanalysis.
11.4.2.2.3 If the surrogate compound recoveries fail to meet the
acceptance criteria in the re-extracted/reanalyzed sample,
then submit data from both analyses. Distinguish between
the initial analysis and the re-extraction/reanalysis on all
deliverables, using the suffixes in Exhibit B.
11.4.3 Corrective Action for Internal Standard Compound Responses which Fail
to Meet their Acceptance Criteria (Sections 11.3.5 and 11.3.6) .
11.4.3.1 If the internal standards fail to meet their acceptance
criteria, check calibrations, internal standard compound
spiking solutions, and instrument operation. If the
calculations were incorrect, correct the calculations and
verify that the internal standard response met their acceptance
criteria. If the internal standard compound spiking solution
was improperly prepared, concentrated, or degraded, re-prepare
solutions and re-extract/reanalyze samples. If the instrument
malfunctioned correct the instrument problem and reanalyze the
sample extract. If the instrument malfunction affected the
calibration, recalibrate the instrument before reanalyzing the
sample extract.
11.4.3.2 If the above actions do not correct the problem, then the
problem may be due to a sample matrix effect. To determine if
there was matrix effect, take the following corrective action
steps.
11.4.3.2.1 Reanalyze the sample extract. EXCEPTION: If internal
standard compound recoveries in a sample used for a matrix
spike and/or matrix spike duplicate were outside the
acceptance windows, then it should be reanalyzed only if
internal standard compound recoveries met the internal
standard acceptance criteria in both the matrix spike and
matrix spike duplicate analysis.
11.4.3.2.2 If the internal standard compound recoveries meet acceptance
criteria in the reanalyzed sample extract, then the problem
was within the Contractor's control. Therefore, submit only
data from the reanalysis.
11.4.3.2.3 If the internal standard compound recoveries fail to meet
their acceptance windows in the reanalyzed sample extract,
then submit data from both analyses. Distinguish between
the initial analysis and the reanalysis on all deliverables
using the suffixes in Exhibit B.
11.4.4 Corrective Action for Surrogate Compound Relative Retention
Times/Internal Standard Compound Retention Times Outside Acceptance
Criteria (Sections 11.3.5 and 11.3.6).
D-53/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 11
Data Analysis and Calculations
Corrective Action
11.4.4.1 If the surrogate compounds relative retention times or internal
standard compounds retention times are not within their
acceptance criteria, check the instrument for malfunctions. If
the instrument malfunctioned, correct the instrument problem
and reanalyze the sample extract. If the instrument
malfunction affected the calibration, recalibrate the
instrument before reanalyzing the sample extract.
11.4.4.2 If the above actions do not correct the problem, then the
problem may be due to a sample matrix effect. To determine if
there was matrix effect, take the following corrective action
steps.
11.4.4.2.1 Reanalyze the sample extract. EXCEPTION: If the surrogate
compounds relative retention times or internal standard
compounds retention times in a sample used for a matrix
spike and/or matrix spike duplicate were outside the
acceptance criteria, then it should be reanalyzed only if
the surrogate compounds relative retention times and
internal standard compounds retention times were within the
acceptance criteria in both the matrix spike and matrix
spike duplicate analysis.
11.4.4.2.2 if the surrogate compounds relative retention times and
internal standard compounds retention times are within the
acceptance criteria in the reanalyzed sample extract, then
the problem was within the Contractor's control. Therefore,
submit only data from the reanalysis with the surrogate
compounds relative retention times and the internal standard
compound retention times within the acceptance limits.
11.4.4.2.3 If the surrogate compounds relative retention times or
internal standard compounds retention times are outside the
acceptance criteria in the reanalyzed sample extract, then
submit data from both analyses. Distinguish between the
initial analysis and the reanalysis on all deliverables,
using the suffixes in Exhibit B.
11.4.5 Corrective action for failure to meet instrument performance checks
and initial .and continuing calibration must be completed before the
analysis of samples.
D-54/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 12
Quality Control
Method Blanks
12.0 QUALITY CONTROL
12.1 Method Blanks - ._.-__ . . . __ _ .
12.1.1 Summary of Method Blanks
A method blank is a volume of a clean reference matrix (reagent water
for water samples, or purified sodium sulfate for soil/sediment
samples) that is carried through the entire analytical procedure.
The volume or weight of the reference matrix must be approximately
equal to the volume of weight of samples associated with the blank.
The purpose of a method blank is to determine the levels of
contamination associated with the processing and analysis of samples.
12.1.2 Frequency of Method Blanks
A method blank must be extracted each time samples are extracted.
The number of samples extracted with each method blank shall not
exceed 20 field samples (excluding matrix spikes/matrix spike
duplicates and PE samples). In addition, a method blank shall:
Be extracted by the same procedure used to extract samples.
Be analyzed on each GC/MS system used to analyze associated
samples.
12.1.3 Procedure for Method Blank Preparation
For semivolatile analyses, a method blank for water samples consists
of 1 L volume of reagent water spiked with 0.5 mL of the surrogate
spiking solution. For medium and low level soil/sediment samples, a
method blank consists of 1 g and 30 g of sodium sulfate spiked with
0.5 mL of the surrogate spiking solution respectively. Extract,
. concentrate, cleanup, and analyze the blank according to procedures
for water and soil samples.
12.1.4 Technical Acceptance Criteria for Method Blank Analysis
12.1.4.1 All blanks must be extracted and analyzed at the frequency
described in Section 12.1.2 on a GC/MS system meeting the
DFTPP, initial calibration, and continuing calibration
technical acceptance criteria.
12.1.4.2 The blank must meet the sample acceptance criteria listed in
Sections 11.3.4 through 11.3.7.
12.1.4.3 For all other target compounds the method blank must contain
less than the CRQL of any single target compound (see Exhibit
C). A method blank for semivolatile analysis must contain less
than five times (5x) the contract required quantitation limit
(CRQL) of the phthalate esters listed in Exhibit C.
12.1.5 Corrective Action for Method Blanks
D-55/SVOA OLM04.2
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Exhibit D Semivolatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.1.5.1 If a method blank does not meet the technical acceptance
criteria for method blank analysis, the Contractor shall
consider the analytical system to be out of control.
12.1.5.2 If contamination is the problem, then the source of the
contamination must be investigated and appropriate corrective
measures must be taken and documented before further sample
analysis proceeds. It is the Contractor's responsibility to
ensure that method interferences caused by contaminants in
solvent, reagents, glassware, and sample storage and processing
hardware that lead to discrete artifacts and/or elevated
baselines in the GC/MS be eliminated. Samples associated with
the contaminated blank must be re-extracted and reanalyzed at
no additional cost to the Agency.
12.1.5.3 If surrogate recoveries in the method blank do not meet the
acceptance criteria listed in Section 11.3.4 and Table 7, first
reanalyze the method blank. If the surrogate recoveries
(except those with advisory limits) do not-meet the acceptance
criteria after reanalysis, the method blank and all samples
associated with that method blank must be re-extracted and
reanalyzed at no additional cost to the Agency.
12.1.5.4 If the method blank does not meet internal standard response
requirements listed in Section 11.3.6, check calculations, the
internal standard spiking solutions, and the instrument
operation. If the calculations were incorrect, correct the
calculations and verify that the internal standard responses
meet their acceptance criteria. If the internal standard
compound spiking solution was improperly prepared,
concentrated, or degraded, re-prepare solutions and re-
extract/reanalyze samples. If the instrument malfunctioned,
correct the instrument problem and reanalyze the method blank.
If the instrument malfunction affected the calibration,
recalibrate the instrument before reanalyzing the blank. The
Contractor shall resolve and document the resolution of the
problem before proceeding with sample analysis.
12.1.5.5 If the method blank does not meet the retention time
requirements for internal standards (Section 11.3.7) or the
surrogates (Section 11.3.5), check the instrument for
malfunction and recalibrate. Reanalyze the method blank.
Sample analyses cannot proceed until the method blank meets
these requirements.
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.1 Summary of MS/MSD
In order to evaluate the effects of the sample matrix on the methods
used for semivolatile analyses, the Agency has prescribed a mixture
of semivolatile target compounds to be spiked into two aliquots of a
sample and analyzed in accordance with the appropriate method.
D-5S/SVOA OLM04.2
-------
Exhibit D Serr.ivolatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.2 Frequency of MS/MSD Analyses
12.2.2.1 A matrix spike and matrix spike duplicate must be extracted and
analyzed for every 20 field samples of a similar matrix in an
SDG whenever samples are extracted by the same procedure ( low
or medium level soil preparation) . ' MS/MSD samples shall be
analyzed unless otherwise specified on the Traffic Report (TR).
If no MS/MSD samples are specified on the TR, the Contractor
shall contact SMO to confirm that MS/MSD analyses are not
required.
12..2.2.2 As part of the Agency's QA/QC program, water rinsate samples
and/or field/trip blanks (field QC) may accompany soil/sediment
samples and/or water samples that are delivered to the
laboratory for analysis. The Contractor shall not perform
MS/MSD analysis on any of the field QC samples.
12.2.2.3 If the EPA Region designates a sample to be used as an MS/MSD,
then that sample must be used. If there is insufficient sample
remaining to perform an MS/MSD, then the Contractor shall
choose another sample on which to perform an MS/MSD analysis.
At the time the selection is made, the Contractor shall notify
the Region (through SMO) that insufficient sample was received
and identify the EPA sample selected for the MS/MSD analysis.
The rationale for the choice of another sample other than the
one designated by the Agency shall be documented in the SDG
Narrative.
12.2.2.4 If there is insufficient sample remaining in any of the samples
in an SDG to perform an MS/MSD, then the Contractor shall
immediately contact SMO to inform them of the problem. SMO
will contact the Region for instructions. The Region will
either approve that no MS/MSD is required, or require that a
reduced sample aliquot be used for the MS/MSD analysis '. SMO
will notify the Contractor of the Region's decision. The
Contractor shall document the decision in the SDG Narrative.
12.2.2.5 If it appears that the Region has requested MS/MSD analysis at
a greater frequency than required by the contract, then the
Contractor shall contact SMO. SMO will contact the Region to
determine which samples should have an MS/MSD performed on
them. SMO will notify the Contractor of the Region's decision.
The Contractor shall document the decision in the SDG
Narrative. If this procedure is not followed, the Contractor
will not be paid for MS/MSD analysis performed at a greater
frequency than required by the contract.'
12.2.2.6 When a Contractor receives only a performance evaluation (PE)
sample(s), no MS/MSD shall be performed within that SDG.
12.2.2.7 When a Contractor receives a performance evaluation (PE) sample
as part of a larger SDG, a sample other than the PE sample must
be chosen for the MS/MSD when the Region did not designate
samples to be used for this purpose. If the PE sample is an
D:57/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
ampulated standard, the ampulated PE sample is not considered
to be another matrix type.
12.2.3 Procedure for Preparing MS/MSD
12.2.3.1 Water Samples
For water samples, prepare two additional 1 L aliquots of the
sample chosen for spiking in two continuous extractors. Add
0.5 mL of surrogate spiking solution and 0.5 mL of the matrix
spiking solution to each aliquot. Extract, concentrate,
cleanup, and analyze the MS/MSD according to the procedures for
water samples.
12.2.3.2 Soil/Sediment Samples - Low Level
For low level soil/sediment samples, prepare two additional 30
g aliquots (record weight to nearest 0.1 g) of the sample
chosen for spiking in the two 400 mL beakers. Add 60 g of
anhydrous powdered sodium sulfate to each aliquot. Mix well.
Add 0.5 mL of the surrogate standard'spiking solution and 0.5
mL of the matrix spiking solution to each aliquot, then
immediately add 100 mL of 1:1 methylene chloride-acetone.
Extract, concentrate, cleanup, and analyze the MS/MSD according
to the procedures for low level soil samples.
12.2.3.3 Soil/Sediment Samples - Medium Level
For medium level soil/sediment samples, prepare two additional
1 g aliquots (record weight to nearest 0.1 g) of the sample
chosen for spiking in two 20 mL vials. Add 2.0 g of anhydrous
powdered sodium sulfate to each aliquot. Mix well. Add 0.5 mL
of surrogate spiking solution, 0.5 mL of matrix spiking
solution, and 9.0 mL of methylene chloride. Extract,
concentrate, cleanup, and analyze the MS/MSD according to the
procedures for medium level samples.
12.2.4 Dilution of MS/MSD
Before any MS/MSD analysis, analyze the original sample, then analyze
the MS/MSD at the same concentration as the most concentrated extract
for which the original sample results will be reported. For example,
if the original sample is to be reported at a 1:1 dilution and a 1:10
dilution, then analyze and report the MS/MSD at a 1:1 dilution only.
However, if the original sample is to be reported at a 1:10 dilution
and a 1:100 dilution, then the MS/MSD must be analyzed and reported
at a 1:10 dilution only. Do not further dilute the MS/MSD samples to
get either spiked or non-spiked analytes within calibration range.
Dilution of the sample must be performed in accordance to the
conditions in Section 10.6.5.
D-58/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.5 Calculations for MS/MSD
12.2.5.1 Calculate the recovery of each matrix spike compound in the
matrix spike and matrix spike duplicate and report on the
appropriate forms. Calculate the concentrations of the matrix
spike compounds using the same equations as used for target
compounds (Equations 6 and 7). Calculate the recovery of each
matrix spike compound as follows:
EQ. 11
SSR ~ SR
Matrix Spike Recovery = x 100
SA
Where,
SSR = Spike Sample Result.
SR = Sample Result.
SA = Spike Added.
12.2.5.2 Calculate the relative percent difference (RPD) of the
recoveries of each compound in the matrix spike and matrix
spike duplicate as follows:
RPD = IMSR-MSDRI x 100
EQ. 12
RPD =
-j (MSR + MSDR)
Where,
RPD = Relative Percent Difference.
MSR = Matrix Spike Recovery.
MSDR = Matrix Spike Duplicate Recovery.
The vertical bars in the formula above indicate the absolute
value of the difference, hence RPD is always expressed as a
positive value.
12.2.6 Technical Acceptance Criteria for MS/MSD
12.2.6.1 All MS/MSD must be prepared and analyzed at a frequency
described in Section 12.2.2. All MS/MSD must be analyzed on a
GC/MS system meeting DFTPP, initial and continuing calibration
technical acceptance criteria, and the method blank technical
acceptance criteria. The MS/MSD must undergo cleanup
procedures, when required on a GPC meeting the technical
acceptance criteria for GPC calibration.
12.2.6.2 The MS/MSD must have an associated method blank meeting the
blank technical acceptance criteria.
D-59/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.6.3 The MS/MSD must be extracted and analyzed within the contract
holding time.
12.2.6.4 The retention time shift for each of the internal standards
must be within ±0.50 minutes (30 seconds) between the MS/MSD
sample and the most recent continuing calibration standard.
12.2.6.5 The relative retention time for the surrogate must be within ±
0.06 RRT units of its standard retention time in the continuing
calibration standard.
12.2.6.6 The limits for matrix spike compound recovery and RPD are given
in Table 6. As these limits are only advisory, no further
action by the laboratory is required; however, frequent
.failures to meet the limits for recovery or RPD warrant
investigation by the laboratory, and may result in questions
from the Agency.
12.2.7 Corrective Action for MS/MSD
Any MS/MSD which fails to meet the technical acceptance criteria for
MS/MSD must be reanalyzed at no additional cost to the Agency.
D-60/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Sections 13-16
Method Performance/Pollution Prevention/Waste Management/References
13.0 METHOD PERFORMANCE
Not Applicable.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or
eliminates the quantity or toxicity of waste at the point of generation.
Numerous opportunities for pollution prevention exist in laboratory
operation. The EPA has' established a preferred hierarchy of
environmental management techniques that places pollution prevention as
the management option of first choice. Whenever feasible, laboratory
personnel should use pollution prevention techniques to address their
waste generation. When wastes cannot be feasibly reduced at the source,
the Agency recommends recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to
laboratories and research institutions, consult Less is Better:
Laboratory Chemical Management for Waste Reduction, available from the
American Chemical Society's Department of Government Relations and
Science Policy, 1155 16th Street, N.W., Washington D.C. .20036, (202)
872-4477.
15.0 WASTE MANAGEMENT
The Environmental Protection Agency requires that laboratory waste
management practices be conducted consistently with all applicable rules
and regulations. The Agency urges laboratories to protect the air,
water, and land by minimizing and controlling all releases from hoods
and bench operations, complying with"the letter and spirit of any sewer
discharge permits and regulations, and by complying with all solid and
hazardous waste regulations, particularly the hazardous waste
identification rules and land disposal restrictions. For further
information on waste management consult The Waste Management Manual for
Laboratory Personnel, available from the American Chemical Society at
the address listed in Section 14.
16.0 REFERENCES
Not Applicable.
D-61/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
17 . 0 TABLES/DIAGRAMS/FLOWCHARTS
Table 1
DFTPP Key Ions and Ion. Abundance Criteria
Mass Ion Abundance Criteria
51 30.0-80.0 percent of mass 198
68 Less than 2.0 percent of mass 69
69 Present
70 Less than 2.0 percent of mass 69
127 25.0 - 75.0 percent of mass 198
197 Less than 1.0 percent of mass.198
198 Base peak 100 percent relative
abundance (see Note)
199 5.0 - 9.0 percent of mass 198
275 10.0 - 30.0 percent of mass 198
365 Greater than 0.75 percent of mass 198
441 Present but less than mass 443
442 40.0 - 110.0 percent of mass 198
443 15.0 - 24.0 percent of mass 442
NOTE: All ion abundances MUST be normalized to m/z 198, the nominal
base peak, even though the-ion abundance of m/z 442 may be up to 110
percent that of m/z 198.
D-62/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 2
Semivolatile Internal Standards With Corresponding
Target Compounds and Surrogates Assigned for Quantitation
1.4-Dichlorobenzene-d,,
Benzaldehyde
Phenol
bis-(2-Chloroethyl
ether
2-Chlorophenol
2-Methylphenol
2,2'-oxybis-(1-
Chloropropane)
Acetophenone
,4-Methylphenol
N-Nitroso-di-n- |
propylamine
Hexachloroethane
2-Fluorophenol (surr)
Phenol-d5 (surr)
2-Chlorophenol-d, (surr)
1,2-Dichlorobenzene-d4
(surr)
Naphthalene-dn
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
bis-(2-Chloro
ethoxy)methane
2,4-Dichlorophenol|
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
Caprolactam
4-Chloro-3-
methylphenol
2-Methylnaphthalene
Nitrobenzene-d5
(surr)
Acenaphthene-din |
Hexachlorocyclo-
pentadiene
2,4,6-Trichloro
phenol
2,4,5-Trichloro
phenol
1,1'-Biphenyl
2-Chloro- |
naphthalene
2-Nitroaniline
Dimethylphthalate
2,6-Dinitrotoluene
Acenaphthylene
3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
Fluorene.
4 -Chlorophenyl-
phenylether
4-Nitroaniline
2 -Fluorobiphenyl
(surr)
Phenanthrene-d,
4,6-Dinitro-2-
methylphenol
4-Bromophenyl-
phenylether
N-Nitroso
diphenylamine
Hexachlorobenzene
Atrazine
Pentachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
2,4,6-Tri-
Bromophenol
(surr)
Chrvsene-d,,
Pyrene
Butylbenzyl
phthalate
3,3'-Dichloro
benzidine
Benzo(a)anthracene
Chrysene
bis-(2-Ethylhexyl)
phthalate
Terphenyl-d14 (surr)
Pervlene-d,,
Di-n-octyl
phthalate
Benzo(b)
fluoranthene
Benzo(k)
fluoranthene
Benzo(a)pyrene
Indenod, 2, 3-cd)
pyrene
Dibenzo(a,h)-
anthracene
Benzo(g,h,i)
perylene
surr = surrogate compound
D-63/SVOA
OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 3
Characteristic Ions for Internal Standards
for Semivolatile Compounds
Primary
Quantitation
INTERNAL STANDARDS Ion Secondary Ions
l,4-Dichlorobenzene-d4 152 115
Naphthalene-d8 136 68
Acenaphthene-dlO 164 162, 160
Phenanthrene-dlO 188 94, 80
Chrysene-dl2 240 120, 236
Perylene-dl2 264 . 260, 265
D-64/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 4
Characteristic Ions for Semivolatile
Target Compounds and Surrogates
Parameter
Benz aldehyde
Phenol
bis- (2-Chloroethyl) ether
2 -Chlorophenol
2 -Methylphenol
2,2' -oxybis (1-Chloropropane)
Acetophenone
4 -Methylphenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2 -Nitrophenol
2 , 4-Dimethylphenol
bis- (2 -Chloroethoxy) methane
2 , 4-Dichlorophenol
Naphthalene
4 -Chloroaniline
Hexachlorobutadiene
Caprolactam
4 - Chloro- 3 -methylphenol
2 -Methylnaphthalene
Hexachlorocyclopentadiene
2,4, 6-Trichlorbphenol
2,4, 5-Trichlorophenol
1,1' -Biphenyl
2 -Chloronaphthalene
2 -Nitroaniline
Dimethylphthalate
2 , 6 -Dinitrotoluene
Acenaphthylene
3 -Nitroaniline
Acenaphthene
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran
2 , 4 -Dinitrotoluene
Diethylphthalate
Fluorene
4-Chlorophenyl-phenylether
4 -Nitroaniline
4 , 6-Dinitro-2-methylphenol
4-Bromophenyl-phenylether
N-Nitrosodiphenylamine
Hexachlorobenzene
Atrazine
Pentachlorophenol
Primary
Quant it at ion
Ion
77
94
93
128
108
45
105
108
70
117
77
82
139
107
93
162
128
127
225
113
107
142
237
196
196
154
162
65
163
165
152
138
153
184
109
168
165
149
166
204"
138
198
248
169
284
200
266
Secondary Ion(s)
105, 106
65, 66
63, 95
64, 130
107
77, 79
77, 51
107
42, 101, 130
201, 199
123, 65
95, 138
65, 109
121, 122
95, 123
164, 98
129, 127
129
223, 227
55, 56
144, 142
141
235, 272
198, 200
198, 200 .
153, 76
164, 127
92, 138
194,- 164
89, 121
151, 153
108, 92
152, 154
63, 154
139, 65
139
63, 182
177, 150
165, 167
206, 141
92, 108
182, 77
250, 141
168, 167
142, 249
173, 215
264, 268
D-65/SVOA
OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagraihs/Flowcharts
Table 4 (cont'd)
Characteristic Ions for Semivolatile
Target Compounds and Surrogates
Primary
Quantisation
Parameter Ion __SecgndaryLjIgiils_L
Phenanthrene 178 179, 1?6
Anthracene 178 179, 176
Carbazole 167 166, 139
Di-n-butylphthalate 149 150, 104
Fluoranthene 202 101, 100
Pyrene 202 101, 100
Butylbenzylphthalate 149 91, 206
3,3'-Dichlorobenzidine 252 254, 126
Benzo(a)anthracene 228 229, 226
Chrysene 228 226, 229
bis-(2-Ethylhexyl)phthalate 149 167, 279
Di-n-Octyl phthalate 149 none
Benzo(b)fluoranthene 252 253, 125
Benzo(k)fluoranthene 252 253, 125
Benzo(a)pyrene 252 253, 125
Indeno(l,2,3-cd)pyrene 276 138, 227
Dibenzo(a,h)anthracene 278 139, 279
Benzo(g,h,i)perylene 276 138, 277
SURROGATES
Phenol-d5 99 42, 71
2-Fluorophenol 112 64
2,4,6-Tribromophenol 330 332, 141
Nitrobenzene-d5 82 128, 54
2-Fluorobiphenyl 172 171
Terphenyl-dl4 244 122, 212
2-Chlorophenol-d4 132 68, 134
1. 2-Dinhl orohgri7:eng-d4 152 115. 150
D-66/SVOA OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 5
Relative Response Factor Criteria for Initial and Continuing
Calibration of Semivolatile Target-Compounds and Surrogates
Semivolatile
Compounds
Benzaldehyde
Phenol
bis- (2-Chloroethyl) ether
2 -Chlorophenol
2 -Methylphenol
2,2' -oxybis- (1-Chloropropane)
Acetophenone
4 -Methylphenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2 -Nitrophenol
2 , 4 -Dimethylphenol
bis- ( 2 -Chloroethoxy) methane
2 , 4 -Dichlorophenol
Naphthalene
4 -Chloroaniline
Hexachlorobutadiene
Caprolactam
4 - Chloro - 3 - Me thylphenol
2 -Methylnaphthalene
Hexachlorocyclopentadiene
2,4,6- Tri Chlorophenol
2,4, 5 -Tri Chlorophenol
1,1' -Biphenyl
2 -Chloronaphthalene
2-Nitroaniline
Dimethylphthalate
2 , 6 -Dinitrotoluene
Acenaphthylene
3 -Nitroaniline
Acenaphthene
2 , 4 -Dinitrophenol
4 -Nitrophenol
Dibenzofuran
2 , 4 -Dinitrotoluene
Diethylphthalate
4 -Chlorophenyl-phenylether
Fluorene
4 -Nitroaniline
4, 6 -Dinitro- 2 -Methylphenol
4-Bromophenyl-phenylether
N-Nitrosodiphenylamine
Hexachlorobenzene
Atrazine
Pentachlorophenol
Phenanthrene
Minimum
RRF
0.010
0.800
0.700
0.800
0.700
0.010
0.010
0.600
0.500
0.300
0.200
0.400
0.100
0.200
0.300
0.200
0.700
0.010
0.010
0.010
0.200
0.400
0.010
0.200
0.200
0.010
0.800
0.010
0.010
0.200
0.900
0.010
0.900
0.010
0.010
0.800
0.200
0.010
0.400
0.900
0.010
0.010
0.100
0.010
0.100
0.010
0.050
0.700
Maximum
%RSD
none
20.5
20.5
20.5
20.5
none
none
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
none
none
none
20.5
20.5
none
20.5
20.5
none
20.5
none
none
20.5
20.5
none
20.5
none
none
20.5
20.5
none
20.5
20.5
none
none
20.5
none
20.5
none
20.5
20.5
Maximum
%Diff
none
±25.0
±25.0
±25.0
±25.0
none
none
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
none
none
none
±25.0
±25.0
none
±25.0
±25.0
none
±25.0
none
none
±25.0
±25.. 0
none
±25.0
none
none
±25.0
±25.0
none
±25.0
±25.0
none
none
±25.0
none
±25.0
none
±25.0
±25.0
D-67/SVOA
OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 5 (cont'd)
Relative Response Factor Criteria for Initial and Continuing
Calibration of Semivolatile Target Compounds and Surrogates
Semivolatile
Compounds
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene
Chrysene
bis- (2-Ethylhexyl)phthalate
Di -n-Octylphthalate
Benzo (b) f luoranthene
Benzo (k) f luoranthene
Benzo (a) pyrene
Indeno ( 1 , 2 , 3 - cd ) pyrene
Dibenzo (a, h) anthracene
Benzo (g,h, i)perylene
SURROGATES
Nitrobenzene -d5
2 - Fluorobiphenyl
Terphenyl - d!4
Phenol -d5
2 - Fluorophenol
2,4, 6 -Tribromophenol
2 - Chlorophenol - d4
1 . 2-Dichlorobenzene-d4
Minimum
RRF
0.700
0.010
0.010
0.600
0.600
0.010
0.010
0.800
0.700
0.010
0.010
0.700
0.700
0.700
0.500
0.400
0.500
0.200
0.700
0.500
0.800
0.600
0.010
0.800
0.400
Maximum
%RSD
20.5
none
none
20.5
20.5
none
none
20.5
20.5
none
none
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
none
20.5
20.5
Maximum
%Diff
±25.0
none
none
±25.0
±25.0
none
none
±25.0
±25.0
none
none
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
none
±25.0
+25.0
D-68/SVOA
OLM04.2
-------
Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 6
Matrix Spike Recovery and
Relative Percent Difference Limits
Compound
%Recovery RPD
%Recovery RPD Soil/ Soil/
Water Water Sediment Sediment
Phenol 12-110 42 26-90 35
2-Chlorophenol 27-123 40 25-102 50
N-Nitroso-di-n-propylamine 41-116 38 41-126 38
4-Chloro-3-Methylphenol 23-97 42 26-103 33
Acenaphthene 46-118 31 31-137 . 19
4-Nitrophenol 10-80 50 11-114 50
2,4-Dinitrotoluene 24-96 38 28-89 47
Pentachlorophenol . 9-103 50 17-109 47
Pyrene 26-127 31 35-142 36
D-69/SVOA
OLM04.2
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Exhibit D Semivolatiles -- Section 17
Tables/Diagrams/Flowcharts
Table 7
.Surrogate Recovery Limits
COMPOUND
Nitrobenzene-d5 (Base/Neutral)
2-Fluorobiphenyl (Base/Neutral)
Terphenyl-dl4 (Base/Neutral)
Phenol -d5 (Acid)
2-Fluorophenol (Acid)
2,4,6 -Tribromophenol (Acid)
2-Chlorophenol-d4 (Acid)
1, 2-Dichlorobenzene-d4
(Base/Neutral)
%Recovery
Water
35-114
43-116
33-141
10-110
21-110
10-123
33-110 (advisory)
16-110 (advisory)
%Recovery
Soil/Sediment
23-120
30-115
18-137
24-113
25-121
19-122
20-130 (advisory)
20-130 (advisory)
D-70/SVOA
OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
APPENDIX A - SCREENING OF SEMIVOLATILE ORGANIC EXTRACTS
1.0 SCOPE AND APPLICATION
1.1 The analytical method described in this section is designed to
characterize soil/sediment samples from hazardous waste sites for the
concentration level of organics.
1.2 The method involves the preparation of soil/sediment samples, which may
contain organic compounds at a level greater than 10,000 ug/kg, and
screening with a gas chromatograph equipped with a flame ionization
detector (GC/FID).
1.3 For soil/sediment samples, the results of the screen are used to
determine which of the two sample preparation procedures (low or medium)
is required, and to determine appropriate dilution factor for GC/MS
analysis. The results of the screen may also be used to assist the
analyst in performing Gel Permeation Chromatography (GPC) cleanup
procedures on extracts of either water or soil/sediment samples.
1.4 The procedure is designed to allow a quantitation limit for screening
purposes as low as 10,000 ug/kg for extractable organics. For analysis
purposes, the quantitation limit is 10,000 ug/kg for extractable
organics. Some samples may contain high concentrations of compounds
that interfere with the analysis of other components at lower levels;
the quantitation limits in those cases may be significantly higher.
1.5 These extraction and preparation procedures were developed for rapid and
safe handling of high concentration hazardous waste samples. The design
of the methods thus does not stress efficient recoveries or low limits
of quantitation of all components. Rather, the procedures were designed
to screen, at moderate recovery and sufficient sensitivity, a broad
spectrum of organic chemicals. The results of the analyses thus may
reflect only a minimum of the amount actually present in some samples.
2.0 SUMMARY OF METHOD
2.1 It is mandatory that all soil/sediment samples be characterized as to
concentration level so that the appropriate analytical protocol is
chosen to ensure proper quantitation limits for the sample. Note that
the terms "low level" and "medium level" are descriptions of the
concentration ranges that are encompassed by the "low" and "medium"
level procedures.
2.2 The laboratory is at liberty to select the method of characterization.
The following two screening methods may be used for soil/sediment sample
characterization.
Screen an aliquot from the "low level" 30 g extract or an aliquot
from the "medium level" 1 g extract.
Screen using GC/FID as the screening instrument.
D-71/SVOA OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
2.3 The concentration ranges covered by these two procedures may be
considered to be approximately 330 ug/kg - 10,000 ug/kg for the low
level analysis and >10,000 ug/kg for medium level analysis for
semivolatile extractables.
2.4 Sample Preparation
2.4.1 Low Level Soil/Sediment
A 30 g portion of soil/sediment is mixed with anhydrous powdered
sodium sulfate and extracted with 1:1 methylene chloride/acetone
using an ultrasonic probe. 5.0 mL of the 300 mL (approximate) total
extract is concentrated to 1.0 mL and screened. If the original
sample concentration is >10,000 ug/Kg the 30 g extract is discarded
and the medium level preparation procedure followed.
2.4.2 Medium Level Soil/Sediment
Approximately 1 g portions of soil/sediment are transferred to vials,
mixed with anhydrous powdered sodium sulfate, and extracted with
methylene chloride. 5.0 mL of the 10.0 mL extract is concentrated to
1.0 mL and screened. If the -sample concentration is <10,000 ug/Kg,
the 1 g extract is discarded and the low level method is followed.
2.5 GC/FID Screening
The concentrated extracts of soil/sediment or water samples are screened
on a gas chromatograph/flame ionization detector using a fused silica
capillary column (FSCC) for semivolatile priority pollutants and related
organics. The results of these screens will determine whether
sufficient quantities of pollutants are present to warrant analysis by
the medium level protocol.
3.0 INTERFERENCES
Method interferences may be caused by contaminants in solvents,
reagents, glassware, and other sample processing hardware that lead to
discrete artifacts and/or elevated baselines in the chromatograms. All
of these materials routinely must be demonstrated to be free from
interferences under the conditions of the analysis by running laboratory
method blanks. Matrix interferences may be caused by contaminants that
are co-extracted from the sample. The extent of matrix interferences
will vary considerably from source to source.
4 . 0 SAFETY
4.1 The toxicity or carcinogenicity of each reagent used in this method has
not been precisely determined; however, each chemical should be treated
as a potential health hazard. Exposure to these reagents should be
reduced to the lowest possible level. The laboratory is responsible for
maintaining a current awareness file of OSHA regulation regarding the
safe handling of the chemicals specified in this method. A reference
file of data handling sheets should be made available to all personnel
involved in these analyses. Specifically, concentrated sulfuric acid
presents some hazards and is moderately toxic and extremely irritating
D-72/SVOA OLM04.2
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Exhibit D Sernivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
to the skin and mucous membranes. Use these reagents in fume hoods
whenever possible, and if eye or skin contact occurs, flush with large
volumes of water.
4.2 Always wear safety glasses or a shield for eye protection, protective
clothing, and observe proper mixing when working with these reagents.
5.0 EQUIPMENT AND SUPPLIES
Brand names, suppliers, catalog and part numbers, are for illustrative
purposes only. No endorsement is implied. Equivalent performance may
be achieved using equipment and supplies other than chose specified
here, but demonstration of equivalent performance meeting the
requirements of this SOW is the responsibility of the Contractor.
5.1 Glassware
5.1.1 Continuous Liquid-Liquid Extractors - equipped with Teflon or glass
connecting joints and stopcocks requiring no lubrications (Hershberg-
Wolf Extractor, Ace Glass Company, Vineland, NJ. P/N 6841 10 or
equivalent).
5.1.2 Beakers - 400 mL
5.1.3 Syringes - 0.5 mL
5.1.4 Glass Scintillation Vials - at least 20 mL, with screw cap and Teflon
or aluminum foil liner.
5.1.5 Vials and Caps - 2 mL capacity for GC auto sampler.
5.1.6 Disposable Pipets - Pasteur, 1 mL.
5.1.7 Drying Column - 19 mm ID chromatographic column with coarse frit
(substitution of a small pad of Pyrex glass wool for the frit will
prevent cross contamination of sample extracts).
5.2 Kuderna-Danish (K-D) Apparatus
5.2.1 Concentrator Tubes - 15 mL and 10 mL graduated (Kontes K-570050-1025
and 570040-1025 or equivalent). Calibrations must be checked at the
volumes employed in the test. Ground-glass stoppers are used to
prevent evaporation of extracts.
5.2.2 Evaporative Flasks - 500 mL (Kontes K-570001-0500 or equivalent).
Attach to concentrator tube with springs.
5.2.3 Snyder Column - Two-ball Micro (Kontes K-569001-0219 or equivalent).
5.3 Spatula - stainless steel or Teflon
5.4 Balances - Analytical, capable of accurately weighing ± 0.0001 g, and
one capable of weighing 100 g to ± 0.01 g. The balances must be
calibrated with class S weights or known reference weights once per each
12-hour work shift. The balances must be- calibrated with class S
D-73/SVOA OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
5.5 Ultrasonic Cell Disrupters - Heat Systems, Ultrasonic Inc., Model W-385
Sonicator (475 watt with pulsing capability, No. 200, M inch tapped
disruptor horn, No. 419 1/8 inch standard tapered Microtip probe, and
No. 305, 3/4 inch tapered high gain "Q" disrupter horn, or No. 208 3/4
inch standard Solid disrupter horn), or equivalent devices with a
minimum of 375 watt output capability.
NOTE: In order to ensure that sufficient energy is transferred to the
sample during extraction, the Microtip probe or horn must be replaced if
the tip begins to erode. Erosion of the tip is evidenced by a rough
surface.
5.6 Sonabox Acoustic Enclosure - recommended with above disruptors for-
decreasing cavitation sound.
5.7 Vacuum Filtration Apparatus
5.7.1 Buchner Funnel
5.7.2 Filter paper - Whatman No. 41 or equivalent.
5.8 Pyrex Glass Wool - rinsed with methylene chloride.
5.9 Silicon Carbide Boiling Chips - approximately 10/40 mesh. Heat to
400 °C for 30 minutes or Soxhlet extract with methylene chloride.
5.10 Water Bath - heated, with concentric ring cover, capable .of temperature
control (±2 °C) . The bath should be used in a hood.
5.11 Nitrogen Evaporation Device - equipped with a water bath that can be
maintained at 35-40 °C. (N-Evap by Organomation Associates, Inc.,
South Berlin, MA, or equivalent). To prevent the release of solvent
fumes into the laboratory, the nitrogen evaporation device must be used
in a hood.
5.12 Gas Chromatograph/Flame lonization Detector (GC/FID System)
5.12.1 Gas Chromatograph - an analytical system complete with a temperature
programmable gas chromatograph and all required accessories including
syringes, analytical columns, and gases. The injection port must be
designed for on-column injection when using packed columns and for
splitless injection when using capillary columns.
5.12.2 Gas Chromatograph Column - 30 m (or longer) X 0.32 mm, 1 micron film
thickness, silicone coated, fused silica capillary column (J&W
scientific DB-5 or Equivalent). Note that this is minimum
requirement for column length. Longer columns.may be used.
5.12.3 Flame ionization Detector
D-74/SVOA OLM04.2
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6.0
Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
REAGENTS AND STANDARDS
6.1 Reagents
6.1.1 Reagent water - defined as water in which an interferant is not
observed at or above the CRQL for each analyte of interest.
6.1.2 Sodium Thiosulfate - (ACS) granular.
6.1.3 Sulfuric Acid Solution (1+1) - slowly add 50 mL of concentrated H 2SO4
(sp. gr. 1.84) to 50 mL of reagent water.
6.1.4 Acetone, methanol, methylene chloride - pesticide residue analysis
grade or equivalent.
6.1.5 Sodium Sulfate - anhydrous powdered reagent grade. Purify by heating
at 400 °C for four hours in a shallow tray. Cool in a desiccator and
store in a glass bottle (Baker anhydrous powder, catalog #73898 or
equivalent).
6.2 Standards
6.2.1 Introduction
The Contractor must provide all the standard solutions to be used
with this contract. These standards may be used only after they have
been certified according to the procedure in Exhibit E. The
Contractor must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must be retained by the
Contractor and presented upon request.
6.2.2 Stock Standard Solutions
6.2.2.1 Prepare or purchase a stock standard solution containing phenol,
phenanthrene, and di-n-octyl phthalate at concentrations of 1
ug/uL. Prepare stock standard solutions by accurately weighing
about 0.01 g of pure material. Dissolve the material in pesticide
quality methylene chloride and dilute to volume in a 10 mL
volumetric flask. Larger volumes may be used at the convenience
of the analyst. If compound purity is assayed at 97.0 percent or
greater, the weight may.be used without correction to calculate
the concentration of the stock standard. If the compound purity
is assayed to be less than 97.0 percent, the weight must be
corrected when calculating the concentration (see Exhibit E,
Analytical Standards Requirements). Commercially prepared stock
standards may be used at any concentration if they are certified
by the manufacturer or by an independent source (see Exhibit E).
6.2.2.2 -Transfer the stock standard solutions into Teflon-sealed screw-cap
bottles. Stock standard solutions should be checked frequently
for signs of degradation or evaporation, especially just prior to
preparing calibration standards from them. Stock standard
solutions must be replaced after six months or sooner if
comparison with quality control check samples indicates a problem.
D-75/SVOA
OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
6.2.3 Working Standard Solutions
6.2.3.1 Surrogate Standard Spiking Solution
Prepare a surrogate standard spiking solution that contains
nitrobenzene-d5, terphenyl-d14/ 2-fluorobiphenylt and 1,2-
dichlorobenzene-d4 at a concentration of 100 ug/mL; phenol-d 5,
2,4,6-tribromophenol, 2-fluorophenol, and 2-chlorophenol-d 4 at a
concentration of 150 ug/mL. Surrogate standards are added to all
samples and calibration solutions. Additional surrogates may be
added at the laboratory's discretion.
6.2.3.2 GC Calibration Standard
Prepare a working standard mixture of phenol, phenanthrene, and
di-n-octylphthalate. The concentration must be such that the
volume injected equals 50 ng of each compound.
6.2.4 Storage of Standards
6.2.4.1 Store the stock standard solutions at 4 °C (± 2°C) in Teflon-lined
screw-cap amber bottles and protect from light.
6.2.4.2 Store the working standards at 4 °C (± 2°C) in Teflon-sealed
containers. The solutions should be checked frequently for
stability. These solutions must be replaced after six months or
sooner if comparison with quality control check samples indicates
a problem.
6.2.4.3 Samples, sample extracts, and standards must be stored separately.
7.0 QUALITY CONTROL
7.1 Method Blank
7.1.1 Summary
A method blank is a volume of a clean reference matrix (reagent water
for water samples, or purified sodium sulfate for soil/sediment
samples) that is carried through the entire analytical procedure.
The volume or weight of the reference matrix must be approximately
equal to the volume or weight of samples associated with the blank.
The purpose of a method blank is to determine the levels of
contamination associated with the processing and analysis of samples.
7.1.2 Frequency
One method blank must be extracted and analyzed on each GC/FID system
used to screen samples for the following, whichever is most frequent.
D-76/SVOA . OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
Each SDG, or
» Each 20 samples in a n SDG, excluding matrix spikes/matrix spike
duplicates, that are of similar matrix (water, soil, or sediment)
or similar concentration (soil only), or
Whenever samples are extracted by the same procedure.
7.1.3 Procedure
For semivolatile analyses, a method blank for water samples consists
of a 1 L volume of reagent water spiked with 0.5 mL of the surrogate
spiking solution. For medium and low level soil/sediment samples,
method blanks consist of 1 g and 30 g of sodium sulfate spiked with
0.5 mL of surrogate -spiking solution, respectively. Extract and
concentrate method blanks at the same time as the samples associated
with the blanks according to Section 12.1. Analyze the method blank
according to Section 12.1. '
8.0 CALIBRATION AND STANDARDIZATION
8.1 GC/FID Operating Condition
Suggested GC operating conditions are as follows:
Initial column temperature hold - 20 °C for 4 minutes.
Column temperature program - 20-280 °C at 8 "C/minute.
Final column temperature hold - 280 °C for 8 minutes.
Injector - Grob-type, splitless.
Sample volume - 1-2 uL.
Carrier gas - Helium at 30 cm/sec.
8.2 GC Calibration
8.2.1 Summary
Prior to sample analysis, each GC/FID system must be initially
calibrated at one concentration level to determine instrument
sensitivity.
8.2.2 Frequency
Each GC/FID system must be calibrated at the beginning of each 12-
hour shift.
8.2.3 Procedure
Inject 1-2 uL of the GC calibration standard prepared in Section
6.2.3.2. The volume injected must equal 50 ng of each of the
calibration compounds.
D-77/SVOA OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
8.2.4 Technical Acceptance Criteria
8.2.4.1 The GC must be standardized for half-scale response from 50 ng of
phenanthrene.
8.2.4.2 The GC must adequately separate phenol from the solvent front.
8.2.4.3 A minimum of quarter-scale response for 50 ng of di-n-
octylphthalate must be exhibited.
8.2.5 Corrective Action
8.2.5.1 If the technical acceptance criteria are not met, recalibrate the
GC instrument. It may be necessary to change the column or take
other corrective actions to achieve the acceptance criteria.
8.2.5.2 GC calibration technical acceptance criteria must be met before
any samples are injected.
9 . 0 PROCEDURE
9.1 Sample Preparation
9.1.1 Low Level Soil/Sediment
9.1.1.1 Decant and discard any water layer on a sediment sample. Mix
samples thoroughly, especially composited samples. Discard any.
foreign objects such as sticks, leaves, and rocks.
9.1.1.2 Weigh approximately 30 g of sample to the nearest 0.1 g into a
400 mL beaker and proceed with low level soil/sediment sample
preparation as described in Section 10.1.4.4 of Exhibit D
(Semivolatiles).
9.1.1.3 Take 5 mL from the 300 mL (approximate) total extract and
concentrate to 1 mL following Section 10.2.2.1 or 10.2.2.2 of
Exhibit D (Semivolatiles,) but note that the final volume for
screening is 1 mL, not 0.5 mL.
9.1.2 Medium Level Soil/Sediment
9.1.2.1 Decant and discard any water layer on a sediment sample. Mix
samples thoroughly, especially composited samples. Discard any
foreign objects such as sticks, leaves, and rocks.
9.1.2.2 Transfer approximately 1 g (record weight to the nearest 0.1 g) of
sample to a 20 mL vial. Wipe the mouth of the vial with a tissue
to remove any sample material and proceed with the medium level
sample preparation procedure described in Section 10.1.4.5 of
Exhibit D (Semivolatiles).
9.1.2.3 Take 5 mL from the 10 mL total extract and concentrate to 1 mL
following Section 10.2.2.1 or 10.2.2.2 of Exhibit D
(Semivolatiles).
D-78/SVOA OLM04.2
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Exhibit D Semivolatiles -- Appendix A
Screening of Semivolatile Organic Extracts
9.2 GC/FID Analysis
Inject 1-2 uL of extract.
9.3 Interpretation Of Chromatograms
9.3.1 Soil/Sediment
9.3.1.1 If no sample peaks from the extract (from low or medium level
preparation) are detected or all are less than 10.0 percent full
scale deflection, the sample must be prepared by the low level
protocol.
9.3.1.2 Peaks are detected at greater than 10.0 percent full scale
deflection and less than or equal to full scale deflection.
If the screen is from the medium level extract, proceed with
GC/MS analysis of this extract with appropriate dilution if
necessary.
If the screen is from the low level extract, discard the
extract and prepare the samples by medium level method for
GC/MS analysis.
9.3.1.3 Peaks are detected at greater than full scale deflection.
If the screen is from the medium level preparation, calculate
the dilution necessary to reduce the major peaks to between
half and full scale deflection. Use this dilution factor to
dilute the extract. This dilution is analyzed by GC/MS for
extractable organics.
If the screen is from the low level preparation, discard the
extract and prepare the samples by the medium level method for
GC/MS analysis.
D-79/SVOA OLM04.2
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EXHIBIT D
ANALYTICAL METHODS
FOR PESTICIDES/AROCLORS
D-l/PEST OLM04.2
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Exhibit D - Analytical Methods for Pesticides/Aroclors
Table of Contents
Section Page
1.0 SCOPE AND APPLICATION 4
2 . 0 SUMMARY OF METHOD 5
2.1 Water 5
2.2 Soil/Sediment 5
3 .0 DEFINITIONS 5
4.0 INTERFERENCES 6
5.0 SAFETY 6
6.0 EQUIPMENT AND SUPPLIES 7
7.0 REAGENTS AND STANDARDS 13
7.1 Reagents 13
7.1.1 Reagent Water 13
7.1.2 Sodium Sulfate 13
7.1.3 Concentrated Sulfuric Acid 13
7.1.4 Sodium hydroxide solution 13
7.1.5 10 Percent Acetone in Hexane 13
7.1.6 Methylene Chloride, Hexane, Acetone, Toluene,
Iso-octane, and Methanol 13
7.1.7 Mercury 13
7.1.8 Copper Powder 13
7.2 Standards 13
7.2.1 Introduction 13
7.2.2 Stock Standard Solutions 14
7.2.3 Secondary Dilution Standards 14
7.2.4 Working Standards 14
7.2.5 Ampulated Standard Extracts 17
7.3 Storage of Standard Solutions 18
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE 19
8.1 Sample Collection and Preservation 19
8.2 Procedure for Sample Storage 19
8.3 Procedure for Sample Extract Storage 19
8.4 Contract Required Holding Times 19
9.0 CALIBRATION AND STANDARDIZATION 20
9.1 Gas Chromatograph Operating Conditions 20
9.2 ' Initial Calibration 20
9.2.1 Summary of Initial Calibration 20
9.2.2 Frequency of Initial Calibration 20
9.2.3 Procedure for Initial Calibration 21
9.2.4 Calculations for Initial Calibration 21
9.2.5 Technical Acceptance Criteria for Initial
Calibration 25.
9.2.6 Corrective Action for Initial Calibration 27
9.3 Calibration Verification . . 28
9.3.1 Summary of Calibration Verification 28
9.3.2 Frequency of Calibration Verification 28
D-2/PEST OLM04.2
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9.3.3 Procedure for Calibration Verification 29
9.3.4 Calculations for Calibration Verification 29
9.3.5 Technical Acceptance Criteria for
Calibration Verification . 29
9.3.6 Corrective Action for Calibration Verification 31
10.0 PROCEDURE . . . ; 33
10.1 Sample Preparation 33
10.2 GC/EC Analysis 54
11.0 DATA ANALYSIS AND CALCULATIONS 59
11.1 Qualitative Identification ..... 59
11.1.1 Identification of Target Compounds 59
11.1.2 GC/MS Confirmation of Pesticides and Aroclors ... 59
11.2 Calculations 62
11.2.1 Target Compounds 62
11.2.2 CRQL Calculation 65
11.2.3 Surrogate Recoveries 65
11.3 Technical Acceptance Criteria for Sample Analysis 66
11.4 Corrective Action for Sample Analysis 67
12.0 QUALITY CONTROL 69
12.1 Blank Analyses 69
12.1.1 Introduction 69
12.1.2 Method Blanks 69
12.1.3 Sulfur Cleanup Blanks 71
12.1.4 Instrument Blanks 73
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD) 74
12.2.1 Summary of MS/MSD 74
12.2.2 Frequency of MS/MSD Analysis 74
12.2.3 Procedure for Preparing MS/MSD 75
12.2.4 Calculations for MS/MSD 76
12.2.5 Technical Acceptance Criteria for MS/MSD 76
12.2.6 Corrective Action for MS/MSD 77
13.0 METHOD PERFORMANCE 78
14.0 POLLUTION PREVENTION 78
15.0 WASTE MANAGEMENT ' 78
16.0 REFERENCES 78
17.0 TABLES/DIAGRAMS/FLOWCHARTS 79
D-3/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 1
Scope and Application
1.0 SCOPE AND APPLICATION
1.1 In 1978, EPA Headquarters and Regional representatives designed
analytical methods for the analysis of chlorinated pesticides and
Aroclors in hazardous waste samples. These methods were based on EPA
Method- 608, Organochlorine Pesticides and PCBs. In 1980, these methods
were adopted for use in the Contract Laboratory Program (CLP). As the
requirements of CERCLA evolved, the CLP methods, as well as their
precedent EPA 600 Series methods, established the basis for other EPA
methods to perform the analysis of chlorinated pesticides and Aroclors
in hazardous waste samples (i.e., SW-846) . The following CLP method has
continuously improved to incorporate technological advancements
promulgated by EPA, and has continued to set the standard for the
preparation, extraction, isolation, identification, and reporting of
chlorinated pesticides and Aroclors at hazardous waste sites.
| 1.2 The analytical method that follows is designed to analyze water,
sediment, and soil from hazardous waste sites to determine the presence
and concentration of the chlorinated pesticides and Aroclors found in
the Target Compound List (TCL) in Exhibit C. The method can be used for
determining analyte concentrations in the range from the contract
required quantitation limits (CRQL) to one million times the CRQL in
| these matrices when appropriate dilutions are made. The method includes
sample extraction, extract cleanup techniques and GC/EC analytical
methods for pesticides and Aroclors.
| 1.3 This analytical method provides the use of SW-846 Methods 3541 (Revision
| 0, September 1994) and 3545 (Revision 0, December 1996) for the
| extraction of soil/sediment samples. However, prior to using either one
| of these alternate extraction procedures, the Contractor must first
| demonstrate that these procedures are equivalent to the existing
| procedures, and obtain approval for use of these alternate extraction
| procedures from the EPA CLP National Program Manager. The process for
| determining and documenting equivalency can be found in Exhibit E
| Section 6.0.
| 1.4 Problems, including resolution difficulties, have been associated with
the following pairs of compounds using this method.
On a DB-608 or equivalent column, DDE and dieldrin; methoxychlor and
endrin ketone; and endosulfan I and gamma-Chiordane.
On a DB-1701 or equivalent column, endosulfan I and gamma-Chlordane,
and methoxychlor and endosulfan sulfate.
| 1.5 There are two isomers of heptachlor epoxide, the endo isomer (isomer A)
and the exo isomer (isomer B). The two isomers are separable using
current GC capillary'columns. Only the exo isomer (isomer B) is of
environmental significance. This is the isomer that must be used as an
analytical standard, identified and quantitated in sample analysis, and
reported on appropriate forms as heptachlor epoxide.
D-4/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Sections 2 & 3
Summary of Method/Definitions
2.0 SUMMARY OF METHOD
2.1 Water
Continuous liquid-liquid or separator/ funnel extraction procedures are
employed for aqueous samples. AIL volume of sample is spiked with the
surrogate solution and extracted with methylene chloride using a
separatory funnel or a continuous extractor. The methylene chloride
extract is dried with anhydrous sodium sulfate, concentrated, and
cleaned up by GPC (GPC is required when higher molecular weight
compounds are present that interfere with the analyses of target
compounds; GPC is optional for all other circumstances). The extract is
then solvent exchanged into hexane, cleaned up by Florisil cartridges,
and the final volume adjusted to 1 mL or 2 mL. The extract is analyzed
using a dual column wide-bore capillary Gas Chromatography/Electron
Capture (GC/EC) technique.
2.2 Soil/Sediment
A 30 g aliquot of sample is spiked with the surrogate and then mixed
with anhydrous sodium sulfate and extracted with a 1:1 acetone/methylene
chloride solvent mixture by sonication. The extract is filtered,
concentrated and solvent-exchanged into methylene chloride. The
methylene chloride extract is then cleaned up by GPC (mandatory).
solvent-exchanged into hexane, cleaned up by Florisil cartridge, and
adjusted to a final volume of 1 mL or 2 mL. The extract is analyzed
using a dual column wide-bore capillary Gas Chromatography/Electron
Capture (GC/EC) technique.
3.0 DEFINITIONS
See Exhibit G for a complete list of definitions.
D-5/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Sections 4 & 5
Interferences/Safety
4.0 INTERFERENCES
4.1 Method interferences may be caused by contaminants in solvents,.
reagents, glassware, and other sample processing hardware. These
contaminants lead to discrete artifacts or to elevated baselines in gas
chromatograms. Routinely, all of these materials must be demonstrated
to be free from interferences under the conditions of the analysis by
running reagent blank. Interferences caused by phthalate esters can
pose a major problem in pesticide analysis. Common flexible plastics
contain-varying amounts of phthalates which are easily extracted during
laboratory operations, so cross-contamination of glassware frequently
occurs when plastics are handled. Interferences from phthalates can
best be minimized by avoiding the use of such plastics in the
laboratory.
4.2 Matrix interferences may be caused by contaminants that are co-extracted
from the sample. The extent of matrix interferences will vary
considerably from source to source, depending upon the nature of the
site being sampled. The cleanup procedures must be used to remove such
interferences in order to achieve the contract required quantitation
limits.
5.0 SAFETY
5.1 The toxicity or carcinogenicity of each reagent used in this method has
not been precisely determined; however, each chemical should be treated
as a potential health hazard. Exposure to these reagents should be
reduced to the lowest possible level. The laboratory is responsible for
maintaining a current awareness file of OSHA regulations regarding the
safe handling of the chemicals specified in this method. A reference
file of data handling sheets should be made available to all personnel
involved in these analyses. Specifically, concentrated sulfuric acid
and the 10 N sodium hydroxide solution are moderately toxic and
extremely irritating to skin and mucous membranes. Use these reagents
in a fume hood whenever possible and if eye or skin contact occurs,
flush with large volumes of water. Always wear safety glasses or a
shield for eye protection, protective clothing, and observe proper
mixing when working with these reagents.
5.2 The following analytes covered by this method have been tentatively
classified as known or suspected human or mammalian carcinogens: 4,4'-
DDT, 4,4'-DDD, the BHCs, and the-Aroclors. Primary standards of these
toxic compounds should be prepared in a hood. A NIOSH/MESA approved
toxic gas respirator should be worn when the analyst handles high
concentrations of these toxic compounds.
' D-6/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
6.0 EQUIPMENT AND SUPPLIES
Brand names, suppliers, and part numbers are for illustrative purposes
only. No endorsement is implied. Equivalent performance may be
achieved using equipment and supplies other than those specified here,
but demonstration of equivalent performance meeting the requirements of
this Statement of Work is the responsibility of the Contractor. The
Contractor must document in its Narrative when it uses equipment and
supplies other than those specified here.
6.1 Glassware
6.1.1 Continuous Liquid-Liquid Extractors - equipped with Teflon or glass
connecting joints and stopcocks requiring no lubrication (Hershberg-
Wolf extractor, Ace Glass Company, Vineland, NJ P/N 6841-10, or
equivalent) or Hydrophobic Membrane-based Extractor (Accelerated One
Step Extractor, Corning series 3195, or equivalent).
6.1.2 Separatory Funnels - 2 L with Teflon stopcock.
6.1.3 Beakers.- 400 inL.
6.1.4 Erlenmeyer Flasks - 250 mL.
6.1.5 Syringes - 10 mL with Luerlok fitting, 1 mL or 2 mL.
6.1.6 Vials and Caps - 20 mL and 10 mL (optional) with screw cap and Teflon
or aluminum foil liner, 2 mL capacity for GC auto sampler.
6.1.7 Pipets - glass volumetric 1 mL or 2 mL.
6.1.8 Centrifuge Tube - 12 to 15 mL with 19 mm ground glass joint
(optional).
6.1.9 Graduated Cylinder - 1 L capacity.
6.1.10 Drying Column - chromatographic column approximately 400 mm long x 19
mm ID, with coarse frit. (Substitution of a small pad of disposable
Pyrex glass wool for the frit will help prevent cross-contamination
of sample extracts).
6.1.11 Volumetric Flasks - 10 mL and 1 or 2 mL.
6.1.12 Bottle or Test Tube - 20 mL with Teflon-lined screw cap for sulfur
removal and a glass bottle - 1 L volume, for use in preparation of
Bio Beads for packing into a column.
6.1.13 Powder Funnels - 10 cm diameter, for filtration/drying.
6.1.14 Buchner Funnels - 9 cm diameter, for filtration.
6.2 Kuderna-Danish (K-D) Apparatus.
6.2.1 Concentrator Tubes - 10 mL, graduated (Kontes K-570040-1029, or
equivalent).
D-7/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
6.2.2 Evaporative Flasks - 500 mL (Kontes K-470001-0500, or equivalent).
6.2.3 Snyder Column - three-ball macro (Kontes K-503000-0121, or
equivalent).
6.2.4 Snyder Column - two-ball micro (Kontes K-569001 -0219, or
equivalent).
6.3 Vacuum System for Eluting Multiple Cleanup Cartridges.
6.3.1 Vac Elute Manifold - Analytichem International, J.T. Baker, or
Supelco (or equivalent). The manifold design must ensure that there
is no contact between plastics containing phthalates and sample
extracts.
6.3.2 Vacuum Trap - made- from a 500 mL sidearm flask fitted with a one-hole
stopper and glass tubing.
6.3.3 Vacuum Pressure Gauge.
6.3.4 Rack for holding 10 mL volumetric flasks in the manifold.
NOTE: Other types of equivalent systems, such as an automated system
using syringe pressure, are considered to be acceptable for elution
of florisil cartridges, as long as all QC-and sample technical
acceptance criteria are met.
6.4 pH Paper - wide range (Hydrion Papers, Micro-essential Laboratory,
Brooklyn, NY, or equivalent).
6.5 Spatula - stainless steel or Teflon.
6.6 Centrifuge - table top (optional).
6.7 Balances - top loading, capable of weighing accurately to ± 0.01 g,
analytical, capable of weighing accurately to ± 0.0001 g. The balances
must be calibrated with class S weights or known reference weights once
per each 12-hour work shift. The balances must be calibrated with class
S weights at a minimum of once per month. The balances must also be
annually checked by a certified technician.
6.8 Ultrasonic Cell Disrupter - Heat Systems, Ultrasonics, Inc., Model W-385
(475 watt with pulsing capability, No. 207 3/4-inch tapered disrupter
horn) or equivalent device with a minimum 375 watt output capability.
NOTE: In order to ensure that sufficient energy is transferred to the
sample during extraction, the horn must be replaced if the tip begins to
erode. Erosion of the tip is evidenced by a rough surface.
6.9 Sonabox Acoustic Enclosure (or equivalent) - for use with disrupter to
decrease noise level.
6.10 Filter Paper - No. 41 Whatmann (or equivalent), 9 cm circles (optional).
6.11 Pyrex Glass Wool - rinsed with methylene chloride and dried before use.
6.12 Boiling chips.
D-8/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
6.12.1 Silicon carbide boiling chips - approximately 10 to 40 mesh. Heat
the chips to 400 °C for 30 minutes or solvent rinse before use.
6.12.2 Teflon boiling chips (optional) - solvent rinse the chips before use.
6.13 Water Bath - heated, with concentric ring cover, capable of temperature
control. NOTE: The water bath should be used in a hood.
6.14 GPC Cleanup System
6.14.1 Gel Permeation Chromatography System - GPC Autoprep Model 1002 A or
B, Analytical Biochemical Laboratories, Inc., or equivalent. Systems
that perform satisfactorily have been assembled from the following
components: an HPLC pump, an auto sampler or a valving system with
sample loops, and a fraction collector. All systems, whether
automated or manual,, must meet the calibration requirements of
Section 10.1.8.1. NOTE: GPC cleanup is required for extracts for
all soils/sediments and for water extracts containing higher
molecular weight contaminants that interfere with the analyses of the
target compounds.
6.14.1.1 Chromatographic column - 700 mm x 25 mm ID glass column. Flow is
upward. To simplify switching from the UV detector during
calibration to the GPC collection device during extract cleanup,
an optional double 3-way valve (Rheodyne Type 50 Teflon Rotary
Valve #10-262 or equivalent) may be attached to that the column
exit flow can be shunted either to the UV flow-through cell or to
the GPC collection device.
6.14.1.2 Guard column (optional) - 5 cm, with appropriate fittings to
connect to the inlet side of the.analytical column (Supelco 5-8319
or equivalent).
6.14.1.3 Bio Beads (SX-3) - 200 to 400 mesh, 70 g (Bio-Rad Laboratories,
Richmond, CA, Catalog 152-2750, or equivalent). An additional 5 g
of Bio Beads is required if the optional guard column is employed.
The quality of Bio Beads may vary from lot to lot because of
excessive fines in some lots. In addition to fines having a
detrimental effect on Chromatography, they can also pass through
the column screens and damage the valve.
6.14.1.4 Ultraviolet detector - fixed wavelength (254 nm) with a semi-prep
flow-through cell.
6.14.1.5 Strip chart recorder - recording integrator or laboratory data
system.
6.14.1.6 Syringe filter assembly, disposable - Bio-Rad "Prep Disc" sample
filter assembly #343-0005, 25 mm, and 5 micron filter discs or
equivalent. Note: Some instrument manufacturer's recommend a
smaller micron filter disc. Consult your instrument operation
manual to determine the proper size filter disc to use in your
system. Check each batch for contaminants. Rinse each filter
assembly (prior to use) with methylene chloride if necessary.
D-9/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
6.15 Florisil - 500 mg or 1 g cartridges with stainless steel or Teflon
frits, (catalog No. 694-313, Analytichem, 24201 Frampton Ave., Harbor
City, CA, or equivalent).
6.16 Nitrogen Evaporation Device - equipped with a heated bath that can be
maintained at 35 to 40 °C (N-Evap by Organomation Associates, Inc.,
South Berlin, MA, or equivalent).
6.17 Oven - drying.
6.18 Desiccator.
6.19 Crucibles - porcelain crucibles or aluminum weighing pans.
6.20 pH Meter - with a combination glass electrode. Calibrate according to
manufacturer's instructions. pH meter must be calibrated prior to each
use.
6.21 Magnetic Stirrer Motor - Model PC 353, Corning Co., Corning, NY, or
equivalent.
6.22 Magnetic Stirrer Bar - Teflon coated, at least 4 cm long.
&.23 Gas Chromatograph/Electron Capture Detector (GC/EC) System.
6.23.1 Gas Chromatograph - must adequately regulate temperature in order to
give a reproducible temperature program and have a flow controller
that maintains a constant column flow rate throughout temperature
program operations. The system must be suitable for split less
injection and have all required accessories including syringes,
analytical columns, and gases..
6.23.2 Gas chromatographs that are available from some manufacturers may
have difficulty in meeting certain method QC requirements because of
endrin and DDT breakdown in the injector. This problem can be
minimized by operating the injector at 200 - 205 °C, using a Pvrex
(not quartz) methyl silicone deactivated injector liner, and
deactivating the metal parts in the injector with dichlorodimethyl
silane. In some cases, using a 0.25 inch packed column injector
converted for use with 0.53 mm capillary columns works better than a
Grob-type injector. If a Grob-type injector is used, a 4 mm liner
may be required to meet breakdown criteria.
6.23.3 Gas Chromatograph Columns - two wide-bore (0.53 mm ID) fused silica
GC columns are required. A separate detector is required for each
column. The specified analytical columns are a 30 m x 0.53 mm ID,
1.0 urn film thickness, DB-1701 (J&W Scientific); SPB 1701 (Supelco);
AT 1701 (Alltech); RTX-1701 (Restek); CP-Sil 19CB (Chrompack); 007-
1701 (Quadrex); BP-10 (SGE); or equivalent, and a 30 m x 0.53 mm ID,
0.5 to 1.0 urn film thickness DB-608 (J&W Scientific); HP-608 (Hewlett
Packard); SPB-608 (Supelco); 007-608 (Quadrex); BP-608 (SGE); CP-Sil
8CB (Chrompack); or equivalent. NOTE: The column length stated
above is the minimum requirement. Longer columns that meet
resolution and calibration requirements may be used. A description
of the GC columns used for analysis shall be provided in the SDG
Narrative.
D-10/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
6.23.3.1 PACKED COLUMNS CANNOT BE USED
. ^
6.23.3.2 A capillary column is considered equivalent if:
The column does not introduce contaminants which interfere with
identification and quantitation of the compounds listed in
Exhibit C (Pesticides)
The analytical results generated using the column meet the
initial calibration and calibration verification technical
acceptance criteria listed in the SOW and the CRQLs listed in
Exhibit C (Pesticides).
The column can accept at least 16 times the low point standard
for individual standard mixtures A and B for each compound
listed in Exhibit C (Pesticides) without becoming overloaded.
The column pair chosen must have dissimilar phases/chemical
properties in order to separate the compounds of interest in
different RT order.
6.23.3.3 Although the instructions included in the SOW are for wide bore
capillary columns, narrower bore capillary columns may be
.evaluated for use. .
6.23.3.4 . As. applicable, follow the manufacturer's instructions for use of
its product.
6.23.3.5 The Contractor must maintain documentation that the column met the
criteria in Section 6.23.3.2. The minimum documentation is as
follows:
6.23.3.5.1 Manufacturer provided information concerning the performance
characteristics of the column;
6.23.3.5.2 Chromatograms and data system reports generated on the GC/ECD
and used for CLP analyses:
From instrument blanks which demonstrate that there are no
contaminants which interfere with the pesticide analysis
when using the alternate columns;
For initial calibration standards analyzed using the column;
.. For calibration verification standards analyzed using the
alternate column.
6.23.3.5.3 Based on the Contractor generated data des.cribed in Section
6.23.3.5.2, the Contractor must complete a written review,
aligned'by the Laboratory Manager certifying that:
The column performance is comparable to the required column
performance in its ability to produce initial calibration
and calibration verifications which meet the technical
acceptance criteria in Sections 9.2.5 and 9.3.5.
D-11/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 6
Equipment and Supplies
The low point initial calibration standard analyses have
adequate sensitivity to meet the pesticide CRQLs.
The high point initial calibration standard analyses were
not overloaded.
The column does not introduce contaminants which interfere
with identification and quantitation of compounds listed in
Exhibit C (Pesticides). '
6.23.3.5.4 The documentation must be made available to the Agency during
on-site laboratory evaluations or sent to the Agency upon
request of the Technical Project Officer or the Administrative
Project Officer.
6.23.3.6 Columns are mounted in a 0.25-inch injector ports, by using glass
adapters available from a variety of commercial sources (J&W
Scientific, Supelco, Inc., Hewlett-Packard, Varian, Inc., Perkin
Elmer, or equivalent) . The two columns may be mounted into a
single injection port with a tee adapter (Supelco, Inc.,
Bellefonte, PA, Catalog No. 2-3660, or equivalent). Use of this
adapter allows simultaneous injection onto both columns. The
laboratory should follow manufacturer's recommendations for
mounting 0.53 mm capillary columns in injector ports.
6.23.3.7 The carrier gas for routine applications is helium.. Laboratories
may choose to use hydrogen as a carrier gas, but they must clearly
identify its use in the SDG Narrative and on all divider pages
preceding raw chromatographic data in submissions to the Agency.
Laboratories that choose to use hydrogen are advised.to exercise
caution in its use. Use of a hydrogen leak detector is highly
recommended when hydrogen is used as the carrier gas. All GC
carrier gas lines must be constructed from stainless steel or
copper tubing. Non-polytetrafluoroethylene (PTFE) thread sealants
or flow controllers with rubber components are not to be used.
6.23.4 Electron Capture Detector (BCD) - the linearity of the response of
the ECD may be greatly dependent on the flow rate of the make-up gas.
The make-up gas must be P-5, P-10 (argon/methane) or nitrogen
according to the instrument specification. Care must be taken to
maintain stable and appropriate flow of make-up gas to the detector.
The GC/EC system must be in a room in which the atmosphere has been
demonstrated to be free of all contaminants which may interfere with
the analysis. The instrument must be vented to outside the facility
or to a trapping system which prevents the release of contaminants
into the instrument room.
6.23.5 Data System - a data system must be interfaced to the GC/EC. The
data system must allow the continuous acquisition of data throughout
the duration of the chromatographic program and must permit, at the
minimum, the output of time vs. intensity (peak height or peak area)
data. Also, the data system must be able to rescale chromatographic
data in order to report chromatograms meeting the requirements listed
within this method.
D-12/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 7
Reagents and Standards
7.0 REAGENTS AND STANDARDS .
7.1 Reagents
7.1.1 Reagent Water - defined as water in which no interferant is observed
at one-half the CRQL of any pesticide/Aroclor when one liter of the
reagent water is extracted and prepared by using the same workup
procedure as for a water sample.
7.1.2 Sodium Sulfate - granular-anhydrous reagent grade, heated at 400 °C
for 4 hours, or at 120 °C for 16 hours, cooled in a desiccator, and
stored in a glass bottle. Each lot must be extracted with hexane and
analyzed by GC/EC to demonstrate that it is free of interference
before use. Baker anhydrous granular, Catalog No. 3375, or
equivalent. CAUTION: An open container of sodium sulfate may become
contaminated during storage in the laboratory.
7.1.3 Concentrated Sulfuric Acid (H2SO4)- 18 N.
7.1.4 Sodium Hydroxide Solution (NaOH) (10 N) - carefully dissolve 40 g of
NaOH in reagent water and dilute the solution to 100 mL.
7.1.5 10 Percent Acetone in Hexane (v/v) - prepare by adding 10 mL of
acetone to 90 mL of hexane. NOTE: Prepare this mixture accurately
or the results from the Florisil cartridge cleanup will be adversely
affected. Water in the acetone also will adversely affect Florisil
performance.
7.1.6 Methylene Chloride, Hexane, Acetone, Toluene, Iso-octane, and
Methanol (optional) - pesticide quality or equivalent. It is
recommended that each lot of solvent used be analyzed to demonstrate
that it is free of interference before use. Methylene chloride must
be certified as acid free or must be tested to demonstrate that it is
free of hydrochloric acid. Acidic methylene chloride must be passed
through basic alumina and then demonstrated to be free of
hydrochloric acid.
7.1.7 Mercury - triple distilled, for sulfur cleanup.
7.1.8 Copper Powder (optional) - fine, granular (Mallinckrodt 4649 or
equivalent). Copper may be used instead of mercury for sulfur
cleanup. Remove oxides by treating with dilute nitric acid, rinse
with distilled water to remove all traces of acid, rinse with
acetone, and dry under a stream of nitrogen.
7.2 Standards
7.2.1 Introduction
The Contractor must provide all standards to be used with this
contract. These standards may be used only after they have been
certified according to the procedure in Exhibit E. The Contractor
must be able to verify that the standards are certified.
Manufacturer's certificates of analysis must be retained by the
Contractor and presented upon request.
.D-13/PEST OLM04.2
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Exhibit D Festicides/Aroclors -- Section 7
Reagents and Standards
7.2.2 Stock Standard Solutions (1 ug/uL) - can be prepared from pure
standard materials or purchased as certified solutions.
7.2.2.1 Prepare stock standard solutions by accurately weighing about
0.0100 g of pure material. Dissolve the material in toluene and
dilute to volume in a 10 mL volumetric flask with toluene or
acetone. Larger volumes may be used at the convenience of the
analyst.
7.2.2.2 When compound purity is assayed to be 97 percent or greater, the
weight may be used without correction to calculate the
concentration of the stock solution. If the compound purity is
assayed to be less than 97 percent, -the weight must be corrected
when calculating the concentration of the stock solution. (See
Exhibit E Analytical Standards Requirements.)
7.2.2.3 Fresh stock standards must be prepared once every six months, or
sooner if standards have degraded or concentrated. Stock
standards must be checked for signs of degradation or
concentration just prior to preparing working standards from them.
7.2.3 Secondary Dilution Standards
Using stock standards, prepare secondary dilution standards in
acetone that contain the compounds of interest either singly or mixed
together. Fresh secondary dilution standards must be prepared once
every six months, or sooner if standards have degraded or
concentrated. Secondary dilution standards must be checked for signs
of degradation or concentration just prior to preparing working
standards from them.
7.2.4 Working Standards
7.2.4.1 Surrogate Standard Spiking Solution
The surrogates, tetrachloro-m-xylene and decachlorobiphenyl, are
added to all standards, samples, matrix spikes, and blanks.
Prepare a surrogate spiking solution of 0.2 ug/mL of each of the
two compounds in acetone.
7.2.4.2 Matrix Spiking Solution
Prepare a matrix spiking solution in acetone or methanol that
contains the following pesticides at the concentrations specified:
Pesticide Concentration ug/mL
gamma-BHC (Lindane) . 0.5
4,4'-DDT 1.0
Endrin 1.0
Heptachlor 0.5
Aldrin 0.5
Dieldrin 1.0
D-14/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 7
Reagents and Standards
| 7.2.4.3 GPC Calibration and Calibration Verification Solutions
| 7.2.4.3.1 Prepare a GPC calibration solution in methylene chloride that
contains the following analytes at the minimum concentrations
listed below:
Analvte Concentration mq/mL
Corn oil . 25.0
Bis-2-ethylhexyl phthalate 0.5
Methoxychlor 0.1
Perylene 0.02
Sulfur . 0.08
7.2.4.3.2 NOTE: Sulfur is not very soluble in methylene chloride, but it
is soluble in warm corn oil. Therefore, one approach is to
weigh out the corn oil, warm it, and transfer .the weighed
amount of sulfur into the warm corn oil. Mix it and then
transfer into a volumetric flask with methylene chloride, along
with the other calibration compounds.
| 7.2.4.3.3 GPC Calibration Verification Solution
Prepare a GPC calibration verification solution in methylene
chloride that contains the following compounds. The
concentrations listed below are for a 5 mL GPC injection loop.
See'section 10.1.8.1.4.3 for compound concentrations if a
smaller size loop is being used.
Compound Concentration UQ/mL
gamma-BHC (Lindane) 0.1
Heptachlor 0.1
Aldrin 0.1
4,4 '-DDT 0.2
Endrin 0.2
Dieldrin 0.2
The Aroclor mixture contains 2 ug/mL each of Aroclor 1016 and
1260 in methylene chloride.
7.2.4.4 Florisil Cartridge Check Solution
Prepare a solution of 2,4,5-Trichlorophenol in acetone, at a
concentration of 0.1 ug/mL.
P-15/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 7
Reagents and Standards
7.2.4.5 Resolution Check Mixture
Prepare a mixture in hexane or iso-octane that contains the
following pesticides and surrogates at the concentrations listed
below.
Compound Concentration (ng/mL)
gamma-Chlordane 10.0
Endosulfan I 10.0
4,4'-DDE 20.0
Dieldrin 20.0
Endosulfan sulfate. 20.0
Endrin ketone 20.0
Methoxychlor 100.0
Tetrachloro-m-xylene 20.0
Decachlorobiphenyl 20.0
7.2.4.6 Performance Evaluation Mixture (PEM)
Prepare the PEM in hexane or iso-octane at the concentration
levels listed below.
Compound Concentration (ng/mL)
gamma-BHC 10.0
alpha-BHC 10.0
4, 4'-DDT 100.0
beta-BHC 10.0
Endrin 50.0
Methoxychlor 250.0
Tetrachloro-m-xylene 20.0
Decachlorobiphenyl 20.0
7.2.4..7 Individual Standard Mixtures A and B
The single component pesticide standards must be prepared in
hexane or iso-octane at three concentrations for each analyte,
including the surrogates. Two separate calibration mixtures, A
and B (listed below), are used to ensure that each peak is
adequately resolved. The low point concentration corresponds to
the CRQL for each analyte. The midpoint concentration must be 4
times the low point concentration. The high point concentration
must be at least 16 times that of the low point, but a higher
concentration may be chosen by the Contractor. The high point
concentration defines the upper end of the concentration range for
which the calibration is valid.
D-16/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 7
Reagents and Standards
Individual Standard Mixture A
Low Point Concentration
alpha-BHC 5.0 ng/mL
Heptachlor 5.0 ng/mL
gamma-BHC 5.0 ng/mL
Endosulfan I 5.0 ng/mL
Dieldrin 10.0 ng/mL
Endrin 10.0 ng/mL
4,4'-DDD 10.0 ng/mL
4,4'-DDT 10.0 ng/mL
Methoxychlor 50.0 ng/mL
Tetrachloro-m-xylene 5 . 0 ng/mL
Decachlorobiphenyl 10.0 ng/mL
Individual Standard Mixture B
Low Point Concentration
beta-BHC
delta-BHC
Aldrin
Heptachlor Epoxide
(exo-epoxy isomer)
alpha-Chlordane
gamma-Chlordane
4,4'-DDE
Endosulfan sulfate
Endrin aldehyde
Endrin ketone
Endosulfan II
Tetrachloro-m-xylene
Decachlorobiphenyl
5.0 ng/mL
5.0 ng/mL
5.0 ng/mL
5.0 ng/mL
5.0 ng/mL
5.0 ng/mL
10.0 ng/mL
10.0 ng/mL
10.0 ng/mL
10.0 ng/mL
10.0 ng/mL
5.0 ng/mL
10.0 ng/mL
NOTE: Only the exo-epoxy isomer (isomer B) of heptachlor epoxide
is used as an analytical standard.
7.2.4.8 Multicomponent Standards
Toxaphene and Aroclor standards must be prepared individually
except for Aroclor 1260 and Aroclor 1016 which may be combined in
one standard mixture. The calibration standards for the Aroclors
must be prepared at concentrations of 100 ng/mL, except for
Aroclor 1221 which must be prepared at 200 ng/mL. Toxaphene must
be prepared at 500 ng/mL. All multicomponent standards must
contain the surrogates at 20 ng/mL. The Aroclor and toxaphene
solutions must be prepared in hexane or iso-octane.
7.2.5 Ampulated Standard Extracts
Standard solutions purchased from a chemical supply house as
ampulated extracts in glass vials may be retained until the
expiration date provided by the manufacturer. If no manufacturer's
expiration date is provided, the standard solutions as ampulated
extracts may be retained and used for 2 years from the preparation
date. Standard solutions prepared by the Contractor which are
D-17/PEST
OLM04.2
-------
Exhibit D festicides/Aroclors -- Section 7
Reagents and Standards
immediately ampulated in glass vials may be retained 2 years from the
preparation date. Upon breaking the glass seal, the expiration times
listed in Sections 7.2.2 through 7.3 will apply. The Contractor is
responsible for assuring that the integrity of the standards have not
degraded (see Section 7.3.5).
7.3 Storage of Standard Solutions
| 7.3.1 Store the stock and secondary dilution standard solutions at
j . 4 °C (± 2°C) in Teflon-lined screw cap amber bottles/vials. Fresh
standards should be prepared every six months, or sooner if
comparison with check standards indicates a problem.
7.3.2 Store the GPC calibration solution in an amber glass bottle with a
| Teflon lined screw-cap at 4°C (± 2°C) and protect from light.
(Refrigeration may cause the corn oil to precipitate. Before use,
allow the calibration solution to stand at room temperature until the
corn oil dissolves.) Replace the calibration standard solution every
six months, or more frequently if necessary.
7.3.3 Store all other working standard solutions in amber glass bottles or
| vials with Teflon lined screw caps at 4°C (± 2°C) and protect from
light. The standard solution must be checked frequently for
stability. Replace all working standard solutions after six months,
or sooner if comparison with quality control check samples indicates
a problem, except for the PEM solution which must be prepared weekly.
CAUTION: Analysts must allow all standard solutions .'to equilibrate
to room temperature before use.
7.3.4 Samples, sample extracts, and standards must be stored separately.
7.3.5 The Contractor is responsible for maintaining the integrity of
standard solutions and verifying prior to use. This means that
standards must be brought to room temperature prior to use, checked
for losses, and checked that all components have remained in the
solution.
D-18/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 8
Sample Collection, Preservation, and Storage
8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 Sample Collection and Preservation
8.1.1 Water samples may be collected in 1 L (or 1 quart) amber glass
containers, fitted with screw-caps lined with Teflon. If amber
containers are not available, the samples should be protected from
light. Soil samples may be collected in glass containers or closed
end tubes (e.g., brass sleeves) in sufficient quantity to perform the
analysis. The specific requirements for site sample collection are
outlined by the Region.
| 8.1.2 All samples must be iced or refrigerated at 4°C (+ 2°C) from the time
of collection until extraction. -.
8.2 Procedure for Sample Storage
8.2.1 The samples must be protected from light and refrigerated at
4 °C (±2 °C) from the time of receipt until 60 days after delivery of
a complete reconciled sample data package to the Agency. After 60
days the samples may be disposed of in a manner that complies with
all applicable regulations.
8.2.2 The samples must be stored in an atmosphere demonstrated to be free
of all potential contaminants.
8.3 Procedure for Sample Extract Storage
8.3.1 Sample extracts must be protected from light and stored at
| 4°C (± 2°C) until 365 days after delivery of a complete reconciled
data package to the Agency.
8.3.2 Sample extracts must be stored in an atmosphere demonstrated to be
free of all potential contaminants.
8.3.3 Samples, sample extracts, and standards must be stored separately.
8.4 Contract Required Holding Times
8.4.1 Extraction of water samples by separatory funnel procedures must be
completed within five days of the Validated Time of Sample Receipt
(VTSR). Extraction of water samples by continuous liquid-liquid
extraction procedures must be started within five days of VTSR.
Extraction of soil/sediment samples by sonication must be completed
within 10 days of VTSR.
8.4.2 As part of the Agency's QA program, the Agency may provide
Performance Evaluation (PE) samples as standard extracts which the
Contractor is required to prepare per instructions provided by the
| Agency. PE samples must be prepared and analyzed concurrently with
| the samples in the SDG. The extraction holding times (five days
after VTSR for water, 10 days after VTSR for soil/sediment) do not
| apply for PE samples received as standard extracts.
8.4.3 Analysis of sample extracts must be completed within 40 days
following the start of extraction.
D-19/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
GC Operating Conditions/Initial Calibration
9.0 CALIBRATION AND STANDARDIZATION
9.1 Gas Chromatograph Operating Conditions
9.1.1 The following are the gas chromatographic analytical conditions. The
conditions are recommended unless otherwise noted.-'
Carrier Gas: . Helium (hydrogen may be used, see Section
6.23.3.7)
Column Flow: 5 mL/min
Make-up Gas: P-5/P-10 or N2 (required)
Injector Temperature: > 200 °C (see Section 9.1.4)
Injection: On-column
Injection Volume: 1 or 2 uL (see Section 9.1.3)
Injector: Grob-type, split less
Initial Temperature: 150 °C
Initial Hold Time: M min
Temperature Ramp: 5 to 6° C/min
Final Temperature: 275 °C
Final Hold Time: Until after decachlorobiphenyl has eluted
(approximately 10 minutes)
9.1.2 Optimize GC conditions for analyte separation and sensitivity. Once
optimized, the same GC conditions must be used for the analysis of
all standards, samples, blanks, and MS/MSD. The linearity of the BCD
may be greatly dependent on the flow rate of the make-up gas. Care
must be taken to maintain stable and appropriate flow of make-up gas
to the detector.
9.1.3 Manual injections must be 2 uL. Auto injectors may use 1 uL volumes.
The same injection volume must be used for all standards, blanks, and
samples, including MS/MSD.
9.1.4 Cold (ambient temperature) on-column injectors that allow injection
directly onto a 0.53 mm ID column may be used as long as the
acceptance criteria for resolution, calibration, and analyte
breakdown are met.
9.2 Initial Calibration
9.2.1 Summary of Initial Calibration
Prior to the analysis of samples, including MS/MSD and required
blanks, each GC/EC system must be initially calibrated at a minimum
of three concentrations to determine instrument sensitivity and the
linearity of response utilizing single component target compound and
surrogate standards. Multicomponent target compounds are calibrated
at a single point.
9.2.2 Frequency of Initial Calibration
Each GC/ECD system must be initially calibrated upon award of the
contract, whenever major instrument maintenance or modification is
D-20/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
performed (e.g., column replacement or repair, cleaning or
replacement of BCD, etc.) or if the calibration verification
technical acceptance criteria have not been met.
9.2.3 Procedure for Initial Calibration
9.2.3.1 Set up the GC/ECD systems as described in Section 9.1.
.9.2.3.2 Prepare the initial calibration standards using the analytes and
the concentrations specified in Sections 7.-2.4.5 through 7.2.4.8.
9.2.3.3 All standards, samples, MS/MSD, blanks, and extracts must be
allowed to warm to ambient temperature before analysis.
9.2.3.4 Analyze the initial calibration sequence as given below. NOTE:
Steps 16 and 17 are used as part of the calibration verification
as well (see Section 9.3).
INITIAL CALIBRATION SEQUENCE
1. Resolution Check
2. Performance Evaluation Mixture
3. Aroclor 1016/1260
4. Aroclor 1221
5. Aroclor 1232
6. Aroclor 1242
7. Aroclor 1248
8. Aroclor 1254
9. Toxaphene
10. Low Point Standard A
11. Low Point Standard B
12. Midpoint Standard A
13. Midpoint Standard B
14. High Point Standard A
15. High Point Standard B
16. Instrument Blank
17. Performance Evaluation Mixture
9.2.4 Calculations for Initial Calibration
9.2.4.1 During the initial calibration sequence, absolute retention times
(RT) are determined for all single component pesticides, the
surrogates, and at least three major peaks of each multicomponent
analyte.
D-21/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
9.2.4.2 For single component pesticides, an RT is measured in each of three
calibration standards and the mean RT is calculated as the average of
the three values. An RT is measured for the surrogates in each of
the three analyses of Individual Standard Mixture A during the
initial calibration and the mean RT is calculated as the average of
the three values. Calculate a mean absolute retention time ("RT)
for each single component pesticide and surrogate using Equation 1.
EQ. 1
^
2-i RTi
RT =
n
Where,
RT = Mean absolute retention time of analyte.
RTi = Absolute retention time of analyte.
n = Number of measurements (3) .
9.2.4.3 A retention time window is calculated for each single component
analyte and surrogate and for the major peaks (3 to 5) of each
multicomponent analyte by using the list in Table 1. Windows are
centered around the mean absolute retention time for the analyte
established during the initial calibrations. Analytes are
identified when peaks are observed in the RT window for the
compound on both GC columns.
9.2.4.4 The linearity of the instrument is determined by calculating a
percent relative standard deviation (%RSD) of the calibration
factors from a three-point calibration curve for each single
component pesticide and surrogate. Either peak area or peak
height may be used to calculate calibration factors used in the
%RSD equation. For example, it is permitted to calculate
linearity for endrin based on peak area and to calculate linearity
for aldrin based on peak height. It is not permitted within a
%RSD calculation for an analyte to use calibration factors
calculated from both peak area and peak height. For example, it
, is not permitted to calculate the calibration factor for the low
point standard for endrin using peak height and calculate the
midpoint and high point standard calibration factors for endrin
using peak area.
9.2.4.5 Calculate the calibration factor for each single component
pesticide and surrogate over the initial calibration range using
Equation 2. The calibration factors for the surrogates are
calculated from the three analyses of Individual Standard Mixture
A only.
D-22/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
9.2.4.6 Calculate the mean and the %RSD of the calibration factors for
each single component pesticide and surrogate over the initial
calibration range using Equations 3 and 4.
EQ. 2
_ Peak area (or height) of the standard
Mass injected (ng)
EQ. 3
CF
CF = -i^-
EQ. 4
%RSD =
SDcp
-
CF
x 100
Where,
K -
(n - 1)
%RSD = Percent relative standard deviation
= Standard deviation of calibration factors
CF. = Calibration factor
CF
= Mean calibration factor
n = Total number of values (3)
9.2.4.7 A calibration factor is calculated for each peak in a selected set
of three to five major peaks for each multicomponent analyte using
Equation 2.
.D-23/PEST
OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
9.2.4.8 Calculate the percent breakdown of DDT, the percent breakdown of
endrin, and the combined breakdown of DDT and endrin in the PEM
using Equations 5, 6, 7, and 8.
EQ. 5 . .
. ,. , . . Peak area (height) of compound in PEM
Amount found (ng) = -'
CFmp
Where,
The calibration factor for the compound determined
from the midpoint standard in the most recent initial
calibration. NOTE: If during the initial
calibration, linearity was determined based on peak
area for the compound, then the midpoint CF must be
based on peak area. If during the initial
calibration, the linearity for the compound was
determined based on peak height for the compound, then
the midpoint CF must be based on peak height .
EQ. 6
, , Amount found (ng) (DDD+DDE)
%Breakdown DDT = - -^ - - xlOO
Amount (ng) of DDT injected
EQ. 7
Amount fo'
in =
Amount (ng) of endrin injected
_ . , , . Amount found (ng) (endrin aldehyde + enrin ketone) , _.-
%Breakdown Endrin = ± £- xlOO
EQ. 8
Combined %Breakdown = %Breakdown DDT + %Breakdown Endrin
9.2.4.9 Calculate the percent difference for each single component
pesticide and surrogate in the PEM using Equations 5 and 9.
EQ. 9 C - C
%D = -^^ ^ x 100
C
nora
Where,
%D = Percent difference
Cnom = Nominal concentration of each analyte
ccaic = Calculated concentration of each analyte from the
analyses of the standards.
D-24/PEST OLM04.2
-------
9.2.4.10
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
Calculate the resolution between the analytes in the Resolution
Check Mixture,, the Performance Evaluation Mixture, and the
midpoint concentration of Individual Standard Mixtures A and B
using Equation 10.
Area or Height
Time-
EQ. 10
V
%Resolution = x 100
H
Where,
V =
H =
Depth of the valley between the two peaks. The depth of
the valley is measured along a vertical line from the
level of the apex of the shorter peak to the floor of the
valley between the two peaks.
Height of the shorter of the adjacent peaks.
9.2.5 Technical Acceptance Criteria for Initial Calibration
All initial calibration technical acceptance criteria apply
independently to both GC columns.
9.2.5.1 The initial calibration sequence must be analyzed according to the
procedure and in the order listed in Section 9.2.3, at the
concentrations listed in Sections 7.2.4.5 through 7.2.4.8, and at
the frequency listed in Section 9.2.2. The GC/ECD operating
conditions optimized in Section 9.1 must be followed.
9.2.5.2 The resolution between two adjacent peaks in the Resolution Check
Mixture must be greater than or equal to 60.0 percent.
9.2.5.3 All single component pesticide and surrogate peaks in both runs of
the PEM must be greater than or equal to 90.0 percent resolved on
each column.
9.2.5.4 The absolute retention times of each of the single component
pesticides and surrogates in both runs of the PEM must be within
D-25/PEST
OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
the retention time windows determined from the three-point initial
calibration in Section 9.2.4.3.
9.2,5.5 The percent difference of the calculated amount (amount found) and
the nominal amount (amount added) for each of the single component
pesticides and surrogates in both of the PEM runs of each GC
column must be greater than or equal to -25.0 AND less than or
equal to 25.0 percent using Equation 9.
9.2.5.6 The percent breakdown of DDT and endrin in each of the PEM runs
must be less than or equal to 20.0 percent. The combined
breakdown of DDT and endrin must be less than or equal to 30.0
percent.
9.2.5.7 The %RSD of the calibration factors for each single component
target compound must be less than or equal to 20.0 percent, except
alpha-BHC and delta-BHC. The %RSD of the calibration factors for
alpha-BHC and delta-BHC must be less than or equal to 25.0
percent. The %RSD of the calibration factors for the two
surrogates must be less than or equal to 30.0 percent. Up to two
single component target compounds (but not surrogates) per column
may exceed the 20.0 percent limit for %RSD (25.0 percent for
alpha-BHC and delta-BHC), but those compounds must have a %RSD of
less than or equal to 30.0 percent.
9.2.5.8 The resolution between any two adjacent peaks in the midpoint
concentrations of Individual Standard Mixtures A and B in the
initial calibration must be greater than or equal to 90.0 percent.
9.2.5.9 All instrument blanks must meet the technical acceptance criteria
in Section 12.1.4.4.
9.2.5.10 The identification of single component pesticides by gas
chromatographic methods is based primarily on retention time data.
The retention time of the apex of a peak can only be verified from
an on-scale chromatogram. The identification of multicomponent
analytes by gas chromatographic methods is based primarily on
recognition of patterns of retention times displayed on a
chromatogram. Therefore, the following requirements apply to all
data presented for single component and multicomponent analytes.
The chromatograms that result from the analyses of the
Resolution Check Mixture, the PEM, and Individual Standard
Mixtures A and B during the initial calibration sequence must
display the single component analytes present in each
standard at greater than 10 percent of full scale but less
than 100 percent of full scale.
The chromatograms for at least one of the three analyses each
of Individual Standard Mixtures A and B from the initial
calibration sequence must display the single component
analytes at greater than 50 percent and less than 100 percent
of full scale.
D-26/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Initial Calibration
The chromatograms of the standards for the multicomponent
analytes analyzed during the initial calibration sequence
must display the peaks chosen for identification of each
analyte at greater than 25 percent and less than 100 percent
of full scale.
For any standard containing alpha-BHC, the baseline of the
chromatogram must return to below 50 percent of full scale
before the elution time of alpha-BHC, and return to below 25
percent of full scale after the elution time of alpha-BHC and
before the elution time of decachlorobiphenyl.
If a chromatogram is replotted electronically to meet
requirements, the scaling factor used must be displayed on
the chromatogram.
If the chromatogram of any standard needs to be replotted
electronically to meet these requirements, both the initial
chromatogram and the replotted chromatogram must be submitted
in the data package.
9.2.6 Corrective Action for Initial Calibration
9.2.6.1 If the technical acceptance criteria for the initial calibration
are not met, inspect the system for problems. It may be necessary
to change the column, bake out the detector, clean the injection
port, or take other corrective actions to achieve the acceptance
criteria.
9.2.6.2 Contamination should be suspected as a cause if the detector
cannot achieve acceptable linearity using this method. In the
case of low level contamination, baking out the detector at an
elevated temperature (350 °C) should be sufficient to achieve
acceptable performance. In the case of heavy contamination,
passing hydrogen through the detector for 1-2 hours at an elevated
temperature may correct the problem. In the case of severe
contamination, the detector may require servicing by the BCD
manufacturer. DO NOT OPEN THE DETECTOR. THE BCD CONTAINS
RADIOCHEMICAL SOURCES.
9.2.6.3 If a laboratory cleans out a detector using an elevated
.temperature, the BCD electronics must be turned off during the
bake out procedure.
9.2.6.4 After bake out or hydrogen reduction, the detector must be
recalibrated using the initial calibration sequence.
9.2.6.5 Initial calibration technical acceptance criteria must be met
before any samples, including MS/MSD or required blanks, are
analyzed. Any samples or required blanks analyzed before the
initial calibration technical acceptance criteria have been met
will, require reanalysis at no additional cost to the Agency.
D-27/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Calibration Verification
9.3 Calibration Verification
9.3.1 Summary of Calibration Verification
Three types of analyses are used to verify the calibration and
evaluate instrument performance. The analyses of instrument blanks,
PEMs, and the midpoint concentration of Individual Standard Mixtures
A and B constitute the continuing calibration. Sample data are not
acceptable unless bracketed by acceptable analyses of instrument
blanks, PEMs, and both Individual Standard Mixtures A and B.
9.3.2 Frequency of Calibration Verification
9.3.2.1 An instrument blank and the PEM must bracket one end of a 12-hour
period during which sample data are collected, and a second
instrument blank and the midpoint concentration of Individual
Standard Mixtures A and B must bracket the other end of the 12-
hour period.
9.3.2.2 For the 12-hour period immediately following the initial
calibration sequence, the instrument blank and the PEM that are
the last two steps in the initial calibration sequence bracket the
front end of that 12-hour period. The injection of the instrument
blank starts the beginning of that 12-hour period (see Section
10.2.2.1). Samples may be injected for 12 hours from the
injection of the instrument blank. The three injections
immediately after that 12-hour, period must be an instrument blank,
Individual Standard Mixture A, and Individual Standard Mixture B.
The instrument blank must be analyzed first, before either
standard. The Individual Standard Mixtures may be analyzed in
either order (A,B or B,A).
9.3.2.3 The analyses of the instrument blank and Individual Standard
Mixtures A and B immediately following one 12-hour period may be
used to begin the subsequent 12-hour period, provided that they
meet the acceptance criteria in Section 9.3.5. In that instance,
the subsequent 12-hour period must be bracketed by the acceptable
analyses of an instrument blank and a PEM, in that order. Those
two analyses may in turn be used to bracket the front end of yet
another 12-hour period. This progression may continue every 12
hours until such time as any of the instrument blanks, PEMs, or
Individual Standard Mixtures fails to meet the acceptance criteria
in Sections 9.3.5. The 12-hour time period begins with the
injection of the instrument blank.
9.3.2.3.1 Standards (PEM or Individual Standard Mixtures), samples and
required blanks may be injected for 12 hours from the time of
injection of the instrument blank.
9.3.2.4 If more than 12 hours have elapsed since the injection of the
instrument blank that bracketed a previous 12-hour period, an
acceptable instrument blank and PEM must be analyzed in order to
start a new sequence. This requirement applies even if no
D-28/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Calibration Verification
analyses were performed since that standard was injected.
9.3.2.5 The requirements for running the instrument blanks, PEM, and
Individual Standard Mixtures A and B are waived when no samples,
dilutions, reanalyses, method/sulfur blanks, MS/MSD, and
multicomponent analytes for the 72-hour confirmation requirement
are analyzed during that 12-hour period. To resume analysis,
using the existing initial calibration, the Contractor first must
analyze an instrument blank and PEM which meet the technical
acceptance criteria.
9.3.2.6 If the entire 12-hour period is not required for the analyses of
all samples to be reported, the sequence must be ended with either
the instrument blank/PEM combination or the instrument
blank/Individual Standard Mixtures A and B combination, whichever
was due to be performed at the end of the 12-hour period.
9.3.3 Procedure for Calibration'Verification
9.3.3.1 Analyze the PEM, instrument blank, and the midpoint concentration
of Individual Standard Mixtures A and B at the required
frequencies (Section 9.3.2).
9.3.3.2 All standards and blanks must be at ambient temperature at the
time of preparation and analysis.
9.3.4 Calculations for Calibration Verification
9.3.4.1 For each analysis of the PEM used to demonstrate continuing
calibration, calculate the percent difference between the amount
of each analyte (including the surrogates) found in the PEM and
the nominal amount using Equations 5 and 9.
9.3.4.2 Calculate the percent breakdown of DDT and endrin, and the
combined breakdown in each PEM analyzed using Equations 5, 6, 7,
and 8.
9.3.4.3 For each analysis of the midpoint concentration of Individual
Standard Mixtures A and B used to demonstrate continuing
calibration, calculate the percent difference between the amount
of. each analyte (including the surrogates) found in the standard
mixture and the nominal amount using Equations 5 and 9. Do not
attempt to calculate the breakdown of Endrin and DDT in the
Individual Standard Mixtures, as these standards contain the
breakdown products as well as the parent compounds.
9.3.5 Technical Acceptance Criteria for Calibration Verification
All calibration verification technical acceptance criteria apply
independently to each column. Each column must meet criteria.
9.3.5.1 The PEMs, Individual Standard Mixtures A and B and instrument
blanks must be analyzed at the required frequency on a GC/EC
D-29/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Calibration Verification
system that has met the initial calibration technical acceptance
criteria.
9.3.5.2 All single component pesticides and surrogates in the PEMs used to
demonstrate continuing calibration must be greater than or equal
to 90.0 percent resolved. The resolution between any two adjacent
peaks in the midpoint concentrations of Individual Standard
Mixtures A and B used to demonstrate initial calibration must be
greater than or equal to 90.0 percent.
9.3.5.3 The absolute retention time .for each of the single component
pesticides and surrogates in the PEMs and midpoint concentration
of the Individual Standard Mixtures used to demonstrate continuing
calibration must be within the retention time window determined
from the three-point initial calibration in Section 9.2.4.3.
9.3.5.4 The percent difference between the calculated amount and the
nominal amount (amount added) for each of the single component
pesticides and surrogates in the PEM must be greater than or equal
to -25.0 percent and less than or equal to 25.0 percent.
9.3.5.5 The percent difference between the calculated amount and the
nominal amount (amount added) for each of the single component
pesticides and surrogates in the INDA and INDB that have been used
as calibration verification must be greater than or equal to -25.0
percent and less than or equal to 25.0 percent.
9.3.5.6 The percent breakdown of DDT in the PEM must be less than or equal
to 20.0 percent on each column. The percent breakdown of endrin
in the PEM must be less than or equal to 20.0 percent on each
column. The combined breakdown of both DDT and endrin must be
less than or equal to 30.0 percent on each column.
9.3.5.7 All instrument blanks must meet the technical acceptance criteria
in Section 12.1.4.4.
9.3.5.8 The identification of single component pesticides by gas
chromatographic methods is based primarily on retention time data.
Since the retention time of the apex of a peak can only be
verified from an on-scale chromatogram, the following requirements
must be met for continuing calibration to be acceptable.
9 . 3 . 5 . 8.. 1 The chromatograms that result from the analyses of the PEM and
the Individual Standard Mixtures must display the single
component analytes present in each standard at greater than 10
percent of full scale but less than 100 percent of full scale.
9.3.5.8.2 For any PEM, Individual Standard Mixture or blank, the baseline
of the chromatogram must return to below 50 percent of full
scale before the elution time of alpha-BHC, and return to below
25 percent of full scale after the elution time of alpha-BHC
and before the elution time of decachlorobiphenyl.
D-30/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Calibration Verification
9.3.5.8.3 If a chromatogram is replotted electronically to meet these
requirements, the scaling factor used must be displayed on the
chromatogram.
9.3.5.8.4 If the chromatogram of any standard or blank needs to be
replotted electronically to meet these requirements, both the
initial chromatogram and the replotted chromatogram(s) must be
submitted in the data package.
9.3.6 Corrective Action for Calibration Verification
9.3.6.1 If the technical acceptance criteria for the calibration
verification are not met, inspect the system for problems and take
corrective action to achieve the acceptance criteria.
9.3.6.2 Major corrective actions such as replacing the GC column or baking
out the detector will require that a new initial calibration be
performed that meets the technical acceptance criteria in Section
9.2.5. _
9.3.6.3 Minor corrective actions may not require performing a new initial
calibration, provided that a new analysis of the standard (PEM or
Individual Standard Mixture) that originally failed the criteria
and an associated instrument blank immediately after the
corrective action do meet all the acceptance criteria.
9.3.6.4 If a PEM or Individual Standard Mixture does not meet technical
acceptance criteria listed above, it must be reinjected
immediately. If the second injection of the PEM or Individual
Standard Mixture meets the criteria, sample analysis may continue.
If the second injection does not meet the criteria, all data
collection must be stopped. Appropriate corrective action must be
taken, and a new initial calibration sequence must be run before
more sample data are collected.
9.3.6.5 If an instrument blank does not meet the technical acceptance
criteria listed in Section 12.1.4.4, all data collection must be
stopped. Appropriate corrective action must be taken to clean out
the system, and an acceptable instrument blank must be analyzed
before more sample data are collected.
9.3.6.6 Analysts are reminded that running an instrument blank and a PEM
or Individual Standard Mixtures once every 12 hours is the minimum
contract requirement. Late eluting peaks may carry over from one
injection to the next if highly complex samples are analyzed or if
the GC conditions are unstable. Such carryover is unacceptable.
Therefore, it may be necessary to run instrument blanks and
standards more often to avoid discarding data.
9.3.6.7 If a successful instrument blank and PEM cannot be run after an
interruption in analysis (Section 9.3.2.5), an acceptable initial
calibration must be run before sample data may be collected. All
acceptable sample analyses must be preceded and followed by
-. . . D-31/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 9
Calibration and Standardization
Calibration Verification
acceptable standards and instrument blanks, as described in
Section 9.3.2.
9.3.6.8 Calibration verification technical acceptance criteria must be met
before any samples, including MS/MSD and required blanks are
reported. Any samples, including MS/MSD and required blanks
associated with a calibration verification which did not meet the
technical acceptance criteria will require reanalysis at no
additional cost to the Agency.
D-32/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
10.0 PROCEDURE
10.1 Sample Preparation
10.1.1 If insufficient sample amount (less than 90% of the required amount)
is received to perform the analyses, the Contractor shall contact SMO
to apprise them of the problem. SMO will contact the Region for
instructions. The Region will either require that no sample analyses
be performed or will require that a reduced volume be used for the
sample analysis. No other changes in the analyses will be permitted.
The Contractor shall document the Region's decision in the SDG '
Narrative.
10.1.2 If multiphase samples (e.g., a two-phase liquid sample, oily
sludge/sandy soil sample) are received by the Contractor, the
Contractor shall contact SMO to apprise them of the type of sample
received. SMO will contact the Region. If all phases of the sample
are amenable to analysis, the Region may require the Contractor to do
any of the following:
Mix the sample and analyze an aliquot from the homogenized
sample.
Separate the phases of the sample and analyze each phase
separately. SMO will provide EPA sample numbers for the
additional phases.
Separate the phases and analyze one or more of the phases, but
not all of the phases. SMO will provide EPA sample numbers for
the additional phases, if required.
Do not analyze the sample.
10.1.2.1 If all of the phases are not amenable to analysis (i.e., outside
scope), the Region may require the Contractor to do any of the
following:
Separate the phase(s) and analyze the phase(s) that is
amenable to analysis. SMO will provide EPA sample numbers
for the additional phases, if required.
Do not analyze the sample.
10.1.2.2 No other change in the analyses will be permitted. The Contractor
shall document the Region's decision in the SDG Narrative.
10.1.3 Extraction of Water Samples
Water samples may be extracted by either a separatory funnel
procedure or a continuous liquid-liquid extraction procedure. If an
emulsion prevents acceptable solvent recovery with the separatory
funnel procedure, continuous liquid-liquid extraction must be
employed.
D-33/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
10.1.3.1 Separatory Funnel Extraction
10.1.3.1.1 Measure out each 1 L sample aliquot in a separate graduated
cylinder. Measure and record pH of the sample with wide range
pH paper and adjust the pH to between 5 and 9 with 10 N sodium
hydroxide or concentrated sulfuric acid, if required. Samples
requiring pH adjustment must be noted in the SDG Narrative.
Place the sample into a 2 L.separatory funnel.
10.1.3.1.2 Using a syringe or a volumetric pipet, add 1.0 mL of the
surrogate solution to all water samples.
10.1.3.1.3 Rinse the graduated cylinder with 30 mL of methylene chloride
and transfer the rinsate to the separatory funnel. If the
sample was received in a 1 L container, rinse the empty
container with 30 mL of methylene chloride and add rinsate to
the separatory funnel. If the sample container is not rinsed,
then add another 30 mL of methylene chloride to the separatory
funnel and extract the sample by shaking the funnel for two
minutes, with periodic venting to release excess pressure.
NOTE: The total volume of solvent used for extraction is 60
mL. Allow the organic layer to separate from the water phase
for a minimum of 10 minutes. If the emulsion interface between
layers is more than one-third the volume of the solvent layer,
the analyst must employ mechanical techniques to complete the
phase separation. The optimum technique depends upon the
sample, and may include stirring, filtration of the emulsion
through glass wool, centrifugation or other physical means.
Drain the methylene chloride into a 250 mL Erlenmeyer flask.
10.1.3.1.4 Add a second 60 mL volume of methylene chloride to the
separatory funnel and repeat the extraction procedure a second
time, combining the extracts in the Erlenmeyer flask. Perform
a third extraction in the same manner.
10.1.3.2 Continuous Liquid-Liquid Extraction
10.1.3.2.1 Continuous Liquid-Liquid Extraction Without Hydrophobic
Membrane
10.1.3.2.1.1 Follow manufacturer's instructions for set-up.
10.1.3.2.1.2 . Add methylene chloride to the bottom of the extractor and
fill it to a depth of at least one inch above the bottom
sidearm.
10.1.3.2.1.3 Measure out each 1 L sample aliquot in a separate, clean
graduated cylinder; transfer the aliquot to the continuous
extractor. Measure the pH of the sample with wide range pH
paper and record pH. Adjust the pH to between 5 and 9 with
10 N sodium hydroxide or concentrated -sulfuric acid, as
required. Samples requiring the pH adjustment must be noted
in the SDG Narrative. NOTE: With some samples, it may be
necessary to place a layer of glass wool between the
D-34/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
methylene chloride and the water layer in the extractor to
prevent precipitation of suspended solids into the methylene
chloride during extraction.
10.1.3.2.1.4 Using a syringe or volumetric pipet, add 1.0 mL of the
surrogate standard spiking solution (Section 7.2.4.1) into
the sample and mix well.
10.1.3.2.1.5 Rinse the graduated cylinder with 50 mL of methylene
chloride and transfer the rancid to the continuous
extractor. If the sample was received in a 1 L container,
rinse the empty container with 50 mL of methylene chloride
and add the rancid to the continuous extractor.
10.1.3.2.1.6 Add sufficient methylene chloride to the continuous
extractor to ensure proper solvent cycling during operation.
Adjust the drip rate to 5 to 15 mL/minute (recommended);
optimize the extraction drip rate. Extract for a minimum of
18 hours. NOTE: When.a minimum drip rate of 10-15
mLs/minute is maintained throughout the extraction, the
extraction time may be reduced to a minimum of 12 hours.
Allow to cool, then detach the distillation flask. Proceed
to Section 10.1.4.
10.1.3.2.1.7 NOTE: Some continuous liquid-liquid extractors are also
capable of concentrating the extract within the extraction
set-up. Follow the manufacturer's instructions for
concentration when using this type of extractor.
10.1.3.2.2 Continuous Liquid-Liquid Extraction With Hydrophobic Membrane
10.1.3.2.2.1 Follow the manufacturer's instructions for set-up.
10.1.3.2.2.2 Measure out each 1 L sample aliquot in a separate, clean
graduated cylinder. If the sample was received in a 1 L
container, rinse the empty container with 50 mL of methylene
chloride and add the rinsate to the continuous extractor.
If the sample was not received in a 1 L container, add 50 mL
of methylene chloride to the continuous extractor. Slowly
transfer the aliquot to the continuous extractor. Measure
the pH of the sample with wide range pH paper and record pH.
Adjust the pH to between 5 and 9 with 10 N sodium hydroxide
or concentrated sulfuric acid, as required. Samples
requiring the pH adjustment must be noted in the SDG
Narrative.
10 .1.3.. 2 .2 . 3 Using a syringe or volumetric pipet, add 1.0 mL of the
surrogate standard spiking solution (Section 7.2.4.1) into
the sample and mix well.
10.1.3.2.2.4 Rinse the graduated cylinder with 50 mL of methylene
chloride and transfer the rinsate to the continuous
extractor.
D-35/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
10.1.3.2.2.5 Add sufficient methylene chloride to the continuous
extractor to ensure proper solvent cycling during operation.
Adjust the drip rate to 15 mL/minute (recommended); optimize
the extraction drip rate. Extract for a minimum of 6 hours.
. (NOTE: Due to the smaller volume of solvent used during the
extraction process, some sample matrices (e.g., oily
samples, samples containing a high concentration of
surfactants) may create an emulsion which will consume the
solvent volume, preventing the efficient extraction of the
sample. When this occurs, add additional solvent to assure
efficient extraction of the sample, and extend the
extraction time for a minimum of 6 hours. If the sample
matrix prevents the free flow of solvent through the
membrane, then the non-hydrophobic membrane continuous
liquid-liquid type extractor must be used.) Allow to cool,
then detach the distillation flask.
10.1.3.2.2.6 NOTE: Some continuous liquid-liquid extractors are also
capable of concentrating the extract within the extraction
act-up. Follow the manufacturer's instructions for
concentration when using this type of extractor. Using the
hydrophobia membrane, it may not be necessary to dry the
extract with sodium sulfate.
10.1.3.2.3 NOTE: If low surrogate recoveries occur, assure 1) the
apparatus was properly assembled to prevent leaks; 2) the drip
rate/solvent cycling was optimized; and 3) there was proper
cooling for condensation of solvent.
10.1.3.2.4 NOTE: Alternate continuous liquid-liquid extractor types that
meet the requirements of the SOW may also be used. If using
alternate extractors or design types, follow the manufacturer's
instructions for set-up. Optimize the extraction procedure.
10.1.4 Extract Drying
10.1.4.1 Assemble a Kuderna-Danish (K-D) concentrator by attaching a 10 mL
concentrator tube to a 500 mL evaporative flask. Other
concentration devices or techniques may be used in place of the
K-D if equivalency is demonstrated for all the pesticide/Aroclor
target compounds listed 'in Exhibit C.
10.1.4.2 Pour the extract through a drying column containing about 10 cm of
anhydrous granular sodium sulfate and collect the extract in the
K-D concentrator. Rinse the Erlenmeyer flask and the column with
at least two additional 20 to 30 mL portions of methylene chloride
to complete the quantitative transfer.
10.1.5 Soil/Sediment Samples
Mix samples thoroughly, especially composited samples. Discard any
foreign objects such as sticks, leaves, and rocks. Also, decant and
discard any standing aqueous phase.
D-36/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
10.1.5.1 pH Determination
10.1.5.1.1 Transfer 50 g of soil/sediment to a 100 mL beaker. Add 50 mL
of water and stir the solution with a magnetic stirrer for 1
hour. Determine the pH of the sample by using a combination
glass electrode and pH meter while the sample is stirred.
Report the pH value on the appropriate data sheet. If the pH
of the soil/sediment is > 9 or < 5, document any subsequent
problems In the analysis related to pH in the SDG Narrative,
but do not attempt to adjust the pH of the sample. Discard the
portion of the sample used for pH determination.
10.1.5.1.2 NOTE: If insufficient volume of soil/sediment is received, use
a smaller 1:1 ratio of grams of sample to mLs of water for the
pH determination, and note in the SDG Narrative.
10.1.5.2 Percent Moisture
Weigh 5 to 10 g of the soil/sediment to the nearest 0.01 g into a
tared crucible or aluminum weighing pan. Determine the weight
percent volatilized by drying overnight at 105 °C (hereafter
referred to as percent moisture). After the sample is dry, remove
the sample and pan and allow them to cool in a desiccator before
weighing. Calculate the percent moisture according to Equation 11
below. Concentrations of individual analytes will be reported
relative to the dry weight of soil/sediment. CAUTION: Gases
volatized from some soil/sediment samples may require that this
drying procedure be carried out in a hood.
EQ. 11
grams of wi
grams of wet sample
...... grams of wet sample - grams of dry sample ,
%Moisture = x 100
10.1.5.3 Soil/Sediment Extraction
The procedure described below is for the extraction of
soil/sediment samples by sonication. The Contractor may also use
Automated Soxhlet Extraction (SW-846 Method 3541 Revision 0,
September 1994) or Pressurized Fluid Extraction (Sff-846 Method
3545 Revision 0, December 1996) techniques for soil/sediment
samples. The above SW-846 methods are provided as reference only
and the laboratory supplied Standard Operating Procedures must be
accepted by the Agency before the laboratory can utilize these
methods (See Exhibit E for required IPR studies). The
requirements of this SOW must be met at all times (i.e., original
sample weight). As applicable, follow manufacturer's instructions
for use of all extraction equipment. If one of the above
alternative extraction procedures is used, the Contractor must
maintain documentation of the procedure utilized and document its
equivalence to the sonication procedure described below. If the
sample weight must be adjusted to utilize one of the alternative
extraction procedures, the Contractor shall immediately contact
D-37/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Sample Preparation
SMO to inform them of the problem. SMO will contact the Region
for instructions.
Note: All soil/sediment samples in a Case must be extracted by the
same procedure.
io.1.5.3.1 Tune the sonicator according to the manufacturer's directions
prior to extracting samples by this procedure.
10.1.5.3.2 Weigh approximately 30 g of sample (to the nearest 0.1 g) into
a 250 or 400 mL beaker and add 60 g of anhydrous sodium sulfate
(granular).
10.1.5.3.3 Add 2.0 mL of surrogate solution to all soil/sediment samples
by using a volumetric pipet or a syringe. Mix the sample well.
The sample and the added sodium sulfate should be a
homogeneous, granular mixture at this point. Twice as much of
the surrogate solution is added to soil/sediment samples than
to water samples.
10.1.5.3.4 Immediately add 80 to 100 mL of 1:1 methylene chloride/acetone
to the sample.
10.1.5.3.5 Place the bottom surface of the sonicator probe about M inch
below the surface of the solvent but above the sediment layer.
10.1.5.3.6 Sonicate for 3 minutes using a 3/4 inch disrupter horn at full
power (output control knob at 10) with pulse on and percent
duty cycle knob set at 50 percent. Do not use a microtip.
NOTE: These settings refer to the Model W-385. When using a
sonicator other then Model W-385, refer to the instructions
provided by the manufacturer for appropriate output settings.
10.1.5.3.7 The extracted sample can be filtered by using gravity or vacuum
filtration.
10.1.5.3.8 For gravity filtration prepare a filtration/drying bed by
placing a plug of glass wool in the neck of a 10 cm powder
funnel and filling the funnel to approximately half its depth
(4 or 5 cm) with anhydrous sodium sulfate (80-100 g). Decant
the extract through the packed funnel and collect it in a
500 mL evaporative (K-D) flask attached to a concentrator tube.
10.1.5.3.9 For vacuum filtration, use Whatman No. 41 paper in the Buchner
funnel. Pre-wet the paper with methylene chloride/acetone .
before decanting the solvent.
10.1.5.3.10 Repeat the extraction two more times with additional 80 to
100 mL portions of the 1:1 methylene chloride/acetone. Before
each extraction, thoroughly mix the solid residue and make
certain that the sodium sulfate is free flowing and not a
consolidated mass. As required, break up large lumps with a
clean spatula. Decant and filter the extraction-solvent after
each sonication by using the same funnel described above.
D-38/PEST ' OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Concentrating the Extract
After the final sonication, pour the entire sample into the,
funnel and rinse the beaker and funnel with 60 mL of 1:1
methylene chloride/acetone.
10.1.6 Concentrating the Extract
10.1.6.1 Concentration by K-D
Other concentration devices or techniques may be used in place of.
the K-D if equivalency is demonstrated for all the
.pesticide/Aroclor target compounds listed in Exhibit C.
10.1.6.1.1 Add one or two clean boiling chips to the evaporative flask and
attach a three-ball Snyder column. Pre-wet the Snyder column
by adding about 1 mL of methylene chloride to the top of the
column. Place the K-D apparatus on .a hot water bath (60 °C to
70 °C recommended) so that the concentrator tube is partially
immersed in the hot water and the entire lower rounded surface
of the flask is bathed with hot vapor. Adjust the vertical
position of the apparatus and the water temperature as required
to complete the concentration in 15 to 30 minutes. At the
proper rate of distillation, the balls of the column will
actively.chatter, but the chambers will not flood with
condensed solvent. When the apparent volume of liquid reaches
3, to 5 mL for water samples (and less than 10 mL for
soil/sediment samples), remove the K-D apparatus. Allow it to
drain and cool for at least 10 minutes. DO NOT ALLOW THE
EVAPORATOR TO GO DRY.
10.1.6.1.2 For water extracts which do not require GPC cleanup, and for
water and soil/sediment extracts which have been through the
GPC cleanup step, proceed with the hexane exchange described in
Section 10.1.6.2.
10.1.6.1.3 For water extracts which require GPC cleanup, remove the Snyder
column, rinse the flask and its lower joint, collect the
rinsate in the concentrator tube, and adjust the volume to
10 mL with methylene chloride. Proceed to Section 10.1.8.1.
10.1.6.1.4 For soil/sediment extracts that have not been cleaned-up using
GPC, it is absolutely necessary to further reduce the volume of
all soil/sediment extracts to 1 mL in order to remove most of
the acetone. This is best accomplished using the nitrogen
evaporation technique (Section 10.1.7.2). The presence of
acetone will cause a dead volume to develop in the GPC column
and thus will cause loss of surrogates and analytes during GPC
cleanups. Adjust the soil/sediment extract volume to 10 mL
with methylene chloride. Proceed to Section 10.1.8.1 for
mandatory GPC. . .
10.1.6.2 Solvent Exchange into Hexane
This procedure applies to both extracts of water samples and
extracts of soil/sediment samples.
Dr39/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Concentrating the Extract
10.1.6.2.1 With the extract in a K-D apparatus, remove the Snyder column,
add 50 mL of hexane and a new boiling chip, and reattach the
Snyder column. Pre-wet the column by adding about 1 mL of
hexane to the top. Concentrate the solvent extract as
described previously (Section 10.1.6.1), but increase the
temperature of the water bath (to between 80 and 90 °C
recommended). When the apparent volume of liquid reaches 3 to
5 mL, remove the K-D apparatus and allow it to drain and cool
for at least 10 minutes. DO NOT ALLOW THE EVAPORATOR TO GO
DRY.
10.1.6.2.2 Remove the Snyder column; using 1 to 2 mL of hexane, rinse the
flask and its lower joint into the concentrator tube. Complete
quantitative transfer of the extract to a 10 mL vial by using
hexane.
10.1.6.2.3 For samples which have not been subjected to GPC cleanup,
adjust the volume of the hexane extract to 10 mL. For samples
which have been subjected to GPC cleanup, concentrate the
hexane extract tb 5 mL using a micro Snyder column or nitrogen
evaporation, as described in Section 10.1.7.1 or 10.1.7.2.
Proceed to Section 10.1.8.2 for Florisil cartridge cleanup.
10.1.7 Final Concentration of Extract
Two different techniques are permitted to concentrate the extract to
volume before Florisil cleanup or extract volume before instrumental
analysis. They are the. Micro Snyder Column and Nitrogen Evaporation
Technique.
10.1.7.1 Micro Snyder Column Concentration
Add another one or two clean boiling chips to the concentrator
tube and attach a two-ball micro Snyder column. Pre-wet the
Snyder column by adding about 0.5 mL of hexane to the top of the
column. Place the K-D apparatus in a hot water bath (80 °C to 90
°C recommended) so that the concentrator tube is partially
immersed in the hot water. Adjust the vertical position of the
apparatus and the water temperature as required to complete the
concentration in 5 to 10 minutes. At the proper rate of
distillation, the balls of the column will actively chatter, but
the chambers will not flood with condensed solvent. When the
apparent volume of liquid reaches 0.5 mL, remove the K-D apparatus
from the water bath and allow it to drain for at least 10 minutes
while cooling. Remove the Snyder column and rinse its flask and
lower joint into the concentrator tube with 0.2 mL of hexane.
Adjust the final volume with hexane to 1 or 2 mL (see Sample
Cleanup by Florisil Cartridge, Section 10.1.8.2.3).
D-40/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.7.2 Nitrogen Evaporation Technique (taken from ASTM Method D 3086)
10.1.7.2.1 Place the Concentrator tube in a warm water bath (30 °C to
35 °C recommended) and evaporate the solvent volume to the
final volume by blowing a gentle stream of clean, dry nitrogen
(filtered through a column of activated carbon) onto the
solvent. DO NOT ALLOW THE EXTRACT TO GO TO DRYNESS. Adjust
the soil/sediment extract volume to 10 mL with methylene
chloride. Proceed to Section 10.1.8 for mandatory GPC cleanup
procedures.
10.1.7.2.2 Gas lines from the gas source to the evaporation apparatus must
be stainless steel, copper, or Teflon tubing. Plastic tubing
must not be used between the carbon trap and the sample as it
may introduce interferences. The internal wall of new tubing
must be rinsed several times with hexane and then dried prior
to use.
10.1.7.2.3 During evaporation, the tube solvent level must be kept below
. the water level of the bath.
10.1.8 Cleanup Procedures
There are three cleanup procedures specified in this method: GPC,
Florisil cartridge, and sulfur cleanup. GPC must- be performed for
all soil/sediment extracts. GPC must be performed for water extracts
that contain higher molecular weight contaminants that interfere with
the analysis of the target analytes. Florisil cartridge cleanup is
mandatory for all extracts. Sulfur cleanup must be performed for all
sample extracts contaminated with sulfur. Blanks and matrix spike
and matrix spike duplicate samples must be subjected to the same
cleanup as the unspiked samples.
10.1.8.1 Sample Cleanup by Gel Permeation Chromatography (GPC)
10.1.8.1.1 Introduction
Gel Permeation Chromatography (GPC) is a size exclusion cleanup
procedure using organic solvents and hydrophobic gels in the
separation of natural (and synthetic) macromolecules. The
packing gel is porous and is characterized by the range or
uniformity (exclusion range) of that pore size. In the choice
of gels, the exclusion range must be larger than the molecular
size of the molecules to be separated.
10.1.8.1.2 GPC Column Preparation
The instructions listed below for GPC column preparation are
for Bio Beads. Alternate column packings may be used if 1) the
column packings have equivalent or better performance than the
Bio Beads and meet the technical acceptance criteria for GPC
calibration and GPC calibration checks, and 2).the column
packings do not introduce contaminants/artifacts into the
sample which interfere with the analysis of the pesticide
D-41/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
compounds. Follow the manufacturer's instructions for
preparation of the GPC column packing.
10.1.8.1.2.1 Weigh out 70 g of Bio Beads (SX-3). Transfer them to a 1 L
bottle with a Teflon-lined cap or a 500 mL separatory funnel
with a large bore stopcock, and add approximately 300 mL of
methylene chloride. Swirl the container to ensure the
wetting of all beads. Allow the beads to swell for a
minimum of 2 hours. Maintain enough solvent to cover the
beads sufficiently at all times. If a guard column is to be
used, repeat the above with 5 g of Bio Beads in a 125 mL
bottle or a beaker, using 25 mL of methylene chloride.
10.1.8.1.2.2 Turn the column upside down from its normal position and
remove the inlet bed support plunger (the inlet plunger is
longer than the outlet plunger). Position and tighten the
outlet bed support plunger as near the end as possible, but
no closer than 5 cm (measured from the gel packing to the
. collar). ;
10.1.8.1.2.3 Raise the end of the outlet tube to keep the solvent in the
GPC column, or close the column outlet stopcock. Place a
small amount of solvent in the column to minimize the
formation of air bubbles at the base of poured column
packing.
10.1.8.1.2.4 Swirl the bead/solvent slurry to get a homogeneous mixture
and, if the wetting was done in a quart bottle, quickly
transfer it to a 500 mL separatory funnel with a large bore
stopcock. Drain the excess methylene chloride directly into
the waste beaker, and then start draining the slurry into
the column by placing the separatory funnel tip against the
.column wall. This will help to minimize bubble formation.
Swirl occasionally to keep the slurry homogeneous. Drain
enough to fill the column. Place the tubing from the column
outlet into a waste beaker below the column, open the
stopcock (if attached), and allow the excess solvent to
drain. Raise the tube to stop the flow, and close the
stopcock when the top of the gel begins to look dry. Add
additional methylene chloride to just rewet the gel.
10.1.8.1.2.5 Wipe any remaining beads and solvent from the inner walls of
the top of the column with a laboratory tissue. Loosen the
seal slightly on the other plunger assembly (long plunger)
and insert it into the column. Make the seal just tight
enough so that any beads on the glass surface will be pushed
forward, but loose enough so that the plunger can be pushed
forward.
CAUTION: Do not tighten the seal if beads are between the
seal and the- glass surface because this can damage the seal
and cause leakage.
D-42/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.1.2.6 Compress the column as much as possible without applying
excessive force. Loosen the seal and gradually pull out the
plunger.- Rinse and wipe off the plunger. Slurry any
remaining beads and transfer them into the column. Repeat
the step in Section 10.1.8.1.2.5 and reinsert the plunger.
If the plunger cannot be inserted and pushed in without
allowing beads to escape around the seal, continue
compression of the beads without tightening the seal, and
loosen and remove the plunger as described. Repeat this
procedure until the plunger is inserted successfully.
10.1.8.1.2.7 Push the plunger until it meets the gel, then compress the
column bed about four centimeters.
10.1.8.1.2.8 Pack the optional 5 cm column with approximately 5 g of pre
swelled beads (different guard columns may require different
amounts). Connect the guard column to the inlet of the
analytical column.
10 .1. 8.. 1. 2 . 9 Connect the column inlet to the solvent reservoir (reservoir
should be placed higher than the top of the column) and
place the column outlet tube in a waste container. Placing
a restrictor in the outlet tube will force air out of the
column more quickly. A restrictor can be made from a piece
of capillary stainless steel tubing of 1/16" OD x 0.010" ID
x 2". Pump methylene chloride through the column at a rate
of 5 mL/min for one hour.
10.1.8.1.2.10 After washing the column for at least one hour, connect the
column outlet tube, without the restrictor, to the inlet
side of the UV detector.. Connect the system outlet to the
.outlet side of the UV detector. A restrictor (same size as
the one in Section 10.1.8.1.2.9 above) in the outlet tube
from' the UV detector will prevent bubble formation which
causes a noisy UV baseline. The restrictor will not affect
flow rate. After pumping methylene chloride through the
column for an additional 1-2 hours, adjust the inlet bed
support plunger until approximately 6-10 psi backpressure is
achieved. Push the plunger in to increase pressure or
slowly pull outward to reduce pressure.
10.1.8.1.2.11 When the GPC column is not to be used for several days,
connect the column outlet line to the column inlet to
prevent column drying and/or channeling. If channeling
occurs, the gel must be removed from the column, reswelled,
and repoured as described above. If drying occurs,
methylene chloride should be pumped through the column until
the observed column pressure is constant and the column
appears wet. Always recalibrate after column drying has
occurred to verify retention volumes have not changed.
NOTE: The description of solvent flow rate and column
pressure applies only to the ABC GPC apparatus.
D-43/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
Laboratories using equivalent equipment must develop the
parameters for their apparatus which give acceptable
performance as described in Section 10.1.8.1.3.
10.1.8.1.3 Calibration of GPC
10.1.8.1.3.1 Summary of GPC Calibration
10.1.8.1.3.1.1 The GPC calibration procedure is based on monitoring the
elution of standards with a UV detector connected to the
GPC column.
10.1.8.1.3.1.2 The UV detector calibration procedure described in
Section 10.1.8.1.3.3 is needed for the analyses of
organochlorine pesticides and Aroclors listed in Exhibit
C. IT MUST NOT BE USED FOR THE ANALYSIS OF GC/MS
EXTRACTABLES OR OTHER ANALYTES WITHOUT A RECOVERY STUDY.
10.1.8.1.3.2 Frequency of GPC Calibration
Each GPC system must be calibrated upon award of the
contract, when the GPC calibration verification solution
fails to meet criteria, when the column is changed, when
channeling occurs, and once every seven days.
10.1.8.1.3.3 Procedure for GPC Calibration
Follow the manufacturer's instructions for operating the GPC
system. Changes in pressure, solvent flow rate, and
temperature conditions can affect analyte retention times
and must be monitored.
10.1.8.1.3.3.1 Using a 10 mL syringe, load the calibration solution
(Section 7.2.4.3) onto the GPC. Determine the elution
times for the phthalate, methoxychlor, and perylene.
Phthalate will elute first; perylene, last.
10.1.8.1.3.3.2 -Choose a "DUMP" time which removes > 85 percent of the
phthalate. Choose a "COLLECT" time so that > 95 percent
of the methoxychlor is collected, and continue to collect
until just prior to the elution time of sulfur. Use a
"WASH" time of 10 minutes.
NOTE: The DUMP and COLLECT times must be adjusted to
compensate for the difference in volume of the lines
; between the detector and the collection flask.
10.1.8.1.3.3.3 Reinject the calibration solution after appropriate
collect and dump cycles have been set, and the solvent
flow and column pressure have been established.
10.1.8.1.3.3.4 Measure and record the volume of collected GPC eluate in
a graduated cylinder. The volume of GPC eluate collected
for each sample extract processed may be used to indicate
D-44/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
problems with the system during sample processing.
10.1.8.1.3.3.5 Analyze a GPC blank of methylene chloride. Concentrate
the methylene chloride that passed through the system
during the collect cycle using Kuderna-Danish (K-D)
evaporator. Exchange the solvent to hexane and analyze
the concentrate by GC/EC according to the procedure in
Section 10.2 (usual protocol). Assuming that the blank
represents the extract from a 1 L water sample, calculate
the analyte concentrations using Equation 13.
10.1.8.1.3.4 Technical Acceptance Criteria for GPC Calibration
10.1.8.1.3.4.1 The GPC system must be calibrated at the frequency
described in Section 10.1.8.1.3.2. The UV trace must
meet the following requirements:
Peaks must be observed and should be symmetrical for
all compounds in the calibration solution.
Corn oil and phthalate peaks must exhibit > 85 percent
resolution.
Phthalate and methoxychlor peaks must exhibit > 85
percent resolution.
Methoxychlor and perylene peaks must exhibit > 85
percent resolution.
Perylene and sulfur peaks must not be saturated and
must exhibit > 90 percent baseline resolution.
10.1.8.1.3.4.2 The solvent flow rate and column pressure must be within
the manufacturer's specified ranges.
10.1.8.1.3.4.3 The retention times for bis (2-ethylhexyl) phthalate and
perylene must not vary more than ± 5 percent between
calibrations. If the retention time shift is > 5
percent, take corrective action. Excessive retention
time shifts are caused by the following:
Poor laboratory temperature control or system leaks.
An unstabilized column that requires pumping methylene
chloride through it for several more hours or
overnight.
Excessive laboratory temperatures causing outgassing
of the methylene chloride.
10.1.8.1.3.4.4 The analyte concentrations in a GPC blank must be less
than.the CRQL of any compound in Exhibit C (Pesticides).
10.1.8.1.3.5 Corrective Action for GPC Calibration
D-45/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.1.3.5.1 If the flow rate and/or column pressure do not fall
within the manufacturer's specified ranges, a new column
should be prepared.
10.1.8.1.3.5.2 A UV trace that does not meet the criteria in Section
10.1.8.1.3.4 would also indicate that a new column should
be prepared. It may be necessary to obtain a new lot of
Bio Beads if the column fails all the criteria.
10.1.8.1.3.5.3 If the GPC blank is equal to or exceeds the CRQL of any
compound in Exhibit C (Pesticides), pump additional
methylene chloride through the system for 1-2'hours.
Analyze another GPC blank to ensure the system is
sufficiently clean. Repeat the methylene chloride
pumping if necessary.
10.1.8.1.4 . GPC Calibration Verification
10.1.8.1.4.1 Summary of GPC Calibration Verification
The GPC calibration must be routinely verified with two
check mixtures (Section 7.2.4.3.3).
10.1.8.1.4.2 Frequency of GPC Calibration Verification
10.1.8.1.4.2.1 The calibration verification must be performed at least
once every 7 days ("immediately following the GPC
Calibration) whenever samples, including matrix spikes,
matrix spike duplicates, and blanks are cleaned up using
the GPC.
10.1.8.1.4.2.2 Some samples may contaminate the SX-3 Bio Beads and
change the retention volume of the GPC column.
Therefore, system calibration and analyte recovery must
be checked whenever a sample causes significant
discoloration of the GPC column. Even if no darkening is
visible, GPC calibration must be checked not less than-
once every seven days.
10.1.8.1.4.3 Procedure for GPC Calibration Verification
The instructions below are for a GPC injection loop of 5 mL.
If a 2 mL injection loop is used, the Contractor will adjust
the volume to 4 mL instead of 10 mL before injection extract
on the GPC.
10.1.8.1.4.3.1 The pesticide GPC calibration verification solution
contains the following six compounds in methylene
chloride: gamma-BHC (Lindane), Heptachlor, and Aldrin
each at a concentration of 0.1 pg/mL for a 5 mL GPC loop
(0.25 ug/mL when a 2 mL GPC loop is used) and 4,4'-DDT ,
Endrin, and Dieldrin at 0.2 ug/mL (0.50 ug/mL for a 2 mL
loop). The Aroclor mixture contains 2 ug/mL each of
D-46/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
Aroclor 1016 and 1260 in methylene chloride (5.0 ug/mL
. when a 2 mL GPC loop is used).
10.1.8.1.4.3.2 Load the first 5 mL sample loop by using a 10 mL syringe
containing 8 mL of the pesticide GPC calibration
verification solution. The Aroclor mixture is loaded
into loop #2 in the same manner. Fractions are collected
in an auto sequence by using the GPC program established
be the UV detector calibration procedure (Section
10.1.8.1.3).
10.1.8.1.4.3.3 The collected GPC calibration verification fraction is
transferred to a K-D apparatus, and the collection vessel
is rinsed with two additional 10 mL portions of methylene
chloride to complete the transfer. The volume of
methylene chloride is reduced according to Section
10.1.6.1. After cooling, the solvent is exchanged to
hexane according to the instructions in Section 10.1.6.2.
The final volume is adjusted to 10 mL, and the sample is
analyzed by GC according to the procedure in Section 10.2
(usual protocol). The analysis must be performed on only
one of the GC columns used for sample analysis.
10.1.8.1.4.3.4 The pattern of the Aroclor quantitation peaks and the
recovery of each single component analyte must be
determined for evaluation and reporting purposes.
10.1.8.1.4.4 Technical Acceptance Criteria for GPC Calibration
Verification
10.1.8.1.4.4.1 The recovery of each of the single component analytes
must be between 80 - 110 percent.
10.1.8.1.4.4.2 The Aroclor patterns must be the same as those from the
Aroclor 1016 and Aroclor 1260 standards in the initial
calibration sequence (Section 9.2.5.10).
10.1.8.1.4.5 Corrective Action for GPC Calibration Verification
Analysts may continue to use the GPC column if the technical
acceptance criteria for the GPC calibration verification are
met. If the recoveries are out of the acceptance window or
if changes in the relative peak heights of the patterns of
the Aroclor are observed, the columns must be replaced and
the GPC recalibrated according to the instructions in
Section 10.1.8.1.3 before proceeding with any GPC cleanup on
samples, including blanks - method and/or sulfur and MS/MSD.
10.1.8.1.5 Daily UV Calibration Check (Optional)
The calibration of the GPC may be monitored daily by use of the
UV-GPC calibration solution (Section 7.2.4.3) and the UV
detector calibration procedure (Section 10.1.8.1.3.3). The UV
detector should be used to monitor the elution times for the
D-47/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
phthalate, methoxychlor and perylene, in that order. The pre-
calibrated GPC program should "dump" > 85 percent of the
phthalate and should "collect" > 95 percent of the methoxychlor
and perylene. Significant changes in elution times of the
analytes (e.g., > 0.5 minutes) indicate that the column is out
of calibration and must be recalibrated or replaced.
10.1.8.1.6 Sample Cleanup by GPC
10.1.8.1.6.1 Introduction to Sample Cleanup by GPC
10.1.8.1.6.1.1 ' It is very important to have consistent laboratory
temperatures during an entire GPC run, which could be 24
hours or more. If temperatures are not consistent,
retention times will shift, and the dump and collect
times determined by the calibration standard no longer
will be appropriate. The ideal laboratory temperature to
prevent out gassing of, the methylene chloride is 22 °C.
10.1.8 ..1-6.1.2 In order to prevent overloading of the GPC column, highly
viscous sample extracts must be diluted prior to cleanup.
Any sample extract with a viscosity greater than that of
1:1 glycerol:water solution must be diluted and loaded
into several loops. Similarly, extracts containing more
than 40 mg/mL of non-volatile residue must be diluted and
loaded into several loops. The non-volatile residue may
be determined by evaporating a 100 uL aliquot of the
extract to dryness in a tared aluminum weighing pan, or
other suitable container. When multiple loops/runs are
necessary for ah individual sample, be sure to combine
all of the sample eluates collected.
10.1.8.1.6.1.3 Systems using automated injection devices to load the
sample on the column must be carefully monitored to
assure that the required amount is injected onto the
column. Viscous extracts, or extracts containing a large
amounts of non-volatile residue, will cause problems with
injecting the- proper amount of sample extract onto the
column using automated injection systems. After the
sample extract has been processed, the remaining sample
extract in an injection vial must be checked to assure
that the proper amount of extract was injected on the
column before proceeding with the sample analysis. If
the proper amount of extract was not injected, the sample
must be reprepared and the sample extract must be either
diluted and loaded into several loops or the sample
extract must be injected manually.
10.1.8.1.6.2 Frequency of Sample Cleanup by GPC
GPC cleanup must be performed at least once for each
soil/sediment extract, water extracts that contain high
D-48/PEST OLM04 .2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
molecular weight contaminants that interfere with the
analysis of the target analytes and all associated QC
(blanks and spikes). If cleanup procedure is inadequate
contact SMO.
10.1.8.1.6.3 Procedure for Sample Cleanup by GPC
10.1.8.1.6.3.1 Particles greater than 5 microns may scratch the valve,
which may result in a system leak .and cross contamination
of sample extracts in the sample loops. To avoid such
problems, filter the extract through a 5 micron filter
disc by attaching a syringe filter assembly containing
the filter disc to a 10 mL syringe. Draw the sample
extract through the filter assembly and into the 10 mL
syringe. Disconnect the filter assembly before
transferring the sample extract into a small glass
container (e.g., a 15 mL culture tube with a Teflon-lined
screw cap). Alternatively, draw the extract into the
syringe without the filter assembly. Attach the filter
assembly and force the extract through the filter and
into the glass container. Draw a minimum of 8 mL of
extract into a 10 mL syringe.
Note: Some GPC instrument manufacturer' s recommend us'ing
a smaller micron size filter disc. In this instance,
follow the manufacturer's recommended operating
instructions.
10.1.8.1.6.3.2 INTRODUCTION OF PARTICULATES OR GLASS WOOL INTO THE GPC
SWITCHING VALVES MAY REQUIRE FACTORY REPAIR OF THE
APPARATUS.
10.1.8.1.6.3.3 Follow the manufacturer's instructions for operation of
the GPC system being utilized. Note: These instructions
were written for a 5 mL GPC injection loop. A 2 mL
injection loop may be used in place of a 5 mL injection
loop. If a 2 mL loop is used, concentrate the 10 mL
extract to 4 mL, and then inject 2 mL from the 4 mL.
10.1.8.1.6.3.4 If the sample is difficult to load, some part of the
system may be blocked. Take appropriate corrective
action following, manufacturer's recommendations. The
problem must be resolved prior to loading sample
extracts.
10.1.8.1.6.3.5 After loading each sample loop, wash the loading port
with methylene chloride to minimize cross contamination.
Inject approximately 10 mL of methylene chloride to rinse
the common tubes.
10.1.8.1.6.3.6 After loading all sample loops, process each sample using
the collect and dump cycle times established in Section
10.1.8.1.3.
D-49/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.1.6.3.7 Collect each sample in a 250 mL Erlenmeyer flask covered
with aluminum foil to reduce solvent evaporation, or
directly into a Kuderna-Danish evaporator. Monitor
sample volumes collected. Changes in sample volumes
collected may indicate one or more of the following
problems:
Change in solvent flow rate, caused by channeling in
the column or changes in column pressure.
Increase in column operating pressure due to the
absorption of particles or gel fines onto either the
guard column or the analytical column gel, if a guard
column is not used.
Leaks in the system or significant variances in room
temperature.
10.1.8.1.6.3.8 After the appropriate GPC fraction has been collected for
each sample, concentrate the extract as per Section
10.1.6.1 and proceed to solvent exchange into hexane as
described in Section 10.1.6.2 and Florisil cleanup in
10.1.8.2.
10.1.8.1.6.3.9 Any samples that were loaded into two or more loops must
be recombined before proceeding with concentration.
10.1.8.2 Florisil Cleanup
10.1.8.2.1 Introduction
Florisil cartridge cleanup significantly reduces matrix
interference caused by polar compounds and is required for all
extracts. The same volume of the concentrated extract taken
for Florisil cleanup must, be maintained after Florisil cleanup
(1 or 2 mL) .
10.1.8.2.2 Florisil Cartridge Performance Check
10.1.8.2.2.1 Summary of Florisil Cartridge Performance Check
Every lot number of Florisil cartridges must be tested
before they are used for sample cleanup.
10.1.8.2.2.2 Frequency of Florisil Cartridge Performance Check
Cartridge performance check must be conducted at least once
on each lot of cartridges used for sample cleanup or every 6
months, whichever is most frequent.
D-50/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.2.2.3 Procedure for Florisil Cartridge Performance Check
Add 0.5 mL of 2,4,5-trichlorophenol solution (0.1 ug/mL in
acetone, Section 7.2.4.4) and 0.5 mL of Standard Mixture A,
midpoint concentration, (Section 7.2.4.7) to 4 mL of hexane.
Reduce the final volume to 0.5 mL using nitrogen (Section
10.1.7.2) . Place the mixture onto the top of a washed
Florisil Cartridge, and elute it with 9 mL of hexane/acetone
[(90:10)(V/V)]. Use two additional 1 mL hexane rinses to
ensure quantitative transfer of standard from the cartridge.
Reduce the final volume to 1 mL using nitrogen (Section
10;1.7.2) and analyze the solution by GC/EC using at least
one of the GC columns specified for sample analysis.
Determine the recovery of each analyte for evaluation and
reporting purposes. Calculate the percent recovery using
Equation 12.
EQ. 12
Percent Recovery = - x 100
Where,
Qd = Quantity determined by analysis
Qa = Quantity added
10.1.8.2.2.4 Technical Acceptance Criteria for Florisil Cartridge
Performance Check
10.1.8.2.2.4.1 The cartridge performance check solution must be analyzed
on a GC/EC meeting the initial calibration and
calibration verification technical acceptance criteria.
10.1.8.2.2.4.2 The lot of Florisil cartridges is acceptable if all
pesticides are recovered at 80 to 120 percent, if the
recovery of trichlorophenol is less than 5 percent, and
if no peaks interfering with the target analytes.are
detected.
10.1.8.2.2.5 Corrective Action for Florisil Cartridge Performance Check
Any lot of Florisil cartridges that does not meet the
criteria above must be discarded and a new lot, meeting
criteria, used for sample cleanup.
D-51/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.2.3 Sample Cleanup by Florisil Cartridge
The required Florisil cartridge size and the final volume of
the extract after Florisil cleanup are a function of the GC
autosampler that a laboratory uses. If the autosampler
operates reliably with 1 mL of sample extract, then a 500 mg
cartridge is used and the required final volume is 1 mL. If
the autosampler requires more sample, prepare 2 mL of sample
extract using a 1 g cartridge. Manual injection requires only
a 1 mL final extract and a 500 mg cartridge.
10.1.8.2.3.1 Frequency of Sample Cleanup by Florisil Cartridge
All sample extracts are required to be cleaned up by the
Florisil cartridge technique.
10.1.8.2.3.2 Procedure for Sample Cleanup by Florisil Cartridge
10.1.8.2.3.2.1 Attach the vacuum manifold .to a water aspirator or to a
vacuum pump with a trap installed .between the manifold
and the vacuum source. Adjust the vacuum pressure in the
manifold to between 5 and 10 pounds of vacuum.
10.1.8.2.3.2.2 Place one Florisil cartridge into the vacuum manifold for
each sample extract.
10.1.8.2.3.2.3 Prior to cleanup of samples, the cartridges must be
washed with hexane/acetone (90:10). This is accomplished
by placing the cartridge on the vacuum manifold, by
pulling a vacuum, and by passing at least 5 mL of the
hexane/acetone solution through the cartridge. While the
cartridges are being washed, adjust the vacuum applied to
each cartridge so that the flow rate through each
cartridge is approximately equal. DO NOT ALLOW THE
CARTRIDGES TO GO DRY AFTER THEY HAVE BEEN WASHED.
10.1.8.2.3.2.4 After the cartridges on the manifold are washed, the
vacuum is released, and a rack containing labeled 10 mL
volumetric flasks is placed inside the manifold. Care
must be taken to ensure that the solvent line from each
cartridge is placed inside of the appropriate volumetric
flask as the manifold top is replaced.
10,. 1. 8 .2 . 3 .2 .5 After the volumetric flasks are in place, the vacuum to
the manifold is restored, and a volume of extract equal
to the required final volume (1 or 2 mL) from each
sample, blank or matrix spike extract is transferred to
the top frit of the appropriate Florisil cartridge. This
must equal the final volume after Florisil cleanup.-
10.1.8.2.3.2.6 Because the volumes marked on concentrator tubes are not
necessarily accurate at the 1 mL level, the use of a
syringe or a volumetric pipet is required to transfer the
extract to the cleanup cartridge.
-D-52/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
Cleanup Procedures
10.1.8.2.3.2.7 The pesticides/Aroclors in the extract concentrates are
then eluted through the column with 8 mL of
hexane/acetone (90:10) and are collected into the 10 mL
volumetric flasks held in the rack inside the vacuum
manifold.
10.1.8.2.3.2.8 Transfer the eluate in each volumetric flask to a clean
centrifuge tube or 10 mL vial. Use two additional 1 mL
hexane rinses to ensure quantitative transfer of the
cartridge eluate.
10.1.8.2.3.2.9 Adjust the extract to the same 1 or 2 mL aliquot volume
as was taken for cleanup using either nitrogen blowdown
(Section 10.1.7.2) or a micro Snyder column (Section
10.1.7.1). Measure the final volume with a syringe or by
transferring the extract to a volumetric flask.
10.1.8.2.3.2.10 If sulfur cleanup is to be performed, proceed to Section
10.1.8.3. Otherwise, transfer the sample to a GC vial
and label the vial. The extract is ready for GC/EC
analysis.
10.1.8.3 Sulfur Cleanup
10.1.8.3.1 Introduction to Sulfur Cleanup
10.1.8.3.1.1 Sulfur contamination will cause a rise in the baseline of a
chromatogram and may interfere with the analyses of the
later eluting pesticides. If crystals of sulfur are evident
or if the presence of sulfur is suspected, sulfur removal
must be performed. Interference which is due to sulfur is
not acceptable. Sulfur can be removed by one of two
methods, according to laboratory preference. If the sulfur
concentration is such that crystallization occurs in the
concentrated extract, centrifuge the extract to settle the
crystals, and remove the sample extract with a disposable
pipette, leaving the excess sulfur in the centrifuge tube.
Transfer the extract to a clean centrifuge tube or clean
concentrator tube before proceeding with further sulfur
cleanup.
10.1.8.3.1.2 If only part of a set of samples require sulfur cleanup,
then, a sulfur cleanup blank is required for that part of
the set (Section 12.1.3).
10.1.8.3.2 Frequency of Sulfur Cleanup
Sulfur removal is required for all sample extracts that contain
sulfur.
D-53/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
GC/EC Analysis
10.1.8.3.3 Procedure for Sulfur Cleanup
10.1.8.3.3.1 Mercury Technique
Add one to three drops of mercury to each hexane extract in
a clean vial. Tighten the top on the vial and agitate the
sample for 30 seconds. Filter or centrifuge the extract.
Pipet the extract to another vial and leave all solid
precipitate and liquid mercury- If the mercury appears
shiny, proceed to Section 10.2 and analyze the extract. If
the mercury turns black, repeat sulfur removal as necessary.
The extract transferred to the vial still represents the 1.0
or 2.0 mL final volume. CAUTION: Waste containing mercury
should be segregated and disposed of properly. NOTE:
Mercury is a highly toxic metal and therefore must be used
with great care. Prior to using mercury, it is recommended
that the analyst become acquainted with proper handling and
cleanup techniques associated with this metal.
10.1.8.3.3.2 Copper Technique
Add approximately 2 g of cleaned copper powder to the
extract in the centrifuge or concentrator tube (2 g will
fill the tube to about .the 0.5 mL mark) . Mix the copper and
extract for at least 1 minute on a mechanical shaker.
Separate the extract from the copper powder by drawing off
the extract with a disposable pipet, and transfer the
extract to a clean vial. The extract transferred to the
vial still represents the 1.0 or 2.0 mL final volume. The
separation of the extract from the copper powder is
necessary to prevent degradation of the pesticides. If the
copper appears bright, proceed to Section 10.2 and analyze
the extracts. If the copper changes color, repeat the
sulfur removal procedure as necessary.
10.2 GC/EC Analysis
10.2.1 Introduction to Sample Analysis by GC/EC
10.2.1.1 Before samples or required blanks can be analyzed, the instrument
must meet the initial calibration and calibration verification
technical acceptance criteria. Sample analysis on both GC columns
is required for all samples, blanks, matrix spikes, and matrix
spike duplicates.
10.2.1.2 Sample extracts, standards, and blanks must be analyzed within an
analytical sequence as defined in Section 10.2.2.1, under the same
instrumental conditions.
10.2.1.3 Set up the GC/EC system per the requirements in Section 9.0.
Unless ambient temperature on-column injection is used (see
Section 9.1.4), the injector must be heated to at least 200 °C.
The optimized gas chromatographic conditions from Section 9.1 must
be used.
D-54/PEST OLM04.2
-------
Exhibit D Pesticides'/Aroclors -- Section 10
Procedure
GC/EC Analysis
10.2.2 Procedure for Sample Analysis by GC/EC
The injection must be made on-column by using either automatic or
manual injection. If autoinjectors are used, 1 uL injection volumes
may be used. Manual injections shall use at least 2 uL injection
volumes. The same injection volume must be used for all standards,
samples, MS/MSD, and blanks associated with the same initial
calibration. If a single injection is used for two GC columns
attached to a single injection port, it may be necessary to use an
injection volume greater than 2 uL. However, the same injection
volume must be used for all analyses.
10.2.2.1 Analytical Sequence
All acceptable samples must be analyzed within a valid analysis
sequence as given below.
Time
0 hr.
Infection #
1-15
16
17
18
Material Injected
First 15 steps of the initial
calibration
Instrument Blank at end of
initial calibration
PEM at end of initial
calibration
First sample
Subsequent samples
12 hr.
1st injection past
12 hr.
2nd and 3rd injections
past 12 hr.
Last Sample
Instrument blank
Individual Standard Mixtures
A and B
Sample
Subsequent samples
Another 12 hr.
1st injection past
12 hr.
2nd injection past
12 hr.
Last Sample
Instrument blank
PEM
Sample
Subsequent samples
D-55/PEST
OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
GC/EC Analysis
Time Injection # Material Injected
Another 12 hr. . Last Sample
1st injection past Instrument blank
12 hr;
2nd and 3rd injections Individual Standard Mixtures
past 12 hr. A and B
Sample
etc.
10.2.2.1.1 NOTE: The first 12 hours are counted from injection #16 (the
instrument blank at the end of the initial calibration
sequence), not from injection #1. Samples may be injected
until 12 hours have elapsed. All subsequent 12-hour periods
are timed from the injection of the instrument blank that
brackets the front end of the samples. Because the 12-hour
time period is timed from injection of the instrument blank
until the injection of the last sample, each 12-hour period may
be separated by the length of one chromatographic run, that of
the analysis of the last sample. While the 12-hour period may
not be exceeded, the laboratory may run instrument blanks and
standards more frequently for instance, to accommodate staff
working 8-hour shifts.
10.2.2.1.2 After the initial calibration, the analysis sequence may
continue as long as acceptable instrument blanks, PEMs and
Individual Standard Mixtures A and B are analyzed at the
required frequency. This analysis sequence shows only the
minimum required blanks and standards. More blanks and
standards may be run at the discretion of the Contractor:
these must also satisfy the criteria presented in Section 9 in
order to continue the run secruence.
10.2.2.1.3 An analysis sequence must also include all required matrix
spike/matrix spike duplicate and method (and/or sulfur) blank
analyses, but the Contractor may decide at what point in the
sequence they are to be analyzed.
10.2.2.1.4 The requirements for the analysis sequence apply to both GC
columns and for all instruments used for these analyses.
10.2.3 Sample Dilutions
10.2.3.1 All samples must be analyzed at the most concentrated level that
is consistent with achieving satisfactory chromatography (defined
in Section 11.3) .
D-56/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 10
Procedure
GC/EC Analysis
10.2.3.2 If the response of any single component pesticide is greater than
the response of that analyte in the initial calibration high point
standard, then the extract must be diluted to have the response of
that analyte between the initial calibration low point and high
point standards.
10.2.3.3 If the response of the largest peak in a multicomponent analyte is
greater than the most intense single component analyte response in
the initial calibration high point standard, then the sample must
be diluted to have the response of the largest peak in the
multicomponent analyte between the responses of the initial
calibration midpoint and high point standards of that single
component pesticide.
10.2.3.4 If dilution is employed solely to bring a peak within the
calibration range or to get a multicomponent pattern on scale, the
results for both the more and the less concentrated extracts must
be reported. The resulting changes in quantitation limits and
surrogate recovery must be reported also for the diluted samples.
10.2.3.5 If the Contractor has reason to believe that diluting the final
extracts will be necessary, a less diluted run may still be
required. If an acceptable chromatogram (as defined in Section
11.3) is achieved with the diluted extract, then:
If the dilution factor is greater than 10, an additional
extract 10 times more concentrated than the diluted sample
extract must be injected and reported with the sample data.
If the dilution factor is less than or equal to 10, then an
undiluted sample extract must be injected and reported with the
sample data.
If the analysis of the most concentrated extract does not meet the
requirement for dilution in Section 11.3.5, then the analysis is
at no additional cost to the Agency.
10.2.3.6 When diluted, the chromatographic data for the single component
pesticides must be able to be reported at greater than 10.0
percent of full scale but less than 100.0 percent of full scale.
10.2.3.7 When diluted, multicomponent analytes must be able to be reported
at greater than 25.0 percent of full scale but less than 100.0
percent of full scale.
10.2.3.8 If a chromatogram is replotted electronically to meet these
requirements, the scaling factor used must be displayed on the
chromatogram. If the chromatogram of any sample needs to be
replotted electronically to meet these requirements both the
initial chromatogram and the replotted chromatogram must be
submitted in the data package.
D-57/PEST OLM04.2
-------
Exhibit D Pesticicies/Aroclors -- Section 10
Procedure
GC/EC Analysis
10.2.3.9 Samples with analytes detected at a level greater than the high
calibration point must be diluted until the response is within the
linear range established during calibration or to a maximum of
1:100,000.
10.2.3.10 If the response is still above the high calibration point after
the dilution of 1:100,000, the Contractor shall contact SMO
immediately.
10.2.3.11 Use the results of the original analysis to determine the
approximate dilution factor required to get the largest analyte
peak within the initial calibration range.
10.2.3.12 The dilution factor chosen should keep the response of the largest
peak for a target compound in the upper half of the initial
calibration range of the instrument.
10.2.3.13 Sample dilutions must be made quantitatively. Dilute the sample
extract with hexane.
| 10.2.3.14 Do not submit data for more than two analyses, i.e., from the
original sample extract and one dilution, or, from the most
concentrated dilution analyzed and one further dilution. This
statement does not refer .to reanalyses required due to failed
technical acceptance criteria.
D-58/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.0 DATA ANALYSIS AND CALCULATIONS
11.1 Qualitative Identification
11.1.1 Identification of Target Compounds
11.1.1.1 The laboratory will identify and quantitate analyte peaks based on
the RT windows and the calibration factors of the midpoint
standard (single component pesticides) established during the
initial calibration sequence.
11.1.1.2 Analytes are identified when peaks are observed in the RT window
for the analyte on both GC columns.
11.1.1.3 A set of three to five major peaks is selected for each
multicomponent analyte. The retention time window for each peak
is determined from the initial calibration analysis.
Identification of a multicomponent analyte in the sample is based
on pattern recognition in conjunction with the elution of three to
five sample peaks within the retention time windows of the
corresponding peaks of the standard on both GC columns.
Calibration factors used to quantitate toxaphene and the Aroclors
are based on the single-point calibration standard analyzed during
the initial calibration. The number of potential quantitation
peaks is listed in Table 2.
11.1.1.4 When any multicomponent analyte is detected in a sample, a
standard must be run within 72 hours of the analyte's detection
(from time of injection), and within a valid 12-hour sequence.
11.1.1.5 The choice of the peaks used for multicomponent analyte
identification and the recognition of those peaks may be
complicated by the environmental alteration of the toxaphene or
Aroclors, and by the presence of co-eluting analytes or matrix
interferences, or both. Because of the alteration of these
materials in the environment, multicomponent analytes in samples
may give patterns similar to, but not identical with, those of the
standards.
11.1.1.6 If more than one multicomponent analyte is observed in a sample,
the Contractor must choose different peaks to quantitate each
multicomponent analyte. A peak common to both analytes present in
the sample must not be used to quantitate either compound.
11.1.2 GC/MS Confirmation of Pesticides and Aroclors
11.1.2.1 Any pesticide or Aroclor analyte listed in Exhibit C for which a
concentration is reported from a GC/EC analysis must have the
identification confirmed by GC/MS if the concentration is
sufficient for that purpose. The following paragraphs are to be
used as guidance in performing GC/MS confirmation. If the
Contractor fails to perform GC/MS confirmation as appropriate, the
Agency may require reanalysis of any affected samples at no
additional cost to the Agency.
D-59/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Qualitative Identification
11.1.2.2 The GC/MS confirmation may be accomplished by one of three general
means:
Examination of the semivolatile GC/MS library search results
(i.e.,TIC data), or
A second analysis of the semivolatile extract, or
Analysis of the pesticide/Aroclor extract, following any
solvent exchange and concentration steps that may be
necessary.
11.1.2.3 The semivolatile GC/MS analysis procedures outlined in Exhibit D
SVOA are based on the injection into the instrument of
approximately 20 ng of a target compound in a 2 uL volume. The
semivolatile CRQL values in Exhibit C are based on the sample
concentration that corresponds to an extract concentration of 10
ng/uL of target analyte. However, these are quantitation limits,
and the detection of analytes and generation of reproducible mass
spectra will routinely be possible at levels 3-10 times lower.
The sample concentration corresponding to 10 ng/uL in extract will
depend on the sample matrix.
11.1.2.3.1 For water samples, 20 ng/2pL corresponds to a sample
concentration of 10 ug/L.
11.1.2.3.2 For soil/sediment samples prepared according to the
semivolatile low level soil/sediment method (i.e., 30 g of
soil/sediment), the corresponding sample concentration is 330
ug/Kg.
11.1.2.3.3 For soil/sediment samples prepared according to the
semivolatile medium'level soil/sediment method (i.e., 1 g of
soil/sediment), the corresponding sample.concentration is
10,000 ug/Kg.
11.1.2.3.4 Therefore, based on the values given above, any pesticide
sample in which compound concentration in the sample extract is
greater than or equal to 10 ng/uL for single component
pesticides, 50 ng/uL for Aroclors, and 125 ng/uL for Toxaphene
should enable the laboratory to confirm the pesticide/Aroclor
by GC/MS analysis of the semivolatile extract.
11.1.2.4 In order to confirm the identification of the target
pesticide/Aroclor, the laboratory must also analyze a reference
standard for the analyte. In order to demonstrate the ability of
the GC/MS system to identify the analyte in question, the
concentration of the standard should be 10 ng/uL for single
component pesticides, 50 ng/uL for Aroclors, and 125 ng/uL for
Toxaphene.
11.1.2.5 To facilitate the confirmation of the single component pesticide
analytes from the semivolatile library search data, the laboratory
may wish to include these analytes in the semivolatile continuing
calibration standard at a concentration of 10 ng/uL or less. Do
D-60/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Qualitative Identification
not include the Aroclors and toxaphene mixture in the semivolatile
initial and continuing calibration standard. If added to this
GC/MS standard, the response factors, retention times, etc. For
these analytes would be reported on the GC/MS quantitation report,
but not on the GC/MS calibration data reporting forms. As only a
single concentration of each analyte would be analyzed, no
linearity (%RSD) or percent difference criteria would be applied
to the response factors for these additional analytes.
11.1.2.6 The laboratory is advised that library search results from the
NIST/EPA/NIH (May 1992 release or later) and Wiley (1991 release
or later) mass spectral library will not likely list the name of
the pesticide/Aroclor analyte as it appears in this SOW, hence,
the mass spectral interpretation specialist is advised to compare
the CAS Registry numbers for the pesticides/Aroclors to those from
the library search routine.
11.1.2.7 If the analyte cannot be confirmed from the semivolatile library
search data for the original semivolatile GC/MS analysis, the
laboratory may analyze another aliquot of the semivolatile sample
extract after further concentration of the aliquot. This second
aliquot must either be analyzed as part of a routine semivolatile
GC/MS analysis, including instrument performance checks (DFTPP),
calibration standards containing the pesticides/Aroclors as
described in Section 11.1.2.5, or it must be analyzed along with
separate reference standards for the analytes to be confirmed.
11.1.2.8 If the analyte cannot be confirmed by either the procedures in
Sections 11.1.2.5 or 11.1.2.7, then an aliquot of the extract
prepared for the GC/EC analysis must be analyzed by GC/MS,
following any necessary solvent exchange and concentration steps.
As in Section 11.1.2.4, analysis of a reference standard is
required if the GC/MS continuing calibration standard does not
contain the analyte to be confirmed.
11.1.2.9 Regardless of which of the three approaches above is used for
GC/MS confirmation, the appropriate blank must also be analyzed by
GC/MS to demonstrate that the presence of the analyte was not the
result of laboratory contamination. If the confirmation is based
on the analysis of the semivolatile extract, then the semivolatile
method blank extracted with the sample must also be analyzed. If
the confirmation is based on the analysis of the extract prepared
for the GC/EC analysis, then the pesticide method blank extracted
with the sample must be analyzed.
11.1.2.10 If the identification of the analyte cannot be confirmed by any of
the GC/MS procedures above and the concentration calculated from
the GC/EC analysis is greater than or equal to the concentration -
of the reference standard analyzed by GC/MS, then report the .
analyte as undetected, adjust the sample quantitation limit (the
value associated with the "U" qualifier) to a sample concentration
equivalent to the concentration of the GC/MS reference standard,
and qualify the results on Form I with one of the laboratory
defined qualifiers ("X," "Y," or "Z"). In this instance, define
D-61/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Calculations
the qualifier explicitly in the SDG Narrative, and describe the
steps taken to confirm the analyte in the SDG Narrative.
11.1.2.11 For GC/MS confirmation of single component analytes, the required
deliverables are copies of the library search results '(best TIC
matches) or analyte spectrum and the spectrum of the reference
standard. For multicomponent analytes, spectra of three
characteristic peaks are required for both the sample component
and the reference standard.
11.1.2.12 The purpose of the GC/MS analysis for the single component
pesticides is for identification. The purpose of the GC/MS
analysis for the multicomponent analytes is to confirm the
presence of chlorinated biphenyls in Aroclor and the presence of
chlorinated camphenes in Toxaphene. The GC/MS analytical results
for the pesticides/Aroclors shall not be used for quantitation and
the GC/MS results shall not be reported on Form I and Form X. The
exception noted in Section 11.1.2.10 applies only to analytes that
cannot be confirmed above the reference standard concentration.
11.2 Calculations
11.2.1 Target Compounds
The concentrations of the single component pesticides and surrogates
are calculated separately for both GC columns by using the following
equations.
11.2.1.1 Water
EQ. 13
(Ax) (Vt) (Df) (GPC)
Concentration ug/L =
(CF) (Vo) (V,)
Where,
AX = Area of the peak for the compound to be measured.
CF = Calibration factor from the initial calibration for the
midpoint concentration external standard (area per ng).
V0 = Volume of water extracted in milliliters (mL).
Vi = Volume of extract injected in microliters (uL). (If a
single injection is made onto two columns, use one half the
volume in the syringe as the volume injected onto each
column.)
Vt = Volume of the concentrated extract in microliters (uL). (If
GPC is not performed, then Vt = 10,000 uL. If GPC is
performed, then Vc = 5,000 uL.)
Df = Dilution factor. The dilution factor for analysis of water
samples by this method is defined as follows:
D-62/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Calculations
uL most cone, extract used to make dilution + uL clean solvent
uL most cone, extract used to make dilution
If no dilution is performed, Df = 1.0.
GPC = GPC factor. (If no GPC is performed, GPC = 1. If GPC is
performed, then GPC =2.0
11.2.1.2 Soil/Sediment
EQ. 14
(Ax) (Vt) (Df) (GPC)
Concentration ug/Kg (Dry weight basis) =
(CF) (V,) (Wa) (D)
Where,
AX and CF are as given for water, above.
Vt = 5,000 uL.
Vi = Volume of extract injected in microliters (uL). (If a
single injection is made onto two columns, use one half the
volume in the syringe as the volume injected onto each
column.)
_ 100 - % moisture
Too
Ws = Weight of sample extracted in grams (g)
Df = Dilution factor. The dilution factor for analysis of
soil/sediment samples by this method is defined as follows:
uL most cone. Extract used to make dilution + uL clean solvent
uL most cone, extract used to make dilution
If no dilution is performed, Df = 1.0.
GPC = GPC factor = 2.
11.2.1.2.1 " The GPC factor is used to account for the amount of extract
that is not recovered from the mandatory use of GPC cleanup.
Concentrating the extract collected after GPC to 5.0 mL rather
than 10.0 mL for water samples not subjected to GPC maintains
the sensitivity of the soil/sediment method comparable to that
of the water method, but correction of the numerical results is
still required.
D-63/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Calculations
11.2.1.2.2 Note that the calibration factors used for the quantitation of
the single component pesticides are the calibration factors
from the midpoint concentration on standard in the most recent
initial calibration.
11.2.1.2.3 Because of the likelihood that compounds co-eluting with the
target compounds will cause positive interferences and increase
the concentration determined by the method, the lower of the
two concentrations calculated for each single component
pesticide is reported on Form I. In addition, the
concentrations calculated for. both the GC columns are reported
on Form X, along with a percent difference comparing the two
concentrations. The percent difference is calculated according
to Equation 15.
EQ. 15
Cone.. - ConcT
%D = x 100
Where, Conc
L
ConcH = The higher of the two concentrations for the target
compound in question.
ConcL = The lower of the two concentrations for the target
compound in question
11.2.1.2.4 Note that using this equation will result in percent difference
values that are always positive. The value will also be
greater than a value calculated using the higher concentration
in the denominator; however, given the likelihood of a positive
interference raising the concentration determined on one GC
column, this is a conservative approach to comparing the two
concentrations.
11.2.1.2.5 The quantitative determination of Toxaphene or Aroclors is
somewhat different from that of single component pesticides.
Quantitation of peaks within the detector linear range CRQL to
> 16 times CRQL is based on a single calibration point assuming
linear detector response. Alternatively, a linear calibration
range may be established during a run sequence by a three-point
calibration curve for any multicomponent analyte. If the
concentration is calculated to be 106 times the CRQL, the
Contractor shall contact SMO immediately.
11.2.1.2.6 The quantitation of toxaphene or Aroclors must be accomplished
by comparing the heights or the areas of each of the three to
five major peaks of the multicomponent analyte in the sample
with the calibration factor for the same peaks established
during the initial calibration sequence. The concentration of
multicomponent analytes is calculated by using Equations 13 and
14, where f^ is the area for each of the major peaks of the
multicomponent analyte. The concentration of each peak is
determined and then a mean concentration for the three to five
major peaks is determined on each column.
D-64/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Calculations
11.2.1.2.7 The reporting requirements for Toxaphene and the Aroclors are
similar to those for the single component analytes, except that
the lower mean concentration (from three to five peaks) is
reported on Form I, and the two mean concentrations reported on
Form X. The two mean concentrations are compared by
calculating the percent difference using Equation 15.
11.2.2 CRQL Calculation
If the adjusted CRQL is less than the CRQL listed in Exhibit C
(Pesticides), report the CRQL in Exhibit C (Pesticides).
11.2.2.1 Water Samples
EQ. 16
Adjusted _ Contract (Vx) (Vt) (Vy) (Df).
CRQL ' CRQL X (v_) (v_) (V.)
Where,
Vt, Df, V0, and V4 are as given in Equation 13.
Vx = Contract sample volume (1000 mL).
Vy = Contract injection volume (1 uL or 2 uL).
Vc = Contract concentrated extract volume (10,000 uL if GPC was
not performed and 5,000 uL if GPC was performed).
11.2.2.2 Soil/Sediment Samples
.EQ. 17
Adjusted . Contract (Wx) (Ve) (Vy) (Df)
CRQL CRQL X (wj (YC) (VA) (D)
Where,
Vt, Df, Ws, V± and D are as given in Equation 14.
Wx = Contract sample weight (30 g).
Vy = Contract injection volume (1 uL or 2 uL).
Vc = Contract concentrated extract volume (GPC is required:
5,000 uL).
11.2.3 Surrogate Recoveries
11.2.3.1 The concentrations of the surrogates are calculated separately for
each GC column in a similar manner as the other analytes, using
Equations 13 and 14. Use the calibration factors from the
midpoint concentration of Individual Standard Mixture A from the
initial calibration. The recoveries of the surrogates calculated
for each GC column according to Equation 12, repeated below.
D-65/PEST OLM04.2
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Exhibit D Pesticicies/Aroclors -- Section 11
Data Analysis and Calculations
Technical Acceptance Criteria for Sample Analysis
EQ. 12
Where,
Percent Recovery = - x 100
>«a
Qd = Quantity determined by analysis
Qa = Quantity added
11.2.3.2 The advisory limits for the recovery of the surrogates are 30-150
percent for both surrogate compounds.
11.2.3.3 As these limits are only advisory, no further action is required
by the laboratory; however, frequent failures to meet the limits
for surrogate recovery warrant investigation by the laboratory,
and may result in questions from the Agency. Surrogate recovery
data from both GC columns are reported (see Exhibit. B).
11.3 Technical Acceptance Criteria for Sample Analysis
The requirements below apply independently to each GC column and to all
instruments used for these analyses. Quantitation must be performed on
each GC column.
11.3.1 Samples must be analyzed under the GC/EC operating conditions in
Section 9. The instrument must have met all initial calibration,
calibration verification, and blank technical acceptance criteria.
Samples must be cleaned-up, when required, on a GPC meeting the
technical acceptance criteria for GPC calibration and GPC calibration
checks. Samples must be cleaned-up using florisil meeting the
technical acceptance criteria for florisil. Sample data must be
bracketed at 12-hour intervals (or less) by acceptable analyses of
instrument blanks, PEMs and Individual Standard Mixtures A and B, as.
described in Section 10.2.2.1.
11.3.2 The samples must be extracted and analyzed within the contract
required holding times.
11.3.3 The samples must have an associated method blank meeting the
technical acceptance criteria for method blanks. When sulfur cleanup
blanks are required, the samples must have associated with it a
sulfur cleanup blank meeting the technical acceptance criteria for
sulfur cleanup blanks.
11.3.4 The retention time for each of the surrogates must be within the
retention time window as calculated in Section 9 for both GC columns.
11.3.5 No target analyte concentrations may exceed the upper limit of the
initial calibration or else the extract must be diluted and
reanalyzed.
11.3.6 A standard for any identified multicomponent analyte must be analyzed
during a valid analytical sequence on the same instrument and column
within 72 hours of its detection in a sample.
D-66/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Corrective Action for Sample Analysis
11.3.7 The identification of single component pesticides by gas
chromatographic methods is based primarily on retention time data.
The retention time of the apex of a peak can be verified only from an
on-scale chromatogram. The identification of multicomponent analytes
is based primarily on recognition of patterns of retention times
displayed on a chromatogram. Therefore, the following requirements
apply to all data presented for single component and multicomponent
analytes.
11.3.7.1 When no analytes are identified in a sample, the chromatograms
from the analyses of the sample extract must use the same scaling
factor as was used for the low point standard of the initial
calibration associated with those analyses.
11.3.7.2 Chromatograms must display single component pesticides detected in
the sample at less than full scale.
11.3.7.3 Chromatograms must display the largest peak of any multicomponent
analyte detected in the sample at-less than full scale.
11.3.7.4 If an extract must be diluted, chromatograms must display single
component pesticides between 10 and 100 percent of full scale.
11.3.7.5 If an extract must be diluted, chromatograms must display the
peaks chosen for quantitation of multicomponent analytes between
25 and 100 percent of full scale.
11.3.7.6 For any sample or blank, the baseline of the chromatogram must
return to below 50 percent of full scale before the elution time
of alpha-BHC, and return to below 25 percent of full scale after
the elution time of alpha-BHC -and before the elution time of
decachlorobiphenyl.
11.3.7.7 If a chromatogram is replotted electronically to meet these
requirements, the scaling factor used must be displayed on the
chromatogram.
11.3.7.8 If the chromatogram of any sample needs to be replotted
electronically to meet these requirements, both the initial
chromatogram and the replotted chromatogram must be submitted in
the data package.
11.4 Corrective Action for Sample Analysis
11.4.1 Sample analysis technical acceptance criteria MUST be met before data
are reported. Samples contaminated from laboratory sources or
associated with a contaminated method blank or sulfur cleanup blank
will require re-extraction and reanalysis at no additional cost to
the Agency. Any samples analyzed that do not meet the technical
acceptance criteria will require re-extraction and/or reanalysis at
no additional cost to the Agency.
11.4.2 If the sample analysis technical acceptance criteria are not met,
check calculations, surrogate solutions, and instrument performance.
D-67/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 11
Data Analysis and Calculations
Corrective Action for Sample Analysis
It may be necessary to recalibrate the instrument or take other
corrective action procedures to meet the technical acceptance
criteria, in which case, the affected samples must be reanalyzed at
no additional cost to the Agency after the corrective action.
11.4.3 The extract from samples which were cleaned-up by GPC using an
automated injection system and have surrogate recoveries outside the
lower advisory surrogate acceptance limits must be.checked to assure
that the proper amount was injected on the GPC column. If
insufficient volume was injected, the sample must be reprepared and
reanalyzed at no additional cost to the Agency.
11.4.4 If sample chromatograms have a high baseline or interfering peaks,
inspect the system to determine the cause of the problem (e.g.,
carryover, column bleed, dirty BCD, contaminated gases, leaking
septum, etc.). After correcting the problem, analyze an instrument
blank to demonstrate that the system is functioning properly.
Reanalyze the sample extracts. If the problem with the samples still
exists, then those samples must be re-extracted and reanalyzed.
Samples which cannot be made to meet the given specifications after
one re-extraction and three-step cleanup (GPC, Florisil, and sulfur
cleanups) are reported in the SDG Narrative and do not require
further analysis.
D-68/PEST OLM04.2
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Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Blank Analyses
12.0 QUALITY CONTROL
12.1 Blank Analyses
12.1.1 Introduction
There are two types of blanks always required by this method: the
method blank and the instrument blank. A separate sulfur cleanup
blank may be required if all samples associated with a given method
blank are not subjected to sulfur cleanup. Samples that are
associated with a sulfur cleanup blank are also associated with the
method blank with which they were extracted. Both the method and
sulfur cleanup blanks must meet the respective acceptance criteria
for the sample analysis acceptance criteria to be met.
12.1.2 Method Blanks
12.1.2.1 Summary of Method Blanks
A method blank is a volume of a clean reference matrix (reagent
water for water samples, or purified sodium sulfate for
soil/sediment samples) that is carried through the entire
analytical procedure. The volume or weight of the reference
matrix must be approximately equal to the volume or weight of
samples associated with the blank. The purpose of a method blank
is to determine the levels of contamination associated with the
processing and analysis of samples.
12.1.2.2 Frequency of Method Blanks
A method blank must be extracted each time samples are extracted.
The number of samples extracted with each method blank shall not
exceed 20 field samples (excluding matrix spikes/matrix spike
duplicates and PE samples). In addition, a method blank shall:
Be extracted by the same procedure used to extract samples.
Be analyzed on each GC/EC system used to analyze associated
samples.
12.1.2.3 Procedure for Method Blank Preparation
12.1.2.3.1 For pesticide/Aroclor analyses, a method blank for water
samples consists of a 1 L volume of reagent water spiked with
1.0 mL of the surrogate spiking solution (Section 7.2.4.1).
For soil/sediment samples, the method blank consists of 30 g of
sodium sulfate spiked with 2.0 mL of the surrogate spiking
solution.
12.1.2.3.2 Extract, concentrate, and analyze method blanks according to
Section 10.
12.1.2.3.3 Calculate method blank results according to Section 11.
12.1.2.4 Technical Acceptance Criteria for Method Blanks
D-69/PEST OLM04.2
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Exhibit D Pesticicies/Aroclors -- Section 12
Quality Control
Blank Analyses
12.1.2.4.1 The requirements below apply independently to each GC column
and to all instruments used for these analyses. Quantitation
must be performed on both GC columns.
12.1.2.4.2 All method blanks must be prepared and analyzed at the
frequency described in Section 12.1.2.2, using the procedure
above and in Section 10 on a GC/EC system meeting the initial
calibration and calibration verification technical acceptance
criteria. Method blanks must undergo cleanup, when required,
on a GPC meeting the technical acceptance criteria for GPC
calibration and GPC calibration checks. Method blanks must be
cleaned-up using Florisil meeting the technical acceptance
criteria for Florisil. Method blanks must be bracketed at 12-
hour intervals (or less) by acceptable analyses of instrument
blanks, PEMS, and individual standard mixtures A and B as
described in Section 10.2.2.1.
I
12.1.2.4.3 The concentration of the target compounds (Exhibit C
(Pesticides)) in the method blank must be less than the CRQL
for each target compound.
12.1.2.4.4 The method-blank must meet all sample technical acceptance
criteria in Sections 11.3.4 to 11.3.7.
12.1.2.4.5 Surrogate recoveries must fall within the acceptance windows of
30-150%. In the case of the method blank(s), these limits are
not advisory.
12.1.2.5 Corrective Action for Method Blanks
12.1.2.5.1 If a method blank does not meet the technical acceptance
criteria, the Contractor must consider the system to be out of
control.
12.1.2.5.2 If contamination is a problem, then the source of the
contamination must be investigated and appropriate corrective
measures must be taken and documented before further sample.
analysis proceeds. It is the Contractor's responsibility to
ensure that method interferences caused by contaminants in
solvents, reagents, glassware, and sample storage and sample
processing hardware that lead to discrete artifacts and/or
elevated baselines be investigated and appropriate corrective
actions be taken and documented before further sample analysis.
All samples associated with a contaminated method blank must be
re-extracted/reanalyzed at no additional cost to the Agency.
12.1.2.5.3 If the surrogate recoveries in the method blank do not meet the
acceptance criteria listed in Section 12.1.2.4.5, first
reanalyze the method blank. If surrogate recoveries do not
meet the acceptance criteria after reanalysis, the method blank
and all samples associated with that method blank must be
re-extracted and reanalyzed at no additional cost to the
Agency.
12.1.2.5.4 If the method blank failed to meet the criteria listed in
D-70/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Blank Analyses
Sections 12.1.2.4.2 and 12.1.2.4.4, then there is an instrument
problem. Correct the instrument problem and reanalyze the
method blank.
12.1.3 Sulfur Cleanup Blanks
12.1.3.1 Summary of Sulfur Cleanup Blanks
The sulfur cleanup blank is a modified form of the method blank.
The sulfur cleanup blank is hexane spiked with the surrogates and
carried through the sulfur cleanup and analysis procedures. The
purpose of the sulfur cleanup blank is to determine the levels of
contamination associated with the separate sulfur cleanup steps.
12.1.3.2 Frequency of Sulfur Cleanup Blanks
The sulfur cleanup blank is prepared separately when only part of
a set of samples extracted together requires sulfur removal. A
method blank is associated with the entire set of samples. The
sulfur cleanup blank is associated with the part of the set which
required sulfur cleanup. If all the samples associated with a
given method blank are subjected to sulfur cleanup, then the
method blank must be subjected to sulfur cleanup, and no separate
sulfur cleanup blank is required.
12.1.3.3 Procedure for Sulfur Cleanup Blank
12.1.3.3.1 The concentrated volume of the blank must be the same as the
final volume of the samples associated with the blank. The
sulfur blank must also contain the surrogates at the same
concentrations as the sample extracts (assuming 100.0 percent
recovery). Therefore, add 0.1 mL of the surrogate solution to
0.9 mL of hexane in a clean vial, or for a sulfur blank with a
final volume of 2 mL, add 0.2 mL of the surrogate solution to
1.8 mL of hexane in a clean vial.
12.1.3.3.2 Proceed with the sulfur removal (Section 10.1.8.3.3.1 or
10.1.8.3.3.2) using the same technique (mercury or copper) as
the samples associated with the blank.
12.1.3.3.3 Analyze the sulfur cleanup blank according to Section 10.2.
Assuming that the material in the sulfur cleanup blank resulted
from the extraction of a 1 L water sample, calculate the
concentration of each analyte using the equation in Section
11.2.1.1. Compare the results to the CRQL values for water
samples in Exhibit C (Pesticides).
12.1.3.4 Technical Acceptance Criteria For Sulfur Cleanup Blanks
12.1.3.4.1 The requirements below apply independently to each GC column
and to all instruments used for these analyses. Quantitation
must be performed on both GC columns. .
D-71/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Blank Analyses
12.1.3.4.2 All sulfur cleanup blanks must be prepared and analyzed at the
frequency described in Section 12.1.3.2 using the procedure
referenced in Section 12.1.3.3 on a GC/EC system meeting the
initial calibration and calibration verification technical
acceptance criteria.
12.1.3.4.3 Sulfur cleanup blanks must be bracketed at 12-hour intervals
(or less) by acceptable analyses of instrument blanks, PEMs,
and Individual Standard Mixtures A and 8, as described in
Section 10.2.2.1.
12.1.3.4.4 The concentration of the target compounds (Exhibit C
(Pesticides)) in the sulfur cleanup blank must be less than the
CRQL for each target compound.
12.1.3.4.5 The sulfur cleanup blank must meet all sample technical
acceptance criteria in Sections 11.3.4 to 11.3.7.
12.1.3.4.6 Surrogate recoveries must fall within the acceptance windows of
30-150%. In the case of the sulfur cleanup blank, -these limits
are not advisory.
12.1.3.5 Corrective Action for Sulfur Cleanup Blanks
12.1.3.5.1 If a sulfur cleanup blank does not meet the technical
acceptance criteria, the Contractor must consider the system to
be out of control.
12.1.3.5.2 If contamination is a problem, then the source of the
contamination must be investigated and appropriate corrective
measures must be taken and documented before further sample
analysis proceeds. It is the Contractor's responsibility to
insure that method interferences caused by contaminants in
solvents, reagents, glassware, and sample storage and sample
processing hardware that lead to discrete artifacts and/or
elevated baselines be investigated and appropriate corrective
actions be taken and documented before further sample analysis.
All samples associated with a contaminated sulfur cleanup blank
must be re-extracted/reanalyzed at no additional cost to the
Agency.
12.1.3.5.3 If the surrogate recoveries in the sulfur cleanup blank do not
meet the acceptance criteria listed in Section 12.1.3.4.5,
first reanalyze the sulfur cleanup blank. If surrogate
recoveries do not meet the acceptance criteria after
reanalysis, the sulfur cleanup blank and all samples associated
with that sulfur cleanup blank must be re-extracted and
reanalyzed at no additional cost o the Agency.
12.1.3.5.4 If the sulfur cleanup blank failed to meet the criteria used in
Sections 12.1.3.4.2 and 12.1.3.4.5, then there is an instrument
problem. Correct the instrument problem and reanalyze the
sulfur cleanup blank.
D-72/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Blank Analyses
12.1.4
Instrument Blanks
12.1.4.1 Summary of Instrument Blanks
An instrument blank is a volume of clean solvent spiked with the
surrogates and' analyzed on each GC column and instrument used for
sample analysis. The purpose of the instrument blank is to
determine the levels of contamination associated with the
instrumental analysis itself, particularly with regard to the
carry over of analytes from standards or highly contaminated
samples into other analyses.
12.1.4.2 Frequency of Instrument Blanks
The first analysis in a 12-hour analysis sequence must be an
instrument blank. All acceptable sample analyses are to be
bracketed by acceptable instrument blanks, as described in Section
10.2.2.1. If more than 12 hours have elapsed since the injection
of the instrument blank that>bracketed a previous 12-hour period,
an instrument blank must be analyzed to initiate a new 12-hour
sequence.
12.1.4.3 Procedure for Instrument Blanks
12.1.4.3.1 Prepare the instrument blank by spiking the surrogates into
.hexane or iso-octane for a concentration of 20 ng/mL of
tetrachloro-m-xylene and decachlorobiphenyl.
12.1.4.3.2 Analyze the instrument blank according to Section 10.2 at the
frequency listed in Section 12.1.4.2.
12.1.4.3.3 For comparing the results of the instrument blank analysis to
the CRQLs, assume that the material in the instrument resulted
from the extraction of a 1 L water sample and calculate the
concentration of each analyte using the equation in Section
11.2.1.1. Compare the results to one-half the GRQL values for
water samples in Exhibit C (Pesticides-) .
12.1.4.4 Technical Acceptance Criteria for Instrument Blanks
12.1.4.4.1 The requirements below apply independently to each GC Column
and to all instruments used for these analyses. Quantitation
must be performed and reported independently (on Form I PEST)
for each GC Column.
12.1.4.4.2 All instrument blanks must be prepared and analyzed at the
frequency described in Section 12.1.4.2, using the procedure in
Section 12.1.4.3 on a GC/EC system meeting the initial
calibration and calibration verification technical acceptance
criteria.
12.1.4.4.3 The concentration of each of the target analytes (Exhibit C
(Pesticides)) in the instrument blank must be less than 0.5
times the CRQL for that analyte.
D-73/PEST
OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.1.4.4.4 The instrument blank must meet all sample technical acceptance
criteria in Sections 11.3.4 to 11.3.7.
12.1.4.5 Corrective Action for Instrument Blanks
12.1.4.5.1 If analytes are detected at greater than half the CRQL, or the
surrogate RTs are outside the RT windows, all data collection
must be stopped, and corrective action must be taken. Data for
samples which were run between the last acceptable instrument
blank and the unacceptable blank are considered suspect. An
acceptable instrument blank must be run before additional data
are collected. After an acceptable instrument blank is run,
all samples which were considered.suspect as defined by the
criteria described above must be reinjected during a valid run
sequence at no additional cost to the Agency and must be
reported.
12.2 Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.1 Summary of MS/MSD
In order to evaluate the effects of the sample matrix on the methods
used for pesticide/Aroclor analyses, the Agency has prescribed a
mixture of pesticide/Aroclor target compounds to be spiked into two
aliquots of a sample, and analyzed in accordance with the appropriate
method.
12.2.2 Frequency of MS/MSD Analysis
12.2.2.1 A matrix spike and matrix spike duplicate must-be extracted and
analyzed for every 20 field samples of a similar matrix in an SDG.
NOTE: There is no differentiation between "low" and "medium"
level soil/sediment samples in this method. Therefore only one
soil/sediment MS/MSD is to be submitted per Sample Delivery Group
(SDG). MS/MSD samples shall be analyzed unless otherwise
specified on the Traffic Report (TR). If no MS/MSD samples are
specified on the TR, the Contractor shall contact SMO to confirm
that MS/MSD analyses are not required.
12.2.2.2 As part of the Agency's QA/QC program, water, rinsate samples
and/or field blanks may be delivered to a laboratory for analysis.
Do not perform MS/MSD analysis on a water rinsate sample or field
blank. =
12.2.2.3 If the EPA Region designates a sample to be used as an MS/MSD,
then that sample must be used. If there is insufficient sample
.volume remaining to perform an MS/MSD, then the Contractor shall
choose another sample to perform an MS/MSD analysis. At the time
the selection is made, the Contractor shall notify the Region
(through SMO) that insufficient-sample was received and identify
the EPA sample selected for the MS/MSD analysis. The rationale
for the choice of another sample other than the one designated by
the Agency shall be documented in the SDG Narrative.
D-74/PEST OLM04.2
-------
Exhibit D Pestrcides/Aroclors -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
12.2.2.4 If there is insufficient sample volume remaining in any of the
samples in an SDG to perform an MS/MSD, the Contractor shall
immediately contact SMO to inform them of the problem. SMO will
contact the Region for instructions. The Region will either
approve that no MS/MSD be performed, or require that a reduced
sample aliquot be used for the MS/MSD analysis. SMO will notify
the Contractor of the Region's decision. The Contractor shall
document the decision in the SDG Narrative. .
12.2.2.5 If it appears that the Region has requested MS/MSD analysis at a
greater frequency then required by the contract, the Contractor
shall contact SMO. SMO will contact the Region to determine which
samples should have an MS/MSD performed on them. SMO will notify
. the Contractor of the Region's decision. The Contractor shall
document the decision in the SDG Narrative. If this procedure is
not followed, the Contractor will not be paid for MS/MSD analysis
performed at a greater frequency than required by the contract.-
12.2.2.6 When a Contractor receives only performance evaluation (PE)
samples, no MS/MSD shall be performed within that SDG.
12.2.2.7 When a Contractor receives a PE sample as part of a larger SDG, a
sample other than the PE sample must be chosen for the MS/MSD when
the Region did not designate samples to be used for this purpose.
If the PE-sample is received as an ampulated standard extract, the
ampulated PE sample is not considered to be another matrix type.
12.2.3 Procedure for Preparing MS/MSD
12.2.3.1 Water Samples
For water samples, measure out two additional 1 L aliquots of the
sample chosen for spiking. Adjust the pH of the samples (if
required) and fortify each with 1 mL of matrix spiking solution.
Using a syringe or volumetric pipet, add 1 mL of surrogate spiking
solution to each sample. Extract, concentrate, cleanup, and
analyze matrix spikes and matrix spike duplicate according to
Section 10.0.
12.2.3.2 Soil/Sediment Samples
For soil/sediment samples weigh out two additional 30 g (record
weight to the nearest 0.1 g) aliquots of the sample chosen for
spiking. Add 1 mL of matrix spiking solution and 2 mL of
surrogate solution. Extract, concentrate, cleanup, and analyze
matrix spikes and matrix spike duplicates according to Section
10.0.
12.2.3.3 Note: Before any MS/MSD analysis, analyze the original sample,
then analyze the MS/MSD at the same concentration as the most
concentrated extract for which the original sample results will be
reported. For example, if the original sample is to be reported
at a 1:1 dilution and a 1:10 dilution, then analyze and report the
MS/MSD at a 1:1 dilution only. However, if the original sample is
to be reported at a 1:10 dilution and a 1:100 dilution, then the
D-75/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
MS/MSD must be analyzed and reported at a 1:10 dilution only. Do
not further dilute the MS/MSD samples to get either spiked or
nonspiked analytes within calibration range.
12.2.4 Calculations for MS/MSD
12.2.4.1 The percent recoveries and the relative percent difference between
the recoveries of each of the compounds in the matrix spike
samples will be calculated and reported by using the following
equations:
EQ. 18
CCTD GT?
Matrix Spike Recovery = x 100
SA-
Where,
SSR
SR
SA
Spike' sample result
Sample result
Spike added
EQ. 19
Where,
RPD
MSR
MSDR =
RPD =
[MSR - MSDR|
- (MSR + MSDR)
x 100
Relative percent difference
Matrix spike recovery
Matrix spike duplicate recovery
12.2.4.2 The vertical bars in the formula above indicate the absolute value
of the difference, hence RPD is always expressed as a positive
value.
12.2.5 Technical Acceptance Criteria for MS/MSD
12.2.5.1 The requirements below apply independently to each GC column and
to all instruments used for these analyses. Quantitation must be
performed on both GC columns.
12.2.5.2 All MS/MSD must be prepared and analyzed at the frequency
described in Section 12.2.2, using the procedure above and in
Section 10 on a GC/EC system meeting the initial calibration,
calibration verification, and blank technical acceptance criteria.
MS/MSD must be cleaned-up, when required, on a GPC meeting the
technical acceptance criteria for GPC calibration and GPC
calibration checks. MS/MSD must be cleaned-up using florisil
meeting the technical acceptance criteria for florisil. MS/MSD
must be bracketed at 12-hour intervals (or less) by acceptable
D-76/PEST
OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 12
Quality Control
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
analyses of instrument blanks, PEMS, and individual standard
mixtures A and B as described in Section 10.2.2.1.
12.2.5.3 The samples must be extracted and analyzed within the contract
required holding times.
12.2.5.4 The retention time for each of the surrogates must be within the
retention time window as calculated in Section 9 for both GC
columns.
12.2.5.5 The limits for matrix spike compound recovery and RPD are given in
Table 3. As these limits are only advisory, no further action by
the laboratory is required. However, frequent failures to meet
the limits for recovery or RPD warrant investigation by the
laboratory, and may result in questions from the Agency.
12.2.6 Corrective Action for MS/MSD
Any MS/MSD which fails to meet the technical acceptance criteria for
MS/MSD must be reanalyzed at no additional cost to the Agency.
D-77/PEST OLM04.2
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Exhibit D Pesticicies/Arociors -- Sections 13-16
Method Performance/Pollution Prevention/Waste Management/References
13.0 METHOD PERFORMANCE
Not Applicable
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or
eliminates the quantity or toxicity of waste at the point of generation.
Numerous opportunities for pollution prevention exist in laboratory
operation. The EPA has established a preferred hierarchy of
environmental management techniques that places pollution prevention as
the management option of first choice. Whenever feasible, laboratory-
personnel should use pollution prevention techniques to address their
waste generation. When wastes cannot be feasibly reduced at the source,
the Agency recommends recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to
laboratories and research institutions, consult Less is Better:
Laboratory Chemical Management for Waste Reduction, available from the
American Chemical Society's Department-of Government Relations and
Science Policy, 1155 16th Street N.W., Washington, D.C. 20036,
(202)872-4477.
15.0 WASTE MANAGEMENT
t
The Environmental Protection Agency requires that laboratory waste
management practices be conducted consistent with all applicable rules
and regulations. The Agency urges laboratories to protect the air,
water, and land by minimizing and controlling all releases from hoods
and bench operations, complying with the letter and spirit of any sewer
discharge permits and regulations, and by complying with all solid and
hazardous waste regulations, particularly the hazardous waste
identification rules and land disposal restrictions. For further
information on waste management consult The Waste management Manual for
Laboratory Personnel, available from the American Chemical Society at
the address listed in Section 14.2. .
16.0 REFERENCES
Not Applicable
D-78/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 17
Tables/Diagrams/Flowcharts
17.0 TABLES/DIAGRAMS/FLOWCHARTS
Table 1
Retention Time Windows for Single and
Multicomponent Analytes and Surrogates
Compound
alpha-BHC
beta-BHC
gamma -BHC (Lindane)
delta-BHC
Heptachlor
Aldrin }
alpha - Chlordane
gamma- Chlordane
Heptachlor epoxide
Dieldrin
Endrin
Endrin aldehyde
Endrin ketone
4,4' -ODD
4,4' -DDE
4,4 '-DDT
Endosulfan I
Endosulfan II
Endosulfan sulfate
Methoxychlor
Aroclors
Toxaphene
Tetrachloro-m-xylene
Decachlorobiphenyl
Retention Time Window (minutes)
± 0.05
±0.05
±0.05
±0.05
± 0.05
±0.05
±0.07
±0.07
±0.07
±0.07
± 0.07
±0.07
± 0.07
±0.07
± 0.07
±0.07
±0.07
± 0.07
±0.07
± 0.07
± 0.07
..± 0.07
±0.05
± 0.10
D-79/PEST OLM04.2
-------
Exhibit D Pesticides/Aroclors -- Section 17
Tables/Diagrams/Flowcharts
Table 2
Number of Potential Quantitation Peaks
Multicomponent Analyte
No. of Potential
Quantitation Peaks
Aroclor 1016/1260
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Toxaphene
5/5
3
4
5
5
5
4
Table 3
Matrix Spike Recovery and
Relative Percent Difference Limits
Compound
gamma -BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4, 4 --DDT
%Recovery
Water
56-123
40-131
40-120
52-126
56-121
38-127
RPD
Water
15
20
22
18
21
27
%Recovery
Soil
46-127
35-130
34-132
31-134
42-139
23-134
RPD
Soil
50
31
43
38
45
50
D-80/PEST
OLM04.2
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EXHIBIT E
QUALITY ASSURANCE/QUALITY CONTROL PROCEDURES AND REQUIREMENTS
E-l OLM04.2
-------
Exhibit E - Quality Assurance/Quality Control Procedures and Requirements
Table of Contents
Section Page
1.0 OVERVIEW 4
2.0 INTRODUCTION 5
3.0 QUALITY ASSURANCE PLAN 7
3.1 Introduction 7
3.2 Required Elements of a Quality Assurance Plan 7
3.3 Updating and Submitting the Quality Assurance Plan 9
3.4 Corrective Actions 10
4.0 STANDARD OPERATING PROCEDURES 11
4.1 Introduction 11
4.2 Format 12
4.3 Requirements 12
4.4 Submitting and Updating SOPs 15
4.5 Corrective Actions 17
5.0 ANALYTICAL STANDARDS REQUIREMENTS 18
5.1 Overview ; 18
5.2 Preparation of Chemical Standards from the Neat High Purity
Bulk Material 18
5.3 Purchase of Chemical Standards Already in Solution 19
5.4 Requesting Standards From the EPA Standards Repository .... 22
5.5 Documentation of the Verification and Preparation of Chemical
Standards 22
5.6 Corrective Actions 23
6.0 DETERMINATION OF METHOD EQUIVALENCY FOR ALTERNATIVE EXTRACTION
PROCEDURES 24
6.1 Initial Precision Recovery (IPR) Study - ... 24
6.2 Analytical Protocol Required 25
6.3 Quantit'ation Limits/Quality Control Requirements 25
6.4 Data Deliverable Requirements 26
7.0 CONTRACT COMPLIANCE SCREENING 27
8.0 REGIONAL DATA REVIEW 28
9.0 PROFICIENCY TESTING 29
9.1 Performance Evaluation Samples 29
9.2 Quarterly Blind Audits . . 30
10.0 GC/MS AND GC/EC TAPE AUDITS ; . . 33
10.1 Overview 33
10.2 Submission of the GC/MS and GC/EC Tapes 35
10.3 Responding to the GC/MS and GC/EC Tape Audit Report 35
10.4 Corrective Actions 36
E-2 OLM04.2
-------
11.0 DATA PACKAGE AUDITS 38
11.1 Overview 38
11.2 Responding to the Data Package Audit Report 38
11.3 Corrective Actions 38
12.0 ON-SITE LABORATORY EVALUATIONS 39
12.1 Overview -39
12.2 Quality Assurance On-Site Evaluation . 39
12.3 Evidentiary Audit 39
12.4 Discussion of the On-Site Team's Findings 40
12.5 Corrective Action Reports for Follow-Through to Quality
Assurance and Evidentiary Audit Repprts ... 40
12.& Corrective Actions 41
13.0 QUALITY ASSURANCE AND DATA TREND ANALYSIS . 42
14.0 DATA MANAGEMENT 43
E-3 . OLM04.2
-------
Exhibit E -- Section 1
Overview
1.0 OVERVIEW
1.1 Quality assurance and quality control are integral parts of the
Environmental Protection Agency's (EPA) Contract Laboratory Program
(CLP). The quality assurance (QA) process consists of management review
and oversight at the planning, implementation, and completion stages of
the environmental data collection activity, and ensures that data
provided are of the quality required. The quality control (QC) process
includes those activities required during data collection to produce the
data quality desired and to document the quality of the collected data.
1.2 During the planning of an environmental data collection program, QA
activities focus on defining data quality criteria and designing a QC
system to measure the quality of data being generated. During the
implementation of the data collection effort, QA activities ensure that
the QC system is functioning effectively, and that the deficiencies
uncovered by the QC system are corrected. After environmental data are
collected, QA activities focus on assessing the quality of data obtained
to determine its suitability to support enforcement or remedial
decisions.
1.3 This exhibit describes the overall quality assurance/quality control
operations and the processes by which the CLP meets the QA/QC objectives
defined above. This contract requires.a variety of QA/QC activities.
These contract requirements are the minimum QC operations necessary to
satisfy the analytical requirements associated with the determination of
the different method analytes. These QC operations are designed to
facilitate laboratory comparison by providing EPA with comparable data
from all Contractors. These requirements do not release the analytical
Contractor from maintaining their own QC checks on method and instrument
performance.
E-4 OLM04.2
-------
Exhibit E -- Section 2
Introduction
2.0 INTRODUCTION
2.1 Appropriate use of data generated under the large range of analytical
conditions encountered in environmental analyses requires reliance on
the QC procedures and criteria incorporated into the methods. The
methods in this contract have been validated on samples typical of those
received by the laboratories in the CLP. However, the validation of
these methods does not guarantee that they perform equally well for all
sample matrices encountered. Inaccuracies can also result from causes
other than unanticipated matrix effects, such as sampling artifacts,
equipment malfunctions, and operator error. Therefore, the quality
control component of each method is indispensable.
2.2 The data acquired from QC procedures are used to estimate and evaluate
the information content of analytical results and to determine the
necessity for or the effect of corrective action procedures. The
parameters used to estimate information content include precision,
accuracy, detection limit, and other quantitative and qualitative
indicators. In addition, QC procedures give an overview of the
activities required in an integrated program to generate data of known
and documented quality required to meet defined objectives.
2.3 The necessary components of a complete QA/QC program include internal QC
criteria that demonstrate acceptable levels of performance, as
determined by QA review. External review of data and procedures is
accomplished by the monitoring activities of the National Program
Office, Regional data users, Sample Management Office (SMO), and the
Quality Assurance Technical Support (QATS) Laboratory. Each external
review accomplishes a different purpose. These reviews are described in
specific sections of this exhibit. Laboratory evaluation samples, GC/MS
and GC/EC tape audits, and data packages provide an external QA
reference for the program. A Contractor on-site evaluation system is
also part of the external QA monitoring. A feedback loop provides the
results of the various review functions to the Contractors through
direct communications with the Technical Project Officers (TPOs) and
Administrative Project Officers (APOs).
2.4 This exhibit does not provide specific instructions for constructing QA
plans, QC systems, or a QA organization. It is, however, an explanation
of the QA/QC requirements of the program. It outlines some minimum
standards for QA/QC programs. It also includes specific items that are
required in a QA plan and by the QA/QC documentation detailed in this
contract. Delivery o'f this documentation provides the Agency with a
complete data package which will stand alone, and limits the need for
contact with the Contractor or with an analyst, at a later date, if some
aspect of the analysis is questioned.
2.5 In order to assure that the product delivered by the Contractor meets
the requirements of the contract, and to improve interlaboratory data
comparison, the Agency requires the following from the Contractor:
Preparation of and adherence to a written quality assurance plan,
the elements of which are designated in Section 3,
E-5 OLM04.2
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Exhibit E -- Section 2
Introduction
Preparation of and adherence to QA/QC standard operating procedures
as described in Section 4,
Adherence to the analytical methods and associated QC requirements
specified in the contract,
Verification of analytical standards and documentation of the purity
of neat materials and the purity and accuracy of solutions obtained
from private chemical supply houses,
Submission of all raw data and pertinent documentation for Regional
review,
Participation in the analysis of laboratory evaluation samples,
including adherence to corrective action procedures,
Submission, upon request, of GC/MS and/or GC/EC tapes and applicable
documentation for tape audits, including a copy of the sample data
package,
Participation in on-site laboratory evaluations, including adherence
to corrective action procedures, and
Submission of all original documentation generated during sample
analyses for Agency review.
E-6 OLM04.2
-------
Exhibit E -- Section 3
Quality Assurance Plan
3.0 QUALITY ASSURANCE PLAN
3.1 Introduction. The Contractor shall establish a quality assurance
program with the objective of providing sound analytical chemical
measurements. This program shall incorporate the quality control
procedures, any necessary corrective action, and all documentation
required during data collection as well as the quality assessment
measures performed by management to ensure acceptable data production.
3.1.1 As evidence of such a program, the Contractor shall prepare a written
quality assurance plan (QAP) which describes the procedures that are
implemented to achieve the following:
Maintain data integrity, validity, and usability,
Ensure that analytical measurement systems are maintained in an
acceptable state of stability and reproducibility,
Detect problems through data assessment and establish corrective
action procedures which keep the analytical process reliable, and
Document all aspects of the measurement process in order to
provide data which are technically sound and legally defensible.
3.1.2 The QAP shall present, in specific terms, the policies, organization,
objectives, functional guidelines, and specific QA and QC activities
designed to achieve the data quality requirements in this contract.
Where applicable, standard operating procedures pertaining to each
element shall be included or referenced as part of the QAP. The QAP
shall be paginated consecutively in ascending order. The QAP shall
be available during on-site laboratory evaluations. Additional
information relevant to the preparation of a QAP can be found in
Agency and American Society for Testing and Materials publications.
3.2 Required Elements of a Quality Assurance Plan. The required elements of
a laboratory's QAP are outlined in this section. This outline should be
used as a framework for developing the QAP.
A. Organization and Personnel
1. QA Policy and Objectives
2. QA Management
a. Organization
b. Assignment of QC and QA Responsibilities
c. Reporting Relationships
d. QA Document Control Procedures
e. QA Program Assessment Procedures
E-7 OLM04.2
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Exhibit E -- Section 3
Quality Assurance Plan
3. Personnel
a. Resumes
b. Education and Experience
c. Training Progress
B. Facilities and Equipment
1. Instrumentation and Backup Alternatives
2. Maintenance Activities and Schedules
C. Document Control
1. Contractor Notebook Policy
2. Sample Tracking/Custody Procedures
3. Logbook Maintenance and Archiving Procedures'
4. Case File Organization, Preparation, and Review Procedures
5. Procedures for Preparation, Approval, Review, Revision, and
Distribution of Standard Operating Procedures
6. Process for Revision of Technical or Documentation Procedures
D. Analytical Methodology
1. Calibration Procedures and Frequency
2. Sample Preparation/Extraction Procedures
3. Sample Analysis Procedures
4. Standards Preparation Procedures
5. Decision Processes, Procedures, and Responsibility for
Initiation of Corrective Action
E. Data Generation
1. Data Collection Procedures
2. Data Reduction Procedures
3. Data Validation Procedures
4. Data Reporting and Authorization Procedures
E-8 OLM04.2
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Exhibit E -- Section 3
Quality Assurance Plan
F. Quality Control
1. Solvent, Reagent, and Adsorbent Check Analysis
2. Reference Material Analysis
3. Internal Quality Control Checks
4. Corrective Action and Determination of QC Limit Procedures
5. Responsibility Designation
G. Quality Assurance
1. Data Quality Assurance
2. Systems/Internal Audits
3. Performance/External Audits
4. Corrective Action Procedures
5. Quality Assurance Reporting Procedures
6. Responsibility Designation
3.3 Updating and Submitting the Quality Assurance Plan
3.3.1 Initial Submission. During the contract solicitation process, the
| Contractor is required to submit their QAP to the Contracting
Officer. Within 60 days after contract award, the Contractor shall
revise the QAP to be in full compliance with the requirements of this
contract. The Contractor shall maintain the QAP on file at the
Contractor's facility for the term of the contract. The revised QAP
will become the official QAP under the contract and may be used
during legal proceedings. Both the initial QAP submission and the
revised QAP shall be paginated consecutively in ascending order. The
revised QAP shall include:
Changes resulting from (1) the Contractor's internal review of
their organization, personnel, facility, equipment, policy, and
procedures and (2) the Contractor's implementation of the
requirements of the contract, and
Changes resulting from the Agency's review of the laboratory
evaluation sample data, bidder-supplied documentation, and
recommendations made during the pre-award on-site laboratory
evaluation.
| 3.3.1.1 The Contractor shall send a copy of the latest version of the QAP
within 7 days of a"request from a Technical Project Officer or
Administrative Project Officer. The Agency requestor will
designate the recipients.
E-9 OLM04.2
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Exhibit E -- Section 3
Quality Assurance Plan
3.3.2 Subsequent Updates and Submissions. During the term of the contract,
the Contractor shall amend the QAP when the following circumstances
occur:
The Agency modifies the contract,
The Agency notifies the Contractor of deficiencies in the QAP,
The Agency notifies the Contractor of deficiencies resulting from
the Agency's review of the Contractor's performance,
The Contractor identifies deficiencies resulting from the
internal review of the QAP,
The Contractor's organization, personnel, facility, equipment,
policy, or procedures change, or
The Contractor identifies deficiencies resulting from the
internal review of changes in their organization, personnel,
facility, equipment, policy, or procedures.
3.3.2.1 The Contractor shall amend the QAP within 30 days of when the
circumstances listed above result in a discrepancy between what
was previously described in the QAP and what is presently
occurring at the Contractor's facility. When the QAP is amended,
all changes in the QAP shall be clearly marked (e.g., a bar in the
margin indicating where the change is found in the document, or
highlighting the change by underlining the change, bold printing
the change, or using a different print font).. The amended pages
shall have the date on which the changes were implemented. The
Contractor shall incorporate all amendments to the latest version
of the QAP. The Contractor shall archive all amendments to the
QAP for future reference by the Agency.
3.3.2.2 The Contractor shall send a copy of the latest version of the QAP
within 7 days of a request from a Technical Project Officer or
Administrative Project Officer. The Agency requestor will
designate the recipients.
3.4 Corrective Actions. If the Contractor fails to adhere to the
requirements listed in Section 3, the Contractor may expect, but the
Agency is not limited to, the following actions: reduction of numbers
of samples sent under this contract, suspension of sample shipment to
the Contractor, a GC/MS and/or GC/EC tape audit, a data package audit,
an on-site laboratory evaluation, a remedial laboratory evaluation
sample, and/or contract sanctions.
E-10 OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
4.0 STANDARD OPERATING PROCEDURES
4.1 Introduction. In order to obtain reliable results, adherence to
prescribed analytical methodology is imperative. In any operation that
is performed on a repetitive basis, reproducibility is best accomplished
through the use of standard operating procedures (SOPs). As defined by
EPA, an SOP is a written document which provides directions for the
step-by-step execution of an operation, analysis, or action which is
commonly accepted as the method for performing certain routine or
repetitive tasks.
4.1.1 SOPs prepared by the Contractor shall be functional (i.e., clear,
comprehensive, up-to-date, and sufficiently detailed to permit
duplication of results by qualified analysts). The SOPs shall be
paginated consecutively in ascending order.
4.1.2 All SOPs shall reflect activities as they are currently performed by
the Contractor. In addition, all SOPs shall be:
Consistent with current Agency regulations, guidelines, and the
CLP contract's requirements.
Consistent with instrument manufacturers' specific instruction
manuals.
Available to the Agency during an on-site laboratory evaluation.
A complete set of SOPs shall be bound together and available for
inspection at such evaluations. During on-site evaluations,
Contractor personnel may be asked to demonstrate the application .
of the SOPs.
Available to the designated recipients within 7 days, upon
request by the Technical Project Officer or Administrative
Project Officer.
Capable of providing for the development of documentation that is
sufficiently complete to record the performance of all tasks
required by the.protocol.
Capable of demonstrating the validity of data reported by the
Contractor and explaining the cause of missing or inconsistent
results.
Capable of describing the corrective measures and feedback
mechanism utilized when analytical results do not meet protocol
requirements.
Reviewed regularly and updated as necessary when contract,
facility, or Contractor procedural modifications are made.
Archived for future reference in usability or evidentiary
situations.
Available at specific work stations as appropriate.
: ' . . E-ll OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
Subject to a document control procedure which precludes the use
of outdated or inappropriate SOPs.
4.2 Format. The format for SOPs may vary depending upon the kind of
activity for which they are prepared; however, at a minimum, the
vfollowing sections shall be included:
Title page,
Scope and application,
Definitions,
Procedures,
QC limits,
Corrective action procedures, including procedures for secondary
review of information being generated,
Documentation description and example forms,
Miscellaneous notes and precautions, and
References.
4.3 Requirements. The Contractor shall maintain the following SOPs.
4.3.1 Evidentiary SOPs for required chain-of-custody and document control
are discussed in Exhibit F.
4.3.2 Sample Receipt and Storage
Sample receipt and identification logbooks
Refrigerator temperature logbooks
Extract storage logbooks
Security precautions
4.3.3 Sample Preparation
Reagent purity check procedures and documentation
Extraction procedures
Extraction bench sheets
Extraction logbook maintenance
4.3.4 Glassware Cleaning
4.3.5 Calibration (Balances)
E-12 ' OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
Procedures
Frequency requirements
Preventative maintenance schedule and procedures
Acceptance criteria 'and corrective actions
Logbook maintenance
4.3.6 Analytical Procedures (for each Analytical System, including GPC)
Instrument performance specifications
Instrumental operating procedures
Data acquisition system operation
Procedures when automatic quantitation algorithms are overridden
QC required parameters
Analytical run/injection logbooks
Instrumental error and editing flag descriptions and resulting
corrective actions
4.3.7 Maintenance Activities (for each Analytical System, including GPC)
Preventative maintenance schedule and procedures
Corrective maintenance determinants and procedures
Maintenance authorization
4.3.8 Analytical Standards
Standard coding/identification and inventory system
Standards preparation logbook(s)
Standards preparation procedures
Procedures for equivalency/traceability analyses and
documentation
Purity logbook (primary standards and solvents)
Storage, replacement, and labeling requirements
QC and corrective action measures
E-13 OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
4.3.9 Data Reduction Procedures
Data processing systems operation
Outlier identification methods
Identification of data requiring corrective action
Procedures for format and/or forms for each operation
4.3.10 Documentation Policy/Procedures
Contractor/analysts' notebook policy, including review policy
Complete SDG File contents
Complete SDG File organization and assembly procedures, including
review policy
Document inventory procedures, including review policy
4.3.11 Data Validation/Self-Inspection Procedures
Data flow and chain-of-command for data review
Procedures for measuring precision and accuracy
Evaluation parameters for identifying systematic errors
Procedures to ensure that hardcopy and electronic deliverables
(e.g., diskette, telefacsimile) are complete and compliant with
the requirements in Exhibits B and'H
Procedures to ensure that hardcopy deliverables are in agreement
with their comparable electronic deliverables
Demonstration of internal QA inspection procedure (demonstrated
by supervisory sign-off on personal notebooks, internal
performance evaluation samples, etc.)
Frequency and type of internal audits (e.g., random, quarterly,
spot checks, perceived trouble areas)
Demonstration of problem identification, corrective actions and
resumption of analytical processing; sequence resulting from
internal audit (i.e., QA feedback)
Documentation of audit reports (internal and external), audit
response, corrective action, etc.
E-14 OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
4.3.12 Data Management and Handling
Procedures for controlling and estimating data entry errors
Procedures for reviewing changes to data and deliverables and
ensuring traceability of updates
Life cycle management procedures for testing, modifying and
implementing changes- to existing computing systems including
hardware, software, and documentation or installing new systems
Database security, backup and archival procedures including
recovery from system failures
System maintenance procedures and response time
Individuals(s) responsible for system operation, maintenance,
data integrity and security
Specifications for staff training procedures
Storage, retrieval, and verification of the completeness and
readability of GC/MS and GC/EC files transferred to magnetic
media
4;.. 4 Submitting and Updating SOPs
4 .-;4.1 Initial Submission. During the contract solicitation process, .the
| Contractor is required to submit their SOPs to the Contracting
-,:- Officer. Within 60 days after contract award, the Contractor shall
j. prepare and maintain on file, at their facility, a complete, revised
set of SOPs fully compliant with the requirements of this contract.
The revised SOPs will become the official SOPs under the contract and
may be used during legal proceedings. Both the initial submission of
SOPs and the revised SOPs shall be paginated consecutively in
ascending order. The revised SOPs shall include:
Changes resulting from (1) the Contractor's internal review of
their procedures and (2) the Contractor's implementation of the
requirements of the contract, and
Changes resulting from the Agency's review of the laboratory
evaluation sample data, bidder-supplied documentation, and
recommendations made during the pre-award on-site laboratory
evaluation.
| 4.4.1.1 The Contractor shall send a complete set of the latest version of
SOPs or individually requested SOPs within 7 days of a request
from a Technical Project Officer or Administrative Project
Officer. The Agency requestor will designate the recipients.
4.4.2 Subsequent Updates and Submissions. During the term of the contract,
the Contractor shall amend the SOPs when the following circumstances
occur:
E-15 OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
The Agency modifies the contract,
The Agency notifies the Contractor of deficiencies in their SOPs,
The Agency notifies the Contractor of deficiencies resulting from
the Agency's review of the Contractor's performance,
The Contractor's procedures change,
The Contractor identifies deficiencies resulting from the
internal review of their SOPs documentation, or
The Contractor identifies deficiencies resulting from the
internal review of their procedures.
4.4.2.1 Existing SOPs shall be amended or new SOPs shall be written within
30 days of when the circumstances listed above result in a
discrepancy between what was previously described in the SOPs and
what is presently occurring at the Contractor's facility. All
changes in the SOPs shall be clearly marked (e.g., a bar in the
margin indicating where the change is in the document, or
highlighting the change by underlining the change, bold printing
the change, or using a different print font). The amended/new
SOPs shall have the date on which the changes were implemented.
4.4.2.2 When existing SOPs are amended or new SOPs are written, the
Contractor shall document the reason(s) for the change, and
maintain the amended or new SOPs -on f-ile at the laboratory
facility. Documentation of the reason(s) for the changes shall be
maintained on file with the amended SOPs or new SOPs.
| 4.4.2.3 The Contractor shall send a complete set of ttie latest version of
SOPs or individually requested SOPs within 7 days of a request
from a Technical Project Officer or Administrative Project
Officer. The Agency requestor will designate the recipients. ,
4.4.2.4 Documentation of the reason(s) for changes to the SOPs shall also
be submitted with the SOPs. An alternate delivery schedule for
submitting the amended/new SOPs and their documentation may be
proposed by the Contractor, but it is the sole decision of the
Agency, represented either by the Technical Project Officer or
Administrative Project Officer, to approve or disapprove the
alternate delivery schedule. If an alternate delivery schedule is
proposed, the Contractor shall describe in a letter to the
Technical Project Officer, Administrative Project Officer, and the
Contracting Officer why he/she is unable to meet the delivery
schedule listed in this section. The Technical Project
Officer/Administrative Project Officer will not grant an extension
for greater than 30 days for amending/writing new SOPs. The
Technical Project Officer/Administrative Project Officer will not
grant an extension for greater than 14 days for submission of the
letter documenting the reasons for the changes and for submitting
amended/new SOPs. The Contractor shall proceed and not assume
E-16 OLM04.2
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Exhibit E -- Section 4
Standard Operating Procedures
that an extension will be granted until so notified by the
Technical Project Officer and/or Administrative Project Officer.
4.5 Corrective Actions. If the Contractor fails to adhere to the
requirements listed in Section 4, the Contractor may expect, but the
Agency is not limited to, the following action: reduction of number of
samples sent under this contract, suspension of sample shipment to the
Contractor, a GC/MS and/or GC/EC tape audit, a data package audit, an
on-site laboratory evaluation, a remedial laboratory evaluation sample,
and/or contract sanctions.
E-17 OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
5.0 ANALYTICAL STANDARDS REQUIREMENTS
5.1 Overview. EPA will not supply analytical reference standards either for
direct analytical measurements or for the purpose of traceability. All
Contractors shall be required to prepare from neat materials or purchase
from private chemical supply houses those standards necessary to
successfully and accurately perform the analyses required in this
protocol.
5.2 Preparation of Chemical Standards from the Neat High Purity Bulk
Material. A Contractor may prepare their chemical standards from neat
materials. Contractors shall obtain the highest purity possible when
purchasing neat chemical standards; when standards are purchased at less
than 97% purity, the Contractor shall document the reason why a higher
purity could not be obtained.
5.2.1 Neat chemical standards shall be kept refrigerated when not being
used in the preparation of standard solutions. Proper storage of
neat chemicals is essential in order to safeguard them from
decomposition.
5.2.2 The purity of a compound can sometimes be misrepresented by a
chemical supply house. Since knowledge of purity is needed to
calculate the concentration of solute in a solution standard, it is
the Contractor's responsibility to have analytical documentation
ascertaining that the purity of each compound is correctly stated.
Purity confirmation, when performed, should use either differential
scanning calorimetry, gas chromatography with flame ionization
detection, high performance liquid chromatography, infrared
spectrometry, or other appropriate techniques. Use of two or more
independent methods is recommended. The correction factor for
impurity when weighing neat materials in the preparation of solution
standards is:
EQ. 1
. , . , . , weight of pure compound
weight of impure compound = T-= ,
[percent purity/100)
where "weight of pure compound" is that required to prepare a
specific volume of a standard solution at a specified concentration.
5.2.3 When compound purity is assayed to be 97% or greater, the weight may
be used without correction to calculate the concentration of the
stock standard. If the compound purity is assayed to be less than
97%, the weight shall be corrected when calculating the concentration
of the stock solution.
5.2.4 Mis-identification of compounds occasionally occurs and it is
possible that a mislabeled compound may be received from a chemical
supply house. It is the Contractor's responsibility to have
analytical documentation ascertaining that all compounds used in the
preparation of solution standards are correctly identified.
E-18 - OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
Identification confirmation, when performed, shall use gas
chromatography/mass spectrometry analysis on at least two different
analytical columns, or other appropriate techniques.
5.2.5 Calculate the weight of material to be weighed out for a specified
volume taking into account the purity of the compound and the desired
concentration. A second person shall verify the accuracy of the
calculations. Check balances for accuracy with a set of standard
weights every 12 hours. All weighing shall be performed on an
analytical balance to the nearest 0.1 mg and verified by a second
person. The solvent used to dissolve the solute shall be compatible
with the protocol in which the standard is to be used; the solute
shall be soluble, stable, and nbnreactive with the solvent. In the
case of a multicomponent solution, the components must not react with
each other.
5.2.6 Transfer the solute to a volumetric flask and dilute to the specified
solution volume with solvent after ensuring dissolution of the solute
in the solvent. Sonication or warming may be performed to promote
dissolution of the solute. This solution shall be called the primary
standard and all subsequent dilutions shall be traceable back to the
primary standard.
5.2.7 Log notebooks shall be kept for all weighing and dilutions. All
-.V subsequent dilutions from the primary standard and the calculations
-'. for determining their concentrations shall be recorded and verified
by a second person. All solution standards shall be refrigerated
.;, when not in use. All solution standards shall be clearly labeled as
;f to the identity of the compound or compounds, concentration, date
:'' prepared, solvent, and initials of the preparer.
5.3 Purchase of Chemical Standards Already in Solution. Solutions of
analytical reference standards can be purchased by"Contractors provided
they meet the following criteria.
5.3.1 Contractors shall maintain the following documentation to verify the
integrity of the standard solutions they purchase:
Mass spectral identification confirmation of the solution,
Purity confirmation of the solution, and
Chromatographic and quantitative documentation that.the solution
standard was QC checked according to the following section.
5.3.2 The Contractor shall purchase standards for which the quality is
demonstrated statistically and analytically. One way this may be
demonstrated is to prepare and analyze three solutions, a high
standard, a low standard, and a standard at the target concentration
(see Sections 5.3.2.1 and 5.3.2.2). The Contractor shall have
documentation to demonstrate that the analytical results for the high
standard and low standard are consistent with the difference in
theoretical concentrations. This is done by the Student's t-test in
Section 5.3.2.4. If this is achieved, the Contractor shall then
E-19 OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
demonstrate that the concentration of the target standard lies midway
between the concentrations of the low and high standards. This is
done by the Student's t-test in Section 5.3.2.5. The standard is
certified to be within 10% of the target concentration using the
equations in Section 5.3.2.6. If this procedure is used, the
Contractor shall document that the following have been achieved.
5.3.2.1 Two solutions of identical concentration shall be prepared
independently from solutions. An aliquot of the first solution
shall be diluted to the intended concentration (the "target
standard"). One aliquot is taken from the second solution and
diluted to a concentration 10% greater than the target standard.
This is called the "high standard." One further aliquot is taken
from the second solution and diluted to a concentration 10,% less
that the target standard. This is called the "low standard."
5.3.2.2 Six replicate analyses of each standard (a total of 18 analyses)
shall be performed in the following sequence: low standard,
target, high standard, low standard, target standard, high
standard, ...
5.3.2.3 The mean and variance of the six results for each solution shall
be calculated.
EQ. 2
Mean =
EQ. 3
..£..-
6 (MEAN)'
tn-
Variance =
The values Y4 represent the results of the six analyses of each
standard. The means of the low, target, and high standards are
designated M1( M2, and M3, respectively. The variances of the low,
target, and high standards are designated V1( V2, and V3,
respectively. Additionally, a pooled variance, Vp, is calculated.
EQ. 4
V V
V, 3
V = 0.81 2 1.21
P ^
If the square root of Vp is less than 1% of M2, then M22/10,000
shall be used as the value of Vp in all subsequent calculations.
E-20 OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
5.3.2.4 The test statistic shall be calculated.
EQ. 5
Test Statistic =
1.1
0.9
5.3.2.5
If the test statistic exceeds 2.13, then a 20% difference between
the high and low standards exists. In such a case, the standards
are not acceptable.
The test statistic shall be calculated.
EQ. 6
Test Statistic =
k-
1.8
2.2
5.3.2.6
If the test statistic exceeds 2.13, then the target standard
concentration has not been demonstrated to be the midway between
the high and low standards. In such a case, the standards are not
acceptable.
The 95% confidence intervals for the mean result of each standard
shall be calculated.
EQ. 7
Interval for Low Standard =
± 2.13 J-J:
6
Interval for Target Standard =
± 2-.13 J -
6
E-21
OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
EQ. 9
Interval for High Standard = M ± 2 .13 .1 £
5.3.2.6.1 These intervals shall not overlap. If overlap is observed, the
ability to discriminate the 10% difference in concentrations
has not been demonstrated. In such a case, the standards are
not acceptable.
5.3.2.6.2 In any event, the Contractor is responsible for the quality of
the standards employed for analyses under this contract.
5.4 Requesting Standards From the EPA Standards Repository. Solutions of
analytical reference materials can be ordered from the U.S. EPA Chemical
Standards Repository, depending on availability. The Contractor can
place an order for standards only after demonstrating.that these
standards are not available from commercial vendors, either in solution
or as a neat material. .
5.5 Documentation of the Verification and Preparation of Chemical Standards.
It is the responsibility of each Contractor to maintain the neces'sary
documentation to show that the chemical standards they have used in the
performance of CLP analysis conform to the requirements previously
listed.
5.5.1 Weighing logbooks, calculations, chromatograms, mass spectra, etc.,
whether produced by the Contractor or purchased from chemical supply
houses, shall be maintained by the Contractor and may be subject to
review during on-site laboratory evaluations. In those cases where
the documentation is supportive of the analytical results of data
packages sent to the Agency, such documentation is to be kept on file
by the Contractor for a period of one year.
5.5.2 Upon request by the Technical Project Officer or Administrative
Project Officer, the Contractor shall submit their most recent
previous year's documentation (12 months) for the verification and
preparation of chemical standards within 14 days of the receipt of
request to the recipients he/she designates.
5.5.3 The Agency may generate a report discussing deficiencies in the
Contractor's documentation for the verification and preparation of
chemical standards or may discuss the deficiencies during an on-site
laboratory evaluation. In a detailed letter to the Technical Project
Officer and the Administrative Project Officer, the Contractor shall
address the deficiencies and the subsequent corrective action
implemented by the Contractor to correct the deficiencies within 14
days of receipt of the report or the on-site laboratory evaluation.
An alternate delivery schedule may be proposed by the Contractor, but
it is the sole decision of the Agency, represented either by the
Technical Project Officer or Administrative Project Officer, to
approve or disapprove the alternate delivery schedule. If an
E-22 ' OLM04.2
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Exhibit E -- Section 5
Analytical Standards Requirements
alternate delivery schedule is proposed, the Contractor shall
describe in a letter to the Technical Project Officer, Administrative
Project Officer, and the Contracting Officer why he/she is unable to
meet the delivery schedule listed in this section. The Technical
Project Officer/Administrative Project Officer will not grant an
extension for greater than 14 days for the Contractor's response
letter to the standards documentation report. The Contractor shall
proceed and not assume that an extension will be granted until so
notified by the Technical Project Officer and/or Administrative
Project Officer.
5.5.4 If new SOPs are required to be written or SOPs are required to be
amended because of deficiencies and the subsequent corrective action
implemented by the Contractor, the Contractor shall write/amend and
submit the SOPs per the requirements listed in Section 4.
5.6 Corrective Actions. If the Contractor fails to adhere to the
requirements listed in Section 5, the Contractor may expect, but the
Agency is not limited to, the following actions: reduction of number of
samples sent under the contract, suspension of sample shipment to
Contractor, a GC/MS and/or GC/EC tape audit, a data package audit, an
on-site laboratory evaluation, a remedial laboratory evaluation sample,
and/or contract sanctions.
E-23 OLM04.2
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Exhibit E -- Section 6
Determination of Method Equivalency for Alternate Extraction Procedures
6.0 DETERMINATION OF METHOD EQUIVALENCY FOR ALTERNATIVE EXTRACTION
PROCEDURES
If the Contractor wishes to use one or both of the alternative
extraction procedures described in Section 1.3 Exhibits D SVOA and D
PEST under Scope and Application, the Contractor must develop and
implement SOPs for performing the alternative extractions in accordance
to Exhibit E Section 4.0. In addition, the Contractor shall maintain
documentation, including raw data, to demonstrate the equivalence of the
alternative extraction procedures to those specified in Sections
10.1.4.4, Exhibit D SVOA and 10.1.5.3, Exhibit D PEST. The required
documentation for demonstrating extraction equivalence include an
Initial Precision Recovery study as described below.
6.1 Initial Precision Recovery (IPR) Study
6.1.1 For the semivolatile fraction, the Contractor shall spike four (4)
solid samples (e.g., anhydrous sodium sulfate) with all the target
compounds at concentrations equal to three (3) times 'the Contract
Required Quantitation Limits (CRQL) listed in Exhibit C under
semivolatiles. For pesticides/Aroclors, the Contractor shall spike
four (4) solid samples with the single component target compounds and
an additional four (4) solid samples with Aroclor 1254 only at
concentrations equal to three (3) times the CRQLs listed in Exhibit C
under pesticides/Aroclors. Each sample must contain the appropriate
surrogates at the concentrations specified in Section 10.1.4.4,
Exhibit D SVOA or Section 10.1.5.3.3, Exhibit D PEST.
6.1.2 The Contractor shall achieve the following recovery limits for the
matrix spike compounds in each of the four replicates of the IPR
study.
| Recovery Limits for_Matrix_S_p_ike Compounds
| Semi vo1atiles
| Compound Recovery Limits
| Phenol 26-90
| 2--Chlorophenol 25-102
| N-Nitroso-di-n-propylamine 41-126
\ 4-Chloro-3-methylphenol 26-103
| Acenaphthene 31-137
| 4-Nitrophenol 11-114
| 2,4-Dinitrotoluene 28-89
| Pentachlorophenol 17-109
I Pyrene 35-142
E-24 OLM04.2
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Exhibit E -- Section 6
Determination of Method Equivalency for Alternative Extraction Procedures
| Pesticides
| Compound Recovery Limits
| Gamma-BHC (Lihdane) 46-127
| Heptachlor 35-130
| Aldrin 34-132
| Dieldrin 31-134
| Endrin 42-139
| 4,4'-DDT 23-134
6.1.3 The advisory limits for the mean percent recoveries (%R) of all other
target compounds in the IPR study is 75% to 125% of the spiked
amount.
6.1.4 The advisory limits for the % Relative Standard Deviation (%RSD) of
the IPR recoveries for each compound is 25% and shall not exceed 50%.
6.2 Analytical Protocol Required
6.2.1 The Contractor shall extract all IPR samples using Stf-846 Methods
3541 (Revision 0, September 1994) and 3545 (Revision 0, December
1996) modified where appropriate to achieve the requirements of this
SOW (i.e., CRQLs and all technical acceptance, criteria). All
modifications to the extraction procedure (e.g., use of methylene
chloride/acetone (1:1, v/v) for pesticide extraction) shall be
adequately documented and submitted with the data package.
6.2.2 The Contractor shall follow the sample cleanup procedures described
in Exhibit D SVOA for semivolatiles and Exhibit D PEST for
pesticides/Aroclors.
6.2.3 The Contractor shall analyze the sample extracts for the IPR study
following the procedures described in Section 10.6, Exhibit D SVOA
for semivolatile compounds and Section 10.2,. Exhibit D PEST for
pesticides/Aroclors compounds.
6.3 Quantitation Limits/Quality Control Requirements
6.3.1 The Contractor shall achieve the CRQLs specified in Exhibit C under
semivolatiles and pesticides/Aroclors.
6.3.2 The Contractor shall follow all QC requirements outlined in Exhibit D
SVOA and Exhibit D PEST including frequency of method blanks,
instrument blanks, instrument performance checks, initial and
continuing calibrations or calibration verifications, internal
standards, and surrogates.
E-25 OLM04.2
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Exhibit E -- Section 6
Determination of Method Equivalency for Alternate Extraction Procedures
6.3.3 All technical acceptance criteria for sample analysis, method blank,
and instrument blank analyses'described in Exhibit D SVOA and Exhibit
D PEST shall be met.
6.3.4 .All semivolatile surrogate recoveries shall be within the limits
specified in Table 7, Exhibit D SVOA.
6.3.5 The advisory limits for the recovery of pesticide surrogates are 30%
to 150%.
6.4 Data Deliverable Requirements
6.4.1 The Contractor shall submit data packages containing all
documentation formatted as required in Exhibits B and H (including,
but not limited to, SDG Narrative, appropriate summary forms, and raw
data). Each IPR replicate shall be reported as a separate sample
(i.e., field sample) on Form I. All tuning data, initial calibration
data, continuing calibration data, and associated blanks with their
raw data must be included in the data package. The Contractor shall
include the source of the blank solid samples used for the IPR study
in the data deliverables.
6.4.2 The Contractor shall include in the SDG Narrative a discussion of any
modifications to the extraction procedures and any problems
encountered along with the resolutions. The Contractor shall provide
an explanation in the SDG Narrative for any of the target compound
recoveries that fall outside the advisory limits. A summary of the
IPR results with all calculations must also be included in the SDG
Narrative.
6.4.3 Simultaneous delivery of the complete Method Equivalency Data Package
shall be made to the following recipients:
EPA: Data Package will be delivered to the laboratory's
Administrative Project Officer (APO).
SMO: USEPA Contract Laboratory Program
Sample Management Office (SMO)1
2000 Edmund Hal ley Drive
Reston, VA 20191-3436
QATS: USEPA Contract Laboratory Program
Quality Assurance Technical Support (QATS) Laboratory2
2700 Chandler Avenue, Building C
Las Vegas, NV 89120
Attn: Data Audit Staff
1The Sample Management Office (SMO) is a contractor operated facility
operating under the CLASS contract awarded and administered by the EPA.
2The Quality Assurance Technical Support (QATS) Laboratory is a
contractor operated facility operating under the QATS contract awarded and
administered by the EPA.
E-26 OLM04.2
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Exhibit E -- Section 7
Contract Compliance Screening
| 7.0 CONTRACT COMPLIANCE SCREENING
| 7.1 Contract compliance screening (CCS) is one aspect "of the Government's
contractual right of inspection of analytical data. CCS examines the
Contractor's adherence to the contract requirements based on the sample
data package delivered to the Agency.
| 7.2 CCS is performed by the Sample Management Office (SMO) under the
direction of the Agency. To assure a uniform review, a set of
standardized procedures has been developed to evaluate the sample data
package submitted by a Contractor against the technical and completeness
requirements of the contract. The government reserves the right to add
and/or delete individual checks. CCS results are used in conjunction
with other information to measure overall Contractor performance and to
take appropriate actions to correct deficiencies in performance.
| 7.3 CCS results are mailed to the Contractor and all other data recipients.
The'Contractor has a period of time to correct deficiencies. The
Contractor shall send all corrections to the Regional client and SMO.
| 7.4 The Agency may generate a CCS trend report which summarizes CCS results
over a given period of time. The Agency may send the CCS trend report
or discuss the CCS trend report during an on-site laboratory evaluation.
In a detailed letter to the Technical Project Officer and Administrative
-Project Officer, the Contractor shall address the deficiencies, and the
^'subsequent corrective action implemented by the Contractor to correct
'-the deficiencies within 14 days of receipt of the report or the pn-site
''laboratory evaluation. An alternate delivery schedule may be proposed
by the Contractor, but it is the sole decision of the Agency,
represented by the Technical Project Officer or Administrative Project
Officer, to approve or disapprove the alternate delivery schedule. If
an alternate delivery schedule is proposed, the Contractor shall
describe in a letter to the Technical Project Officer, Administrative
Project Officer, and Contracting Officer why he/she is unable to meet
the delivery schedule listed in this section. The Technical Project
Officer/Administrative Project Officer will not grant an extension for
greater than 14 days for the Contractor's response to the CCS trend
report. The Contractor shall proceed and not assume that an extension
will be granted until so notified by the Technical Project Officer
and/or Administrative Project Officer.
| 7.5 If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective action
implemented by the Contractor, the Contractor shall write/amend and
submit the SOPs per the requirements listed in Section 4.
If the Contractor fails to adhere to the requirements listed in Section
7, the Contractor may expect, but the Agency is not limited to, the
following actions: reduction of number of samples sent under the
contract, suspension of sample shipment to the Contractor, a GC/MS
and/or GC/EC tape audit, a data package audit, an on-site laboratory
evaluation, a remedial laboratory evaluation sample, and/or contract
sanctions.
E-27 OLM04.2
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I Exhibit E -- Section 8
Regional Data Review
| 8.0 REGIONAL DATA REVIEW
| 8.1 Contractor data are generated to meet the specific needs of the EPA
Regions. In order to verify the usability of data for the intended
purpose, each Region reviews data from the perspective of the end user,
based upon functional aspects of data quality. General guidelines for
data review have been developed jointly by the Regions and the National
Program Office. Each Region uses these guidelines as the basis for data
evaluation. Individual Regions may augment the basic guideline review
process with additional review based on Region-specific or site-specific
concerns. Regional reviews, like the sites under investigation, vary
based on the nature of the problems under investigation and the Regional
response appropriate to the specific circumstances.
| 8.2 Regional data reviews, relating usability of the data to. a specific
site, are part of the collective assessment process. They complement
the review done at the Sample Management Office, which is designed to
identify contractual discrepancies, and the review done by the Program
Office, which is designed to evaluate Contractor and method performance.
These individual evaluations are integrated into a collective review
that is necessary for Program and Contractor administration and
management and may be used to take appropriate action to correct
deficiencies in the Contractor's performance.
E-28 OLM04.2
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Exhibit E -- Section 5
Proficiency Testing
9.0 PROFICIENCY TESTING
As a means of measuring and evaluating both the Contractor's and the
method's analytical performance, the Contractor must participate in
EPA's Proficiency Testing Program. EPA's Proficiency Testing Program
involves the analysis of case specific Performance Evaluation (PE)
samples and the participation in interlaboratory Quarterly Blind (QB)
Audits. The Contractor's analytical PE samples and QB results will be
used by EPA to assess and verify the Contractor's continuing ability to
produce acceptable analytical data in accordance with the contractual
requirements.
9.1 Performance Evaluation Samples
9.1.1 The Performance -Evaluation sample(s) maybe scheduled with the
Contractor as frequently as on an SDG-by-SDG basis. The PE samples
may be sent either by the Regional Client or the National Program
Office. PE samples will assist EPA in monitoring Contractor
performance.
9.1.2 PE samples will be provided as either single-blinds (recognizable as
a PE sample but of unknown composition), or as double-blinds (not
recognizable as a PE sample and of unknown composition) '. The
Contractor will not be informed of either the analytes or the
concentrations in the PE samples.
9.1.3 The Contractor may receive the PE samples as either full volume
samples or ampulated/bottled concentrates from EPA or a designated
EPA Contractor. The PE samples shall come with instructions
concerning the unique preparation procedures, if any, required to
reconstitute the PE samples (i.e., the required dilution of the PE
sample concentrate). .PE samples are to be extracted and/or analyzed
with the rest of the routine samples in the SDG. The Contractor
shall prepare and analyze the PE sample using the procedure described
in the sample preparation and method analysis sections of Exhibit D.
All contract required QC shall also be met. The PE sample results
are to be submitted in the SDG deliverable package per normal
reporting procedures detailed in Exhibit B.
9.1.4 In addition to PE sample preparation and analysis, the Contractor
shall be responsible for correctly identifying and quantitating the
analytes included in each PE sample. When PE sample results are
received by EPA, the PE sample results will be evaluated for correct
analytical identification'and quantitation. EPA will notify the
Contractor of unacceptable performance. EPA reserves the right to
adjust the PE sample acceptance windows in order to compensate for
any unanticipated difficulties with a particular PE sample.
9.1.5 The Contractor shall demonstrate acceptable analytical performance
for both identification and quantitation of PE sample analytes. For
unacceptable PE sample performance, EPA may take, but is not limited
to the following actions: reduce value or rejection of data for the
samples, SDG, or Case impacted; Show Cause and/or Cure Notice;
reduction in the number of samples shipped to the laboratory;
E-29 OLM04.2
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I Exhibit E -- Section 3
| Proficiency Testing
suspension of sample shipment; an on-site laboratory inspection; a
full data package audit; and/or require the laboratory to analyze a
Remedial QB.
9.2 Quarterly Blind Audits
9.2.1 Quarterly Blind (QB) Audits may be scheduled concurrently with all
contract laboratories up to a frequency of four times a year. A
Quarterly Blind Audit is a unique analytical case containing only
Performance Evaluation samples (i.e., referred to as Quarterly Blind
(QB) samples). The QB samples will be scheduled by the National
Program Office through the CLASS Contractor. QB samples will assist
EPA in monitoring Contractor performance.
9.2.2 QB samples will be provided as single-blinds (recognizable as a PE
sample but of unknown composition). The Contractor will not be
informed of either the analytes or the concentrations in the PE
samples.
9.2.3 The Contractor may receive the QB samples as either full volume
samples or ampulated/bottled concentrates from EPA or a designated
EPA Contractor. The QB samples shall come with instructions
concerning the unique preparation procedures, if any, required to
reconstitute the QB samples (i.e., the required dilution of the QB
sample concentrate). The Contractor shall prepare and analyze the QB
samples using the procedure described in the sample preparation and
method analysis sections of Exhibit D. All contract required QC
shall also be met. The QB sample results are to be submitted in the
SDG deliverable package per normal reporting procedures detailed in
Exhibit B.
9.2.4 In addition to QB sample preparation and analysis, the Contractor
shall be responsible for correctly identifying and quantitating the
analytes included in each QB sample. When QB sample results are
received by EPA, the QB sample results will be scored for correct
analytical identification and quantitation. The QB sample scoring
will be provided to the Contractor via coded evaluation sheets, by
analyte. EPA will notify the Contractor of unacceptable performance.
EPA reserves the right to adjust the PE sample acceptance windows in
order to compensate for any unanticipated difficulties with a
particular PE sample. The Contractor's QB sample performance will be
assessed into one of the following three categories:
9.2.4.1 Acceptable, No Response Required: Score greater than or equal to
90 percent. The data meets most or all of the scoring criteria.
No -response is required.
9.2.4.2 . Acceptable, Response Explaining Deficiencies Required: Score
greater than or equal to 75 percent, but less than 90 percent.
Deficiencies exist in the Contractor's performance. Corrective
action response required.
E-30 OLM04.2
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Exhibit E -- Section 9
Proficiency Testing
9.2.4.3 Unacceptable Performance, Response Explaining Deficiencies
Required: Score less than 75 percent. Deficiencies exist in the
Contractor's performance to the extent that the National Program
Office has determined that the Contractor has not demonstrated the
capability to meet the contract requirements. Corrective action
response required.
9.2.5 In the case of Section 9.2.4.2 or 9.2.4.3, the Contractor shall
describe the deficiency(ies) and the action (s) taken to correct the
deficiency(ies) in a corrective action letter to the Administrative
Project Officer, the Technical Project Officer, and the CLP Quality
Assurance Coordinator within 14 days of receipt of notification from
the Agency. .
9.2.5.1 An alternate delivery schedule for the corrective action letter
may be proposed by the Contractor, but it is the sole decision of
the Agency, represented either by the Technical Project Officer or
Administrative Project Officer, to approve or disapprove the
alternate delivery schedule. If an alternate delivery schedule is
proposed, the Contractor shall describe in a letter to the
Technical Project Officer, Administrative Project Officer, and
Contracting Officer why the laboratory is unable to meet the
original delivery schedule listed in Section 9.2.5. The Technical
Project Officer/Administrative Project Officer will not grant an
extension for greater than 14 days for the Contractor's corrective
action letter. The Contractor shall proceed and hot assume that
-~ an extension will be granted until so notified by the Technical
?" Project Officer or Administrative Project Officer.
9.2.6 In the case of Section 9.2.4.2 or 9.2.4.3, if new SOPs are required
to be written, or if existing SOPs are required to be rewritten or
amended because of deficiencies and subsequent corrective action
implemented by the Contractor, the Contractor shall write/amend the
SOPs per the requirements listed in Exhibit E, Section 4.
9.2.7 For unacceptable QB sample performance (Section 9.2.4.3), the EPA may
take, but is not limited to the following actions: reduction in the
number of samples shipped to the laboratory; suspension of sample
shipment; an on-site laboratory inspection; a full data package
audit; and/or require the laboratory to analyze a Remedial QB sample;
and/or contract sanctions.
9.2.8 A Remedial QB Audit is a unique analytical case containing only QB
samples. A Remedial QB Audit may be scheduled by the National
Program Office with the Contractor(s) for any of the following
reasons: unacceptable PE sample performance, unacceptable QB sample
performance, and/or major change in the laboratory (e.g., relocation,
new owner, or high turn-over of key personnel). Sections 9.2.2
through 9.2.7 apply to the Remedial QB Audit process.
E-31 OLM04.2
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I Exhibit E -- Section
| Proficiency Testing
9.2.9 If the Contractor fails to adhere to the requirements listed in
Section 9, the Contractor may expect, but the Agency is not limited
to, - the following actions: reduction in the number of samples sent
under the contract; suspension of sample shipment to the Contractor;
a full data package audit; an on-site laboratory inspection; a
Remedial QB sample; and/or contract sanctions.
E-32 OLM04.2
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I Exhibit E -- Section 10
j GC/MS and GC/EC Tape Audits
| 10.0 GC/MS AND GC/EC TAPE AUDITS
| 10.1 Overview. Periodically, the Agency requests the GC/MS and GC/EC
magnetic tapes from Contractors for a specific Case iri order to
accomplish tape audits. Generally, tape submissions and audits are
requested for the following reasons.
Program overview,
Indication of data quality problems,
Support for on-site audits, and
Specific Regional requests.
| 10.1.1 Depending upon the reason for an audit, the tapes from a recent Case,
a specific Case, or a laboratory evaluation sample may be requested.
Tape audits provide a mechanism to assess adherence to contractual
requirements and to ensure the consistency of data reported on the
| hardcopy/electronic deliverables with that generated on the GC/MS and
| GC/EC tapes. This function provides external monitoring of Program
QC requirements and checks adherence of the Contractor to internal QA
procedures. In addition, tape audits enable the Agency to evaluate
the utility, precision, and accuracy of the analytical methods.
| 10.1.2 The Contractor shall store all raw and processed GC/MS and GC/EC data
on magnetic tape, in appropriate instrument manufacturer's format,
| uncompressed, and with no security codes. This tape shall include
| data for samples, all QC samples, blanks, matrix spikes, matrix spike
duplicates, initial calibrations, continuing calibrations,
| calibration verification standards, including resolution check
| samples and performance evaluation mixtures, GPC single component and
| multicomponent and Florisil cartridge check samples and associated
| calibrations, and instrument performance check solutions (BFB and
DFTPP) as well as all Contractor-generated spectral libraries and
quantitation reports required to generate the data package. The
Contractor shall maintain a written reference logbook of tape files
of the EPA sample number, calibration data, standards, blanks, matrix
spikes, and matrix spike duplicates. The logbook shall include EPA
sample numbers and standard and blank IDs, identified by Case and
Sample Delivery Group.
| 10.1.3 The Contractor is required to retain the GC/MS and GC/EC tapes for
365 days after submission of the reconciled Complete SDG File. When
| submitting GC/MS and GC/EC tapes to the Agency, the following
materials shall be delivered in response to the request.
| 10.1.3.1 All associated raw data files for samples, all QC samples, blanks,
matrix spikes, matrix spike duplicates, initial calibrations,
| continuing calibrations, calibration verification-standards,
| including resolution check samples and performance evaluation
| mixtures, GPC single component and multicomponent Florisil
| cartridge check samples and associated calibrations, and
instrument performance check solutions (BFB and DFTPP).
E-33 OLM04.2
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I Exhibit E -- Section 10
I GC/MS and GC/EC Tape Audits
| 10.1.3.2 All processed data files and quantitation output files associated
| with the raw data files described in Section 10.1.3.1.
| 10.1.3.3 All associated identifications and calculation files (method
| files) used to generate the data submitted in the data package.
| 10.1.3.4 All Contractor-generated mass spectral library files (NIST/EPA/NIH
and/or Wiley, or equivalent, library not required).
| 10.1.3.5 A copy of the Contractor's written reference logbook relating tape
files to EPA sample number, calibration data, standards, blanks,
matrix spikes, and matrix spike duplicates. The logbook shall
include EPA sample numbers and lab file identifiers for all
samples, blanks, and standards, identified by Case and Sample
Delivery Group.
| 10.1.3.6 A directory of all files on each tape, including all
| subdirectories and the files contained therein.
I
| 10.1.3.7 A copy of the completed sample data package.
| 10.1.3.8 A statement attesting to the completeness of the GC/MS and GC/EC
data tape submission, signed and dated by the Contractor's
laboratory manager. The Contractor shall also provide a statement
attesting that the data reported have not been altered in any way.
These statements shall be part of a cover sheet that includes the
following information relevant to the data tape submission-
Contractor name,
Date of submission,
Case number,
SDG number,
| GC/MS and GC/EC make and model number,
<
Software version,
Disk drive type (e.g., CDC, PRIAM, etc.),
File transfer method (e.g., DSD, DTD, FTP, Aquarius, etc.),
and
| Data System Computer,
| System Operating Software,
| Data System Network,
| . Tape Backup Software,
| Tape Backup Hardware,
E-34 OLM04.2
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Exhibit E -- Section 10
GC/MS and GC/EC Tape Audits
| Data Analysis Software,
| Fraction, and
| Volume of data (in Mb) backed up on each tape
Names and telephone numbers of two Contractor contacts for
further information regarding the submission.
| 10.2 Submission of the GC/MS and GC/EC Tapes. Upon request of the
Administrative Project Officer, the Contractor shall send the required
| GC/MS and/or GC/EC tapes and all necessary documentation to the EPA
designated recipient (e.g., QATS) within seven. (7) days of notification.
An alternate delivery schedule may be proposed by the Contractor, but it
is the sole decision of the Agency, represented either by the Technical
Project Officer or Administrative Project Officer, to approve or
disapprove the alternate delivery schedule. If an alternate delivery
schedule is proposed, the Contractor shall describe in a letter to the
Technical Project Officer, Administrative Project Officer, and the
Contracting Officer why he/she is unable to meet the delivery schedule
listed in this section. The Technical Project Officer/Administrative
Project Officer will not grant an extension for greater than seven days
| for submission of the GC/MS and/or GC/EC tape. The Contractor shall
"proceed and not assume that an extension will be granted until so
.^notified by the Technical Project Officer and/or Administrative Project
a Officer.
| NOTE: The GC/MS and GC/EC tapes shall be shipped according to the
procedures in Exhibit F.
| 10.3 "Responding to the GC/MS and GC/EC Tape Audit Report. After completion
| of the GC/MS and GC/EC tape audit, the Agency may send a copy of the
I GC/MS and GC/EC tape audit report to the Contractor or may discuss the
| GC/MS and GC/EC tape audit report at an on-site laboratory evaluation.
In a detailed letter to the Technical Project Officer and Administrative
Project Officer, the Contractor shall discuss the corrective actions
| implemented to resolve the deficiencies listed in the GC/MS and GC/EC
tape audit report within 14 days of receipt of the report.
| 10.3.1 An alternate delivery schedule may be proposed by the Contractor, but
it is the sole decision of the Agency, represented either by the
Technical Project Officer or Administrative Project Officer, to
approve or disapprove the alternate delivery schedule. ""If an
alternate delivery schedule is proposed, the Contractor shall
describe in a letter to the Technical Project Officer, Administrative
Project Officer, and the Contracting Officer why he/she is unable to
meet the delivery schedule listed in this section. The Technical
Project Officer/Administrative Project Officer will not grant an
extension for greater than 14 days for the Contractor's response
| letter to the GC/MS and GC/EC tape report. The Contractor shall
proceed and not assume Jthat an extension will be granted until so
notified by the Technical Project Officer and/or Administrative
Project Officer.
E-35 OLM04.2
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I Exhibit E -- Section 10
| GC/MS and GC/EC Tape Audits
| 10.3.2 If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective
action implemented by the Contractor, the Contractor shall
write/amend and submit the SOPs per the requirements listed in
Section 4.
| 10.3.3 Maintenance of the Magnetic Tape Storage Device
| 10.3.3.1 The Contractor shall certify that the tape head alignment on the
magnetic tape storage device is in compliance with the ANSI
standards for nine track magnetic tapes. If the Contractor does
not have documentation of alignment within the last 12 months, the
Contractor must perform or have performed the manufacturer's
documented head alignment procedure within 60 days of contract
award. This is generally performed with a "skew" tape, certified
to be in conformance with ANSI standards. The alignment must be
performed by qualified personnel. The tape head alignment must be
performed at a minimum once every 12 months or when there is
evidence that the tape head may be out of alignment.
| 10.3.3.2 The tape system, including recording head, must be in conformance
with the manufacturer's physical and electrical standards.
Alignment of the remaining components of the tape system such as
the retracting arms, must be performed at intervals not to exceed
24 months. If the Contractor cannot demonstrate that the
remaining components of the tape system are in alignment, then the
Contractor must perform or have performed the manufacturer's
recommended alignment procedure.
| 10.3.4 Record of Maintenance'of the Magnetic Tape Storage Device
Documentation of maintenance, alignment, and repair procedures must
be kept in an instrument maintenance log book for each tape device
and data system. Also include any local area network components that
provide a means for the transmission of data to or from the
instrument data system and the tape system. Maintenance entries must
include serial number, property number (if applicable), data and time
of repair, name of person performing maintenance, problem
description, problem resolution, date and time of failure (if
applicable), and date and time placed back in service. Copies of
repairs shall be kept in the maintenance documentation.
Documentation of 1) data system, and 2) tape system maintenance and
alignments, for the last 24 months must be made available upon
| " written request of ""the Technical Project Officer or Administrative
| Project Officer or during a laboratory on-site evaluation. The
j Contractor shall always submit a GC/MS and GC/EC tape from a tape
system in conformance with the manufacturer's physical and electrical
standards and alignment according to manufacturer's procedures.
| 10.4 Corrective Actions. If the Contractor fails to adhere to the
| requirements listed in Section 10, the Contractor may expect, but the
Agency is not limited to, the following actions: reduction in the
number of samples sent under the contract, suspension of sample shipment
| to the Contractor, an on-site laboratory evaluation, a GC/MS and/or
E-36 OLM04.2
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Exhibit E -- Section 10
GC/MS and GC/EC Tape Audits
GC/EC tape audit, a data package audit, a remedial laboratory evaluation
sample, and/or contract sanctions.
E-37 OLM04.2
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Exhibit E -'- Section 11
Data Package Audits
I 11.0 DATA PACKAGE AUDITS
| 11.1 Overview. Data package audits are performed by the Agency for program
overview and specific Regional concerns and to assess the technical
quality of the data and evaluate overall Contractor performance. They
provide the Agency with an in-depth inspection and evaluation of the
Case data package with regard to achieving QA/QC acceptability. Data
packages are periodically selected from recently received Cases. They
are evaluated for the technical quality of hardcopy raw data, quality
assurance, and adherence to contractual requirements. A thorough review
of the raw data is completed, including: a check of instrument
printouts, quantitation reports, chromatograms, spectra, library
searches and other documentation for deviations from the contractual
requirements, a check for transcription and calculation errors, a review
of the qualifications of the Contractor personnel involved with the
| Case, and a review of the latest version of all SOPs on file.
Standardized procedures have been established to assure uniformity of
the auditing process.
| 11.2 Responding to the Data Package Audit Report. After completing the data
package audit, the Agency may send a copy of the data package audit
report to the Contractor or may discuss the data package audit report.at
an on-site laboratory evaluation. In a detailed letter to the Technical
Project Officer and the Administrative Project Officer, the Contractor
shall discuss the corrective actions implemented to resolve the
deficiencies listed in the data package audit report within 14 days of
receipt of the report.
| 11.2.1 An alternate delivery schedule may be proposed by the Contractor, but
it is the sole decision of the Agency, represented either by the
Technical Project Officer or Administrative Project Officer, to
approve or disapprove the alternate delivery schedule. If an
alternate delivery schedule is proposed, the Contractor shall
describe in a letter to the Technical Project Officer, Administrative
Project Officer, and the Contracting Officer, why he/she is unable to
meet the delivery schedule listed in this section. The Technical
Project Officer/Administrative Project Officer will not grant an
extension for greater than 14 days for the Contractor's response
letter to the data package report. The Contractor shall proceed and
not assume that an extension will be granted until so notified by the
Technical Project Officer and/or Administrative Project Officer.
| 11.2.2 If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective
action implemented by the Contractor, the Contractor shall
write/amend and submit the SOPs per the requirements listed in
Section 4.
| 11.3 Corrective Actions. If the Contractor fails to adhere to the
j requirements listed in Section 11, the Contractor may expect, but the
Agency is not limited to, the following actions: reduction in the
numbers of samples sent under the contract, suspension of sample
shipment to the Contractor, an on-site laboratory evaluation, a GC/MS
| and/or GC/EC tape audit, a data package audit, a remedial laboratory
evaluation sample, and/or contract sanctions.
E-38 OLM04.2
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I Exhibit E -- Section 12
On-Site Laboratory Evaluations
| 12.0 ON-SITE LABORATORY EVALUATIONS
| 12.1 Overview. At a frequency dictated by a Contractor's performance, the
Administrative Project Officer, Technical Project Officer, or the
Contracting Officer will conduct an on-site laboratory evaluation. On-
site laboratory evaluations are carried out to monitor the Contractor's
ability to meet selected terms and conditions specified in the contract.
The evaluation process incorporates two separate categories: a quality
assurance evaluation and an evidentiary audit.
| 12.2 Quality Assurance On-Site Evaluation. Quality assurance evaluators
inspect the Contractor's facilities to verify the adequacy and
maintenance of instrumentation, the continuity of personnel meeting
experience or education requirements, and the acceptable performance of
analytical and QC procedures.
| 12.2.1 The Contractor shall expect that items to be monitored will include,
but not be limited to, the following items:
Size and appearance of the facility,
Quantity, age, availability, scheduled maintenance, and
performance of instrumentation,
Availability, appropriateness, and utilization of the QAP and
SOPs,
Staff qualifications and experience, and personnel training
programs,
Reagents, standards, and sample storage facilities,
Standard preparation logbooks and raw data,
Bench sheets and analytical logbook maintenance and review, and
Review of the Contractor's sample analysis/data package
inspection/data management procedures.
| 12.2.2 Prior to an on-site evaluation, various documentation pertaining to
performance of the specific Contractor is integrated in a profile
package for discussion during the evaluation. Items that may be
included are previous on-site reports, laboratory evaluation sample
| scores, Regional review of data, Regional QA materials, GC/MS and
| GC/EC tape audit reports, data audit reports, results of CCS, and
data- trend reports.
| 12.3 Evidentiary Audit. Evidence auditors conduct an on-site laboratory
evaluation to determine if Contractor policies and procedures are in
place to satisfy evidence handling requirements as stated in Exhibit F.
The evidence audit comprises a procedural audit, an audit of written
SOPs, and an audit of analytical project file documentation.
E-39 OLM04.2.
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I Exhibit E -- Section 12
On-Site Laboratory Evaluations
| 12.3.1 Procedural Audit. The procedural audit consists of review and
examination of actual standard operating procedures and accompanying
documentation for. the following Contractor operations: sample
receiving, sample storage, sample identification, sample security,
sample tracking (from receipt to completion of analysis), and
analytical project file organization and assembly.
| 12.3.2 Written SOPs Audit. The written SOPs audit consists of review and
examination of the written SOPs to determine if they are accurate and
complete for the following Contractor operations: sample receiving,
sample storage, sample identification, sample security, sample
tracking (from receipt to completion of analysis), and analytical
project file organization and assembly.
| 12.3.3 Analytical Project File Evidence Audit. The analytical project file
evidence audit consists of review and examination of the analytical
project file documentation. The auditors review the files to
determine:
The accuracy of the document inventory,
The completeness of the file,
The adequacy and accuracy of the document numbering system,
Traceability of sample activity,
Identification of activity recorded on the documents, and
Error correction methods.
| 12.4 Discussion of the On-Site Team's Findings. During the debriefing, the
auditors present their findings and recommendations for corrective
actions necessary to the Contractor personnel.
| 12.5 Corrective Action Reports for Follow-Through to Quality Assurance .and
Evidentiary Audit Reports. Following an on-site laboratory evaluation,
quality assurance and/or evidentiary audit reports which discuss
deficiencies found during the on-site evaluation may be sent to the
Contractor. In a detailed letter, the Contractor shall discuss the
corrective actions implemented to resolve the deficiencies discussed
during the on-site evaluation and discussed in the report(s) to the
Technical Project Officer and the Administrative Project Officer within
14 days of receipt of the report.
| 12.5.1 An alternate delivery schedule may be proposed by the Contractor, but
it is the sole decision of the Agency, represented either by the
Technical Project Officer or Administrative Project Officer, to
approve or disapprove the alternate delivery schedule. If an
alternate delivery schedule is proposed, the Contractor shall
describe in a letter to the Technical Project Officer, Administrative
Project Officer, and the Contracting Officer why he/she is unable to
meet the delivery schedule listed in this section. The Technical
Project Officer/Administrative Project .Officer will not grant an
E-40 OLM04.2
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I Exhibit E -- Section 12
On-Site Laboratory Evaluations
extension for greater than 14 days for the Contractor's response
letter to the quality assurance and evidentiary audit report. The
Contractor shall proceed and not assume that an extension will be
granted until so notified by the Technical Project Officer and/or
Administrative Project Officer.
| 12.5.2 If new SOPs are required to be written or SOPs are required to be
amended because of the deficiencies and the subsequent corrective
.action implemented by the Contractor, the Contractor shall
write/amend and submit the SOPs per the requirements listed in
Section 4.
| 12.6 Corrective Actions. If the Contractor fails to adhere to the
| requirements listed in Section 12, the Contractor may expect, but the
Agency is not limited to, the following actions: reduction in the
number of samples sent under the contract, suspension of sample shipment
| to the Contractor, an on-site laboratory evaluation, a GC/MS and/or
| GC/EC tape audit, a data package audit, a remedial laboratory evaluation
sample, and/or contract sanctions.
E-41 OLM04.2
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Exhibit E -- Section 13
Quality Assurance and Data Trend Analysis
| 13.0 QUALITY ASSURANCE AND DATA TREND ANALYSIS
| 13.1 Data submitted by Contractors are subject to review from several
aspects: compliance with contract-required QC, usability, and full data
package evaluation. Problems resulting from any of these reviews may
| determine the need for a GC/MS and GC/EC tape audit, an on-site
laboratory evaluation and/or a remedial laboratory evaluation sample.
In addition, QC prescribed in the methods provides information that is
continually used by the Agency to assess sample data quality, Contractor
data quality and Program data quality via data trend analysis. Trend
analysis is accomplished by entering data into a computerized database.
Statistical reports that evaluate specific anomalies or disclose trends
in many areas, including the following, are generated from this
database:
Surrogate spike recovery, .
Laboratory evaluation sample results,
Blanks,
GC/MS instrument performance checks (BFB and DFTPP),
Initial and continuing calibration data, and
Other QC and method parameters.
| 13.2 Program-wide statistical results are used to rank Contractors in order
to observe the relative performance of each Contractor using a given
protocol against its peers. The reports are also used to identify
trends within Contractors. The results of many of these trend analyses
are included in the overall evaluation of a Contractor's performance,
and are reviewed to determine if corrective action or an on-site
laboratory evaluation may be required to ensure that the Contractor can
meet the QA/QC requirements of the contract. Contractor performance
over time is monitored using these trend analysis techniques to detect
departures of Contractor output from required or desired levels of
quality control, and to provide an early warning of Contractor QA/QC
problems which may not be apparent from the results of an individual
Case.
| 13.3 As a further benefit to the Program, the database provides the
information needed to establish performance-based criteria in updated
analytical protocols, where advisory criteria have been previously used.
The vast empirical data set produced by Contractors is carefully
analyzed, with the results augmenting theoretical and research-based
performance criteria. The result is a continuously monitored set of
quality control and performance criteria specifications of what is
routinely achievable and expected of environmental chemistry Contractors
engaged in mass production analysis of environmental samples. This, in
turn, assists the Agency in meeting its objectives of obtaining data of
known and documented quality.
E.-42 OLM04.2
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I Exhibit E -- Section 14
Data Management
| 14.0 DATA MANAGEMENT
| 14.1 Data management procedures are defined as procedures specifying the
acquisition or entry, update, correction, deletion, storage, and
security of computer-readable data and files. These procedures shall be
in written form and contain a clear definition for all databases and
files used to generate or resubmit deliverables. Key areas of concern
include system organization (including personnel and security),
documentation operations, traceability, and quality control.
| 14.2 Data manually entered from hardcopy shall be subject to quality control
and the error rates estimated. Systems shall prevent entry of incorrect
or out-of-range data and alert data entry personnel of errors. In
addition, data entry error rates shall be estimated and recorded on a
monthly basis by reentering a statistical sample of the data entered and
calculating discrepancy rates by data element.
| 14.3 The record of changes in the form of corrections and updates to data
originally generated, submitted, and/or resubmitted shall be documented
to allow traceability of updates. Documentation shall include the
following for each change.
Justification or rationale for the change.
Initials of the person making the change(s). Data changes shall be
implemented and reviewed by a person or group independent of the
source generating the deliverable.
Documentation of changes shall be retained according to the schedule
of the original deliverable.
Resubmitted diskettes or other deliverables shall be reinspected as
a part of the Contractor's internal inspection process prior to
resubmission. The entire deliverable, not just the changes, shall
be inspected.
The Contractor's laboratory manager shall approve changes to
originally submitted deliverables.
Documentation of data changes may be requested by Contractor
auditors.
| 14.4 Life cycle management procedures shall be applied to computer software
systems developed by the Contractor to be used to generate and edit
contract deliverables. Such systems shall be thoroughly tested and
documented prior to utilization.
| 14.4.1 A software test and acceptance plan including test requirements, test
results, and acceptance criteria shall be developed, followed, and
available in written form.
E-43 OLM04.2
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Exhibit E -- Section 14
Data Management
14.4.2 System changes shall not be made directly to production systems
generating deliverables. Changes shall be made first to a
development system and tested prior to implementation.
14.4.3 Each version of the.production system will be given an identification
number, date of installation, date of last operation, and archived.
14.4.4 System and operations documentation shall be developed and maintained
for each system. Documentation shall include a user's manual and an
operations and maintenance manual.
14.4.5 This documentation shall be available for on-site review and/or upon
written request by the Technical Project Officer or Administrative
Project Officer.
14.5 Individual(s) responsible for the following functions shall be
identified.
System operation and maintenance, including documentation and
training,
Database integrity, including data entry, data updating and quality
control, and
Data and system security, backup, and archiving.
E-44 OLM04.2
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EXHIBIT F
CHAIN-OF-CUSTODY, DOCUMENT CONTROL,
AND WRITTEN STANDARD OPERATING PROCEDURES
F-l OLM04.2
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Exhibit F - Chain-of-Custody, Document Control, and
Written Standard Operating Procedures
Table of Contents
Section Page
1.0 INTRODUCTION 3
2.0 STANDARD OPERATING PROCEDURES 4
2.1 Sample Receiving 4
2.2 Sample Identification 5
2.3 Sample Security 5
2.4 Sample Storage 6
2.5 Sample Tracking and Document Control . 6
2.6 Computer-Resident Sample Data Control . . . 7
2.7 Complete Sample Delivery Group File (CSF) Organization and
Assembly 7
3.0 WRITTEN STANDARD OPERATING PROCEDURES (SOPS) 10
3.1 Sample Receiving 10
3.2 Sample Identification 11
3.3 Sample Security 12
3.4 Sample Storage 12
3.5 Sample Tracking and Document Control 12
3.6 Computer-Resident Sample Data Control 13
3.7 CSF Organization and Assembly 14
F-2 OLM04.2
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Exhibit F -- Section 1
Introduction
1.0 INTRODUCTION
1.1 A sample is physical evidence collected from a facility or from the
environment. Controlling evidence is an essential part of the hazardous
waste investigation effort. "To ensure that the Environmental Protection
Agency's (EPA) sample data and records supporting sample-related
activities are admissible and have weight as evidence in future
litigation, Contractors are required to maintain EPA samples under
chain-of-custody and to account for all samples and supporting records
of sample handling, preparation, and analysis. Contractors shall
maintain sample identity, sample custody, and all sample-related records
according to the requirements in this exhibit.
1.2
The purposes of the evidence requirements include:
Ensuring traceability of samples while in the possession of the
Contractor.
Ensuring custody of samples while in the possession of the
Contractor.
Ensuring the integrity of sample identity while in the possession of
the Contractor.
Ensuring sample-related activities are recorded on documents or in
other formats for EPA sample receipt, storage, preparation,
analysis, and disposal.
Ensuring all laboratory records for each specified Sample Delivery
Group will be accounted for when the project is completed.
Ensuring that all laboratory records directly related to EPA samples
are assembled and delivered to EPA or, prior to delivery, are
available upon EPA's request.
F-3 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
2.0 STANDARD OPERATING PROCEDURES
The Contractor shall implement the following standard operating
procedures for sample receiving, sample identification, sample security,
sample storage, sample tracking and document control, computer-resident
sample data control, and complete sample delivery group file
organization and assembly to ensure accountability of EPA sample
chain-of-custody as well as control of all EPA sample-related records.
2.1 Sample Receiving
2.1..1 The Contractor shall designate a sample custodian responsible for
receiving EPA samples.
2.1.2 The Contractor shall designate a representative to receive EPA
samples in the event that the sample custodian is not available.
2.1.3 Upon receipt, the condition of shipping containers and sample
containers shall be inspected and recorded on Form DC-1 by the sample
custodian or his/her representative.
2.1.4 Upon receipt, the condition of the custody seals (intact/broken)
shall be inspected and recorded on Form DC-1 by the sample custodian
or his/her representative.
2.1.5 The sample custodian or his/her representative shall verify and
record on Form DC-1 the presence or absence of the following
documents accompanying the sample shipment:
Custody seals,
Chain-of-custody records,
Traffic reports or packing lists,
Airbills or airbill stickers, and
Sample tags.
2.1.6 The sample custodian or his/her representative shall verify and
record on Form DC-1 the agreement or disagreement of information
recorded on all documents received with samples and information
recorded on sample containers.
2.1.7 The sample custodian or his/her representative shall record the
following information on Form DC-1 as samples are received and
inspected:
Custody seal numbers when present,
Airbill or airbill sticker numbers,
Sample tags listed/not listed on chain-of-custody records,
Cooler temperature,
F-4 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
Date of receipt,
Time of receipt,
EPA sample numbers,
Sample tag numbers,
Assigned laboratory numbers,
Samples delivered by hand, and
Problems and discrepancies.
2.1.8 The sample custodian or his/her representative shall sign, date, and
record the time on all accompanying forms, when applicable, at the
time of sample receipt (for example, chain-of-custody records,
traffic reports or packing lists, and airbills). Note: Initials are
not acceptable.
2.1.9 The Contractor shall contact the Sample Management Office (SMO) to
resolve problems and discrepancies including, but not limited to,
absent documents, conflicting information, absent or broken custody
seals, absent temperature indicator bottle, and unsatisfactory sample
condition.(for example, leaking sample container).
2.1.10 The Contractor shall record resolution of problems and discrepancies
by SMO.
2.2 Sample Identification
2.2.1 The Contractor shall maintain the identity of EPA samples and
prepared samples (including extracted samples, digested samples, and
distilled samples) throughout the laboratory.
2.2.2 Each sample and sample preparation container shall be labeled with
the SMO number or a unique laboratory sample identification number.
2.3 Sample Security
2.3.1 The Contractor shall demonstrate that EPA sample custody is
maintained from receiving through retention or disposal. A sample is
in custody if:
It is in your possession; or
It is in your view after being in your possession; or
It is locked in a secure area after being in your possession; or
It is in a designated secure area. (Secure areas shall be
accessible only to authorized personnel.)
2.3.2 The Contractor shall demonstrate security of designated secure areas.
-P-5 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
2.4 Sample Storage
The Contractor shall designate storage areas for EPA samples and
prepared samples.
2.5 Sample Tracking and Document Control
2.5.1 The Contractor shall record all activities performed on EPA samples.
2.5.2 Titles which identify the activities recorded shall be printed on
each page of all laboratory documents. (Activities include, but are
not limited to, sample receipt, sample storage, sample preparation,
and sample analysis.) When a document is a record of analysis, the
instrument type and parameter group (for example, GC/MS-VOA) shall be
included in the title.
2.5.3 When columns are used to organize information recorded on laboratory
documents, the information recorded in the columns shall be
identified in a column heading.
2.5.4 Reviewers' signatures shall be identified on laboratory documents
when reviews are conducted. Note: Individuals recording review
comments on computer-generated raw data are not required to be
identified unless the written comments address data validity.
2.5.5 The laboratory name shall be identified on preprinted laboratory
documents.
2.5.6 Each laboratory document entry shall be dated with the month/day/year
(for example, 01/01/90) and signed (or initialed) by the
individual(s) responsible for performing the recorded activity at the
time the activity is recorded.
2.S.I Notations on laboratory documents shall be recorded in ink.
2.5.8 Corrections to laboratory documents and raw data shall be made by
drawing single lines through the errors and entering the correct
information. Information shall not be obliterated or rendered
unreadable. Corrections and additions to information shall be signed
(or initialed) and dated.
2.5.9 Unused portions of laboratory documents shall be lined-out.
2.5.10 Pages in bound and unbound logbooks shall be sequentially numbered.
2.5.11 Instrument-specific run logs shall be maintained to enable the
reconstruction of run sequences.
2.5.12 Logbook entries shall be in chronological order.
2.5.13 Logbook entries shall include only one Sample Delivery Group (SDG)
per page, except in the events where the SDGs "share" QC samples (for
example, instrument run logs and extraction logs).
2.5.14 Information inserted into laboratory documents shall be affixed
permanently in place. The individual responsible for inserting
F-6 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
information shall sign and date across the insert and logbook page at
the time information is inserted.
2.5.15 The Contractor shall document disposal or retention of EPA samples,
remaining-portions of samples, and prepared samples.
2.6 Computer-Resident Sample Data Control
2.6.1 Contractor personnel responsible for original data entry shall be
identified at the time of data input.
2.6.2 The Contractor shall make changes to electronic data in a manner
which ensures that the original data entry is preserved, the editor
is identified, and the revision date is recorded.
2.6.3 The Contractor shall routinely verify the accuracy of manually
entered data, electronically entered data, and data acquired from
instruments.
2.6.4 The Contractor shall routinely verify documents produced by the
electronic data collection system to ensure accuracy of the
information reported.
2.6.5 The Contractor shall ensure that the electronic data collection
system is secure.
2.6.5.1 The electronic data collection system shall be maintained in a
secure location.
2.6.5.2 Access to the electronic data collection system functions shall be
limited to authorized personnel through utilization of software
security techniques (for example, log-ons or restricted
passwords).
2.6.5.3 Electronic data collection systems shall be protected from the
introduction of external programs or software (for example,
viruses).
2.6.6 The Contractor shall designate archive storage areas for electronic
data and the software required to access the data.
2.6.7 The Contractor shall designate an individual responsible for
maintaining archives of electronic data, including the software.
2.6.8 The Contractor shall maintain the archives of electronic data and
necessary software in a secure location. (Secure areas shall be
accessible only to authorized personnel.)
2.7 Complete Sample Delivery Group File (CSF) Organization and Assembly
2.7.1 The Contractor shall designate a document control officer responsible
for the organization and assembly of the CSF.
2.7.2 The Contractor shall designate a representative responsible for the
organization and assembly of the CSF in the event that the document
control officer is not available.
F-7 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
2.7.3 The Contractor shall maintain documents relating to the CSF in a
secure location.
2.7.4 All original laboratory forms and copies of SDG-related logbook pages
shall be included in the CSF.
2.7.5 Copies of laboratory documents in the CSF shall be photocopied in a
manner to provide complete and legible replicates.
2.7.6 Documents 'relevant to each SDG including, but not limited to, the
following shall be included in the CSF:
logbook pages, records of failed or attempted analysis,
benchsheets, custody records,
mass spectra, sample tracking records,
chromatograms, . raw data summaries,
screening records, computer printouts,
preparation records, correspondence,
re-preparation records, FAX originals,
analytical records, library search results, and
re-analysis records, other.
2.7.7 The document control officer or his/her representative shall ensure
that sample tags are encased in clear plastic bags before placing
them in the CSF.
2.7.8 . CSF documents shall be organized and assembled on an SDG-specific
basis.
2.7.9 Original documents which include information relating to more than
one SDG (for example, chain-of-custody records, traffic reports,
calibration logs) shall be filed in the CSF of the lowest SDG number,
and copies of these originals shall be placed in the other CSF(s).
The document control officer or his/her representative shall record
the following statement on the copies in dark ink:
COPY
ORIGINAL DOCUMENTS ARE INCLUDED IN CSF
Signature
Date
2.7.10 All CSFs shall be submitted with a completed Form DC-2. All
resubmitted CSFs shall be submitted with a new or revised Form DC-2.
2.7.11 Each item in the CSF and resubmitted CSFs shall be inventoried and
assembled in the order specified on Form DC-2. Each page of the CSF
shall be stamped with a sequential number. Page number ranges shall
F-8 OLM04.2
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Exhibit F -- Section 2
Standard Operating Procedures
be recorded in the columns provided on Form DC-2. Intentional gaps
in the page numbering sequence shall be recorded in the "Comments"
section on Form DC-2. When inserting new or inadvertently omitted
documents, the Contractor shall identify them with unique accountable
numbers. The unique accountable- numbers and' the locations of the
documents shall be recorded in the "Other Records" section' on Form
DC-2.
2.7.12 Before shipping each CSF, the document control officer or his/her
representative shall verify the agreement of information recorded on
all documentation and ensure that the information is consistent and
the CSF is complete.-
2.7.13 The document control officer or his/her representative shall document
the shipment of deliverable packages including what was sent, to
whom, the date, and the carrier used.
2.7.14 Shipments of deliverable packages, including resubmittals, shall be
sealed with custody seals by the document control officer or his/her
representative in a manner such that opening the packages would break
the seals.
2.7.15 Custody seals shall be signed and dated by the document control
officer or his/her representative when sealing deliverable packages.
F-9 OLM04.2
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Exhibit F -- Section 3
Written Standard Operating Procedures
3.0 WRITTEN STANDARD OPERATING PROCEDURES (SOPS)
The Contractor shall develop and implement the following written SOPs
for sample receiving, sample identification, sample security, sample
storage, sample tracking and document control, computer-resident sample
data control, and CSF file organization and assembly to ensure
accountability for EPA sample chain-of-custody and control of all EPA
sample-related records.
3.1 Sample Receiving
3.1.1 The Contractor shall have written SOPs for sample receiving which
accurately reflect the procedures used by the laboratory.
3.1.2 The written SOPs for sample receiving shall ensure that the
procedures listed below are in use at the laboratory.
3.1.2.1 The condition of shipping containers and sample containers are
inspected and recorded on Form DC-1 upon receipt by the sample
custodian or his/her representative.
3.1.2.2 The condition of custody seals are inspected and recorded on Form
DC-1 upon receipt by the sample custodian or his/her
representative.
3.1.2.3 The presence or absence of the following documents accompanying
the sample shipment is verified and recorded on Form DC-1 by the
sample custodian or his/her representative:
Custody seals,
Chain-of-custody records,
Traffic reports or packing lists,
Airbills or airbill stickers, and
Sample tags.
3.1.2.4 The agreement or disagreement of information recorded on shipping
documents with information recorded on sample containers is
verified and recorded on Form DC-1 by the sample custodian or
his/her representative.
3.1.2.5 The following information is recorded on Form DC-1 by the sample
custodian or his/her representative as samples are received and
inspected:
Custody seal numbers when present,
Airbill or airbill sticker numbers,
Sample tag numbers listed/not listed on chain-of-custody
records,
Cooler temperature,
F-10 OLM04.2
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Exhibit F -- Section 3
Written Standard Operating Procedures
Date of receipt,
Time of receipt,
EPA sample numbers,
Sample tag numbers,
Assigned laboratory numbers,
Samples delivered by hand, and
Problems and discrepancies.
3.1.2.6 All accompanying forms are signed, dated, and the time is
recorded, when applicable, at the time of sample receipt (for
example, chain-of-custody records, traffic reports or packing
lists, and airbills) by the sample custodian or his/her
representative.
3.1.2.7 SMO is contacted to resolve problems and discrepancies including,
but not limited- to, absent documents, conflicting information,
| absent or broken custody seals, absent temperature indicator
| bottle, and unsatisfactory sample .condition (for example, leaking
sample container).
3.1.2.8 The resolution of problems and discrepancies by SMO is recorded.
3.2 Sample Identification
3.2.1 The Contractor shall have written SOPs for sample identification
which accurately reflect the procedures used by the laboratory.
3.2.2 The written SOPs for sample identification shall ensure that the
procedures listed below are in use at the laboratory.
3.2.2.1 The identity of EPA samples and prepared samples is maintained
throughout the laboratory:
When the Contractor assigns unique laboratory sample
identification numbers, the written SOPs shall include a
description of the procedure used to assign these numbers,
t
" When the Contractor uses prefixes or suffixes in addition to
laboratory sample identification numbers, the written SOPs
shall include their definitions, and
When the Contractor uses methods to uniquely identify
fractions/parameter groups and matrix type, the written SOPs
shall include a description of these methods.
3.2.2.2 Each sample and sample preparation container is' labeled with the
SMO number or a unique laboratory sample identification number.
F-ll OLM04.2
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Exhibit F -- Section 3
Written Standard Operating Procedures
3.3 Sample Security
3.3.1 The Contractor shall have written SOPs for sample security which
accurately reflect the procedures used by the laboratory.
3.3.2 The written.SOPs for sample security shall include the items listed
below.
3.3.2.1 Procedures which ensure the following:
Sample custody is maintained, and
The security of designated secure areas is maintained.
3.3.2.2 A list of authorized personnel who have access to locked storage
areas.
3.4 Sample Storage . /
3.4.1 The Contractor shall have written SOPs for sample storage which
accurately reflect the procedures used by the laboratory.
3.4.2 The written SOPs for sample storage shall describe locations,
contents, and identities of all storage areas for EPA samples and
prepared samples in the laboratory.
3.5 Sample Tracking and Document Control
3.5.1 The Contractor shall have written SOPs for sample tracking and
document control which accurately reflect the procedures used by the
laboratory.
3.5.2 The written SOPs for sample tracking and document control shall
include the items listed below.
3.5.2.1 Examples of all laboratory documents used during sample receiving,
sample storage, sample transfer, sample analyses, CSF organization
and assembly, and sample retention or disposal.
3.5.2.2 Procedures which ensure the following:
All activities performed on EPA samples are recorded;
Titles which identify the activities recorded are printed on
, each page of all laboratory documents;
Information recorded in columns is identified with column
headings,- .
Reviewers' signatures are identified on laboratory documents;
The laboratory name is included on preprinted laboratory
documents;
Laboratory document entries are signed and dated with the
F-12 OLM04.2
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Exhibit F -- Section 3
Written Standard Operating Procedures
month/day/year (for example, 01/01/90);
Entries on all laboratory documents are recorded in ink;
Corrections and additions to- laboratory documents are made by
drawing single lines through the errors, entering the correct
information, and initialing and dating the new information;
Unused portions of laboratory documents are lined-out;
Pages in bound and unbound logbooks are sequentially numbered;
Instrument-specific run logs are maintained to enable the
reconstruction of run sequences;
Logbook entries are recorded in chronological order;
Entries are recorded for only one SDG on a page, except in the
events where SDGs "share" quality control (QC) samples (for
example, instrument run logs and extraction logs);
Information inserted in laboratory documents is affixed
permanently, signed, and dated across the insert; and
The retention or disposal of EPA samples, remaining portions
of samples, and prepared samples is documented.
3.6 Computer-Resident Sample Data Control
3.6.1 The Contractor shall have written SOPs for computer-resident sample
data control which accurately reflect the procedures used by the
laboratory.
3.6.2 The written SOPs for computer-resident sample data control shall
include the items listed below.
3.6.2.1 Procedures which ensure the following:
Contractor personnel responsible for original data entry are
identified;
Changes to electronic data are made such that the original
data entry is preserved, the editor is identified, and the
revision date is recorded;
The accuracy of manually entered data, electronically entered
data, and data acquired from instruments is verified;
Report documents produced by the electronic data collection
system are routinely verified to ensure the accuracy of the
information reported;
. 'Electronic data collection system security is maintained; and
Archives of electronic data and accompanying software are
maintained in a secure location.
F-13 OLM04.2
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Exhibit F -- Section 3
Written Standard Operating Procedures
3.6.2.2 Descriptions of archive storage areas for the electronic data and
the software required to access data archives.
3.6.2.3 A list of authorized personnel who have access to electronic data
collection system functions and to archived data.
3.7 CSF Organization and Assembly
3.7.1 The Contractor shall have written SOPs for CSF organization and
assembly which accurately reflect the procedures used by the
laboratory.
3.7.2 The written SOPs for CSF organization and assembly shall ensure that
the procedures listed below are in use at the laboratory.
Documents relating to the CSF are maintained in a secure
location.
All original laboratory forms and copies of SDG-related logbook
pages are included in the CSF.
Laboratory documents are photocopied in a manner to provide
complete and legible replicates.
All documents relevant to each SDG are included in the CSF.
Sample tags are encased in clear plastic bags by the document
control officer or his/her representative before placing them in
the CSF.
The CSF is organized and assembled on an SDG-specific basis.
Copies are referenced to originals in the event that an original
document contains information relating to more than one SDG.
Each CSF is submitted with a completed Form DC-2, and resubmitted
CSFs are submitted with a new or revised Form DC-2.
Each page of the CSF is stamped with a sequential number and the
page number ranges are recorded in the columns provided on Form
DC-2.
Consistency and completeness of the CSF is verified by the
document control officer or his/her representative.
Shipments of deliverable packages are documented by the document
control officer or his/her representative.
Deliverable packages are shipped by the document control officer
or his/her representative using custody seals in a manner such
that opening the packages would break the seals.
Custody seals are signed and dated by the document control
officer or his/her representative before placing them on
deliverable packages.
F-14 OLM04.2
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EXHIBIT G
GLOSSARY OF TERMS
G-l OLM04.2
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Exhibit G -- Glossary of Terras
ALIQUOT - a measured portion of a sample, or solution, taken for sample
preparation and/or analysis.
ANALYSIS DATE/TIME - the date and military time of the injection of the
sample, standard, or blank into the GC/MS or GC system.
BAR GRAPH SPECTRUM - a plot of the mass-to-charge ratio (m/e) versus relative
intensity of the ion current.
BLANK - an analytical sample designed to assess specific sources of laboratory
contamination. See individual types of Blanks: Method Blank; Instrument
Blank, Storage Blank, and Sulfur Blank.
BREAKDOWN - a measure of the decomposition of certain analytes (DDT and
Endrin) into by-products.
4-BROMOFLUOROBENZENE (BFB) - the compound chosen to establish mass spectral
instrument performance for volatile (VOA) analyses. It is also used in the
VOA fraction as a system monitoring compound (SMC).
CALIBRATION FACTOR (CF) - a measure of the gas chromatographic response of a
target analyte to the mass injected. The calibration factor is analogous to
the Relative Response Factor (RRF) used in the Volatile and Semivolatile
fractions.
CASE - a finite, usually predetermined number of samples collected over a
given time period from a particular site. Case numbers are assigned by the
Sample Management Office. A Case consists of one or more Sample Delivery
Groups.
CHARACTERIZATION - a determination of the approximate concentration range of
compounds of interest used to choose the appropriate analytical protocol.
CONCENTRATION LEVEL (low or medium) - characterization of soil samples or
sample fractions as low concentration or medium concentration is made on the
basis of the laboratory's preliminary screen, not on the basis of information
entered on the Traffic Report by the sampler.
CONTAMINATION - a component of a sample or an extract that is not
representative of the environmental source of the sample. Contamination may
stem from other samples, sampling equipment, while in transit, from laboratory
reagents, laboratory environment, or analytical instruments.
CONTINUING CALIBRATION - analytical standard run every 12 hours to verify the
initial calibration of the system.
CONTINUOUS LIQUID-LIQUID EXTRACTION - used herein synonymously with the terms
continuous extraction, continuous liquid extraction, and liquid extraction.
This extraction technique involves boiling the extraction solvent in a flask
and condensing the solvent above the aqueous sample. The condensed solvent
drips through the sample, extracting the compounds of interest from the
aqueous phase.
G-2 OLM04.2
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Exhibit G -- Glossary of Terms
(CLASS) CONTRACT LABORATORY ANALYTICAL SERVICES SUPPORT - contract that
operates the Sample Management Office (SMO) and is awarded and administered by
the EPA.
DATE -
Hardcopy Reporting - MM/DD/YY - where MM = 01 for January, 02 for
February, ... 12 for December; DD = 01 to 31; YY = 96, 97, 98, 99, etc.
Electronic Reporting - MM/DD/YYYY - where MM = 01 for January, 02 for
February, ... 12 for December; DD = 01 to 31; YYYY = 1996, 1997, 1998,
1999, etc.
DAY - unless otherwise specified, day shall mean calendar day.
>
DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP) - compound chosen to establish mass
spectral instrument performance for semivolatile analysis.
EXTRACTABLE - a compound that can be partitioned into an organic solvent from
the sample matrix and is amenable to gas chromatography. Extractables include
semivolatile (BNA) and pesticide/Aroclor compounds.
EXTRACTED ION CURRENT PROFILE (EICP) - a plot of ion abundance versus time (or
scan number) for ion(s) of specified mass(es).
FIELD SAMPLE - a portion of material to be analyzed that is contained in
single or multiple containers and identified by a unique sample number.
GAS CHROMATOGRAPH (GC) - the instrument used to separate analytes on a
stationary phase within a chromatographic column. The analytes are volatized
directly from the sample (VOA water and low-soil), volatized from the sample
extract (VOA medium soil), or injected as extracts (SVOA and PEST). In VOA
and SVOA analysis, the compounds are detected by a Mass Spectrometer (MS). In
PEST analysis, the compounds are detected by an Electron Capture (EC)
detector. ' In the screening procedure (all fractions), the Flame lonization
Detector (FID) is used as the detector.
GEL PERMEATION CHROMATOGRAPHY (GPC) - a size-exclusion chromatographic
technique that is used as a cleanup procedure for removing large organic
molecules, particularly naturally occurring macro-molecules such as lipids,
polymers, viruses, etc.
IN-HOUSE - at the Contractor's facility.
INITIAL CALIBRATION - analysis of analytical standards for a series of
different specified concentrations; used to define the linearity and dynamic
range of the response of the mass spectrometer or electron capture detector to
the target compounds.
INTEGRATION SCAN RANGE - the scan number of the scan at the beginning of the
area of integration to the scan number at the end of the area of integration.
Performed in accordance with Exhibit D VOA, Sections 11.2.1:9 and 11.2.1.10
and Exhibit D SVOA, Sections 11.2.1.2 and 11.2.1.3.
G-3 OLM04.2
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Exhibit G -- Glossary of Terms
INTEGRATION TIME RANGE - the retention time at the beginning of the area of
integration to the retention time at the end of the area of integration.
INTERNAL STANDARDS - compounds added to every standard, blank, matrix spike,
matrix spike duplicate, sample (for volatiles), and sample extract (for
semivolatiles) at a known concentration, prior to analysis. Internal
standards are used as the basis for quantitation of the target compounds.
INSTRUMENT BLANK - a blank designed to determine the level of contamination
associated with the analytical instruments.
INSUFFICIENT QUANTITY - when there is not enough volume (water sample) or
weight (soil/sediment) to perform any of the required operations: sample
analysis or extraction, percent moisture, MS/MSD, etc. Exhibit D provides
guidance for addressing this situation.
LABORATORY - synonymous with Contractor as used herein.
m/z - Mass to charge ratio, synonymous with "m/e".
MATRIX - the predominant material of which the sample to be analyzed is
composed. For the purpose of this SOW, a sample matrix is either water or
soil/sediment. Matrix is not synonymous with phase (liquid or solid).
MATRIX EFFECT - in general, the effect of a particular matrix (water or
soil/sediment) on the constituents with which it contacts. This is
particularly pronounced for clay particles which may adsorb chemicals and
catalyze reactions. Matrix effects may prevent extraction of target analytes,
and may affect surrogate recoveries. In addition, non-target analytes may be
extracted from the matrix causing interferences.
MATRIX SPIKE - aliquot of a matrix (water or soil) fortified (spiked) with
known quantities of specific compounds and subjected to the entire analytical
procedure in order to indicate the appropriateness of the method for the
matrix by measuring recovery.
MATRIX SPIKE DUPLICATE - a second aliquot of the same matrix as the matrix
spike (above) that is spiked in order to determine the precision of the
method.
METHOD BLANK - an analytical control consisting of all reagents, internal
standards, and surrogate standards (or SMCs for VOA), that is carried
throughout the entire analytical procedure. The method blank is used to
define the level of laboratory, background, and reagent contamination.
NARRATIVE (SDG Narrative) - portion of the data package which includes
laboratory, contract, Case, and sample number identification, and descriptive
documentation of any problems encountered in processing the samples, along
with corrective action taken and problem resolution. Complete SDG Narrative
specifications are included in Exhibit B.
PERCENT DIFFERENCE (%D) - As used-in this SOW and elsewhere to compare two
values, the percent difference indicates both the direction and the magnitude
of the comparison, i.e., the percent difference may be either negative,
positive, or zero. (In contrast, see relative .percent difference.)
G-4 OLM04.2
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Exhibit G -- Glossary of Terms
PERCENT MOISTURE - an approximation of the amount of water in a soil/sediment
sample made by drying an aliquot of the sample at 105 °C. The percent
moisture determined in this manner also includes contributions from all
compounds that may volatilize at or below 105 °C, including water. Percent
moisture may be determined from decanted samples and from samples that are not
decanted.
PERFORMANCE EVALUATION MIXTURE - a calibration solution of specific analytes
used to evaluate both recovery and percent breakdown as measures of
performance.
PRIMARY QUANTISATION ION - a contract specified ion used to quantitate a
target analyte.
PROTOCOL - describes the exact procedures to be followed with respect to
sample receipt and handling, analytical methods, data reporting and
deliverables, and document control. Used synonymously with Statement of Work
(SOW).
PURGE AND TRAP (DEVICE) - analytical technique (device) used to isolate
volatile (purgeable) organics by stripping the compounds from water or soil by
a stream of inert gas, trapping the compounds on an adsorbent such as a porous
polymer trap, and thermally desorbing the trapped compounds onto the gas
chromatographic column.
PURGEABLES - volatile compounds.
| QUALITY ASSURANCE TECHNICAL SUPPORT (QATS) LABORATORY - a contractor operated
j facility operated under the QATS contract, awarded and administered by the
| EPA.
REAGENT WATER - water in which an interferant is not observed at or above the
minimum quantitation limit of the parameters of interest.
RECONSTRUCTED ION CHROMATOGRAM (RIC) - a mass spectral graphical
representation of the separation achieved by a gas chromatograph; a plot of
total ion current versus retention time.
RELATIVE PERCENT DIFFERENCE (RPD) - As used in this SOW and elsewhere to
compare two values, the relative percent difference is based on the mean of
the two values, and is reported as an absolute value, i.e., always expressed
as a positive number or zero. In contrast, see percent difference.
RELATIVE RESPONSE FACTOR (RRF) - a measure of the relative mass spectral
response of an analyte compared to its internal standard. Relative Response
Factors are determined by analysis of standards and are used in the
calculation of concentrations of analytes in samples. RRF is determined by
the following equation:
Ax Cis
RRF = ^- x
A. C
IB X
Where,
G-5 OLM04.2
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Exhibit G -- Glossary of Terms
A = area of the characteristic ion measured
C = concentration, or amount (mass)
is = internal standard
x = analyte of interest
RELATIVE RETENTION TIME (RRT) - the ratio of the retention time of a compound
to that of a standard (such as an internal standard).
RRT =
RT
RT
is
Where,
RTC = Retention time for the semivolatile target or surrogate compound
in continuing calibration.
RTis= Retention time for the internal standard in calibration standard
or in a sample.
| REPRESENTATIVE - alternate or designee who has the knowledge and authority to
| perform a specific task.
RESOLUTION - also termed separation or percent resolution, the separation
between peaks on a chromatogram, calculated by dividing the depth of the
valley between the peaks by the peak height of the smaller peak being
resolved, multiplied by 100.
Am (or Height)
For pesticide analysis the X-axis shall be displayed such that a data reviewer
can calculate the % Resolution.
RESOLUTION CHECK MIXTURE - a solution of specific analytes used to determine
resolution of adjacent peaks; used to assess instrumental performance.
RESPONSE - or Instrumental Response: a measurement of the output of the GC
detector (MS, EC, or FID) in which the intensity of the signal is
proportionate to the amount (or concentration) detected. Measured by peak
area or peak height.
G-6
OLM04.2
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Exhibit G -- Glossary of Terms
RETENTION TIME (RT) - the time a target analyte is retained on a GC column
before elution. The identification of a target analyte is dependent on a
target compound's retention time falling within the specified retention time
window established for that compound. Retention time is dependent on the
nature of the column's stationary phase, column diameter, temperature, flow
rate, and other parameters.
SAMPLE DELIVERY GROUP (SDG) - a unit within a single Case that is used to
identify a group of samples for delivery. An SDG is a group of 20 or fewer
| field samples within a Case, received over a period of up. to 7 calendar days.
Data from all samples in an SDG are due concurrently. A Sample Delivery Group
is defined by one of the following, whichever occurs, first:
All samples within a Case; or
| Every set of 20 field samples (excluding PE samples) within a Case; or
| All samples received within 7 calendar days, excluding Sundays and
| Government holidays. However, PE samples received within a Case shall
| be assigned to an SDG containing field samples for the Case.
| In addition, all samples and sample fractions assigned to an SDG must have
| been scheduled under the same contractual turnaround time.
Samples may be assigned to Sample Delivery Groups by matrix (i.e., all soil
samples in one SDG, all water samples in another), at the discretion of the
laboratory.
| SAMPLE MANAGEMENT OFFICE (SMO) - a contractor operated facility operated by
| the CLASS contract, awarded and administered by the EPA.
SAMPLE NUMBER (EPA Sample Number) - a unique identification number designated
by EPA to each sample. The EPA sample number appears on the sample Traffic
Report which documents information on.that sample.
SECONDARY QUANTITATION ION - contract specified ion(s) to be used in
quantitation of target analytes when interferences prevent the use of the
primary quantitation ion.
SEMIVOLATILE COMPOUNDS - compounds amenable to analysis by extraction of the
sample with an organic solvent. Used synonymously with Base/Neutral/Acid
(BNA) compounds.
SOIL - used herein synonymously with soil/sediment and sediment.
SONIC CELL DISRUPTOR (SONICATOR) - a device that uses the energy from
controlled ultrasound applications to mix, disperse, and dissolve organic
materials from a given matrix.
STANDARD ANALYSIS - an analytical determination made with known quantities of
target compounds; used to determine response factors.
STORAGE BLANK - reagent water (two 40.0 mL aliquots) stored with samples in an
SDG. It is analyzed after all samples in that SDG have been analyzed; and is
used to determine the level of contamination acquired during storage.
G-7 OLM04.2
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Exhibit G -- Glossary of Terms
SULFUR BLANK - a modified method blank that is prepared only when some of the
samples in a batch are subjected to sulfur cleanup. It is used to determine
the level of contamination associated with the sulfur cleanup procedure. When
all of the samples are subjected to sulfur cleanup, then the method blank
serves this purpose. When none of the samples are subjected to sulfur
cleanup, no sulfur blank is required.
SURROGATES (Surrogate Standard) - for semivolatiles and pesticides/Aroclors,
compounds added to every blank, sample, matrix spike, matrix spike duplicate,
and standard; used to evaluate analytical efficiency by measuring recovery.
Surrogates are brominated, fluorinated, or isotopically labeled compounds not
expected to be detected in environmental media.
SYSTEM MONITORING COMPOUNDS - compounds added to every blank, sample, matrix
spike, matrix -spike duplicate, and standard for volatile analysis, and used to
evaluate the performance of the entire purge and trap-gas chromatograph-mass
spectrometer system. These compounds are brominated or deuterated compounds
not expected to be detected in environmental media.
TARGET COMPOUND LIST (TCL) - a list of compounds designated by the Statement
of Work (Exhibit C) for analysis.
TENTATIVELY IDENTIFIED COMPOUNDS (TIC) - compounds detected in samples, that
are not target compounds, internal standards, system monitoring compounds, or
| surrogates. TICs must have peak areas or heights greater than 10% of the peak
| areas or heights of nearest internal standard. TICs must be subjected to mass
| spectral library searches and be deemed acceptable by a mass spectral
| interpretation specialist.
TIME - when required to record time on any deliverable item, time shall be
expressed as Military Time, i.e., a 24-hour clock.
TRAFFIC REPORT (TR) - an EPA sample identification form filled out by the
sampler, which accompanies the sample during shipment to the laboratory and
which documents sample condition and receipt by the laboratory.
TWELVE-HOUR TIME PERIOD - The twelve'(12) hour time period for GC/MS system
instrument performance check, standards calibration (initial or continuing
calibration), and method blank analysis begins at the moment of injection of
the DFTPP or BFB analysis that the laboratory submits as documentation of
instrument performance. The time period ends after 12 hours have elapsed
according to the system clock. For pesticide/Aroclor analyses performed by
GC/EC, the twelve hour time period in the analytical sequence begins at the
moment of injection of the instrument blank that precedes sample analyses, and
ends after twelve hours have elapsed according to the system clock.
VALIDATED TIME OF SAMPLE RECEIPT (VTSR) - the date on which a sample is
received at the Contractor's facility, as recorded on the shipper's delivery
receipt and Sample Traffic Report.
VOLATILE COMPOUNDS - compounds amenable to.analysis by the purge and trap
technique. Used synonymously with purgeable compounds.
G-8 OLM04.2
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Exhibit G -- Glossary of Terms
WIDE BORE CAPILLARY COLUMN - a gas chromatographic column with an internal
diameter (ID) that is greater than or equal to 0.53 mm. Columns with lesser
diameters are classified as narrow bore capillary columns.
G-9 OLM04.2
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EXHIBIT H
AGENCY STANDARD IMPLEMENTATION
H-l OLM04.2
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Exhibit H - Agency Standard Implementation
Table of Contents
Section Page
1.0 FORMAT CHARACTERISTICS 3
2.0 RECORD TYPES 5
3.0 PRODUCTION RUNS 6
4.0 RECORD SEQUENCE 8
5.0 ' FILE/RECORD INTEGRITY 9
6.0 DATES AND TIMES 9
7.0 MULTIPLE VOLUME DATA 9
8.0 DELIVERABLE 10
9.0 RECORD LISTING 12
9.1 Production Run Header Record (Type 10) 12
9.2 Chromatography Record (Type 11) 13
9.3 Sample Header Data Record (Type 20) 14
9.4 Sample Header Data Record (Type 21) 16
9.5 Sample Condition Record (Type 22) 18
9.6 Associated Injection and Counter Record (Type 23) 20
9.7 Sample Cleanup Record (Type 27) 23
9.8 Results Data Record (Type 30) . . . .- 25
9.9 Auxiliary Data Record (Type 32) 28
9.10 Name Record (Type 33) 29
9.11 Instrumental Data Readout Record (Type 36) 30
9.12 Comment Record (Type 90) 33
10.0 DEFINITIONS OF VARIOUS CODES USED IN AGENCY STANDARD RECORDS . . . . 34
10.1 Quality Control and Related Codes (QCC) in Type 20 Records . . 34
10.2 Codes For Sample Medium (Matrix, Sources) 36
10.3 List of Sample and Result Qualifiers 36
APPENDIX A -- FORMAT OF RECORDS FOR SPECIFIC USES 38
Table of Contents 39
H-2 OLM04.2
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Exhibit H -- Section 1
Format Characteristics
1.0 FORMAT CHARACTERISTICS
1.1 This constitutes an implementation of the EPA Agency Standard for
Electronic Data Transmission based upon analytical results and ancillary
information required by the contract. All data generated by a single
analysis are grouped together, and the groups are aggregated to produce
files that report data from an SDG. Because this implementation is only
a subset of the Agency Standard, some fields have been replaced by
delimiters as place holders for non-CLP data elements.
1.2 This implementation includes detailed specifications for the required
format of each record. The position in the record where each field is
to be contained relevant to other fields is specified, as well as the
maximum length of the field. Each field's required contents are
specified as literal (contained in quotes), which must appear exactly as
shown (without quotes), or as a variable for which format and/or
descriptions are listed in the format/contents column. Options and
examples are listed for most fields. For fields where more than three
options are available, a list and description of options are supplied on
a separate page following the record descriptions. Fields are separated
from each other by the delimiter "|" (ASCII 124) . Fields that do not
contain data should be zero length or a blank field (empty with no space
or additional delimiters between the delimiters before and after the
field) with the delimiter as a place holder. For the purposes of
Section 9 of this exhibit, wherever "blank" is given as an option under
the "Format/Contents" column, it refers to a blank field as explained
above.
1.3 Numeric fields may contain numeric digits, a decimal place, and a
leading minus sign. A positive sign is assumed if no negative sign is
entered in a numeric field and shall not be entered into any numeric
field. Values that exceed the maximum length allowed shall be reported
to the maximum possible, maintaining the specified decimal place and
maximum field length restrictions.
1.4 Requirements for significant figures and number of decimal places are
specified in Exhibit B. The numeric field lengths are specified such
that all possible numeric values can be written to the file. The size
of the numeric field indicates the maximum number of digits, including a
decimal place and negative sign (if appropriate), that can appear in the
field at the same time. Therefore, the number reported may need.to be
rounded (using rounding rules described in Exhibit B) to fit into the
field. The rounding shall maintain the greatest significance possible
providing the field length limitation. In addition, the rounded number
that appears on the form, and therefore in the field on the diskette
file, must be used in any calculation that may result in other numbers
reported on the same form or other forms in the SDG. The numbers/values
reported by the Contractor are used by CCS to calculate a result (e.g.,
CRQL). The final value calculated by CCS is then rounded according to
rounding rules described in Exhibit B and is used for comparison to the
final value (e.g., CRQL) reported by the Contractor. Field lengths
should only be as long as necessary to contain the data; packing with
blanks is not allowed.
H-3 OLM04.2
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Exhibit H -- Section 1
Format Characteristics
1.5 The CLP is currently developing a data delivery strategy that may be
used as an alternative to the requirements stated in Exhibit H. This
strategy's intent is to provide a neutral data delivery structure to the
Contractor that will further facilitate the exchange of analytical
information, generated under this analytical protocol. The proposed
strategy is intended to accommodate laboratories that generate data
transmission files under multiple data formats. Upon implementation of
this alternate electronic data delivery strategy by the CLP and prior to
submission of data in alternate format(s), the Contractor must first
demonstrate its ability to provide electronic data as stated in this
Exhibit H and obtain written permission from the CLP for the submission
of data in alternate format(s). The Contractor will receive a written
response to its request within 90 calendar days. However, until the
implementation of this alternate electronic data delivery strategy by
the CLP, all electronic data deliverables must be provided as specified
in this Exhibit H.
H-4 OLM04.2
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Exhibit H -- Section 2
Record Types
2.0 RECORD TYPES
2.1 The Agency Standard consists of variable length ASCII records. Maximum
field length specifications match the reporting requirements in Exhibit
B. The last two bytes of each record shall contain "carriage return"
and "line feed", respectively.
2.2 This implementation consists of twelve record types that can be
summarized in four groups, designated by the first record type in each
group:
Type Type ID Contents
Run Header 10 Information pertinent to a group of
samples processed in a continuous
sequence; usually several per SDG
Sample Header 20 Sample identifying, qualifying, and
linking information
Results Record 30 Analyte results and qualifications
Comments Record 90 Free form comments
2.3 A separate run header is used for volatiles (VGA), semivolatiles (SV),
and for each column analysis for pesticides (PEST) (minimum of four type
10 series for VOA/SV/PEST SDG). The 20 series records contain sample
characteristics and link samples within an SDG to the corresponding
calibrations, blanks, and other QCs. The 30 series records contain the
actual analytical results by analyte within each sample. The 10, 20,
and 30 records are associated with each other by their position in the
file (i.e., 30 series records follow the corresponding 20 series, which
in turn follow the 10 series run header records).
H-5 OLM04.2
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Exhibit K -- Section 3
Production Runs
3.0 PRODUCTION RUNS
3.1 A production run represents a "group" or "batch" of samples that are
processed in a continuous sequence under relatively stable conditions.
Specifically:
3.1.1 Calibration - All samples in a run use the same initial calibration
data.
3.1.2 Method number - Constant throughout a run.
3.1.3 Instrument conditions - Constant throughout a run.
3.2 Each instrumental analysis consists of a separate production run and is
reported in a separate file. There will be a separate production run
for each of the two pesticide GC columns utilized. Thus, a full three
fraction analysis will consist of a minimum of four production runs.
' Hr6 OLM04.2
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Exhibit H -- Section 3
Production Runs
3.3 Example of the Sequence of Record Types in a File1
10 Contains Run Header information.
11 Contains additional run-wide information.
20 Occurs once for each sample, calibration, mean response
factor, matrix spike duplicate result, etc. Acts as a
header.
21
22 Contains additional information for samples.
23
27
30 Occurs once for each final analytical result. Reports
the value being determined as defined by the type 20.
32 Reports any auxiliary data necessary.
33 Reports compound names for tentatively identified
compounds (TICs) if necessary.
36 Reports any instrumental data necessary.
30 Values for the next analyte or parameter being measured.
32 Additional data may vary for each parameter, and may
33 occur in any order. Multiple occurrences of the same
36 record type, however, must be consecutive.
30 Continues for as many as are necessary.
32
33
36
30
32
33
36
20 Next Sample Header record. The following applies to the
21 next sample or other group of data.
22
30
32
33
36
30
32
33
36
etc.
20
21
30
32
33
36
etc.
Appendix A provides a detailed set of examples for the use of the
different record types, and their relationship to other record types.
H-7 OLM04.2
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Exhibit H -- Section 4
Record Sequence
4.0 RECORD SEQUENCE
4.1 The sequence of records for Agency Standard files is as follows: A Run
Header (type 10) record shall be present once and once only (per file)
as the first record in a file. Therefore, a complete VOA/SV/PEST SDG
will consist of several files.
4.2 Each environmental sample, calibration standard, or quality control
sample is represented by a group composed of type 20, 21, 22, 23, and 27
records, that hold sample level identifying information, followed by
type 30, 32, 33, and 36 records for each method analyte including
surrogates, system monitoring compounds, and internal standards in the
sample. The type 20 record holds a count for the number of method
analytes being determined and includes all target compounds, surrogates,
system monitoring compounds, and internal standards plus each peak of
the multi-component pesticides (do not include TICs in this count). A'
separate field on the type 23 record contains the number of TICs found.
Type 20 records shall occur in the order of sample analysis. In
addition, a type 20 record with a QC code "MNC", followed by a type 30
record for each method analyte (reporting values such as mean response
factors) will appear after the type 10 or type 11 record and before the
type 20 record that initiates the analytical sequence. Similarly, for
pesticide runs, a type 20 record with a QC code "GPC" for GPC recovery,
followed by type 30 records for each of the method analytes spiked; and
a type 20 record with a QC code "FLO" for Florisil recovery, followed by
type 30 records for each of the method analytes (and the two surrogates)
included in the Florisil check will appear before the type 20 record
that initiates the analytical sequence.
4.3 Type 90 comment records may be defined to occupy any position after the
type 10 (header) record.
H-8 OLM04.2
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Exhibit H -- Sections- 5-7
File/Record Integrity/Dates and Times/Multiple Volume Data
5.0 FILE/RECORD INTEGRITY
All record types shall contain the following check fields to ensure file
and record integrity:
Record Field Field
Position Length Contents Remarks
First Field 2 Record type "10" or as appropriate
Last Field 5 Record sequence number 00001-99999, numbered
within file sequentially
4 Record checksum1 Four hexadecimal digits
2 Must contain CR and LF
6.0 DATES AND TIMES
Date or time-of-day information consists of successive groups of two
decimal digits (except year, which is four decimal digits), each
separated by delimiters. Dates are given in the order 1TYY MM DD, and
times as HH MM. All hours shall be given as 00 to 23 using a 24-hour
clock and shall be local time. All days shall be given as 01 to 31.
All months shall be given as 01 to 12 (e.g., 01 is January, 02 is
February).
7.0 MULTIPLE VOLUME DATA . '
There is no requirement under this format that all the data from an
entire sample delivery group fit onto a single diskette. However, each
single production run must fit onto a single diskette if possible. If
that is not possible, then it is necessary that all files start with a
type 10 record, and that the multiple type 10 records for each file of
the same production run be identical. Information for a single sample
shall not be split between files.
The checksum is the sum of the ASCII representation of the data on the
record up to the Record Sequence Number (not including the Record
Sequence Number) plus the checksum of the previous record. The sum is
taken modulo 65536 (216) and is represented as four hexadecimal digits
(i.e., the remainder of the sum divided by 65536 represented as four
hexadecimal digits).
H-9 OLM04.2
-------
Exhibit H -- Section 8
Deliverable
8.0 DELIVERABLE
8.1 The file shall be submitted on IBM-compatible, 3.5 inch high density
1.44 M-byte diskettes. The diskettes shall be formatted and recorded
using MS-DOS Operating System. The diskettes shall contain all
information relevant to one and only one SDG. An alternative means of
electronic transmission may be utilized if approved in advance by the
EPA.
8.2 Agency Standard data from an entire SDG may not fit onto a single
diskette. If a single production run is being split onto multiple
diskettes, then all files shall start with a type 10 record, and the
multiple type 10 records for each file of the same production run shall
be identical. Do not split the data from a .single sample.onto multiple
diskettes.
8.3 Information on the diskette must correspond to information submitted in
the hardcopy raw data package and on the hardcopy raw data package
forms. For example, type 30 results field specifies maximum length of
13. When reporting CRQLs or results on Form 1, maximum length is 13 as
is specified in this exhibit; when reporting 'calculated amounts' on
Form 7D, hardcopy specified maximum length is 8. Unused records shall
not be included on the diskettes. If the information submitted in the
hardcopy data package forms is changed, the information in the
electronic file (e.g., diskette) shall be changed accordingly, and a
complete electronic deliverable containing all the information for the
SDG shall be resubmitted along with the hardcopy at no additional cost
to the EPA.
8.4 Each diskette shall be identified with an external label containing (in
this order) the following information:
Disk Density
File Name(s)
Laboratory Name (optional)
Laboratory Code
Contract Number
Case Number/SDG
SAS Number (where applicable)
Initial Submission or Resubmission (as applicable) and Date
8.5 The format for File Name shall be XXXXX.O01 to XXXXX.O99. Where XXXXX
is the SDG identifier, O designates Organics, and 01 through 99 is .the
file number.
8.6 Dimensions of the label must be in the range of 2-1/2" to 2-3/4" long by
2" to 2-1/8" wide for a 3-1/2 inch IBM-compatible diskette.
8.7 Section 9.0 (Record Listing) provides information for the usage of each
of the record types. Where specified, labels indicate the nature of the
value(s) that follow on that record. If the value(s) will not be
reported, the label shall be omitted.
H-10 OLM04.2
-------
Exhibit H -- Section 8
Deliverable
8.7.1 A record type 30 for each TCL compound, surrogate, system monitoring
compound, and internal standard quantitated for shall be reported.
If the^TCL is not detected, the 'U' qualifier in the appropriate
field shall be indicative of that.
8.7.2 For multicomponent analytes (Aroclors/toxaphene), if the
multicomponent analyte is detected, a record type 30 and 32 shall be
reported for each peak identified.
H.-ll OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.0 RECORD LISTING
The following lists every record type required to report data from a
single SDG.
9.1 Production Run Header Record (Type 10)
Use: Each production run will start with a record type 10.
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
2 RECORD. TYPE "10"
6 Delimiters I I I I I I
5 INSTRUMENT/DETECTOR Character1
1 Delimiter |
8 METHOD NUMBER Character2
2 Delimiters ||
6 LAB CODE Character
4 Delimiters ||||
11 CONTRACT NUMBER Character
1 Delimiter |
10 INSTRUMENT ID Character
2 Delimiters | |
25 LABORATORY NAME Character
2 Delimiters . | | '
5 RECORD SEQUENCE NUMBER Numeric
4 CHECKSUM Character
General descriptor (GC/MS for VOA/SVOA analysis or GC for pesticide
analysis on GC/EC).
OLM04.2V For Volatiles; OLM04.2B for semivolatiles; OLM04.2P for
pesticides. (O for Organic, L for Low, M for Medium, zero four for
document number, zero V for volatiles, zero B for semivolatiles, zero P
for pesticides.)
H-12 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.2 Chroraatography Record (Type 11)
Use: To describe chromatograph condition. Must be present once for
each production run immediately following the record type 10.
CONTENTS FORMAT/CONTENTS
RECORD TYPE "11"
Delimiter |
GC COLUMN IDENTIFICATION Character
Delimiters ||
GC COLUMN ID1 Numeric (mm)
Delimiters I I I I I I I I 1 I I
RECORD'SEQUENCE NO. Numeric
CHECKSUM Character
Internal Diameter of the GC column used.
H-13 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.3 Sample Header Data Record (Type 20)
1
1
1
3
1
3
1
5
1
6
1
4
1
2
1
2
1
2
1
2
2
2
1
5
CONTENTS
RECORD TYPE
Delimiters
EPA SAMPLE NUMBER
Delimiter
MATRIX
Delimiter
QC CODE
Delimiter
SAMPLE QUALIFIER
Delimiter
CASE NUMBER
Delimiter
SDG NO.
Delimiter
SAMPLE/BLANK/STANDARDS YEAR ANALYZED
Delimiter
SAMPLE/BLANK/STANDARDS MONTH ANALYZED
Delimiter
SAMPLE/BLANK/STANDARDS DAY ANALYZED
Delimiter
SAMPLE/BLANK/STANDARDS HOUR ANALYZED
Delimiter
SAMPLE/BLANK/STANDARDS MINUTE ANALYZED
Delimiters
SAMPLE WT/VOL UNITS
Delimiter
SAMPLE WT/VOL
FORMAT/CONTENTS
"20"
II
As is exactly on the
hardcopy form
I
CHARACTER1
I
Character (See Section 10)
I
RIN/REX/REJ/SRN/blank2
I
Numeric
I
Character
I
iTYY
I
MM
I
DD
I
HH
I
MM
II
"G"/"ML"/blank3
I
Numeric4
"0" if not applicable (calibration,
soil.
tune, etc.); "1" for water; "H" for
"RIN" for reinjection,- "REX" for re -extract ions; "REJ" for rejected
samples; "SRN" for dilutions; and leave blank (empty field with zero
length) when none of the previous conditions apply. In case of multiple
operations on a sample, the final operation will be indicated (e.g.,
reinjection of a dilution; AAA12DLRE would have a QC Code of "RIN") .
Sample WT/VOL unit is mL (milliliters) for liquids and G (grams) for
solids. The sample units code indicates which units are in use for the
current sample. Leave blank (zero length) if not applicable.
Sample WT/VOL is the volume in milliliters for liquid or the wet weight
in grams for solids. Sample WT/VOL includes the purge volume. .
H-14
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Sample Header Data Record (Type 20) (Cont.)
CONTENTS FORMAT/CONTENTS
Delimiter |
ANALYTE COUNT Numeric5
Delimiters . || |
RECORD SEQUENCE NO. Numeric
CHECKSUM Character
1-3 decimal digits. Counts TCL analytes, surrogates, system monitoring
compounds (SMC), internal standards, and all peaks reported for multi-
component PCBs. Do not include the count for TICs in this field. For
calibrations, also count DFTPP, if included in calibration solution.
H-15 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.4 Sample Header Data Record (Type 21)
Use: Continuation of Type 20.
Position: Follows the Type 20 to which it applies.
MAXIMUM
LENGTH
2
1
1
1
1
2
1
1
1
2
6
1
14
1
4
1'
2
1
2
2
4
1
2
1
2
2
CONTENTS
RECORD TYPE
Delimiter
PURGE
Delimiter
LEVEL
Delimiters
EXTRACTION
Delimiters
SAS NUMBER
Delimiter
LAB FILE/ SAMPLE ID
Delimiter
YEAR EXTRACTED
Delimiter
MONTH EXTRACTED
Delimiter
DAY EXTRACTED
Delimiters
YEAR RECEIVED
Delimiter
MONTH RECEIVED
Delimiter
DAY RECEIVED
Delimiters
I 2
FORMAT/CONTENTS
"21"
I
"N" for not heated; "Y" for heated;
blank if SV or PEST
I
"L"/"M"/blank1
II
S/C/H/N/X/P/T/blank (for all other
volatile samples)2
II
Character
I
Character3
I
ITYY/blank (for volatiles)
I
MM/blank (for volatiles)
I
DD/blank (for volatiles)
II
YYYY/blank (for standards, tunes, and
blanks)
I
MM/blank (for standards, tunes, and
blanks)
I
DD/blank (for standards, tunes, and
blanks)
II
"L" for low level samples and "M" for medium level samples for volatile
and semivolatile analyses. Leave blank for pesticides, all
calibrations, and all tunes.
"S" for separatory funnel; "C" for continuous liq-liq without
hydrophobia membrane; "H" for continuous liq-liq with hydrophobia
membrane; "N" for sonication; "X" for automated soxhlet; "P" for
pressurized fluid; "T" for volatile low level soils^ by the Modified
Sff-846 Method 5035;.blank (zero length field) for all other volatile
samples.
Lab File ID for volatile and semivolatile analyses. Lab Sample ID for
pesticides in same format as on:-forms.
H-16
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Sample Header Data Record (Type 21) (Cont.)
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
8 INJECTION/ALIQUOT VOLUME Numeric/blank (for low level VOA)4
2 Delimiters . | |
5 RECORD SEQUENCE NO. Numeric
4 CHECKSUM Character
Injection volume, in uL, for SVOAs and PESTs; Soil Aliquot Volume for
medium level VOA.
H-17 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.5 Sample Condition Record (Type 22)
Use: Continuation of type 20. Used to describe additional Sample
Conditions.
Position: Follows the type 20'and 21 to which it applies.
MAXIMUM
LENGTH
2
1
1 ^
1
2
1
2
\
2
1
2
1
14
1
4
1
5
1
1
1
8
1
8
3
CONTENTS
RECORD TYPE
Delimiter
CALIBRATION YEAR
Delimiter
CALIBRATION MONTH
Delimiter
CALIBRATION DAY
Delimiter
CALIBRATION HOUR
Delimiter
CALIBRATION MINUTE
Delimiter
CALIBRATION FILE ID
Delimiter
PH
Delimiter
PERCENT MOISTURE
Delimiter
DECANTED
Delimiter
EXTRACT VOLUME
Delimiter
DILUTION FACTOR
Delimiters
FORMAT/CONTENTS
"22"
I
yyYY/blank (for PEST)1
I
MM/blank (for PEST)
I
DD/blank (for PEST)
I
HH/blank (for PEST)
I
MM/blank (for PEST)
I
Character/blank (for PEST)2
I
Numeric/blank (for aqueous samples
and volatiles)
I
Numeric
I
"Y"/"N"/blank (for volatiles)
I
Numeric/blank (for low level VOA)3
I
Numeric4
III
For volatiles and semivolatiles, enter the date and time of analysis of
the most recent 50 ug/L (VOAs) or the 50 ng (SVGAs) standard run prior
to the sample reported in the associated type 20 record. Leave blank
for pesticides.
Lab File ID of standard specified in 1 above (volatiles/semivolatiles
only). This field must match the Lab File ID on Type 21 for the
associated calibration (VSTD050/SSTD050). Leave blank for pesticides.
Enter the Soil Extract Volume for medium level VOA, and Concentrated
Extract Volume for all SVOA and PEST. The value should be reported in
microliters.
Dilution factor of sample analyzed (omit contract-mandated dilutions).
H-18 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Sample Condition Record (Type 22) (Cont.)
'CONTENTS FORMAT/CONTENTS
LEVEL Numeric/blank (for VOA/SV)5
Delimiter |
RECORD SEQUENCE NO. Numeric
CHECKSUM Character
Concentration level of Pesticide Individual Mix A and B standards.
Concentration of low point, mid point and high point calibration
standards as a multiplier of low point. Low point = 1.0; Mid point =
4.0; High point 2 16.0.
H-19 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.6 Associated Injection and Counter Record (Type 23)
Use: Continuation of type 20. Used to identify associated blanks
and tunes, and the number of surrogates/SMCs and spikes
outside of the QC limits and the number of TICs.
Position: Follows the type 20, 21, and 22 to which it applies.
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
2 RECORD TYPE "23"
1 Delimiter |
1 INSTRUMENT PERFORMANCE "P" (for BFB and DFTPP IPC) or blank (for
CHECK (IPC/TUNE) LABEL pesticides)
1 Delimiter |
| 4 IPC/TUNE INJECTION YEAR YYYY/blank (for PEST)
1 Delimiter |
2 IPC/TUNE INJECTION MM/blank (for PEST)
MONTH
1 Delimiter |
2 IPC/TUNE INJECTION DAY DD/blank (for PEST)
1 Delimiter |
2 IPC/TUNE INJECTION HOUR HH/blank (for PEST)
1 Delimiter |
2 IPC/TUNE INJECTION MM/blank (for PEST)
MINUTE
1 Delimiter |
14 DFTPP/BFB LAB FILE ID Character/blank (for PEST)
1 Delimiter |
2 VOLATILE STORAGE BLANK "HB" (for VOA) or blank (for SV and PEST)
LABEL
1 Delimiter |
| 4 STORAGE BLANK INJECTION ITYY/blank (for SV and PEST)
YEAR
1 Delimiter |
' 2 STORAGE BLANK INJECTION MM/blank (for SV and PEST)
MONTH
1 Delimiter |
2 STORAGE BLANK- INJECTION DD/blank (for SV and PEST)
DAY
1 Delimiter |
2 STORAGE BLANK INJECTION HH/blank (for SV and PEST)
HOUR
1 Delimiter |
2 STORAGE BLANK INJECTION MM/blank (for SV and PEST)
MINUTE
1 Delimiter |
14 STORAGE BLANK LAB Character
.FILE ID (VOA ONLY)
4 . Delimiters
H-20 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Associated Injection and Counter Record (Type 23) (Cont.)
MAXIMUM
LENGTH
2
1
1 ^
1
2
1
2
1
2
1
2
1
14
1
1
1
2
1
1
1
2
1
1
1
CONTENTS
METHOD BLANK LABEL
Delimiter
METHOD BLANK INJECTION
YEAR
Delimiter
METHOD BLANK INJECTION
MONTH
Delimiter
METHOD BLANK INJECTION
DAY
Delimiter
METHOD BLANK INJECTION
HOUR
Delimiter
METHOD BLANK INJECTION
MINUTES
Delimiter
METHOD BLANK LAB
FILE (for VOA and
SV) /SAMPLE ID (for
PEST)
Delimiter
SURROGATE (for SV and
PEST) /SMC (for VOA)
RECOVERY LABEL
Delimiter
SURROGATE (for SV and
PEST) /SMC (for VOA)
RECOVERIES OUT
Delimiter
TIC LABEL
Delimiter
NO. OF TICS
Delimiter
SPIKE RECOVERY LABEL
Delimiter
FORMAT/CONTENTS
"MB"/blank (for standard, tune, and
method blanks)
I
YYYY/blank (for standard, tune, and
method blanks)
I
MM/blank (for standard, tune, and method
blanks)
I
DD/blank (for standard, tune, and method
blanks)
HH/blank (for standard, tune, and method
blanks)
I
MM/blank (for standard, tune, and method
blanks)
I
CHARACTER
"P" for % recoveries/blank (for STD/IPC)
Numeric1
"T" (for VOA and SV TICs)/blank (for
PEST)
I
Numeric
I
"S" for Matrix Spikes and Matrix Spike
Duplicates/blank for anything else
This will be the number of surrogate (for SV or PEST) or SMC (for VOA)
recoveries outside QC limits for a specific column. It should not be
cumulative of the two columns for pesticides.
H-21
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Associated Injection and Counter Record (Type 23) (Cont.)
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
2 SPIKE RECOVERIES OUT Numeric/blank2
1 Delimiter |
1 RPD LABEL "R" for RPD/blank3
1 Delimiter |
2 RPD OUT Numeric
1 Delimiter |
5 RECORD SEQUENCE 'NO. Numeric
4 CHECKSUM Character
Enter the number of spike recoveries out. Enter "0"(zero) if none of
the spike recoveries are outside of the QC limit.
"R" for Matrix Spike/Matrix Spike Duplicate Recovery Relative Percent
Differences. Leave blank for all other samples (only report for
MS/MSD).
H-22 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.7 Sample Cleanup Record (Type 27)
Use: Continuation of type 20. Used to identify sample/blank cleanup
procedures and QC results.
Position: Follows type 20, 21, 22, and 23 to which it applies.
FORMAT/CONTENTS
"27"
I
"G" for GPC/blank (for VGA}1
I
ITYY/blank (for VGA)
I
MM/blank (for VGA)
I
DD/blank (for VGA)
I
HH/blank (for VGA)
I
MM/blank (for VGA)
I
Character/blank (for VGA and
SV)2
I
"F" (for PEST) or blank (for
VGA and SV)
I
ITYY/blank (for VGA and SV)
I
MM/blank (for VGA and SV)
I
DD/blank (for VGA and SV)
I
HH/blank (for VGA and SV)
I
MM/blank (for VGA and SV)
I
Character3
"G" indicates that GPC was performed. If GPC was not performed,.leave
the field blank.
Lab Sample ID of associated GPC. This is a unique identifier assigned
to the spike recovery results for a specific GPC calibration check for
pesticides. Leave blank for volatiles and semivolatiles.
Lab Sample ID of associate Florisil lot check. This is a unique
identifier assigned to a lot of Florisil cartridges.
MAXIMUM
LENGTH
2
1
1
1
1 «
1
2
1
2
1
2
1
2
1
14
1
1
1
1 *
1
2
1
2
1
2
1
2
1
14
CONTENTS
RECORD TYPE
Delimiter
FIRST CLEANUP TYPE
Delimiter
GPC CALIBRATION CHECK YEAR
Delimiter
GPC CALIBRATION CHECK MONTH
Delimiter
GPC CALIBRATION CHECK DAY
Delimiter
GPC CALIBRATION CHECK HOUR
Delimiter
GPC CALIBRATION CHECK MINUTE
Delimiter
GPC Data Descriptor
Delimiter
.FLORISIL CLEANUP TYPE
Delimiter
FLORISIL LOT CHECK YEAR
Delimiter
FLORISIL LOT CHECK MONTH
Delimiter
FLORISIL LOT CHECK DAY
Delimiter
FLORISIL LOT CHECK HOUR
Delimiter
FLORISIL LOT CHECK MINUTE
Delimiter
FLORISIL DATA DESCRIPTOR
H-23
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Sample Cleanup Record (Type 27) (Cont.)
MAXIMUM
LENGTH . CONTENTS
1 Delimiter
1 SULFUR CLEANUP
1 Delimiter
2 SULFUR BLANK LABEL
1 Delimiter
4 SULFUR BLANK INJECTION YEAR
1 Delimiter
2 SULFUR BLANK INJECTION MONTH
2 Delimiters
2 SULFUR BLANK INJECTION DAY
1 Delimiter
2 SULFUR BLANK INJECTION HOUR
1 Delimiter
2 SULFUR BLANK INJECTION MINUTE
1 Delimiter
14 SULFUR BLANK LABORATORY/
SAMPLE ID
1 Delimiter
5 RECORD SEQUENCE NO.
4 CHECKSUM
FORMAT/CONTENTS
I
Y/N (for PEST)/blank (for VOA
and SV)
11 SB"/blank (if no separate
sulfur blank was prepared for
pesticides; also blank for VOA
and SV)
I
iTYY/blank (for VOA and SV)
I
MM/blank (for VOA and SV)
II
DD/blank (for VOA and SV)
I
HH/blank (for VOA and SV)
I
MM/blank (for VOA and SV)
I
Character
I
Numeric
Character
H-24
OLM04.2
-------
9.8 . Results Data Record (Type 30)
Exhibit H -- Section 9
Record Listing
CONTENTS
RECORD TYPE
Delimiter
ANALYTE LABEL
1 Delimiter
9 CAS NUMBER
1 Delimiter
9 INTERNAL STD. CAS NUMBER
1 Delimiter
5 CONCENTRATION UNITS
1 Delimiter
3 RESULT QUALIFIER
1 Delimiter
13 RESULTS
1 Delimiter
5 FLAGS
1 Delimiter
1 AMOUNT ADDED LABEL
1 Delimiter
13 AMOUNT ADDED
1 -Delimiter
FORMAT/CONTENTS '
"30"
I
"C" for CAS Number (blank for
unknown TICs)
I
Numeric (for TCL, surrogates,
DFTPP, BFB, SMC, internal.
standards, and identified TICs)
Numeric
Character "ug/L" (aqueous);
"ug/Kg" (soil) ,- "ng" (amount
added)
Character1'2
I
Numeric3
I
Character4
I
"A" for Amt. added5
I
Numeric
1 When a Type 20 Record is used for calibration summary (MNC), the
associated Type 30 Record uses "AVG" for average RRFs and Mean
Calibration Factors. See Exhibit H Section 10.3.2.
2 For pesticide sample analysis, if an analyte is detected in only one of
the two column analyses, report the analyte as "not detected." in both
runs. Report result qualifier, for each column, as BDL. See Section
10.3.2 for result qualifiers.
3 Leave this field blank only when reporting non-detects.
4 A maximum of five flags (D,E,J,B,A,P,C,X,Y,Z, or N) with no space
between the flags can be reported, each representing a qualification of
the result as described in Exhibit B. For surrogates, the "D" flag will
indicate surrogates diluted out.
5 For Matrix Spike/Matrix Spike Duplicate analysis, surrogate, SMC for
VOA, SV, and PEST (Form 3s). Nominal Amount for Pesticides (Form
7E/7F) . Spike added for florisil and GPC (Form 9A/9B) .
H-25
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Results Data Record (Type 30) (Cont.)
MAXIMUM
LENGTH CONTENTS
1
I
13
1
1
1
5
1
1
1
5
1
5
1
1
1
5
1
1
1
5
CRQL LABEL
Delimiter
CRQL
Delimiter
RSD LABEL
Delimiter
RSD VALUE
Delimiter
MS/MSD REC LABEL
Delimiter
MS % RECOVERY
Delimiter
MSD % RECOVERY
Delimiter
RPD LABEL
Delimiter
RPD VALUE
Delimiter
SURR/ SPIKE RECOVERY LABEL
Delimiter
SURR/SPIKE RECOVERY
FORMAT/CONTENTS
"U" for "undetected" or blank when
analyte is detected
I
Numeric
"R" for % Resolution/RSD6
I
Numeric
I
"P" for % recovery [MS/MSD] /blank
(for sample [except MS/MSD] ,
standard, tune, blanks,
calibration)
Numeric/blank (for everything
except MS)
I
Numeric/blank (for everything
except MSD)
I
"D" for MS/MSD or for pesticide
calibration verification
(%D) /blank
I
Numeric/blank7
I
"S" for % recovery/blank (for non-
surrogate/SMC and non-spike
analytes
I
% Recovery/blank8
"R" for % Resolution (Forms 6H, 61, 6J, and 6K) or for RSD of Response
factors under Calibration summary (MNC) Type 20. (Blank for VOA and SV
fractions.)
RPD for MS/MSD recoveries, or %D for pesticides. Calibration
Verification (Form 7E/7F). Otherwise, leave blank.
Surrogate (for SV and PEST)/SMC (for VOA) or Spike (Forms 2, Form 9A/9B)
recovery. Leave blank for non-surrogate and non-spike analytes.
H-26
OLM04.2
-------
Results Data Record (Type 30) (Cont.)
Exhibit H -- Section 9
Record Listing
MAXIMUM
LENGTH CONTENTS
1 Delimiter
FORMAT/CONTENTS
MEAN CONCENTRATION LABEL
1 Delimiter
13 MEAN CONCENTRATION
1 Delimiter
1 PERCENT DIFFERENCE.LABEL
1 Delimiter
5 PERCENT DIFFERENCE
1 Delimiter
1 INTERNAL STANDARD AREA LABEL
1 Delimiter
13 INTERNAL STANDARD AREA
1 Delimiter
5 RECORD SEQUENCE NO.
4 CHECKSUM
"M" for Mean cone, (for
multicomponent PEST only)/blank
(for VOA and SV)
I
Numeric (for PEST)/blank (for VOA
and SV)9
"F" or "P" (PEST)/blank (for VOA
and SV field sample analysis)10
I
Numeric
I
"I" for IS Area (for VOA and
SV)/blank (for PEST)
I
Numeric (for VOA and SV)/blank
(for PEST)
I
Numeric
Character
9 Mean Concentration for Multicomponent analytes detected in pesticide
analyses.
10 "P" for Percent Difference between concentrations from two columns in
pesticide analyses, or "F" for Percent Difference between average RRF
(initial, calibration) and RRF50 (continuing calibration) in VOA/SVOA
analyses. Leave blank for volatile and semivolatile sample, blank, and
tune analysis.
H-27
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.9 Auxiliary Data Record (Type 32)
Use: Used to report retention time (in minutes) for Internal
Standards and for TICs (for Volatiles and Semivolatiles). Used
to report retention time data and percent breakdown (for
pesticides).
Position: Follows type 30. (Record will only be required as specified
above.)
MAXIMUM
LENGTH . CONTENTS
2 RECORD TYPE
3 Delimiters
2 RETENTION TIME LABEL
1 Delimiter
5 RETENTION TIME
1 Delimiter
3 FIRST LIMIT LABEL
1 Delimiter
5 RT WINDOW LOWER LIMIT
1 Delimiter
3 SECOND LIMIT LABEL
1 Delimiter
5 RT WINDOW UPPER LIMIT
2 Delimiters
2 % BREAKDOWN LABEL
1 Delimiter
5 % BREAKDOWN
FORMAT/CONTENTS
"32"
Ml
"RT"
I
Numeric
I
"RTF"
I
Numeric
I
"RTT"
I
Numeric
II
"PB" for % breakdown/blank (for
VOA and SV)
I
Numeric (DDT/ENDRIN)/blank (for
VOA and SV)
1 Delimiter
5 COMBINED % BREAKDOWN
2 Delimiters
1 PEAK
1 Delimiter
5 RECORD SEQUENCE NO.
4 CHECKSUM
Numeric/blank (for VOA and SV)1
II
1 THROUGH 5 (for pesticide
multicomponent compounds)/blank
(for VOA and SV)2 .
I
Numeric
Character
The combined %breakdown will be reported on both the record type 32s
(for DDT and Endrin).
For positively identified compounds, a minimum of 3 peaks and a maximum
of 5 peaks are allowed. Types 30 and 32 will be repeated for each peak
that is reported (a minimum of three, a maximum of five times). This is
for multicomponent analytes in pesticide analyses.
H-28
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.10 Name Record (Type 33)
Use: This record type is used for volatile and semivolatile
analyses only to carry an analyte name for TICs. This record
is not used for pesticide analysis.
Position: Follows types 30 and 32 for TICs.
CONTENTS FORMAT/CONTENTS
RECORD TYPE "33"
Delimiter |
NAME OF COMPOUND Character
Delimiter |
RECORD SEQUENCE NO. Numeric
CHECKSUM Character
H--29 OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.11 Instrumental Data Readout Record (Type 36}
Use: This record type is only used for volatile and semivolatile
analyses to describe DFTPP/BFB percent abundances. This
record is not used for pesticide analysis.
Position: Follows type 30 for DFTPP/BFB data.
MAXIMUM
LENGTH CONTENTS
2 RECORD TYPE
1 Delimiter
1 MASS LABEL
3 Delimiters
3 FIRST MASS (DFTPP/BFB)
2 Delimiters
5 FIRST PERCENT RELATIVE
ABUNDANCE
1 Delimiter
3 SECOND MASS
1 Delimiter
5 SECOND PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 69
1 Delimiter
3 THIRD MASS
1 Delimiter
5 THIRD PERCENT RELATIVE
ABUNDANCE
2 Delimiters
3 FOURTH MASS
1 Delimiter
5 FOURTH PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 69
1 Delimiter
3 FIFTH MASS
1 Delimiter
5 FIFTH PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 174
1 Delimiter
3 SIXTH MASS
1 Delimiter
FORMAT/CONTENTS
"36"
I
"M"
III ,
Numeric (DFTPP for SV or BFB for VGA)
II
Numeri'c
I
Numeric
I
Numeric
I
Numeric, DFTPP only/blank (for VOA)
I
Numeric
I
Numeric
II .'
Numeric
I
Numeric
I
Numeric, DFTPP only/blank (for VOA)
Numeric
I
Numeric
I
Numeric, BFB only/blank (for SV)
Numeric
H--30
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Instrumental Data Readout Record (Type 36) (Cont.)
MAXIMUM
LENGTH CONTENTS
5 SIXTH PERCENT RELATIVE
ABUNDANCE
2 Delimiters
3 SEVENTH MASS
1 Delimiter
5 SEVENTH PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 174
1 Delimiter
3 EIGHTH MASS
1 Delimiter
5 EIGHTH PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 174
1 Delimiter
3 NINTH MASS
1 Delimiter
5 NINTH PERCENT RELATIVE
ABUNDANCE
1 Delimiter
5 PERCENT MASS OF 176
1 Delimiter
3 TENTH MASS
1 Delimiter
5 TENTH PERCENT RELATIVE
ABUNDANCE
2 Delimiters
3 ELEVENTH MASS
1 Delimiter
5 ELEVENTH PERCENT
RELATIVE ABUNDANCE
2 Delimiters
3 TWELFTH MASS
1 Delimiter
'5 TWELFTH PERCENT RELATIVE
ABUNDANCE
2 Delimiters
3 THIRTEENTH MASS
2 Delimiters
FORMAT/CONTENTS
Numeric
Numeric
Numeric
I "
Numeric, BFB only/blank (for SV)
I
Numeric
I
Numeric
I
Numeric, BFB only/blank (for SV)
I
Numeric
I
Numeric
Numeric, BFB only/blank (for SV)
I
Numeric/blank (for VOA)
I
Numeric/blank (for VOA)
II
Numeric/blank (for VOA)
Numeric/blank (for VOA)
II
Numeric/blank (for VOA)
I
Numeric/blank (for VOA)
Numeric/blank (for VOA)
II
H-31
OLM04.2
-------
Exhibit H -- Section 9
Record Listing
Instrumental Data Readout Record (Type 36) (Cont.)
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
5 THIRTEENTH PERCENT Numeric/blank (for VOA)
RELATIVE ABUNDANCE
1 Delimiter |
5 PERCENT MASS OF 442 Numeric, DFTPP only (blank for VOA)
1 Delimiter |
5 RECORD SEQUENCE NO. Numeric
4 CHECKSUM Character
H-32 . OLM04.2
-------
Exhibit H -- Section 9
Record Listing
9.12 Comment Record (Type 90)
Use: To provide for operator-entered comments.
Position: May occur anywhere in the file after the type 10 record.
MAXIMUM
LENGTH CONTENTS FORMAT/CONTENTS
2 RECORD TYPE "90"
1 Delimiter |
67 ANY COMMENT Character
1 Delimiter |
5 RECORD SEQUENCE NO. Numeric
4 CHECKSUM Character
-H-33 OLM04.-2
-------
Exhibit H -- Section 10
Definitions of Various Codes
10.0 DEFINITIONS OF VARIOUS CODES USED IN AGENCY STANDARD RECORDS
10.1 Quality Control and Related Codes (QCC) in Type 20 Records
10.1.1 Note: These codes appear in the QC code fields of type 20 records.
They are. used to indicate the type of data that is being reported.
QCC Name
LRB LABORATORY (REAGENT)
BLANK
LIB LABORATORY INSTRUMENT
BLANK
LSB LABORATORY SULFUR BLANK
LHB LABORATORY STORAGE BLANK
FRB FIELD BLANK
FRM FIELD REFERENCE SAMPLE
Definition
The "Method Blank" (see Exhibit G).
The "Instrument Blank".
If different from "Method Blank"
(pesticides).
The storage blank (volatiles).
This is any sample that is submitted
from the field and is identified as
a blank. This includes trip blanks,
rinsates, equipment blanks, etc.
This is any sample that is submitted
for a Case and is identified as a
Performance Evaluation (PE) sample.
An 'environmental sample which is
analyzed according to the analytical
method, and subsequently used for
the matrix spike and the matrix
spike duplicate (see Exhibit G).
The "Matrix Spike" (see Exhibit G);
must precede LF2.
The "Matrix Spike Duplicate" (see
Exhibit G).
LSD LABORATORY SPIKE
DUPLICATE BACKGROUND
(ORIGINAL) VALUES
LF1 LABORATORY SPIKED SAMPLE
- FINAL - FIRST MEMBER
LF2 LABORATORY SPIKED SAMPLE
- FINAL - SECOND MEMBER
LPC LABORATORY PERFORMANCE
CHECK SOLUTION
A solution of DFTPP (SVGA) or BFB
(VGA) or method analytes (PEST/PCB)
used to evaluate the performance of
an instrument with respect to a
defined set of criteria (Tune or
Resolution Check Sample) (see
Exhibit G).
FLO FLORISIL CHECK SOLUTION
A solution of pesticides used to
check recovery from each lot of
Florisil cartridges. These recovery
results will be provided in every
production run where associated
samples are analyzed.
H-34
OLM04.2
-------
Exhibit H -- Section 10
Definitions of Various Codes
GPC GPC CHECK SOLUTION
A solution of pesticides used to
check recovery from each new GPC
calibration. These recovery results
will be provided in every production
run where associated samples are
CLM INITIAL CALIBRATION -
MULTI-POINT
CLS INITIAL CALIBRATION
SINGLE POINT
CLC CONTINUING CALIBRATION
CHECK
CLE CONTINUING PERFORMANCE
CHECK
10.1.2
The Initial Calibration for GC/MS
(see Exhibit G), or the Initial
Individual Standard Mixes (A, B) for
pesticides (see Exhibit D PEST).
Response factors (GC/MS) or
Calibration Factors (pesticides)
will be reported on the following
type 30 records.
The Initial Toxaphene/Aroclor Mixes
used to determine all calibration
factors (see Exhibit D PEST).
The continuing calibration
(VSTDOSO/SSTD050) for GC/MS.
The subsequent Individual Standard
Mixes (A,B), Performance Evaluation
Mixture, and for subsequent
injections of Toxaphene/Aroclor
mixes for pesticides (see Exhibit D
PEST).
A calibration solution as above used
both as an initial calibration (CLM)
and a continuing check (CLC). (50
level initial calibration if needed
for Form 8.)
The following QCC values are used on type 20 records which act as a
header, and indicate that additional (usually calculated) analyte
specific data will be present on type 30 (and following' type)
records. Usually, these data will apply to an entire production run,
in which case they will appear immediately following the type 10
record or type 11 record if present. If the data apply to only a
portion of the samples in the run, they shall be placed immediately
preceding the samples to which they apply. Much of the rest of the
information in the type 20 record may be blank, indicating that these
data do not apply to these results.
CLD DUAL PURPOSE CALIBRATION
MNC MEAN VALUES FROM
CALIBRATIONS
The data following represent mean
values and percent RSDs from the
initial calibration (GC/MS) or the
mean calibration factors, mean
retention times and retention time
windows (pesticides).
H-35
OLM04.2
-------
Exhibit H -- Section 10
Definitions of Various Codes
10.2 Codes For Sample Medium (Matrix, Sources)
Medium Code
All Media, Specific Medium not Applicable. 0 (zero)
Use for Calibrations, Tunes, etc.
Water 1
Soil H
10.3 List of Sample and Result Qualifiers
Definition: A sample qualifier consists of three characters which act
as an indicator of the fact and the reason that the subject analysis (a)
did not produce a numeric result, or (b) produced a numeric result for
an entire sample but it is qualified in some respect relating to the
type or validity of the result.
10.3.1 Sample Qualifiers
Oualifier Full Name Definition
RIN RE-ANALYZED The indicated analysis results were
generated from a re-injection of the same
sample extract or aliquot (RE SUFFIX).
REX RE-PREPARED The indicated analysis results were
generated from a re-extraction of the same
sample (RE SUFFIX).
REJ REJECTED The results for the entire sample analysis
have been rejected for an unspecified
reason by the laboratory. For initial
calibration data, these data were not
utilized in the calculation of the mean.
SRN DILUTED The indicated analysis results were
generated from a dilution of the same
sample (DL SUFFIX).
10.3.2 Result Qualifiers in Type 30 Records
A result qualifier consists of three characters which act as an
indicator of the fact and the reason that the subject analysis (a)
did not produce a numeric result, or (b) produced a numeric result
for a single analyte but it is qualified in some respect relating to
the type or validity of the result. This qualifier is complementary
to the flags field on a type 30 record. A TIC must have either a
TIE, TFB, ALC, or PRE result qualifier.
BDL ' BELOW DETECTABLE Indicates compound was analyzed for but
LIMITS not detected (Form 1 "U" Flag).
NAR NO ANALYSIS RESULT There is no analysis result required
for this subject parameter.
H-36 OLM04.2
-------
Exhibit H -- Section 10
Definitions of Various Codes
AVG AVERAGE VALUE
CBC CANNOT BE CALCULATED
LTL LESS THAN LOWER
CALIBRATION LIMIT
GTL GREATER THAN UPPER
CALIBRATION LIMIT
LLS LESS THAN LOWER
STANDARD
TIE TENTATIVELY IDENTIFIED
ESTIMATED VALUE
REJ REJECTED
STD INTERNAL STANDARD
STB INTERNAL STANDARD
BELOW DETECTION LIMITS
FBK FOUND IN BLANK
TFB TENTATIVELY IDENTIFIED
| AND FOUND IN BLANK
ALC ALDOL CONDENSATION
NRP NON-REPRODUCIBLE
PRE PRESUMPTIVE PRESENCE
Average value -- used to report a range
of values (e.g., relative response
factors).
The analysis result cannot be
calculated because an operand value is
.qualified (e.g., identifies analytes
whose internal standard is not found)
(Form 1 "X" Flag).
Analysis result is from a diluted
sample (DL suffix) and may be less
accurate than the result from an
undiluted sample (Form 1 "D" Flag).
Actual value is known to be greater
than the upper calibration range (Form
1 "E" Flag).
The analysis result is less than the
sample guantitation limit (Form 1 "J"
Flag).
The indicated analyte is a tentatively
identified analyte; its concentration
has been'estimated (Form 1-F.or 1-G
"J" Flag).
Results for the analyte are rejected by
the laboratory.
The indicated compound is an internal
standard.
A combination of "STD" and "BDL".
The indicated compound was found in the
associated method blank (LRB) as well
as the sample (Form 1 "B" Flag).
A Combination of "TIE" and "FBK" (Form
1-F or 1-G "B" Flag).
Labels a suspected Aldol Condensation-
product for TICs (Form 1-G "A" Flag).
Results of two or more injections are
not comparable (Form l-£ "P" flag),
e.g., Aroclor target analyte with
greater than 25% difference between
mean concentrations of the two column
analyses.
Presumptive evidence of presence of
material for TIC (Form 1-F or 1-G "N"
Flag).
H-37
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
APPENDIX A -- FORMAT OF RECORDS FOR SPECIFIC USES
The USEPA does not warrant or guarantee the completeness and/or accuracy of the
representative examples of record type uses provided in this appendix. This
appendix serves as an example for the usage of record types and in no way
redefines or supersedes the specifications or requirements stated in Exhibits A
through H of OLM04.2. NOTE: Examples are representative and are not typically
provided for both columns used in the pesticide analysis.
H-38 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
Appendix A -- Format of Records for Specific Uses
Table of Contents
Section ' Page
1.0 VOLATILES 42
1.1 Record Type '10 for Volatiles 42
1.2 Record Type 11 for Volatiles 42
1.3 Record Type 20s and 30s for Volatiles --
Initial Calibration Mean Values (QC Code 'MNC') 42
1.4 Record Type 20s and 30s for Volatiles --
BFB Tune (QC Code 'LPC') 42
1.5 Record Type 20s and 30s for Volatiles --
Initial Calibration Standard (QC Code 'CLM') 42
1.6 Record Type 20s and 30s for Volatiles --
Dual Purpose Calibration Standard (QC Code 'CLD') 43
1.7 Record Type 20s and 30s for Volatiles --
Continuing Calibration Standard (QC Code 'CLC') 43
1.8 Record Type 20s and 30s for Volatiles --
Method Blank (QC Code 'LRB') 44
1.9 Record Type 20s and 30s for Volatiles --
Storage Blank (QC Code 'LHB') 45
1.10 Record Type 20s and 30s for Volatiles --
Instrument Blank (QC Code 'LIB') 46
1.11 Record Type 20s and 30s for Volatiles --
Regular Field Sample (QC Code field is blank) 47
1.12 Record Type 20s and 30s for Volatiles --
Field Sample chosen for MS/MSD (QC Code 'LSD') ... 48
1.13 Record Type 20s and 30s for Volatiles --
Matrix Spike Sample (QC Code 'LF1') 48
1.14 Record Type 20s and 30s for Volatiles --
Matrix Spike Duplicate Sample (QC Code 'LF2') 50
2.0 SEMIVOLATILES 52
2.1 Record Type 10 for Semivolatiles 52
2.2 Record Type 11 for Semivolatiles 52
2.3 Record Type 20s and 30s for Semivolatiles --
Initial Calibration Mean Values (QC Code 'MNC1) 52
2.4 Record Type 20s and 30s for Semivolatiles --
DFTPP Tune (QC Code 'LPC') 52
2.5 Record Type 20s and 30s for Semivolatiles --
Initial Calibration Standard (QC Code 'CLM') 52
2.6 Record Type 20s and 30s for Semivolatiles --
Dual Purpose Calibration Standard (QC Code 'CLD') 53
2.7 Record Type 20s and 30s for Semivolatiles --
Continuing Calibration Standard (QC Code 'CLC1) . . ... . . . .54
2.8 Record Type 20s and 30s for Semivolatiles --
Method Blank (QC Code 'LRB') 55
2.9 Record Type 20s and 30s for Semivolatiles --
Regular Field Sample (QC Code field is blank) 56
2.10 Record Type 20s and 30s for Semivolatiles --
Field Sample Chosen for MS/MSD (QC Code 'LSD') 57
H-39 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
2.11 Record Type 20s and 30s for Semivolatiles --
Matrix Spike Sample (QC Code 'LF1') 58
2.12 Record Type 20s and 30s for Semivolatiles --
Matrix Spike Duplicate Sample (QC Code 'LF2') 59
3.0 PESTICIDES (COL. 1) 62
3.1 Record Type 10 for Pesticides (Col 1) 62
3.2 Record Type 11 for Pesticides (Col 1) 62
3.3 Record Type 20s and 30s for Pesticides (Col 1) --
Initial Calibration Mean Values (QC Code 'MNC') ........ 62
3.4 Record Type 20s and 30s for Pesticides (Col 1) --
Florisil Cartridge Check Recovery Values (QC Code 'FLO') ... 63
3.5 Record Type 20s and 30s for Pesticides (Col 1) --
GPC Recovery Values (QC Code 'GPC1.) . . 64
3.6 Record Type 20s and 30s for Pesticides (Col 1) --
Resolution Check Standard (QC Code 'LPC') 64
3.7 Record Type 20s and 30s for Pesticides (Col 1) --
Performance Evaluation Mixture (QC Code 'CLE') 65
3.8 Record Type 20s and 30s for Pesticides (Col 1) --
. Initial Calibration Multicomponent Standard (QC Code 'CLS') . . 66
3.9 Record Type 20s and 30s for Pesticides (Col 1) --
Initial Calibration Single Component --
Individual Standard A (QC Code 'CLM') 67
3.10 Record Type 20s and 30s for Pesticides (Col 1) --
Initial Calibration Single Component --
Individual Standard Mix B (QC Code 'CLM') 68
3.11 Record Type 20s and 30s for Pesticides (Col 1) --
Instrument Blank (QC Code 'LIB') 69
3.12 Record Type 20s and 30s for Pesticides (Col 1) --
Method Blank (QC Code 'LRB') 70
3.13 Record Type 20s and 30s for Pesticides (Col 1) --
Matrix Spike Sample (QC Code 'LF1') 70
3.14 Record Type 20s and 30s for Pesticides (Col 1) --
Matrix Spike Duplicate Sample (QC Code 'LF2') 71
3.15 Record Type 20s and 30s for Pesticides (Col 1) --'
Continuing Performance Check --
Individual Standard Mix A (QC Code 'CLE') 73
3.16 Record Type 20s and 30s for Pesticides (Col 1) --
Continuing Performance Check --
Individual Standard Mix B (QC Code 'CLE') 73
3.17 Record Type 20s and 30s for Pesticides (Col 1) --
Continuing Performance Check --
Performance Evaluation Mixture (QC Code 'CLE') c 74
3.18 Record Type 20s and 30s for Pesticides (Col 1) --
Field Sample chosen for MS/MSD (QC Code 'LSD') 75
4.0 PESTICIDES (COL. 2) . 77
4.1 Record Type 10 for Pesticides (Col 2) 77
4.2 Record Type 11 for Pesticides (Col 2) 77
4.3 Record Type 20s and 30s for Pesticides (Col 2) --
Initial Calibration Mean Values (QC Code 'MNC') 77
4.4 Record Type 20s and 30s for Pesticides (Col 2) --
Resolution Check Standard (QC Code 'LPC') 78
H-40 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
4.5 Record Type 20s and 30s for,Pesticides (Col 2) --
Performance Evaluation Mixture (QC Code 'CLE') 79
4.6 Record Type 20s and 30s for Pesticides (Col 2) --
Initial Calibration Multicomponent Standard (QC Code 'CLS') . . 80
4.7 Record Type 20s and 30s for Pesticides (Col 2) --
Initial Calibration Single Component --
Individual Standard A (QC Code 'CLM') .80
4.8 Record Type 20s and 30s for Pesticides (Col 2) --
Instrument Blank (QC Code 'LIB') 82
4.9 Record Type 20s and 30s for Pesticides (Col 2) --
Method Blank (QC Code 'LRB') 82
4.10 Record Type 20s and 30s for Pesticides --
Matrix Spike Sample (QC Code 'LF1') 83
4.11 Record Type 20s and 30s for Pesticides --
Matrix Spike Duplicate Sample (QC Code 'LF2') 84
4.12 Record Type 20s and 30s for Pesticides (Col 2) --
72 Hours Aroclor Standard (QC .Code 'CLE') 86
4.13 Record Type 20s and 30s for Pesticides (Col 2) --
Field Sample chosen for MS/MSD (QC Code 'LSD') 86
5.0 TYPE 90 -- COMMENTS RECORD 88
H-41 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
1.0 VOLATILES
1.1 Record Type 10 for Volatiles
10||||||GC/MS|OLM04.2V\ \TESLAB||||68D00001|INSTV1||TEST LABS
INC.||000012C33
1.2 Record Type 11 for Volatiles
11|DB-5| |0.53| | | | | | | | | | |000024CD9
1.3 Record Type 20s and 30s for Volatiles -- Initial Calibration Mean Values
(QC Code 'MNC')
20|||0|MNC||18000|X1201|||||||||36|||000036668
30|C|74873|||AVG|0.53l||||||R|17.0||||||||||||||0000486BE
30|C|74839|||AVG|l.536||||||R|11.1||||||||||||||00005A717
1.4 Record Type 20s and 30s for Volatiles -- BFB Tune (QC Code 'LPC')
20|||0|LPC||18000|X1201|1532|04|25|01|01||||l|||0004011E3
21|N||||||BFB01|||||| MM |0004121B2
30|C|460004||||||||||||||||||||MII|00042388C
36|M| | |50| 118.8|75|45.5| |95|100.0| |96|7.2| 1173|0.0|0.01174|72.8| 1175 J5.7
|7.8|176|71.6|98.3|177|4.9|6.8|MM M M M M|000439122
1.5 Record Type 20s and 30s for Volatiles -- Initial Calibration Standard (QC
Code 'CLM')
20 | | VSTD020|0|CLM| 118000|X120111992103|25|09|42| M I36M |00044B8F2
2i|N|| M IISTDOIJ M M M M I|ooo45C944
23 I P I 1992 |.04 | 25 | 011 011 BFB01 M M M M M M M M M M M M M 00046EA64
30 I C| 74873 I 74975 I | |0.563| M M M M M M M M M I | 000470F21
H-42 OLM04.2
-------
1.6
1.7
30 IC|74839 I 74975 I | 11.528|
Exhibit H -- Appendix A
Format of Records for Specific Uses
I0004833E2
Record Type 20s and 30s for Volatiles -- Dual Purpose Calibration Standard
(QC Code 'CLD')
20||VSTD050|0|CLD||18000|X1201|1992\05|25|10|25||||39|| J0014300AA
. 21|N||||||CSTD01|||||||||||00144117D
23|P|15S2|05|30|05|01|BFB02|| | | | | | | I 1 | | | | I ! M I I I ! 1 I I I0014532A2
30|C|74873|74975|||0.931|||||||||||||||||||||001465B66
30|C|74839|74975| | |l.82l| | | | | I I I I I I I I I I I I I I I I00147842C
30|C|17060070|74975| | |2.089|
| 001810B47
30|C|3114554| | | STD | | |A|50.0| || I I I I I I I I I I I I 1 1 1 109281 j 001822EDB
32| | |RT|15.74| | | | | | | | | | | 001833EF5
30 | C| 5403 63 | | | STD | | | A| 50 . 0 | | | | | | | | . | | | |
32| | |RT|9.97| | | | | | | | | | (0018570D13
30 | C| 74975 | | | STD | | | A| 50 . 0 | | | | | | | | | | | |
32 | | |RT|8.00| | | | | | | | | | |00187A10C
1 125103 00184618CB
| I | 26084 | 0018691EDC
Record Type 20s and 30s for Volatiles -- Continuing Calibration Standard
(QC Code 'CLC1 )
20| |VSTD050|0|CLC| 1 18000 |X1201 1 1992 \ 05 | 30 | 05 | 25 | |.| |39| |.|0024300AD
2l|N| | | | | JCSTDOI) | | | | | | | | | |00244117F
H-43
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
23|P|1S52|05|30|05|01|BFB02| | || I I I
30 |C| 74873 | 74975 | | |0.96l| | | | | | | | | |
30 | C| 74839 | 74975 | | |l.803| | | | | | | | | |
1.8
I I M I I I I! I I I |0024532A1
| F| 81 . 0 | | | 002465B65
| F| 17 . 4 | | |00247842A
I I I I I I I I I |F|l0.6| | |002810B46
| I I I I I I I 1 1 1 109281 1 002822EDA
| I | 125103 | 00284618C
30|C|17060070|74975| | |2.089| | | | || I
30|C|3114554| | |STD| | |A|50.0| | | | | | |
32 | | |RT| 15. 74) | | | | | | | | | |002833EF3
30 | C| 540363 | | |STD| | | A| 50 . 0 | | | | | | | |
'
32| | |RT|9.97| | | | | | | | | | |0028570D1
30|C|74975| | | STD | | |A|50.0| | | | | | | | | || I I I I 1 1 1 26084 | 0028691ED
32| | |RT|8.00| | M I I I I I I |00287A10D
Record Type 20s and 30s for Volatiles -- Method Blank (QC Code 'LRB')
20| |VBLK01|1|LRB| | 18000 |X1201 | 1992\ 05 | 30 | 06 | 11 | |ML|5.0|39| | | 00288CB9F
2l|N|L| | | | |FBLK01| | | I I I I I I I | 00289DCF6
22|l$52|05|30|05|25|CSTDOl| | | | |l.0| | | |00290F6D3
23|P|l552|05|30|05|Ol|BFB02| | | | | | | || | | I I I I I I I p I ° I T I ° I I I I | 002911B17
30 | C| 74873 | 74575 | UG/L | BDL | |u| | |u| 10 | | | | | | | | | | | | | | | | 002923881
30|C|74839| 74575 1 UG/L | BDL | |u| | |U|lO| | | | | | I I I I I I I I I I 0029355ED
30 | C| 2037265 | 3114554 | UG/L| | 47 . 9 | | A| 50 . 0 |
30|C|460004|3114554|UG/L| | 47 . 0 | | A| 50 . 0 | |
| | S | 96 |
S 94
| | 003251E4B
0032647E1
H-44
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|17060070|74975|UG/L| | 50 . 3 | | A| 50 . 0 | | | | | | | |.| |S|lOl| | | | | | | 003277241
30|C|3114554| | | STD | | |A|50.0| | | | | | | | | | | | | | | | I | 104439 | 0032895DF
32 | | | RT | 15. 70 | | | | | | | | | | |00329A5EA
30 | C| 540363 | | | STD | | | A| 50 . 0 | | | | | | | | | | | | | | | | I | 135938 | 00330C8A8
32| | |RT|9.92| | | | | | | | | | | 00331D7DE
30|C|74975| | | STD | | |A|50.0| | | | | | | | || II I I I | 1 1 26488 | 00332F90C
32| | |RT|8.00| | | | | | | | | | |00333082C
1.9 Record Type 20s and 30s for Volatiles -- Storage Blank (QC Code 'LHB')
20 | |VHBLKOl|l|LHB| | 18000 |X1201 | 1592 | 05 | 30 | 06 | 21 | |ML|5.0|39| | | 00688CB9F
2i|N|L| 1 1 1 IFHBLKOI) || M 1 1 I I I |oo689DCF6
22 | 1992 | 05 | 30 | 05 | 25 | CSTD01 1 | | | | 1 . 0 | | | | 00690F6D3
23 | P| 1952 | 05 | 30 | 05 | 01 | BFB02 | | | | | | | | | | |MB | 1992 | 05 | 30 | 06 | 11 | FBLK01 | P | 0 | T | 0
| | | | |006911B17
30 | C| 74873 | 74975 |UG/L |BDL | |U| | |u| 10 | | | | | | | | | | | | | | | | 006923881
30|C|74839| 74975|UG/L | BDL | |u| | |u|lO| || I I I II I I I I I I I I 0069355ED
30|C|2037265|3114554|UG/L| |47.9| |A|50.0| | || | I I I I IS|96| | | | I I I007251E4B
30|C|460004|3114554|UG/L| | 47 . 0 | |A|50.0| | | | | | | | | |S|94| | | | | | |0072647E1
30|C|17060070|74975|UG/L| |50 .3 | |A|50.0| | | | | | | | | |S1101| | | | | | |007277241
30|C|3114554| | |STD| | |A|50.0| | | | | I I I I I I I I I I 111104439|0072895DF
32|||RT|15.70|||||||||||00729A5EA
30|C|540363|||STD|||A|50.0||||||||||||||||I|135938|00730C8A8
32|||RT|9.92|||||||||||00731D7DE
H-45 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|74975| | |STD| | |A|50.0| || I Ij I I I M I I M 11|26488|00732F90C
32|||RT|8.00|||||||||||00733082C
1.10 Record Type 20s and 30s for Volatiles -- Instrument Blank (QC Code 'LIB')
20||VIBLKOl|l|LIB||18000|X1201|1992\05|30|06|30||ML|5.0|39|||00688CB9F
21|N|L| | | | |FIBLK01| | | I I I I I I I |00689DCF6
22|1992|05|30|05|25|CSTD01| | | | |l.0| | | |00690F6D3
23|P|1992|05|30|05|01|BFB02| | | | || I I I I I MB\1992\05|30|061111FBLK01|P|0|T|0
I I I I I006911B17
30|C|74873|74975|UG/L|BDL||u|||u|lO|||||||||||||||
30|C|74839|74975|UG/L|BDL||u|||u|10||||||||||||||||0069355ED
30|C|2037265|3114554|UG/L||47.9||A|50.0||||||||||S|96|||||||007251E4B
30|C|460004|3114554|UG/L||47.0||A|50.0||||||||||S|94|||||||0072647E1
30|C|17060070|74975|UG/L| |50.3| |A|50.0| || | I I I I I ls|!0l| I I I I I |007277241
30|C|3114554| | |STD| | |A|50.0| | || I I I I I I I I I I I 111104439|0072895DF
32 | | |RT|15.70| | | | | | | | |,| |00729A5EA
30|C|540363| | |STD| | |A|50.0| | | I I I I I I I I I I I I 111135938|00730C8A8
32|||RT|9.92|||||||||||00731D7DE
30|C|74975| | |STD| | |A|50.0| | | | | | || I I I I I I I 11126488|00732F90C
32| | |RT.|8.00| | | | | | | | | | |00733082C
H-:46 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
1.11 Record Type 20s and 30s for Volatiles -- Regular Field Sample (QC Code
field is blank)
20| |X1200|l| | |18000|X1201|1992|05|30|06|37| |ML|5.0|39| | | 0033432DB
21 |N | L | | | | |FX1200| | | | 1 1592 | 05 | 27 I | | |003354C2D
22 | 1992 | 05 | 30 | 05 | 25 | CSTD01 | | | | |l.0| | | |00336660A
23|P|1992|05|30|05|01|BFB02|HB|1992|05|30|06|21|FHBLK01| | | |MB | 1992 | 05 | 30
|06|ll|FBLKOl|P|0|T|2| | | | 0 | 003379931
30 | C| 74873 | 74975 |UG/L |BDL | |U| | |U| 10 |
30|C|74839| 74975 |UG/L| BDL | |U| | |U| 10 |
J00338B69B
00339D407
30|C|2037265|3114554|UG/L| | 51 . 8 | | A| 50 . 0
30|C|460004|3114554|UG/L| |59.0| |A|50.0|
30|C|17060070|74975|UG/L| | 54 . 3 | |A|50.0|
30|C|3114554| | | STD | | |A|50.0| | | | | | I I I I I I
32| | |RT|15.66| | | | | | | | | | [00275277B
30 |C| 540363 | | | STD | | | A| 50 . 0 | | | | | | | | | | | | |
32| | |RT|9.91| | | | | | | | | | [002775948
30 |C | 74975] | | STD | | | A| 50 . 0 | | |'| | | | | | | | | | |
32| | |RT|7.96| | | | | | | | | | J00279898B
30|C| | |UG/L|TIE|9| | | | | | | | | | | | | | | | | || I |002807A4A
| | S | 102 |
|S|98| | |
|S|l07| |
| | | 00271A07D
|00272CA19
| | 00273F48C
I 96179 002741762
| I | 123502 | 002764A14
| 1 1 26331 1 002787A4A
32| | |RT|2.90|
|00281898B
33 | UNKNOm\ 00281898B
30|C|74630527| |UG/L | TIE 1 1 1 JN|
| 002827A4.A
H-47
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
32| | |RT|25.20| | | |.| | | | | | |00283898B
33|3-UNDECENE, 6-METHYL-, (E)-|00284898B
1.12 Record Type 20s and 30s for Volatiles -- Field Sample chosen for MS/MSD
(QC Code 'LSD1)
20| |X120l|l|LSD| 118000|X120111552|05|30|06|37 | |ML|5.0|39| | |0033432DB
21|N|L|||||FX1201LSD||||\1992\05\27\\\|003354C2D
22|1552|05|30|05|25|CSTD01|||||l.0||||00336660A
23|P|1552|05|30|05|01|BFB02|HB|1552|05|30|06|21|FHBLK01||||MB|1552|05|30
|06|11|FBLK01|P|0|T|0||||0|003379931
30|C|74873|74575|UG/L|BDL||u|||u|10||||||||||||||||00338B69B
30|C|74839|74575|UG/L|BDL||u|||u|10||||||||||||||||00339D407
30|C|2037265|3114554|UG/L||50.8||A|50.0||||||||||s|l02|||||||00371A07D
30|C|460004|3114554|UG/L| |49.0| |A|50.0| | || I I I I I |S|98| | | | | | |00372CA19
30|C|17060070|74975|UG/L| |53.3| |A|50.0| | | | | | I I I |S|l07| | | | | | |00373F48C
30|C|3114554.| | | STD | | |A|50.0| | | | | | I I I I I I I I II * I 96178 | 003741762
32|||RT|15.65|||||||||||00375277B
30|C|540363 | | |STD| | |A|50.0| | | | | | | | | | | | | | | 1111235011003764A14
32|||RT|9.90|||||||||||003775948
30|C|74975|||STD|||A|50.0||||||||||||||||I|26330|003787A4A
32|||RT|7.95|||||||||||00379898B
1.13 Record Type 20s and 30s for Volatiles -- Matrix Spike Sample (QC Code
1LF1')
20||X1201MS|1|LF1||18000|X1201|1992\05|30|07|14||ML|5.0|39|||00380B5C1
H-48 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
2l|N|L| | | | |FX1201LF1| | | | \1992\QS\21\ | | |00381CF38
22 | 1992 | 05 | 30 | 05 | 25 | CSTD01 | | | | |l.0| | | |00382E915
23 | P | 1992 | 05 | 30 | 05 | 01 1 BFB02 | HB | 1992 1 05 | 30 | 06 | 21 j'FHBLKOl | | | |MB 1 1992 1 05 | 30
|06|11|FBLK01|P|0| | |S|0|R|0|003831CEC
30|C|74873| 74 795 \ UG/L | BDL |
003843A56
30|C|75354|74975|UG/L||40||A|50.00|||||P|80||D|4|||||||||003911212
30|C|79016|540363|UG/L||46||A|50.00|||||P|92||D|4|||||||||004026477
30|C|71432|540363|UG/L||46||A|50.00|||||P|92||D|2|||||||||00405C84B
30|C|108883|3114554|UG/L||45||A|50.00|||||P|9l||D|6|||||||||00412ABC4
30|C|108907|3114554|UG/L||44||AJ50.00|||||P|88||D|7|||||||||00413D5FF
30|C|2037265|3114554|UG/L| |46.l| |A|50.0|
30|C|460004|3114554|UG/L| | 46 . 7 | | A| 50 . 0 | |
30 | C| 17060070 | 74975 | UG/L | | 54 .3 | | A| 50 . 0 | |
| | S | 92 | | | | | | |004175BA7
| S | 93 | | | | | | | 004188542
|S|l09| | | | | | J00419AFC2
30|C|3114554| | |STD| | |A|50.0|
32 |RT|15.70
00421E35B
30 |C| 540363 | | | STD | | | A| 50 . 0 | | | | | | |
32| | |RT|9.92| | | | | | | | | | |004231549
30|C|74975| | | STD | | |A|50.0| | | | | | | |
32| | |RT|7.98| | | | | | | | | | |00425459B
I I I I I I 1 1 1 101076 | 00420D350
| I | 125573 | 004220613
26701 004243657
H-49
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
1.14 Record Type 20s and 30s for Volatiles -- Matrix Spike Duplicate Sample (QC
Code ' LF2 ' )
20| |X1201MSD|l|LF2| | 18000 |X1201 | 1992 \ 05 | 30 | 07 | 55 | |MLJ5.0|39| | | 00426726B
2l|N|L| | | | |FX1201LF2 | | | | \1992\ 05 |27| | | J004278BE3
22 | 1992 | 05 | 30 | 05 | 25 | CSTD01
l.0 00428A5CO
23 | P | 1992 1 05 | 3 0 | 05 | 01 | BFB02 | HB 1 1952 1 05 | 30 | 06 | 21 1 FHBLK01 | | | | MB | 1992 1 05 | 3 0
|06|ll|FBLKOl|P|0| | |S|0|R|0|00429D997
30 | C| 74873 | 74975 |UG/L |BDL|
10 |
00430F701
30|C|75354|74975|UG/L||38||A|50.00|||||PJ|77|D|4||||
30|C|79016|540363|UG/L||44||A|50.00|||||P||88|D|4||j
30|C|71432|540363|UG/L||47||A|50.00|||||P||94|D|2|||
30|C|108883|3114554|UG/L||48||A|50.00|||||P||97|D|6|
30|C|108907|3114554|UG/L||47||A|50.00|||||P||94JD|7|
[00437CED4
||004482146
||004518527
||| J0045868B3
I I I I0045992EE
| |S|98| | | | | | |0046318AA
| S | 95 | | | | | | | 004644251
004656CBF
30|C|2037265|3114554|UG/L| |49.2| |A|50.0| | | | |
30 | C| 460004 | 3114554 | UG/L | | 47 . 6 | | A| 50 . 0 | | | | | |
30|C|17060070|74975|UG/L| | 55 . 2 | |A|50.0| | | | | |
30|C|3114554| | | STD | | |A|50.0| | || I I I I I I I I I I I | I 1 101145 | 00466904A
32| | |RT|15.70| | | | | | | | | | |00467A055
30 |C| 540363 | | | STD | | | A| 50 . 0 | | | | | | | | | | | | | | | 1 1 1 124184 | 00468C30A
H-50
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
32|||RT|9.94||||||||||(00469D24C
30|C|74975| | |STD| | |A|50.0| | | 1 | 1 | | | I II I I I |1126683|00470F36D
32RT7.980047102B1
H-51 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
2.0 SEMIVOLATILES
2.1 Record Type 10 for Semivolatiles
10||||||GC/MS|OLM04.2B\\TESLAB||||68D00001|INSTB1||TEST LABS
INC.||000002BA9
2.2 Record Type 11 for Semivolatiles
,ll|XRT-l||0.52||||||||||J000024C8D
2.3 ' Record Type 20s and 30s for Semivolatiles -- Initial Calibration Mean
Values (QC Code 'MNC')
20|||0|MNC||18000|X1201|||||||||72|||00003661C
30|C|108952|3855821||AVG|l.817||||||R|7.2||||||||||||||000048677
30|C|111444|3855821| |AVG|l.607| | | | | | R | 6 .2 | | | | | | | | | | | | | | 00005A6C4
30|C|95578|3855821||AVG|l.375||||||R|3.l||||||||||||||00006C650
30|C|93951736|3855821||AVG|l.22l|||MIRI5-3IIIIIIIIIIIIII000745BDE
30|C|2199691|3855821||AVG|0.91l||||||R|2.0||||||||||||||000757DOA
2.4 Record Type 20s and 30s for Semivolatiles -- DFTPP Tune (QC Code 'LPC')
20|||0|LPC||18000|X1201|1552|05|01|00|32||||l|||000769E6E
21|||||||DFTPP01|||||||||||00077AF43
30|C|5074715|||||||||||||||||||||||||0007BC71C
36|M| | | 511 |41.9|68 | 0.5 11.3|69|37.6| |70|0.0|0.01127|45.2| |l97|0.4| |l98|lO
0.0| 1199|8.0| |275|25.0| |365|3.69| |44l|l3.7| |442J99.l| |443| | 20.8|21.0|000
793554
2.5 Record Type 20s and 30s for Semivolatiles -- Initial Calibration Standard
(QC Code 'CLM')
20||SSTD080|0|CLM||18000|X1201|1992\05|01|02|01||||72|||00155B94D
21|||||||STD02|||||||||||00156C8F3
H-52 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
23 | P |1992|05|01100|32|DFTPP011 | | || I I I I I I I I I I I I I I I I I II I I00157EBBA
30|C|108952|3855821| | |l.853| | | | || I I I I I I I I I I I I I I I0015812F5 .-
30|C|11144438558211.599' | | | 001593A37
30|C|93951736|385582l| | |l.248J |A|40.000| | || I II II I I I I I I I I |00228C51D
30|C|2199691|3855821| | |0.928| |A|40.000| | | | | I I I I I I I I I II I (00229ED4C
2.6 Record Type 20s and 30s for Semivolatiles -- Dual Purpose Calibration
Standard (QC Code 'CLD')
20||SSTD050|0|CLD|| 18000|X120111992|05|01102|40||||72|||0045914F6
211 | | | | | |STD03| | | | | | | | | | |00460249D
23|P|1992|05|01|00|32|DFTPP01| || I I I I I I I I I I I I I I I I I I I I I I I 004614764
30|C|108952|3855821| | |l.462| | |l I I I I I I I II I I I I I I I |004623B3A
30|C|111444|3855821| | |l.233| || I I I M II I I I I I I M I I |00463664C
30|C|2199691|3855821| | |0.828| | | || I I I I I I I I I I I I M I I0053318FO
30|C|1146652| | |STD| | |A|20.0| | || I I I I I I I I I I I |I|58474|005343BC2
32|||RT|7.23|||||||||||005354AE6
30|C|15067262| | |STD| | |A|20.0| || I I I I I I I I I I I I |I|27242|005366E6F
32|||RT|9.17||||||||||(005377DA2
30|C|1517222| | |STD| | |AJ20.0| | || I I I I I I I I I I I 11|38472|00538A043
32| | |RT|10.82| | | M | I I M |00539B042
30|C|1520963| | | STD | | |Al200| | I I I I I I I I I I I I I 11118770|00540D2F2
H-53 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
32|||RT|17.95|||||||||||00541E310
30|C|171903.5| | |STD| | |A|20.0| | | | | | | | | | | I I I I II I 24292 | 0054205B2
32|||RT|14.22|||||||||||0054315AF
30|C|385582l| | |STD| | |A|20.0| | | | I I I I I I I I I I I 11 117522|00544385F
32|||RT|5.87|||||||||||00545479F
2.7 Record Type 20s and 30s for Semivolatiles -- Continuing Calibration
Standard (QC Code 'CLC')
20||SSTD050|0|CLC||18000|X1201|1992\06|01|11|30||||78|||00459DC7F
21|||||||CCSTD01|||||||||||00460ED24
23|P|lS32|06|Ol|ll|Ol|DFTPP02| | | | | | I | | | | | | | | I I | I I | | | | | [004610FEB
30|C|108952|3855821| | |l.462| | | | | | | | | | | I I I | I |F|l9.5| | [004623B3A
30C1114443855821|l.233F|23.300463664C
30|C|2199691|3855821| | |0.828| | || I I I I I I I I I I I I IFI9-1| I |0053318FO
30|C|1146652| | |STD| | |A|20.0| | | | | | || I I I I I I I |I|58474|005343BC2
32|||RT|7.23|||||||||||005354AE6
30|C|15067262| | |STD| | |A|20.0| | || I I I I I I I I I I I |1127242|005366E6F
32|||RT|9.17|||||||||||005377DA2
30|C|1517222| | |STD| | |A|20.0| | | | | | | | | | | | | | | |I | 38472|00538A043
32|||RT|10.82|||||||||||00539B042
30|C|1520963 | | |STD| | |A|20.0| | | | | | | | | | | | | | | 11118770|00540D2F2
32|||RT|17.95|||||||||||00541E310
30|C|1719035| | |STD| | |A|20.0| | | | | | | | | | | | | I I 11|24292|0054205B2
H-54 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
32 | | |RT|14.22| | | | | | | | | | |0054315AF
30|C|385582l| | | STD | | |A|20.0| | | | | | |
1 17522 | 00544385F
32| | |RT|5.87| | | | | | | | | | J00545479F
2.8 Record Type 20s and 30s for Semivolatiles -- Method Blank (QC Code 'LRB')
20| |SBLK32|l|LRB| | 18000 |X1201 | 1552| 06 | 01 | 12 | 10 | |ML|lOOO|78| | |005467308
21 1 |L| |C| | |FSBLK01|1952|03|30| | | | | |2.0| | 005478CBB
22 | 1552 | 06 | 01 | 11 | 30 | CCSTD01 | | | |lOOO|l.O| | | | 00548AA6D
23|P|l952|06|Ol|ll|Ol|DFTPP02| | | | | | | | | |
30 | C| 108952 | 3855821 1 UG/L | BDL| |u| | |u| 10 |
30 | C| 4165600 | 1520963 | UG/L | | 40 . 9 | | A| 50 . 0 | | |
30|C|321608|15067262|UG/L| |42.8| |A|50.0| | |
30|C|98904439|1719035|UG/L| | 52 . 0 | |A|50.0| |
30|C|4165622|3855821|UG/L| |67.2| |A|75.0| | |
30 |C| 367124 | 3855821 1 UG/L | | 61 . 7 | | A| 75 . 0 | | |
30|C|118796|15067262|UG/L| | 70 . 9 | |A|75.0| |
30|C|93951736|3855821|UG/L| |69.2| |A|75.0|
30|C|219969l|385582l|UG/L| |38.9| |A|50.0| |
30 | C| 1146652 | | | STD | | | A| 20 . 0 | | | | | | | | | | | | | |
32| | |RT|7.72|
|00623CF6A
30 C 15067262 STD A 20 . 0
|P|0|T|0| | | | | 00549D056
| | | | | 00550EE8E
S | 82 |
S 86
|S|l04|
S 90
S 82
S 95
| S | 92
S 78
006147181
| 006159BF9
| 00616C83A
| 00617F2D2
|006181C81
| 00619472C
0062072BF
| 006219D66
I 94564 00622C038
I 46152 00624F2FE
32| | |RT|9.65|
| 00625023E
H-55
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30 | C| 1517222 | | | STD | | | A| 20 . 0 |
2.9
32 | | RT | 11 . 32
0062734DF
30|C|1520963| | | STD | | |A|20.0| | | | | | |
32| | |RT|18.44| | | | | || I I I I 0062967B8
30|C|1719035| | |STD| | |A|20.0| | | | | | |
32 | | | RT | 14. 70 | | | | | | | | | | |006319A71
30|C|3855821| | | STD | | |A|20.0| | | | | | |
32.| | |RT|6.35| | || | | | | | | | 00633CC63
| I | 65936 | 0062624EE
| 35768 | 00628579F
43708 006308A67
1 29752 | 00632BD33
Record Type 20s and 30s for Semivolatiles -- Regular Field Sample (QC Code
field is blank)
20| |X120l|l| | |18000|X1201|15S2|06|01|12|20| | ML 1 1000 | 78 | | | 00434F7E4
21| |L| |C| | |FX1201|1SS>2|05|30| \1992\05\27\ \2.0\ | 0043518E4
22 | 1992 | 06 | 01 | 11 | 30 |CCSTD01 | | | |lOOO|l.O| | | |004363696
23 | P | 1992 1 06 | 01 1 11 | 01 1 DFTPP02 | | | I I I I I I I I MB I 1992 | 04 | 01 1 15 1 14 | FSBLK01 1 P | 0 |
T|0| | | |0|004376C26
30 | C| 108952 | 3855821 |UG/L|BDL| |U| | |U|10|
004388A5E
30|C|4165600|1520963|UG/L| | 43 . 0 | | A| 50 . 0 | |
30 | C| 321608 | 15067262 | UG/L| | 48 . 3 | | A| 50 . 0 | |
30|C|98904439|1719035|UG/L| |51.8| |A|50.0|
30 | C| 4165622 | 3855821 | UG/L| | 69 . 8 | | A| 75 . 0 | |
30 |C| 367124)3855821 | UG/L | | 69 . 6 | | A| 75 . 0 | | |
30|C|118796|15067262|UG/L| |79.5| |A|75.0| |
H-56
| S 86
| S | 97 |
I I I I I |S|l04|
S 93
| S | 93 |
|S|l06|
005020B12
00503358D
0050461DF
005058C8C
| 00506B64E
| 00507E1D3
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30 |C| 93951736 | 3855821 |UG/L| | 73 . 0 | | A| 75 . 0 |
30|C|219969l|385582l|UG/L| |45.6| |A|50.0| |
30|C|385582l| | | STD | | |A|20.0| | | | | | | | | | | | | |
32| | |RT|6.38| | | | | | | | | | |0051169E8
30|C|1146652| | | STD | | |A|20.0| | | || | | | | | | ||
32| | |RT|7.75| | | | | | | | | | |005139BCF
30|C|15067262| | | STD | | |A|20.0| | | | | | | | | | | |
| S | 97 |
S 91
| 005080D64
|005093801
30288 | 005105AB5
96100 005128C90
1 47432 | 00514BF65
32 RT 9 . 67
00515CEA7
30|C|1517222| | | STD | | |A|20.0| | | | | || I I I I I I I I 1 1 1 71076 | 00516F145
32| | |RT|11.34| | M I M|] ||005170142
30|C|1719035| | |STD| | |A|20.0| | | | | | I I I I I I I II | I | 36728 | 0051823F5
32| | |RT|14.74| || M I I I I I |00519340D
30 | C| 1520963 | | |STD| | | A| 20 . 0 | | | | | | | | | | | | | | | | I | 27356 | 0052056BD
32 RT 18. 49
| 0052166DB
2.10 Record Type 20s and 30s for Semivolatiles -- Field Sample Chosen for
MS/MSD (QC Code 'LSD')
20| |X120l|l|LSD| |18000|X1201|1992|06|01|12|50| |ML|lOOO|78| | | 00634F7E4
21| |L| |C| | |FX1201LSD|1992|05|30| |l992|05|27| |2.0| |0063518E4
22 | 1992\ 06 | 01 1 11 1 30 | CCSTD01 1 | | |lOOO|l.O| | | |006363696
23 | P | 1992 | 06 | 01 | 11 | 01 | DFTPP02 |
T|0| | | |0|006376C26
| MB | 1992 | 04 | 01 15 14 FSBLK01 P 0
30|C|108952|3S55821|UG/L|BDL| |u| | |u|lO| M I I I I I I M I I I I I 006388A5E
H-57
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|4165600|1520963|UG/L| |43.0| |A|50.0| |
30|C|321608|15067262|UG/L| |48.3| |A|50.0| |
30|C|98904439|1719035|UG/L| | 51 . 8 | |A|50.0|
30|C|4165622|3855821|UG/L| |69.8| |A|75.0| |
30 | C| 367124 | 3 855821 | UG/L | | 69 . 6 | | A| 75 . 0 | | |
30|C|118796|15067262|UG/L| |79.5| |A|75.0| |
30|C|93951736|3855821|UG/L| | 73 . 0 | | A| 75 . 0 |
30|C|219969l|385582l|UG/L| |45.6| |A|50.0| |
30|C|3855821| | | STD | | |A|20.0| | | | | | | | | | | | | |
32| | |RT|6.38| | | | | || I I I I 0071169E8
30 | C| 1146652 | | | STD | | | A| 20 . 0 | | | | | | | | | | | | | |
32 | | |RT| 7. 75) | | | | | | | | | |007139BCF
30|C|15067262| | |STD| | |A|20.0| | | | | | | | | | | | |
|S|86|
| S | 97 |
S 104
93
S 93
| S | 106 |
| S | 97 |
S 91
J007020B12
'00703358D
0070461DF
| 007058C8C
00706B64E
| 00707E1D3
| 007080D64
007093801
30288 007105AB5
| I | 96100 | 007128C90
47432 00714BF65
32 RT | 9 . 67
00715CEA7
I 71076 00716F145
| 36728 | 0071823F5
I 27356 0072056BD
30 | C| 1517222 | | | STD | | | A| 20 . 0 | | | | | | | | | | | | |
32) | |RT|11.34| | | | | | | | | | |007170142
30|C|1719035| | |STD| | |A|20.0| | | | | | | | | | || I
32 | | |RT| 14 .74 | | | | | | | | | | | 00719340D
30 | C| 1520963 | | | STD | | | A| 20 . 0 | | | | | | | | | | | |
32| | |RT|18.49| | | | | | | | | | | 0072166DB
2.11 Record Type 20s and 30s for Semivolatiles -- Matrix Spike Sample (QC Code
'LF1')
20 | |X1201MS|l|LFl| 1 18000 |X1201 1 1992 \ 06 | 01 1 13 | 34 | |MLJ500|78| | | 00722931C
21 | |L| |C| | |FX1201LF1|1352|05|30| \1992\05\2T\ |2.0| | 00723B441
H-58 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
22|1352|06|01111130|CCSTD011 | | |50011.0 | | | |00724D125
23|P|1992|06|01|11|01|DFTPP02|||||||||||MB|1332|06|01|12|10|FSBLK01|P|0|
||S|0|R|0|00725074C
30|C|108952|3855821|UG/L||61||A|75.00|||||P|82||D|2|||||||||007263177
30|C|111444|3S55S21|UG/L|BDL||U|||U|10||||||||||||||||007274FA5
30|C|95578|3855821|UG/L||61||A|75.00|||||P|81||D|1|||||||||00728790F
30 | C| 4165600 | 1520963 | UG/L | | 37 . 8 | | A| 50 . 0 |
30 | C| 321608 | 15067262 |UG/L| | 40 . 3 | j A| 50 . 0 |
| S | 76 |
S 81
|0079035AC
007916004
30|C|2199691|3855821|UG/L| |38.4| |A|50.0| | | | | | | | | | S | 77 | | | | | | | 007976162
30|C|1146652| | | STD | | |A|20.0| | | I I I I I I I I I I I I 1 1 1 101044 | 0079884EO
32| | |RT|7.70|
|007999410
30|C|1719035| | |STD| | |A|20.0| | | | | | | | | | | | | | | | I | 37488 | 008064F42
32 | | |RT|14.69| | | | | | | | | | | 008075F5E
30|C|3855821| | | STD | | |A|20.0| | | | || I I I I I I I II 1 1 1 30512 | 0080881FE
32| | |RT|6.33| | | | | | | | | | | 008099122
2.12 Record Type 20s and 30s for Semivolatiles -- Matrix Spike Duplicate Sample
(QC Code 'LF2')
20 | |X1201MSD|l|LF2| | 18000 JX1201 | 1992 \ 06 | 01 | 14 | 05 | |ML|500|78| | | 00810BDF7
H-59
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses .
21 | |L| |C| | |FX1201LF2|1992|05|30| \1992\05\27\ \2.0\ |00811DF1D
22 | 1392 | 06 | 01 | 11 | 30 | CCSTD01 | | | | 500 | 1 . 0 | | | | 00812FC01
23 | P | 1992 | 06 | 01 1 11 1 01 1 DFTPP02 | || I I I I I I I I MB I ^992 | 06 | 01 1 12 1 10 | FSBLK01 1 P | 0 |
| |S|0|R|0|008133228
30|C|108952|3855821|UG/L| | 63 | | A| 75 . 00 | | | | | P | | 84 |D | 2
30 |c| 111444 | |UG/L|BDL| |u| | |u|io| | | | | | | | | | | | | | |
30|C|95578|385582l|UG/L| | 61 | | A| 75 . 00 | | | | | P| | 82 | D | 1
| 008145C61
| 00816A3FA
30 | C| 4165600 | 1520963 |UG/L| | 39 .2 | | A| 50 . 0 |
30 |C| 321608 | 15067262 | UG/L | | 40 . 1 | | A| 50 . 0 |
| S | 78 |
| S | 80 |
| 0087865AD
| 008799002
30|C|1146652| | | STD | | |AJ20.0| || I I I I I I I I I I I I | I 1 100060 | 00886B4FA
32| | |RT|7.73|
00887C42D
||||| | I | 50488 | 00888E7D2
| 77500 | 0089019AE
30 |C | 15067262 | | | STD | ||A|20.0|||||||
32| | |RT|9.65| | | | | | | | I | | 00889F712
30|C|1517222| | |STD| | |A|20.0| | | | 1 || |
32| | |RT|ll.32| | | | | | | | | | |00891299F
30|C|1520963| | | STD | -| |A|20.0| | || I I I I I I I I I I I | 1 1 29384 | 008924C52
32| | |RT|18.44| | | | | | | | | | | 008935C6B
30 |C| 1719035 | | | STD | | | A| 20 . 0 | | | | | | | | |
32| | |RT|14.70| | | | | | | | | | |008958F2D
H-60
| I | 39388 | 008947F23
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|3855821|||STD|||A|20.0||||||||||||||||I|29976|0089SB201
32|||RT|6.37|||||||||||00897C133
H-61 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
3.0 PESTICIDES (COL. 1)
3.1 Record Type 10 for Pesticides (Col 1)
10 | | | | | \GC\OLM04.2P\ | TESLAB | | | |68DOOOOl| INSTP11 | TEST LABS INC. | |000002A30
3.2 Record Type 11 for Pesticides (Col 1) . -
ll|DB-5||0.53||||||||||J0000249FA
3.3 Record Type 20s and 30s for Pesticides (Col 1) -- Initial Calibration Mean
Values (QC Code 'MNC')
20|||0|MNC||18000|X1201|||||||||61|||000036387
30|C|319846| | |AVG|834490| | | | | |R|6| | | | | | | | | | | | | |000048346
32|||RT|6.92|RTF|6.87|RTT|6.97|||||||000059DCB
30|C|319857| | |AVG|272332| | | | | |R|l2| | | | | | | | | | || I I00006BE34
32||RT|8.24RTF8.19|RTT8.29||||00007D89C
30|C|5103742|||AVG|706395||||||R|13||||||||||||||00042FD21
32 | | |RT111.87|RTF111.80|RTT111.94| | | | | | |000431AOA
30|C|8001352| | | |l3757| | | I I I I I I I ! I I I I I I I I I |00044363C
32|||RT|14.84|RTF|14.77|RTT|14.91||||||l|000455429
30|C|8001352| | | | 7373 | | || I ! I I I I I 1 I I i ! 1 I I M000466F72
32|||RT|15.47|RTF|15.40|RTT|15.54||||||2|000478D57
30|C|8001352| | | |10643| | | | | | | | | | | | | | | | | | | | |00048A976
32|||RT|16.04|RTF|15.97|RTT|16.11||||||3J00049C748
30|C|8001352 | | | J17393| | | | | | | | | | | | | | | | || I I |00050E370
32|||RT|17.23|RTF|17.16|RTT|17.30||||||4|000510136
H-62 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|11096825| | | |48393|
32 | | | RT | 14. 01 | RTF | 13. 94 | RTT | 14. 08 |
| 00120C450
500121E21E
30|C|877098| | |AVG|344348| | | | | |R|lO| || I I I I I I I I I I I 0012202BA
32 | | | RT | 5. 04 | RTF | 4. 99 | RTT | 5. 09 | | | | | | | 001231D26
30|C|2051243| | |AVG| 455516 | | | | | |R| 10 | | | | | | | | | |
32| | |RT|22.53|RTF|22.43|RTT|22.63| | | | | | | 001255B43
001243E74
3.4 Record Type 20s and 30s for Pesticides (Col 1) -- Florisil Cartridge Check
Recovery Values (QC Code 'FLO')
20 | \FLOP1248A100\0\FLO\ \ 18000 | X1201 | 1991 \ 11 | 14 | 09 | 19 | | | | 11 | | | 00126852C
21
| P1248A1
2 . 0 00127993B
30|C|319846| |NG| |8.695| |A|lO.OOO| | |
30 | C| 58899 | |NG| |8.816| |A|lO.OOO| | | |
30|C|76448| |NG| |8.690| |A|lO.OOO| | | |
30 | C| 959988 | |NG | | 8 . 891 1 | A| 10 . 000 | | |
30|C|6057l| |NG| |17.498| |A|20.000| | |
30|C|72208| |NG | | 16. 576 | |A|20.000| | |
30|C|72548| |NG| |23.206| |A|20.000| | |
30 | C| 50293 | |NG| |16.551| |A|20.000| | |
30|C|72435| |NG| | 84 . 668 | | A| 100 . 000 | |
30 | C| 877098 | |NG| |9.882| | A| 10 . 000 | | |
30 |C | 2051243 | |NG| | 20 . 032 | | A| 20 . 000 |
| |S|87.0| | | |
| S | 88 .2 | | | | |
|S|86.9| | | | |
| | S | 88 . 9 | | | |
| |S|87.5| | | |
| | S | 82 . 9 | | | |
| | S 1 116 . 0 | | |
| |S|82.8| | | |
| | | S | 84 . 7 | | |
| | | S | 98 . 8 | | | |
S 100 . 2
| |00128BFC9
|00129E581
J001300B3E
| |0013131F9
| | 001325882
| | 001337EF2
| | | 00134A61A
| | 00135CC78
| | |00136F3EA
| | 001371A93
| | 001384337
30/C/35954//WG//2//A/50.000//////////S/4///////001384338
H-63
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
3.5 Record Type 20s and 30s for Pesticides (Col 1) -- GPC Recovery Values (QC
Code 'GPC')
20)\GPC1242A112B\0\GPC\\18000|X1201|1991\11|13|09|19||||11|||00139852C
21| | | | | | |G1242A1| | | I | | | | |2.0| |00140993B
30|C|58899||NG||9.816||A|lO.OOO||||||||||S|98.2|||||||00141E581
30|C|76448||NG||9.690||A|lO.OOO||||||||||S|96.9|||||||001420B3E
30|C|309002||NG||9.89l||A|lO.OOO||||||||||S|98.9|||||||0014331F9
30|C|60571||NG||18.498||A|20.000||||||||||S|92.5|||||||001445882
30|C|72208||NG||17.576||A|20.000||||||||||S|87.9|||||||001457EF2
30|C|50293||NG||17.581||A|20.000)|||||||||S|87.9|||||||00146CC78
3.6 Record Type 20s and 30s for Pesticides (Col 1) -- Resolution Check
Standard (QC Code 'LPC')
20||RESC01|0|LPC||18000|X120l|1992\04|20|04|44||||9|||001396901
21|||||||RESC01|||||||||2.0||001407BA9
30|C|877098| | | | | | | | | |R|98.9| | | | | | || I I I I I |0014196FF
32|||RT|5.06|||||||||||00142A62C
30|C|5103742| | | | | | | | | |R|lOO.O| | | || I I 1 ! 1 I I I I00143C2DE
32|||RT|11.88|||||||||||00144D2EE
30|C|959988| | | | | | | | | |R|lOO.O| | | | M I I I I I I I I00145EEFC
32|||RT|12.40|||||||||||00146FEF7
30|C|72559||||||||||R|92.3||||||||||||||00147193C
32|||RT|13.10|||||||||||00148292B
30|C|60571| | | | | | | | | |R|100.0| | || I i I I 1 I I I I |001494422
32| | |RT|13.26| | | | | | | | || I 001505422
H-64 OLM04.2
-------
30|C|1031078| |
32| | |RT|16.03|
30|C|72435| | | |
32| | |RT|17.87|
| | |R|100.0| | | | |
| I I I |0015280C6
|R|98.6| M | | | | |
00154AB36
Exhibit H -- Appendix A
Format of- Records for Specific Uses
0015170C8
001539B17
30|C|53494705| | | || I II I |R|lOO.O| | | | I I I I I I I I I |00155C8F1
32 RT 18. 15
30|C|2051243|
32| | |RT|22.53|
00156D8FE
||||||||||||||||||||00157FOAD
(0015800AD
3.7 Record Type 20s and 30s for Pesticides (Col 1)
Mixture (QC Code 'CLE')
--Performance Evaluation
20 | |PEM01|0|CLE| | 18000 |X1201 | 1992\ 04 | 20 | 06 | 26 | | | | 12 | | | 001592687
|PEM01|
|2.0| |00160389F
30 | C| 319846 | |NG| | 0.020 | |A|0.020| | | R| 97 . 5 | | | |D | 0 . 0 |
32| | |RT|6.94| | | | | | | | | | |001626C20
30 | C| 319857 | |NG| | 0 . 022 | |A|0.020| | |R|94.0| | | |D|-10.
32 RT 8 . 25
00164AOED
30 | C| 58899 | |NG | | 0 . 020 | |A| 0 . 020 | | |R| 93 . 4 | | | | D | 0 . 0 | | |
32 | | | RT | 8. 03 | | | | | | | | | | |00166D388
30 | C| 72208 | |NG| |0.117| |A|0.100| | |R|98.5| | | |D|-17.0|
| 001615CE1
0016391BC
| 00165C465
| 0017048D9
32) | | RT | 14. 26 |
PB | 11 . 0 13 . 5 0017160EC
30 | C| 50293 | |NG||0.201||A|0.200|||R|94.6||||D|-0.5|||||||| | 0017284BB
32| | | RT 1 15 .'44 | | | | | | PB | 2 . 5 1 13 . 5 | | |001739COC
30 | C| 72435 | |NG| |0.54l| |A|0.500| | |R|97.4||||D|-8.2|||||||| | 00174C014
32| | |RT|17.86| | | | | | | | | | |00175D032
H-65 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
| 001806222
0018296ED
30 |C| 877098 | |NG| | 0 . 038 | | A| 0 . 040 | | |R| 92 . 6 | | | |D| 5 . 0 | |
32 | | |RT|5.06| | | | | | | | | | |00181714F
30|C|2051243| |NG| |0.042| |A|0.040| | | | | | | |D|-5.0| | | | |
32| | |RT|22.53| | | | | | | | | | |00183A6ED
3.8 Record Type 20s and 30s for Pesticides (Col 1) -- Initial Calibration
Multicomponent Standard (QC Code 'CLS')
20| |AR16600l|0|CLS| | 18000 |X1201 | 1992\ 04 | 20 | 06 | 58 | | | | 12 | | | 00184CFD8
21| | | | | | |AR16600l| | | | | | | | |2.0| | 00185E4C3
30|C|12674112| | | |27928| |A|0.200| | | | | | | | | | | | | | | | | | 0018606AO
32| | |RT|9.00| | | | | | | | | |l|00187169E
30|C|12674112|.| | |694l| |A|0.200| | | | I | | I | | | | | | | | | | 001883797
32| | |RT|10.80|
|2|001894872
30|C|12674112| | | |6398| |A|0.200|
I 001906971
32 | | | RT | 11 . 14 |
3 001917A4B
30|C|12674112| | | | 9007 | |A|0.200| | | | I I I I I I I I I I I I I I 001929B36
32| | |RT|9.46| | | | | | | | | |4|00193AB5F
30|C|12674112| | | |l082l| |A|0.200| | | | I I I I I I I I M I I II 00194CD18
32 RT 7 . 99 |
| 5 | 00195DD48
30 |C| 11096825 | | | | 94264 | | A| 0 . 200 | | | | | | |
32| | |RT|16.86| | | || I I II |l|001971038
30 | C| 11096825 | | | | 74552 | | A| 0 . 200 | | | | | | |
32| | |RT|14.23| | | | | | | | | |2|001994308
30|C|11096825| | | |32609| |A|0.200| | Ml I I
32 | | | RT | 18. 14 | | | | | | | | | |3|0020175DO
H-66
00196FF3E
-|00198322C
I I I I I I I 0020064E5
OLM04.2
-------
30|C|11096825| | | |34595| |A|0.200|
32 RT 19.661
|4|00203A8CF
30|C|11096825| | | |48393| |A|0.200|
32 RT 14. 01
|5|00205DBA2
Exhibit H -- Appendix A
Format of Records for Specific Uses
0020297C7
00204CABD
00206FCDA
30|C|877098| | | |344348| |A|0.040| | | | | | | | | | |
32| | |RT|5.05| | | I | | | M I |002070C06
30|C|2051243| | | |455516| |A|0.040| || I I I II I I I I I I I II I 002082DFO
32| | |RT|22.54| | | | | | | | | | |002093DFB
3.9 Record Type 20s and 30s for Pesticides (Col 1) -- Initial Calibration
Single Component -- Individual Standard A (QC Code 'CLM')
20 | |INDAL13|0|CLM| | 18000 |X1201 | 1992 \ 04 | 20 | 11 | 41 | | | | 11 | | |00304C753
21 | | | | | | |INDAL13| | | | | | | | | 2.0 | |00305DA70
22||||||||||||||1.0|00306E736
30 |C | 319846 | | | | 867823 | |A|0.010| | | | || I I I I I
32| | |RT|6.9l| | | | | | | | | | |003081789
30|C|58899| | | |807087| |A|0.010| I I || I I I I I I I
I I I | 003070857
|0030937DC
32 RT8.0l
0031046FD
30|C|76448| | | | 827300 | |A|0.010| | || I I I I I I I I I I I I I |003116728
32| | |RT|8.89| | || I I I II I |00312766D
30|C|959988| | | |605148| |A|0.010| || I I I I I I I I I I I I I I |0031397A9
32| | |RT|12.38| | || I I I I I I |00314A7AB
30|C|6057l| || |638273J |A|0.020| | | | I I I I I I I I I I I I I |00315C7CC
32 | | | RT 1 13. 24 | | | || I I I I I |00316D7CA
30|C|72208| | | |444069| |A|0.020| | | | | | | | I I I II I M I |00317F7F3
H-67 '
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
32|||RT|14.25|||||||||||0031807FD
30|C|72548| | | |444235| |A|0.020| | | | | | | | | I I II I I I I I 003192832
32|||RT|14.62|||||||||||00320383D
30|C|50293||||401902||A|0.020||||||||||||j|||||00321583D
32|||RT|15.43|||||||||||003226848
30|C|72435| | | |174490| |A|0.100| | | I I I I I I I I I I I I I I |003238870
32|||RT|17.85|| | | | | | || I|00324988D
30|C|877098| | | |373538| |A|0.010| | | I I I I I I I I I I I I I I |00325B9B1
32|||RT|5.03|||||||||||00326C8D1
30|C|2051243| | | |496702| |A|0.020| I I I | I I I I I I | 1 | | | | |00327EAA7
- 32|||RT|22.52|||||||||| J00328FAA6
3.10 Record Type 20s and 30s for Pesticides (Col 1) -- Initial Calibration
'' Single Component -- Individual Standard Mix B (QC Code 'CLM')
/-. 20 | |INDBL15|0|CLM| |18000|X1201|1992|04|20|12|13| | | 113 | | | 003292199
21|||||||INDBL15|||||||||2.0||0033034C3
22|-|| | || | | I'll | ||1.0|003314189
30|C|319857| | | |301500| |A|0.010| | II I I I I I I I I I I I I I |003326275
32| | |RT|8.25| | | || I I I I I |0033371A6
30|C|319868| | | |946215| |A|0.010| | I I II I II I I I I I I I I I0033492C4
32| | |RT|9.27| | | | | I I I I I I00335A1F8
30|C|7421934| | | |461669 | |A|0.020| | || I I I I I I i I I I I I I (00348EE52
32| | |RT|15.69| | | | | || | I I |00349FE6F
H-68 . OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|5103719| | | |781319| |A|0.010| | || I I I I I I I I I I I I I |00350204E
32| | |RT|12.33| MINIMI |003513041
30|C|5103742| | | |804407| |A|0.010| | | | | | | | | | I I I I I I I I 003525220
32|||RT|ll.87|||||||||||00353622F
30|C|877098| | | |373538) |A|0.010| || M I M I I I I II M I |003548353
32|||RT|5.04|||||||||||00355927E
30|C|2051243| | | |496702| |A)0.020) | | | I I I I I M I I I I I I |00356B454
32| | |RT|22.53| | | | | I I I I I I00357C454
3.11 Record Type 20s and 30s for Pesticides (Col 1) -- Instrument Blank (QC
Code 'LIB')
| 20||PIBLKX1|1|LIB||18000|X1201|1992\04|21|12|19||ML|lOOO|30|||004663C44
21|||||||PIBLKX1|||||||||2.0||004674F64
22) | | | | | | | | |10000|1.0| | | [004686077
| 30|C|319846| |UG/L|BDL| | | | |U|0.050\ M M I I I M M I I I I00469809D
| 30|C|319857| |UG/L|BDL| | | | |U| 0.050\ | | I | I | | I | l'| || I I 00470AOC5
| 30|C|319868| |UG/L|BDL| | | | |u|0.050\ | | | M M I M II I I |00471COEF
30|C|11096825| |UG/L|BDL| | | | |u|1.0\ \ \ \ \ \ \ \ \ \ \ \ \ \ | |00496E7D1
30|C|877098| |UG/L| |0.040| |A/0.2/| | | I I.I I I I I I I I I I I I I I 0049708D6
32|||RT|5.06|||||||||||004981803
30|C|2051243| |UG/L|NRP|0.042| |A/0.2/| | | | I I I I I I I I M I I I I I004993E4D
32| | |RT|22.54| | | I I I I I I I I005004E58
H-69 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
3.12 Record Type 20s and 30s for Pesticides (Col 1) -- Method Blank (QC Code
LRB' )
20 | |PBLK58|l|LRB| | 18000 |X1201 | 1552 | 04 | 21 | 14 | 31 | |ML|lOOO|30| | (0052620A8
|S| | |FPBLKOl|l992|04 |17 | | | | | |2.0| |0052739F9
21
22
|10000|1.0| | | J005284BOC
27| | | | | | | |F|1991|11|14|09|19|P1248A1|N| | | | | | | | |005308E9E
30 | C| 319846 | |UG/L|BDL| | | | |U| 0 . 050 | | | | | | | | | | | | | | | |00531AEC2
30 | C| 319857 | |UG/L|BDL| | | | |U|0.050| 11111111111111 I 00532CEE8
30|C|11096825| |UG/L|BDL| | | | |U|l.O| || I I I I I I I I I I I I I 00558082B
: 30 | C| 877098 | |UG/L| | 0 . 19 | | A| 0. 2\ \ \ \ \ \ \ \ \ \ S | 94 | | | | | | | 005592E19
" 32| | |RT|5.06| | | | | | | | | | |005603D46
30 | C| 2051243 | |UG/L| | 0 . 21 | | A| 0.2 \ \ \ \ \ \ \ \ \ \ B \ 100 | | | | | | | 005616468
32| | |RT|22.53| | | | | | | | | | | 005627468
3.13 Record Type 20s and 30s for Pesticides (Col 1) -- Matrix Spike Sample (QC
Code ' LF1 ' )
20| |X1201MS|1|LF1| | 18000 JX1201 | 1992 | 04 | 21 | 16 | 08 | |ML|300|30| | | 00563A08B
21 | | | |S| | | 488920 | 1992 | 04 | 17 | |l992|04|l5| |2.0| |00564BFE5
22
23
| 5000 1 1 . 0 | | | | 00565D2D6
| | | | | | | | | | | | | | |MB|1992|04|21|14|31|FPBLK01|P|0| | | S | 5 | R| 5 | 005660949
27 | | | | | | | |F|1991|11|14|09|19|P1248A1|N| | | | | | | | |00567285F
30 | C| 319846 | |UG/L|BDL| | | | \\J\0.050\ 1 | | | | | | | || I I I I I 005684889
H-70
OLM04.2
-------
Exhibit H -- Appendix A
Format of-Records for Specific Uses
30|C|58899| |UG/L| | 0 . 82 | |A|l.667| | | | |P|49| |D|l
32| | |RT|8.01| | | | | | | | | | J00572B839
30|C|76448| |UG/L| |0.69| |A|l.667| | | | | P | 41 | |D|2|
|Pl2.3| | | 00571A918
|P|6.2| | | 00573D7A3
32| | |RT|8.90|
00574E6D6
30|C|50293| |UG/L| |l.5| |A|l.667| | | | |P|90| |D|6| | | | |P|0.0| | | 005875913
32| | |RT|15.43|
|00588691E
30 | C| 72435 | |UG/L|BDL| | | | |u| 0. 50 \ \ \ \ \ \ \
30|C|53494705| |UG/L | LLS | 0 . 094 | J | | | | | | |
|00589877C
|P|6.4 | 00590AD22
32| | |RT|18.14|
|00591BD2E
30|C|7421934| |UG/L | LLS | 0 . 091 1 j|
I I I I I I IPI2-2I I I 00592E1B6
32 |RT|15.68
| 00593F1D2
30 |C| 5103719 | |UG/L|BDL| | | | |u| 0. 050 \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ | 0059412C9
30 | C| 877098 | |UG/L| | 0. 20\ \ A| 0. 20 \ \ \ \ \
32 | | |RT|5.03| | | | | | | | | | |0060568AC
30 | C| 2051243 | |UG/L| | 0. 20\ \ A| 0.20\ \ \ \ \ \ \ \ \ \ S | 100
\ \ S \ 100\ \ \ \ \ \ | 00604598C
006068FOA
32| | |RT|22.52|
006079F09
3.14 Record Type 20s and 30s for Pesticides (Col 1) -- Matrix Spike Duplicate
Sample (QC Code 'LF2')
20| |X1201MSD|l|LF2| | 18000 JX1201 | 1592 | 04 | 21 | 16 | 4i | |ML|300|30| | |00608CBB4
2l| | | |S| | |488921|1992|04|17| |1992|04|15| |2.0| | 00609EBOF
H-71 OLM04.2
-------
Exhibit K -- Appendix A
Format of Records for Specific Uses
22| | | | | | | | | |5000|l.0| | | |00610FEOO
23||||||||||||||||||MB|1552|04|21|14|31|FPBLK01|P|0|||S|5|R|5|006113473
27 | | | | | | | |F|1S91|11|14|09|19|P1248A1|N| | | | | | | | |006125389
30 |C| 319846 | |UG/L|BDL| | | | \\J\0.050\ | | | | | || | | | | | | | | 0061373B3
30|C|76448||UG/L||0.70||A|l.667|||||P||42|D|2|||||P|6.l||[0061802BC
32|||RT|8.9l|||||||||||0061911FO
.30 | C| 50293 | |UG/L| |l.6| |A|l.667| ||||
:32| | | RT 1 15. 45 | | | | | | | | | | |00633944F
?30|C|72435| |UG/L|BDL| | | | |U| 0. 50 | | | |
K.30|C| 53494705 | | UG/LJLLS | 0 . 098 | J| | | |
32| | |RT|18.16| | | | | | | | | | |00636E928
30 |C| 7421934 | JUG/L | LLS | 0 . 096 | J| ||||
32 | | | RT | 15. 70 | | | | | | | | | | (006381DD7
30|C|5103719| |UG/L|BDL| | | | |U| 0.050\
006328438
00634B2AD
|P|l2.2| | |00635D91A
|006370DCC
006393ECE
30 |C | 877098 | |UG/L| | 0. 19\ \ A| 0. 20 \ \
32| | |RT|5.04| | | | | | | | | | |0065094B5
30 |C | 2051243 | |UG/L| |0.18||A|0.20|
I I I I IsI97I I I I I I |00649858A
00651BB13
32 | | | RT | 22 . 53 |
| 00652CB13
-H-72
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
3.15 Record Type 20s and 30s for Pesticides (Col 1) -- Continuing Performance
Check -- Individual Standard Mix A (QC Code 'CLE')
20 | | INDAM72 | 0 | CLE | | 18000 | X1201 | 1992 \ 04 | 21 | 22 | 12 | | | | 11 | | |006882FOF
21 1 | | | | | | INDAM72 || I I I I II I 2 ° I I 00689423C
22| | | | | | | | | | | | | |4.0|006904FOF
30 |C| 319846 | |NG| | 0 . 039 | | A| 0 . 040 | | | | | | | |D | 2 . 5 | | | | | | | | | 006917382
32 | | |RT|6.94| || I I I I I I I I 0069282C1
30|C|58899| |NG| | 0 . 035 | |A|0.040| | | |
32 | | | RT | 8. 03 | | | | | | | | | | |00694B666
|D|l2.5|
00693A743
30|C|72435| |NG||0.438||A|0.400||||||||D|-9.5||
32| | |RT|17.86| | | | | I I I I I |00708234C
30 | C| 877098 | |NG| |0.037| |A|
|D|23.8|
32| | |RT|5.05| | | | | | | | | | |00710570A
30|C|2051243| |NG| |0.06l| |A|0.080| |
32| | |RT|22.52| | | | I I I I I I |007128D17
| 00707132E
| 0070947DE
007117D18
3.16 Record Type 20s and 30s for Pesticides (Col 1) -- Continuing Performance
Check -- Individual Standard Mix B (QC Code 'CLE1)
- 20 | |INDBM78|0|CLE| | 18000 |X1201 | 1392 | 04 | 21 | 22 | 51 | | | | 13 | | J00713B40B
21 1 | | | | | | INDBM78 | | | | | | I I I 2 ° I I 00714C749
22|||||||||||i||4.0|00715D41C
30 | C| 319857 | |NG| | 0 . 036 | | A| 0 . 040 | | | | | | | | D 1 10 . 0 |.| | | | | | | | 00716F95A
32| | |RT|8.26| | | Ml I I I I | 00-717088C
H-73
OLM04.2
-------
Exhibit K -- Appendix A
Format of Records for Specific Uses
30 |C| 319868 | |NG| | 0 . 038 | | A| 0 . 040 | |
32| | |RT|9.28| | | | | | | | | | [007193C35
30 |C| 309002 | |NG| |0.038| |A|0.040| |
32| | |RT|9.83| | | | | | | | | | | 007216FAC
|D | 5 ..0 |
|D|5.0|
| 007182DOO
007206076
30|C|5103742| |NG| |0.038| |A|0.040| |
32| | |RT|ll.88| MINIMI |007371E78
30 | C| 877098 | |NG| |0.042| |A|0.040|||
32| | |RT|5.06| || || || | || |00739529B
. 30 |C| 2051243 | |NG| |0.067| |A|0.080| |
|D|5.0|
D 16 . 2
|007360E68
|00738436E
|0074078B5
. 32| | |RT|22.54|
I 0074188CO
3.17 Record Type 20s and 30s for Pesticides (Col 1) -- Continuing Performance
'"Check -- Performance Evaluation Mixture (QC Code 'CLE')
20| |PEM90|0 |CLE| | 18000 |X1201 | 1992\ 04 | 23 | 13 | 47 | | | | 12 | | | 00777E850
2l||||||| PEM90 | | | | || || | 2 . 0 || 00778FA7A
007792031
| 00781551E
|OO783891F
|007880CB5
30 |C| 319846 | |NG| |0.025| |A|0.020| | |j?/99.4/| | | | |D|-25.0|
32| | |RT|6.93| | | | | | | | | | |007802F65
30 |C| 319857 | |NG| |0.025| |A|0.020| | |R| 99.4 | | | |D| -25.0J | |
32| | |RT|8.25| M I I I I I M | 00782644F
30 | C| 58899 | |NG| |0.022| |A|0.020| | |R|98.7| | | |DJ-10.0| | | |
32| | |RT|8.03| | | | | | | M I |007849842
'30|C|72208| |NG| |0.108| |A.|0.100| | |R|98.9| | | |D|-8.0| | | ||
32 | | | RT | 14. 27 |
| PB | 20 . 0 | 24 . 0 | | | 0078924C6
H-74 '
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|50293||NG||0.201||A|0.200|||R|95.9||||D|-0.5|||||||||007904895
32|||RT|15.45||||||PB|4.0|24.0|||007915FE1
30|C|72435| |NG| |0.518| |A|0.500| | |R|97.9| | | |D|-3.6| | | | | | | | |0079283EC
32| | |RT|17.86| | | | | | | | | | |00793940A
30|C|877098||NG||0.044||A|0.040|||R|98.7||||D|-10.0|||||||||007982735
32|||RT|5.05|||||||||||007993661
30|C|2051243| |NG| |0.04l| |A|0.040| | | | | | | |D|-2.5| | | | | | | | |008005COO
32| | |RT|22.53| | | | | | | | | | |008016COO
3.18 Record Type 20s and 30s for Pesticides (Col 1) -- Field Sample chosen for
MS/MSD (QC Code 'LSD')
J 20||X120l|l|LSD||18000|X1201|1SS2|04|23|15|42||ML|400|34|||0080296B4
| 21||||S|||FX1201|1932|04|17||l332|04|l5||2.0||00803B55E
22| | | | | | | | | |500011.0 | | | |00804C84F
| 23||||||||||||||||||MB|1392|04|2l|l4|31|FPBLKOl|P|2| | I I I I I00805FBAE
| 27| | | | M | |F|19Sl|11|14|09|19|P1248A1|N| | | I I II I |008061AC4
| 30|C|319846| |UG/L|BDL| | | | |u|0.050\ | | | || I I I I I I I I I I008073AEB
| . 30|C|319857||UG/L|BDL|||||U|0.050||||||||||||||||008085B14
| 30|C|319868| |UG/L|BDL| | | | |u|0.050\ | | | I I I I I I I I I I I I008097B3F
30|C|72559||UG/L|LLS|0.014|JP||||||||||||||||P|27.3|||008165DD3
32|||RT|13.03|||||||||||008176DC4
30|C|72208| |UG/L|BDL| | | | \U\0.10\ | | | I | I I I I I | | | | |008188C04
30|C|33213659||UG/L|BDL|||||u|0.10\|||||||||||||||00819ACEF
H-75 OLM04.2
-------
Exhibit K -- Appendix A
Format of Records for Specific Uses
30 |C| 877098 | |UG/L| |0.10||A|0.20|||
32 | | | RT | 5. 04 | | | | || | | | | |00847F5F6
30 | C| 2051243 | |UG/L| | 0.10\ |A|0.20| |
32| | |RT|22.53| | | | | | | | | | |008492C7E
|00846E6CB
|S|53| | |P|7.7| | |008481C7E
H-76
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
4.0 PESTICIDES (COL. 2)
4.1 Record Type 10 for Pesticides (Col 2)
10 | | | | | |GC| OLM04.2P\ | TESLAB | | | | 68D000011INSTP2 | | TEST LABS INC. | | 000002A31
4.2 Record Type 11 for Pesticides (Col 2)
11|DB-608| I 0.53 I | | | | | | | | | |000024AD7
4.3 Record Type 20s and 30s for Pesticides (Col 2) -- Initial Calibration Mean
Values (QC Code 'MNC')
20|||0|MNC||18000|X1201|||||||||62|||000036465
30|C|319846|||AVG|1137869||||||R|16||||||||||||||0000485E4
32| | |RT|4.56RTF|4.51 | RTT|4.611 | | | | | |00005A047
30|C|12674112| | | |35883| | | | || I I I I I I I I I I I II I I00054566A
32|||RT|5.69|RTF|5.62|RTT|5.76||||||l|0005571C3
30|C|12674112| | | 1161411 | | | II II I I I I I I I I I I I ||000568ECC
32|||RT|4.70|RTF|4.63|RTT|4.77|||||I2I00057AA13
30|C|12674112| | | 118842 | | | I I I I I I I I I I I I I I I I I |00058C730
32|||RT|6.51|RTF|6.44|RTT|6.58||||||3|00059E285
30|C|12674112| | | |l5946| | | | I I I I I II I I I I I I I I I |00060FFAE
32| | |RT|7.30|RTF|7.23 |RTT|7.37||||||4|000611AEO
30|C|12674112| | | |l6309| | | | | | | | | I I I I I I I I I I I I0006237EF
32|||RT|8.01|RTF|7.94|RTT|8.08||||||5|00063533C
30|C|11104282| | | |9686| | | | | | I I I I I I I I I 1 I I I I I000646F7E
32|||RT|3.89|RTF|3.82|RTT|3.96||||||l|000658AB9
H-77 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|11104282| | | |3312 | | I 1 | I || I I I I I I I I 1 I I | |00066A6BF
32|||RT|3.49|RTF|3.42|RTT|3.56||||||2|00067C1EF
4:4
30|C|877098| | |AVG|559374| | | | |.|R|2l| 1 | | | | | | | | I I I (001242054
32 | | | RT | 2. 87 | RTF | 2. 82 | RTT | 2. 92 | | | | | | | 001253A9F
30 |C| 2051243 | | |AVG| 594715 | | | | | | R| 16 | | | | | | | | | | | | | |001265C02
32| | |RT|16.34 | RTF | 16. 24 | RTT | 16. 44 |
| 0012778FF
Record Type 20s and 30s for Pesticides (Col 2) -- Resolution Check
Standard (QC Code 'LPC')
20 | |RESC01|0|LPC| | 18000 |X1201 | 1992 | 04 | 20 | 04 | 44 | | | |9| | | 0014186BD
211 | | | | | |RESC01|
30|C|877098 Mill
32| | |RT|2.89| | I I
30|C|959988| | | |-|
32|||RT|8.71||||
30|C|5103742||||
32| | |RT|8.89| | | |
30|C|72559| | | II I
32| | |RT|9.35| | | |
30|C|60571||| N I
32| ||RT|9.611| | |
30|C|1031078| | | |
32M IRT|13.17| I I
| | | |2.0| [001429965
|R|100.0||||||||||||||00143B560
| | | 00144C495
| R | 97 . 0 |
00146EF1C
| | | |001481B13
|R|99.0MNNMII
| | | | 001504499
|R|IOO. OMNIUM
| | | |001526EC2
M|R|96.3|||||NI
| | | | |001549AB1
H-78
00145DFEA
|001470BCE
| | 001493566
|001515F90
|001538AB1
OLM04.2
-------
30|C|72435| | | |
32| | |RT|13.35|
|R|lOO.O|
Exhibit H -- Appendix A
Format of -Records for Specific Uses
00155B5AA
00156C5AA
30|C|53494705| | | | | | | | | |R|lOO.O| | | | | | | | | | | | | | 00157E365
32| | |RT|14.06| | | | | | | M | |00158F36E
30|C|2051243|||||||||||||||||||||||||001590B1D
32 | | |RT|16.35| | | | | | | | | | |001601B2A
4.5 Record Type 20s and 30s for Pesticides (Col 2) -- Performance Evaluation
Mixture (QC Code 'CLE')
20| |PEM01|0|CLE| | 18000 JX1201 | 1992 | 04 | 20 | 06 | 26 | | | | 12 | | | 001614104
21
PEM01
2.0 00162531C
30 | C| 319846 | |NG| |0.02l| |A|0.020| | |R|99.l| | | |D|-5.0|
32| | |RT|4.59| | | || I I I I I |001648725
30 | C| 319857 | |NG| |0.02l| |A|0.020| | |R|94.9| | | |D|-5.0|
32 | | | RT | 7. 31 1 | | | | | | | | | |00166BB15
30 | C| 58899 | |NG| |0.020| |A|0.020| ||R|97.8||||D|0.0|||
32| | |RT|5.47| MINIMI I 00168EDC9
30 | C| 72208 | |NG | | 0.103 | | A | 0.100 | | |R | 95 . 6 || | |D | -3 . 0 | |
32| | |RT|10.09| || II |PB|11.0|12.0| | | 0017379E1
30|C|50293| |NG | | 0.182 | |A| 0 . 200 | | | R| 96 . 3 | | | | D | 9 . 0 | | |
32| | |RT|11.68| | | | | |PB|1.0|12.0| | | 00175B476
30 | C| 72435 | |NG|| 0 . 501 | | A| 0 . 500 | | | R| 94 . 8 | | | | D | -0 . 2 | |
32 | | | RT | 13. 34 || | | | | | | | | |00177E85D
30|C|877098| |NG| |0.037| |A|0.040| | |R|95.8| | | |D|7.5| |
32| | |RT|2.89|| | | | M I I I |001838971
H-79
0016377E7
00165ABF2
00167DE8D
|0017261EB
| 00174 9D4D
00176D85E
001827A3C
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30 |C| 2051243 | |NG| | 0 . 039 | | A| 0 . 040 | |
32| | |RT|16.34| | | | | | | | | | | 00185BEAA
4.6
4.7
|D| 2 . 5
Record Type 20s and 30s for Pesticides (Col 2)
Multicomponent Standard (QC Code ' CLS ' )
20| |AR122102|0|CLS| |'18000 |X1201 1 1992 | 04 | 20 | 07 | 31 1
00184AE9E
-- Initial Calibration
J002128054
21
|AR122102|
| 2.0 | | 002139525
30 | C| 11104282 |
32| | |RT|3.89| |
30 |C| 11104282 |
32| | |RT|3.49| |
30|C|11104282|
32 | RT|5.67| |
| 9686 | | A| 0 .400 |
1 00215C641
| 3312 | |A| 0.400 |
|2|00217F71E
|3087| |A|0.400|
002192825
30 | C| 11104282 | | | |2207| |A|0.400| | | |
32| | |RT|7.05| | | | | | | | | |4|002215916
30|C|11104282| | | |2134| |A|0.400| | | |
32 | | |RT| 8. 02 |
|5|0022389FB
30 | C| 877098 | | | | 559374 | | A| 0 . 040 | | | |
32 | | |RT|2.86| | | | | | | | | | |00225BA76
30|C|2051243| | | |594715| |A|0.040| | |
32| | |RT|16.33| | | | | | | | | | (00227EC66
| 00214B62E
00216E70E
I I I I I 002181808
0022048FE
I I I I I I I I I I I 0022279EE
00224AB44
I 00226DC65
Record Type 20s and 30s for Pesticides (Col 2) -- Initial Calibration
Single Component -- Individual Standard A (QC Code 'CLM')
20 | |INDAM16|0|CLM| | 18000 JX1201 | 1992 | 04 | 20 | 12 | 46 | | | | 11 | | | 00362366C
21 | | | | | | |INDAM16| | | | | | || | 2.0 | | 003634997
H-80
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
22
4.000364566A
30 | C| 319846 | | | | 1128992 | |A|0.040| | | R| 94 . 7 |
32| | |RT|4.56| | | | | | | | | | |0036687A3
30|C|58899| | | |l040769| |A|0.040| | |R|96.3| |
32| | |RT|5.44|
00368B815
30|C|76448| | | |l070468| |A|0.040| | |R|96.8|
I I I I I |003657868
I 00367A8DC
00369D943
32| | |RT|5.81| | | | | | | M | |00370E873
30|C|959988| | | | 834736 | |A|0.040| | |R|95.7| || | || | I I I I I I I 0037109C3
32| | |RT|8.68| | | || I I I I I |003721905
30|C|60571| | | |842038| |A|0.080| | |R|95.7|
32| | |RT|9.58| | | | | | | | | | [003744874
30 | C| 72208 | | | | 630027 | | A| 0 . 080 | | | R| 98 . 1 |
I II M I (003733932
003756886
32 RT 10. 07
003767882
30|C|72548| | | | 599176 | |A|0.080| | |R|92.6| | || I I I I I I I I I |0037798EO
32| | |RT|11.29|
00378A8E1
30|C|.50293| | | |572605| |A|0.080| | |R|99.2|
32 | | RT | 11. 66 |
00380D91A
'30|C|72435| | | | 237.099 | |A|0.400| | |RI 95 5 I I
32| | |RT|13.33| MINIMI | 00382093E
30 | C| 877098 | | | | 558724 | | A| 0 . 040 | | |R| 96 . 3 |
32| | |RT|2.87| || I I I I I I I |0038439B8
30 |C| 2051243 | | | | 595863 | |A|0.080| I I I I I I I I
32| | |RT|16.33| | | | | | | | | | |003866BB1
H-81
M I 00379C90E
I |00381F94A
003832A85
I I I I |003855BBO
OLM04.2
-------
Exhibit H -- Appendix A
.Format of Records for Specific Uses
4.8 Record Type 20s and 30s for Pesticides (Col 2) -- Instrument Blank (QC
Code 'LIB')
20||PIBLKB2|l|LIB||18000|X1201|1592|04|21|12|19||ML|lOOO|30||[004708102
21| | | | | | |PIBLKB2| | | | | | | | | 2 . 0| |004719422
22 | | | | | | | | | 11000011.0| | | |00472A535
30|C|319846||UG/L|BDL||||\V\0.050\|||||||||||||||00473C55B
30|C|319857||UG/L|BDL|||||U|0.050||||||||||||||||00474E583
30|C|319868||UG/L|BDL|||||U|0.050||||||||||||||||0047505AD
I 30|c|no9769i||UG/L|BDL|11||u|i.o|11 M I M M M 11 I|oo4990B8E
| 30|C|11096825| |UG/L|BDL| | | | |U|l.O| M M M I I M I I II I005002C8F
| ?~30|C|877098||UG/L||0.040\\AJO.2\||||||||||||||M M I005014D94
32| | |RT|2.89| M I M I I I I |005025CC9
| 30|C|2051243| |UG/L|NRP|0.Oil| |A/0.2/| | II I M!| | I | I I | | | I |005038305
32| ||RT|16.35| | | || I I II I I 005049312
4.9 Record Type 20s and 30s for Pesticides (Col 2) -- Method Blank (QC Code
1LRB')
| 20||PBLK58|l|LRB||18000|X1201|1992|04|21|14|31||ML|lOOO|30|||005306672
| 21M | |S| | |FPBLK01|1992|04|17| || | ||2.0| |005317FC3
22||||||||||10000|1.0||||0053290D6
23|||||||||||||||||||||||||P|0|||||||00533B552
| 27| M II I I |F|1991|11|14|09|19|P1248A1|N| M M I I I |00534D468
30|C|319846||UG/L|BDL|||||u|0.050| M M M IM M M I|00535F48C
H-82 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|319857| |UG/L|BDL| | | | |u|0.050| | | | | | | | | I I II I I I0053614B2
30|C|319868| |UG/L|BDL| | | | |u|0.050| | | | | | | | | I I I I I I |0053734DA
30|C|58899||UG/L|BDL|||||U|0.050|||||||||||| MI[005385434
30|C|11096825||UG/LJBDL|||||u|1.0||||||||||||||||005624DF5
30|C|877098||UG/L||0.18||A|0.20||||||||||S|89|||||||0056373E6
32| | |RT|2.89| | | | | || I I I I 00564831B
30|C|2051243| |UG/L| |0 .211 |A|0.20| | | | | | | | | |S|lOO| | | | | | |00565AA3D
32 | | | RT | 16 . 35 | | | | | | | ] | | | 00566BA4A
4.10 Record'Type 20s and 30s for Pesticides -- Matrix Spike Sample (QC Code
LF11)
20||X1201MS|l|LFl||18000|X1201|1992\04|21|16|08||ML|300|30|||00567E66D
2l||||S|||488920|1552|04|17||l952|04|l5||2.0||0056805C7
22| | | | | | | | | |5000|1.0| | | |0056918B8
23||||||||||||||||||MB|1992|04|21|14|31|FPBLK01|P|0|||S|1|R|1|005704FOF
27| | | | | | | |F|1991|11|14|09|19|P1248A1|N| | | | | || I I005716E25
30|C|319846 | |UG/L|BDL| | | | |U|0.050| | | | | | || I I I I I I I |005728E4F
30|C|319857| |UG/L|BDL| | | | |u|0.050| | | | | || II I I I I I I |00573AE7B
30|C|319868| |UG/L|BDL| | | | \U\0.050\ || | I I I I I I I I I I I I00574CEA9
30|C|58899| |UG/L| |0.73 | |A|0.833| | | | |P|88| |D|0| | | | |P112.3| | |00575F7AO
32|||RT|5.43|||||||||||0057606CE
30|C|76448||UG/L||0.65||A|0.833|||||P|78||D|1|||||P|6.2|||005772EF6
32| | |RT|5.81| | M I I I I I I |005783E26
H-83 OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30|C|50293| |UG/L| | 1 . 5 | |A|l.667| | | | | P | 90 | |D | 6 | | | | | P | 0 . 0 | | |00591C120
32 | | |RT|11.66| | | | | | | | | | |00592D12C
30|C|72435| |UG/L|BDL| | | | |U| 0. 50\ \ \ \ \ \ \ \ \ \ \ \ \ \ \ |00593EF8A
30 |C| 53494705 | |UG/L| LLS | 0 . 10 | j| ||||||||
32| | |RT|14.03| | | | |'| | | | | (005952430
30 |C| 7421934 | (UG/L | LLS | 0 . 089 | j| | | | || I I I
32| | |RT|12.34| | | | | | | | | | (0059758C7
005941434
I I I I p I 2 2 I I I 0059648C9
| S | 97 |
(00608C07E
4.11
330 |C| 877098 | |UG/L| | 0. 19\ \ A\ 0. 20 \ \ \ \ | |
^32 | | |RT|2.86| | | | | | | | | | |00609CFBO
30 |C| 2051243 | |UG/L| | 0. 20\ \ A\ 0.20\ \ \ \ \ \ \ \ \ \ S \ 100 \ \ \ \ \ \ | 00610F61C
32| | |RT|16.33| | | | | | | | | | |00611061D
Record Type 20s and 30s for Pesticides -- Matrix Spike Duplicate Sample
(QC Code 'LF2')
20 | |X1201MSD|1|LF2| | 18000 (X1201 | 1952 | 04 | 21 | 16 | 41 | |ML|300|30| | | 0061232C8
21| | | |S| | |488921|1S92|04|17| |1952|04|15| |2.0| (006135223
22| | | | | | | | | |5000|l.0| | | |006146514
23 | | | | | | | | | | | | | | | | | | MB | 1992 | 04 | 21 1 14 | 31 1 FPBLK01 |P|0| | | S'| 1 1 R 1 1 1 006159B6B
27 | | | | | | | |F|1391|11|14|09|19|P1248A1|N| | | | | | | | | 00616BA81
30 |C|319846 | |UG/L|BDL| | | | |U| 0. 050\ | | | | | | | | | | | | | | | 00617DAAB
H-84
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
30 | C| 76448 | |UG/L| |0.66| |A|0.833| |
32| | |RT|5.82| | | | | | | | | | |006238A90
30 | C| 50293 | |UG/L| |l.6||A|
32| | |RT|ll.67| | | | | | | | | | |006371D9D
30|C|72435| |UG/L|BDL| | | | |U|0.50| | |
30 | C| 53494705 | |UG/L| LLS | 0 . 11 | j| | | |
32| | |RT|14.05| | | | | | | | | | |006407171
30|C|7421934| | UG/L | LLS | 0 . 092 | J | | | |
32| | |RT|12.36|
00642A607
30|C|5103719| |UG/L|BDL| | | | |U| O.OSO\\
30|C|5103742| |UG/L|BDL| | | | \\S\0.050\ |
30 | C| 877098 | |UG/L| | 0. 19\ \ A| 0.20 | | |
32| | |RT|2.87| | | | | | | | | | | 006541CEC
30 |C| 2051243 | |UG/L| | 0. 19\ \ A\ 0. 20\ \
32| | |RT|16.35| | | || I I I I I |006565365
|79|D|l|
006227B5F
I I
||||P|0.0|| |006360D90
| | 006383BFB
| P | 12 . 2 | | | 0063 96169
|P|4.3| | | 006419607
| | | | |00643C6FE
I I I I I 00644E7F1
S 96
\ \ \ \ S | 94 |
006530DB9
006554358
H-85
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
4.12 Record Type 20s and 30s for Pesticides (Col 2) -- 72 Hours Aroclor
Standard (QC Code 'CLE')
20 | |AR122102|0|CLE| 1 18000 | X1201 1 1532 1 07. | 20 | 06 | 23 | | | |?| |
21| | | | | | |VAR1221V2| | || II I I I2-0| |002139525
30|C|11104282| |DB/L| \200\ | | | | | | | M | | I I I I I I I I |00214B62E
32| | |RT|3.89| | | || I I I I 1 1 1 00215C641
30|C|11104282| | C7G/L| |200| | | | | | | | | | | | | | | | | | | | |00216E70E
32| | |RT|3.49| | | | | | | | | |2|00217F71E
30|C|lll04282||aG/L||200| | | || || | IIIIIIIIIIH |002181808
32| | |RT|5.67| | | | | | | | | |3|002192825
30|Cllll04282| |C7G/L| |200| | | | | | | | | | | | | | | | | |
| 002128054
32 | | | RT | 7. 05 |
| 4 | 002215916
30 | C| 11104282 | \UG/L\ \200\
| RT | 8. 02 |
|5|0022389FB
30 | C| 877098 | \UG/L\ \ 20 \ \ A| 0 . 040 | | |
32 | | |RT | 2. 86) | | | | | | | | | |00225BA76
30|C|2051243| |DG/L| |20| |A|0.040| |
0022048FE
|0022279EE
| 00224AB44
|00226DC65
32 | | | RT | 16 . 33 |
| 00227EC66
4.13 Record Type 20s and 30s for Pesticides (Col 2) -- Field Sample chosen for
MS/MSD (QC Code 'LSD')
20 | |X120l|l|LSD| | 18000 | X1201 | 1552 | 04 | 23 | 15 | 42 | |ML|400|34| | | 008061655
21
22)
23
| FX1201 | 1992 | 04 | 17 | | 1992 | 04 | 15 | | 2 . 0 | | 0080734FF
|5000|l.0 | 0080847FO
MB 1552 04 21 14 31 FPBLK01 P 2
008097B4F
H-86
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
27| | | | | | | |F|1991|11|14|09|19|P1248A1|N|
30|C|319846| |UG/L|BDL| | | | |u| O.OSO\ | | | | |
30 | C| 319857 | |UG/LJBDL| | | | |U|O.OSO| | | | | |
30|C|6057l| |UG/L|BDL| ||||U|0.
30|C|72559| |UG/L |LLS | 0 . Oil | JP |
32 | | |RT|9.27|
00821EC9B
30|C|72208| |UG/L|BDL| | | | |u| 0.10\ || I I I
30 |C| 33213659 | |UG/L|BDL| | | | |U| 0. 10 \ \ \
30|C|72548| |UG/L|BDL| | | | |U| 0.10\ | | | | |
30|C|11096825| |UG/L|BDL| | | | |U|l.O
30 |C| 877098 | |UG/L| | 0 . 26 | | A| 0.20\ \
32| | |RT|2.86| | | | | | || I I |00851720A
30 | C| 2051243 | |UG/L| | 0 . 28 | | A| 0. 20\
| 008109A65
| I |00811BA8C
00812DAB5
|| | 00819B90E
|P|27.3| | | 00820DD67
I I I 008220ADB
| | | | | j 008232BC6
| | | 008244A21
IIIIIIMI008493D1C
|S|130|||||||0085062D8
|S|140|.
I0085298AO
32| | |RT|16.34|
00853A8AC
H-87
OLM04.2
-------
Exhibit H -- Appendix A
Format of Records for Specific Uses
5.0 TYPE 90 -- COMMENTS RECORD
This record could appear anywhere after the Record Type 10. The comment
on this record will usually apply to the most previous record type. The
example of Record Type 90 below would appear after the Record Type 10 -
indicating the software and version number that was used to generate this
data.
90|CCS SYSTEMS SOFTWARE VERSION 3.5|000023A75
\
H-88 OLM04.2
-------
OLM04.2A
Corrections/Modifications/Clarifications
Corrections:
Exhibit C, Section 1.0 Volatiles Target Compound and contract Required Quantitation Limits
All values under the column "Med. Soil ug/Kg" should be changed from 1200 to 1300. The reason for
this change lies in the fact that the CLP rounding rule has been changed from that used in previous
Statement of Work. The numbers in the "med. Soil" column are derived from calculations based on the
sample preparation protocol of the SOW'. The calculated "non-rounded" value under this column is
1250 ug/Kg. Based upon the previous SOW rounding rule (if number to be retained is an even number
preceding a 5, then number is to be unchanged), 1250 ug/Kg would be rounded to 1200 ug/Kg. The
new rounding rule ( as outlined in Exhibit B, Section 3.3.9, page B-33) stipulates that if the number to
be dropped is 5 or greater, then the number retained should be increased by 1. Based upon this '
requirement, 1250 ug/Kg becomes 1300 ug/Kg.
Contract Modifications:
Exhibit D - Volatiles Appendix B
Modified SW-846 Method 5035 for Volatiles in Low Level Soils
V
1.1 The following statement should be added to the end of the paragraph: (It has been
Superfund's desire to make Method 5035 the predominant method for low level volatile soil analysis.
However, due to technical uncertainties and logistic problems, the method has so far had limited use.
AOC now believes that most of the technical and logistic issues have been resolved, at least on an
interim basis, and therefore will be requesting the Regions to specify the use of the CLP Method 5035.)
7.1.1 Delete 7.1.1 as written and insert the following: Soil/sediment samples should be collected
in the field in either field core sampling/storage containers (i.e. Encore or equivalent) or pre-
prepared closed-system purge-and-trap sample vials as described in Section 9.3. If field core sampling
containers are used, the field should send at least three containers per field sample containing
approximately 5 g each, and at least one 60 mL sealed glass vial containing sample with minimum
headspace. The Contractor shall transfer the contents of the field core sampling containers immediately
upon receipt into the closed-system sample vial prepared as described in Section 9.3 below and record
the date and time of transfer. If pre-prepared closed-system purge-and-trap sample vials are used to
collect samples in the field, the field should send at least two closed-system containers per field sample
containing approximately 5 g each, and at least one 60 mL sealed glass vial containing sample with
minimum headspace. The Contractor is then to proceed to Section 9.3.9 and determine final sample
weight If me minimurn amount of containers have not been sent by the field, the Contractor is to
immediately contact SMO for instructions, note. If MS/MSD analysis are required for a particular
sample, 2 additional field core sampling/storage containers or two additional closed-system purge-and-
trap sample vials should be sent by the field. Contact SMO if insufficient sample for MS/MSD analysis
has been sent by the field.
-------
7.1.2 Change wording to include the following: All samples received in closed-system purge-and-
trap sample vials must be iced or refrigerated at 4° C (+/- 2° Q from time of collection until time of
analysis. Any sample received in field core sampling/storage containers that are not immediately
transferred to a closed-system purge-and-trap sample vial containing sodium bisulfate preservation
solution must be placed in a freezing compartment and held at
-12 ° C (+/- 2 ° C) until time of analysis (see Section 9.3).
7.2.1 Add the following language: The samples must be protected from light and refrigerated at 4
0 C (+/- 2 ° C) ( -12 ° C , +/- 2 ° C, if placed in freezing compartment as stated in 7.1.2) from the time
of receipt until 60 days after delivery of a reconciled, complete sample data package to the Agency.
After 60 days, the samples may be disposed of in a manner that complies with all applicable
regulations.
9.3.1 Add the following note to the end of the paragraph: Note: There should be three field
core sampling/storage containers for each field sample. The contents of two of the field core containers
are to be processed using the steps outlined in 9.3.2 through 9.3.9. One of these prepared samples is
then to be used as the primary sample, while the other is to be used as a back-up sample, if necessary.
The contents of the third field core container shall be transferred to a tared dry closed-system purge-
and-trap container (i.e. no preservative solution or stirring bar is to be added), weighed according to
9.3.9, and then stored in a freezing compartment at -12 ° C (+/- 2 ° C). This sample shall be used for
the medium concentration level methanol extraction procedure as described in Exhibit D-VOA Section
10.1.4.2 if results of the original analysis indicate that medium level extraction is warranted.
9.3.8 Change the language for "Note" to the following: NOTE: Soil samples that contain
carbonate minerals may effervesce upon contact with the acidic preservative solution in the sample vial.
Therefore, if samples are known or suspected to contain high levels of carbonates, a test sample (from
the 60 mL glass vial) should be added to a clean vial and checked for effervescence. If a rapid or
vigorous reaction occurs, the Contractor may discard the test sample and proceed with sample
preparation by transferring the contents of each of the three field core sampling/storage containers into
separate tared dry closed -system purge-and-trap vials (i.e. contains no preservative solution), two of
which should contain stirring bars.§Weigh the vials as per 9.3.9, and then transfer all three vials to a
freezing compartment at -12 ° C (+/- 2 ° Q. If analysis is to begin immediately on the sample, the
contents of one of the field core sampling/storage containers may be transferred to a tared closed-
system purge-and-trap vial containing 5 mL reagent water (no sodium bisulfate). The sample is then
analyzed by the procedure starting at 9.3.9.
9.4 Sample Purge-and-Trap
9.4.1 Change the language to the following: Prior to sample purge, all soil/sediment samples
must be allowed to warm to ambient temperature. For those samples that have been stored in freezing
compartments and that will be analyzed by the low concentration level protocol, 5 mL of reagent water
must be added to the vials without disturbing the hermetic seal of the sample vial (note: an additional 5
mL of reagent water will be added to the vial as per 9.4.2). Shake all vials containing aqueous
solutions gently, to ensure that the contents move freely and that stirring will be effective. Place the
sample vial in the instrument carousel according to the manufacturer's instruction.
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requested to use the preliminary results option judiciously. An attempt will be made to ensure that
appropriate turnaround options are requested and that unnecessary QC and reporting packages are not
performed. Under the new SOW, MS/MSD analysis is not required if the Agency requests that it not
be performed. The lab is requested to make sure that SMO is contacted if there is any question or
concern at all over assigning SDGs.
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