REGION I
LABORATORY DATA VALIDATION
FUNCTIONAL GUIDELINES FOR EVALUATING INORGANICS ANALYSES
Prepared for the
HAZARDOUS SITE EVALUATION DIVISION
U.S. ENVIRONMENTAL PROTECTION AGENCY
Compiled by
Ruth Bleyler
Sample Management Office
VIAR i COMPANY
Prepared by
THE USEPA DATA REVIEW WORKGROUP
Scott Siders - EPA HQ - Co-Chairperson
>e Hankins - EPA Region III - Co-Chairperson
Messina - Laura Scalise - EPA Region II
Gary Bennet - EPA Region IV
Ida Levin - EPA Region V
Mahmoud El Feky - EPA Region VI
Larry Marchin - EPA Region VII
June 13, 1988
Modified by
Deborah Szaro - EPA Region I
Karol-Anne O'Leary - ESAT Region I
EPA Contract No. 68-01-7443
February 1989
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TABLE OF CONTENTS
Pa e
Title Page .1
Table ef Contents ii
List of Appendices IV
Preface . V
Scope of the CLP Routine Analytical Services.... 1
Role of the Reviewer
1.0 INTRODUCTION a
1.1 Overview of the Data Revlew Process 2
1.2 Information Available to the Reviewer 2
1.2.1 The Data Package 2
1.2.2 Information Supplied by the Sampling Team 3
1.2.2.1 Field QA/QC Samples 3
1.2.2.2 Sample De’scr ptions 4
1.2.3 Laboratory Contract Compliance Screening (CCS) 5
1.2.4 Performance Evaluation Samples 6
1.3 The RegIonal/Laboratory Communication Network 6
1.4 The DPO Communication Network 6
1.5 The Data Validation Report &
2.0 PRELIMiNARY REVIEW 18
2.1 The Data Su ary 16
2.2 Usage of Qualifier Codes on the Data Sui riary 16
3.0 INORGANiC VALIDATION PROCEDURE 20
I. Data completeness 21
II. Nolding times 21
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TABLE OF CONTENTS (concluded)
3.0 INORGANIC VALIDATION PROCEDURE
III. Calibration 22
IV. Blanks 2
V. ICP Interference Check Sample 28
VI. Matrix Spike Analysis
VII. Laboratory Duplicate Sample Analysis 33
VIII. Field Duplicate Sample Analysis 34
IX. Laboratory Control Sample Analysis 35
X. Furnace Atomic Absorption Analysis 37
XI. IC? Serial Dilution Analysis 38
XI I. Detection Limits
XIII. Sample Result Verification 41
XIV. Overall Assessment of Data for a Case 42
GLOSSARY A: Data Qualifier Definitions 43
GLOSSARY B: Other Terms 44
LIST OF APPENDICES
Appendix A: Contract Compliance Screening Procedures for RAS
Inorganics Data Package
Appendix B: Contract Compliance Screening — Listing of Defect
Statements
Appendix C: Completed Data Validation Report
Appendix D: Figures
Fig .ire 1: Region I Data Validation Roles
and Responsibilities
Figure 2: Overview of the Data Validation Process
Figure 3: Inorganic Traffic Report
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Figure 4: C1 ain-of-Custody For
Figure 5: Contract Laboratory Program Telephone Record
Log
Figure 6: Data Quality Objectives $u znary Forui
Figure 7: Data Suary Tables
Figure 8: Standard Worksheets
Figure 9: inorganic Regional Data Assessr ent Forn
Appendix E: A Con pleted Inorganic Regional Data Assesst ent ForiT
(IRDA) and Guidance for Completing the IRDA.
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PREFACE
The Laboratory Data Validation Functional Guidelines for
Evaluating Inorgariics Analyses (June 1988 revision) have been modified
for use within Region I. The modifications were performed to delineate
regionally required actions that were not specified in the June 1988
revision. Formats and procedures relating to information transfer
within Region I have also been incorporated. By presenting additional
guidance, this document will assist the reviewer in using profess onai
udgement to make more informed decisions and in better serving the
needs of the data users.
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SCOPE 07 TEE COWTRACT LABOBJiTORY PROGR)J4
ROUTIXE MIkLYTICAL SERVICES
Samples from hazardous waste sites are generally unpredictable,
and may contain high concentrations of contaminants, complex mixtures
of contaminants, and constituents that interfere with the analytical
method. The Routine Analytical Services (RAS) Statement of Work (SOW)
for the Contract Laboratory Program (CL.P) is a contractual step-by-step
method intended to obtain characterization of the contaminants present
at the highest concentration and identification of samples that may
need special methods for proper analysis. The CL? SOW requires a
substantial amount of quality control and complete documentation of all
steps employed during the analysis. This information is necessary for
a reliable validation process, and is essential for litigation.
A major driving force of the CLP is to provide routine analysis
of a large number of samples. For the majority of samples, valid,
usable data are obtained. For those difficult samples, however, CL?
provides sufficient documentation to indicate the nature of the
problem. CL? Special Analytical Services (SAS) can then be employed
to target the analysis problem. The risk of obtaining unusable data
is highest when little site information is known or when interferences
are present. EPA recognizes that the quality of the analytical results
obtained by the same method may not be consistent for all samples.
As presented in this document, the reviewer assumes that the
precision and accuracy of the CLP meets or exceeds the Data Quality
Objectives (DQOs) for the sampling event. it is beyond the scope of
this docunient to compare site-specific DQOs to the data quality
obtained. } owever, the DQO Summary Form enclosed with each data
package should enable the data reviewer to assess site-specific data
usability for particular data sets.
Sumn a rv
1. The CL? analyzes large numbers of potentially complex environ-
mental samples.
2. The SOW requires that analysis be attempted via a rigid protocol.
Under normal circumstances, proper analysis is achieved. When
complex or difficult samples are analyzed, the SOW focuses the
laboratory’s effort on the constituents present at the highest
concentrations. For these samples, the SOW does not require that
minimum detection limits be achieved.
3. The SOW requires a substantial amount of quality control and
documentation as part of the analysis.
4. The required documentation permits full—scale data review by EPA.
ROLE OF TEE RXVIEWER
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Upon completion of analysis, the CLP laboratory sends a replicate
data package to each of the following: the Region requesting the
analysis, EPA’s Sample Management Office (Sf0), and the Environmental
Monitoring Systems Laboratory (ZMSL-LV). It is SMO’s responsibility
to determine whether the laboratory was contractually compliant w t
the SOW through Contract Compliance Screening (CCS) as part of the
government’s right of inspection. On the other hand, the Regional data
reviewer takes the results from the Statement of Work (SOW) analysis,
receives input from the user as to objectives of the sampling effort,
and attempts to determine if the data meet the user’s needs. The
driving force for Regional data validation is that contractually
compliant data are not always technically useful and that contractually
non—compliant data are sometimes very useful.
Throughout this document, date validation criteria are discussed
from four perspectives; technical objective of the criteria, the
criteria itself, evaluation of the criteria, and actions resulting fro-
the review. Once the entire data set has been reviewed, a narrative
report indicating the data quality and identifying specific proble-
areas is written for the user.
Summary
Data review requires that four ob)ectives be simultaneously ccr-
sidered:
1. To assess end summarize the quality and reliability of
CL? data for the user (usability);
2. To document (for the historical record of the site)
factors affecting usability:
a. discrepancies in the data,
b. poor laboratâry practice not regulated in the SOW,
and
c. site locations which are difficult to analyze;
3. To assist regional DPOs in monitoring CL? laboratory
performance and maintaining good lab practices; and
4. To provide program personnel with information concerning
the effectiveness of SOW methods and the CL?, and to
identify problems requiring resolution by headquarters.
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LABORATORY DATA VALIDATXON
ItINCflOWAL GtflDELW B POR ZYALUATING INORGANXCB ANALYSES
1.0 INTRODUCTION
This document is designed to offer guidance in laboratory data
evaluation and validation. In some aspects, it is equivalent to a
Standard Operating Procedure (SOP). In other, more subjective areas,
only general guidance is offered due to the complexities and uniqueness
of data relative to specific samples. These Guidelines have been
updated to include all requirements in the 7/87 Statement of Work (SOW)
for Inorganics.
Those areas where specific SOPs are possible are primarily areas
in which definitive performance requirements are established. These
areas also correspond to specific requirements in Agency contracts and
these requirements are concerned with specifications that are not
sample dependent; they specify performance requirements on matters that
should be fully under a laboratory’s control. These specific areas
include blanks, calibration standards, performance evaluation standard
materials, and tuning. In particular, mistakes such as calculation and
transcription errors must be rectified by resubmission of corrected
data sheets.
This document is intended to provide guidance for technical data
review. Some areas of overlap exist between technical review and
Contract Compliance Screening (CCS); however, contract compliance is
not intended to be a goal of these guidelines. It is assumed that the
CCS is available and can be utilized to assist in the data revie
procedure.
Some requirements are not identical for every Case or batch of
samples. Requirements for frequency of Quality Control (QC) actions
are dependent on the number of samples, sample preparation technique,
time of analysis, etc. Specific Case requirements and the impact of
non-conformance must be addressed on a case by case basis; no specific
guidance is provided.
At times, there may be an urgent need to use data which do not
meet all contract requirements and technical criteria. Use of these
data does constitute either a new requirement standard or full
accQ tance of the data. Any decision to utilize data for which
per±: -zance criteria have not been met is strictly to facilitate the
progress of projects requiring the availability of the data. A
contract laboratory submitting data which are out of specification may
be required to re-run or submit data even if the previously submitted
data have been utilized due to urgent program needs; data which do not
meet specified requirements are never fully acceptable.
The only exception to this requirement is in the area of
requirements for individual sample analysis; if the nature of the
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sample ‘itself limits the attainment of specifications, appropriate
allowances must be made. The overriding concern of the Agency is to
obtain data which are technically valid and legally defensible.
All data reviews must have, as a cover sheet, the inorganic
regional data assessment (IRDA) form (see Appendix D, Figure 9). If
mandatory actions are required, they should be specifically noted on
this form. In addition, this form is to be used to summarize overall
deficiencies requiring attention, as well as general laboratory
performance and any discernible trends in the quality of the data.
(This form is not a replacement for the data review.) Sufficient
supplementary documentation must accompany the form to clearly identify
the problems associated with a Case. The form and any attachments must
be submitted to the Contract Laboratory Program Quality Assurance
Officer (CLP QAO), the Regional Deputy Project Officer (DPO), and the
Environmental Monitoring Systems Laboratory in Las Vegas (EMSL/LV).
It is the responsibility of the data reviewer to notify the
Regional DPO concerning problems and shortcomings with regard to
laboratory data in writing. If there is an urgent requirement, the
DPO may be contacted by telephone to expedite corrective action. it
is recommended that all items regarding a specific case needing DP
action be presented at one time. In any case, the inorganic regional
data assessment form must be completed and submitted.
1.]. Overview of the Data Review Process
in Region I, the CLP DPO provides all data validation training
and oversight of contractor work. The DPO approves data reviewer
qualifications, presents workshops to teach step-by—step data
validation and to introduce new regional guidelines and procedures,
and audits data validation packages for technical content, format, and
accuracy.
Appendix D, Figures 1 and 2 illustrate the normal flow of the data
review process. Sources of information are noted, as well as
communication channels and key decision points in the review process.
1.2 Information ? vpjlable to the Reviewer
1.2.1 The Data Package
A. Objective
The CLP data package is designed to provide all necessary
documentation to verify compliance to the Statement of
Work (SOW) and to enable verification of the accuracy and
reliability of the reported results.
B. Requirements
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Items examined during CCS and contractual quality control
requirements are presented in Appendix A and B of this
document, respectively. A list of the required
deliverables is contained in the 50W.
C. Evaluation Procedure
Procedures for the evaluation of specific deliverables
are referenced in Sections 3 of this document.
D. Action
When contract-required information necessary for data
validation is missing from the date package, the reviewer
should call the laboratory and request the omitted data
according to the procedure referenced in Section 1.3.
Only authorized regional personnel may contact the
laboratory.
1.2.2 Information Supplied by the Saruplinc Team
In order to use this document effectively, the reviewer should
have a general overview of the case at handy the exact number of
samples, their assigned numbers, their matrix, and the number of
laboratories involved for the analysis are essential inforrnatio .
Additional useful information includes the types of waste disposal,
the overall purpose and goals of the sampling investigation, sarple
locations/descriptions (particularly identification of any residential
wells within the sample set), and knowledge of any positive results
from prior on-site sampling efforts. Background information on the
site is very helpful and an effort should be made to obtain these data.
The EPA site project officer or contractor site project manager are the
best sources for answers or further direction.
1.2.2.). Field OA/OC Samoles
A. Objective
Field QA/QC samples, such as trip blanks, equipment
blanks, and field duplicates, enable data reviewers to
evaluate sampling conditions, techniques, and precision.
B. At a minimum, equipment blanks and duplicates must be
included at a frequency of five percent.
C. Evaluation Procedure
The reviewer should evaluate the contamination found in
the blanks as part of the lab method blank review, and
the field duplicate precision concurrent with lab
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duplicate precision evaluation.
D. Action
1. If the laboratory has not provided results for any
of the samples that were shipped, the reviewer should
check the case narrative for a possible explanation
(broken sample, insufficient sample or re-analysis,
etc.). If no explanation is found, the P.5CC should
be contacted to further investigate and resolve the
issue.
2. The sampler should be called if any of the following
problems are noted:
a. equipment blanks or field duplicates not
identified; and
b. anomalies such as traffic report numbers listed twice,
etc.
1.2.2.2 Sarple DescriotJ. ons
A. Objective
Sample descriptions/locations are necessary information
for preparing the data summary tables and for the
evaluation of holding times (see Section 3.2). (In
addition, sai ple descriptions are useful as supplementary
information for the consideration and discussion of
matrix problems and chemical constituents identified in
particular samples.)
B. Requirements
Copies of the traffic reports (see Appendix D, Figure 3)
are mandatory deliverables in the laboratory data
package. In addition, a copy of the chain—of-custody
form (COC) (see Appendix D , Figure 4) may be provided in
the data package or may be available to the reviewer from
the sampling team. Both forms contain the date of
sampling as well as the sampling locations.
C. Evaluation Procedure
Traffic reports and the COC form must be compared for
consistency with respect to the designation of quality
control samples (blanks and field duplicates) and the
identification numbers for field samples.
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D. Action
1. If discrepancies are identified, the sampler should
be contacted for resolution.
2. If information is illegible (sample descriptions or
sampling date), the sampler should also be contacted
to provide a legible copy of this information.
3. If traffic reports are missing, the laboratory should
be contacted for this required deliverable.
1.2.3 Laboratory Contract Comr liance Screening (CCS )
A. Objective
CCS provides a rapid, high volume assessment of
deliverables for technical compliance to contract
requirements. The primary application is to enable a
determination of payment recommendation. Because of this
direct link to payment, CCS fosters a somewhat timely
resolution of contractual problems.
B. Requirements
Items examined by CCS are listed in Appendix A. The
Sample Management Office (SMO) performs CCS on 100
percent of data packages submitted. Laboratories are
required to submit all missing data, and resubmit or
explain all data identified as non—compliant during CCS.
C. Evaluation Procedure
CCS must be used by the reviewer, when available, to
evaluate those technical criteria that are also
contractual criteria and to determine the completeness
of the data package. The CCS results should be previewed
to determine important compliance issues. The reviewer
should compare the findings of the CCS to the laboratory
data package in the course of data validation. A list
of defect statements utilized by CCS is contained in
Appendix B.
D. Action
1. If the CCS is not provided with the data package, it
should be requested through the RSCC. )1owever, data
review can still be initiated without CCS results,
provided the reviewer assesses non- compliance issues
which may affect the usability of the data.
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2. If errors are noted on the CCS, they should be flagged
and forwarded to the attention of the Region I DPO.
3. When a contract—required re-analysis or deliverable
was noted as missing by CCS, the reviewer Should call
the laboratory to find out the expected delivery
date.
1.2.4 Performance Evaluation Samtles
The reviewer should contact the sampler to determine if any PE
Samples were sent with the case. If they were, the reviewer should
obtain all pertinent identification information (i.e. Traffic Report
Nos., EPA identification no., etc.). Once this information s
obtained, the data reviewer should call Cheryl O’Halloran at (617)
860-4614 to obtain the true values of the sample for comparison to the
laboratory results.
1.3 The Regjonal/L.aboratorv Coinnunication Network
A. Objective
In January 1983, the National Program Office established
a system of direct com unication between the regions and
contract laboratories as a routine method for regional
data review staff to obtain answers to technical
questions concerning program data in the timeliest and
most direct manner possible.
B. Requirements
The ground rules for this system are as follows:
1. Regional contact of laboratories is permissible only
after laboratory data submission.
2. Al]. logistical questions involving data delivery?
contractual requirements, procedural recommendations,
and other general matters are to be referred to the
RSCC, to SMO, or to program management (i.e.? OPO)
as appropriate. In addition, re- analysis requests
originating from the data reviewer must be channeled
through the RSCC or the Region I DPO.
3. Only authorized regional personnel may contact
laboratories and they may contact only the specified
laboratory personnel.
C. Procedure
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2.. All conversations between the regions aiid the
laboratories are recorded by both the laboratory and
the regional contact on the CLP telephone record log
(Appendix D, Figure 5).
2 One copy of the telephone record log is forwarded by
the reviewer to each of the following:
- SMO
- the Region I laboratory DPO
— the laboratory
— RSCC
D. Action
1. When requesting information tro the laboratory, the
insistence on short deadlines by the data reviewer
during the initial contact has been shown to be the
priu ary factor in nini izing the time required to get
an answer.
2. The four types of proble ns that require direct
contact between the reviewer and the laboratory for
resolution are illustrated in the attached flow chart
(Appendix D, Figure 2) and are described below:
a. In the case of fussing or illegible deliverables,
the reviewer should call the laboratory to
establish and record the expected due date for
the requested deliverable.
b. When a contract—required re-analysis necessary
for data-validation is nissing, the reviewer
should checX to see if the problenu was noted by
the CCS. If so, the reviewer should call the
laboratory to find out the expected due date.
If the problem was not noted by CCS, the
reviewer, in conjunction with the site project
nuanager, nuust decide whether initiation of a
re-analysis request would provide usable data
(weighing a consideration of holding tinues,
etc.). To initiate a re—analysis request, the
reviewer must contact the RSCC or the Region I
laboratory t PO.
c. Clarification of discrepancies or errors in the
reported data usually requires correction and
re-submission of results by the laboratory. If
the laboratory does not verify the error, then
the reviewer should doublecheck his work to
insure the accurate reporting and qualification
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of data.
d. In some cases, it may be necessary to have the
laboratory provide certain explanations or
details of the conditions of analysis that do
not correspond to any of the SOW required
deliverables. In such cases, a verbal answer is
all that is required of the laboratory.
1.4 The DPO Communication 1 Ietwork
Similar to the above, DPO communications involve contact ‘.ith
pro)ect officers, laboratories, SMO, and data reviewers. The DPO
receives numerous reports from SMO and EMSL-LV. Those which relate
directly and specifically to data review will be forwarded to reviewers
as appropriate. The DPOs will also provide updates to SOW protocols
as they are received.
Inter-regional questions or problems with laboratory performance
are referred to DPOs for resolution. For instance, if Region 1 data
reviewers uncovered a possible contamination problem in a laboratcry
assigned to Region 2, the problem is first referred to the Region 1
DPO who then contacts the DPO in Region 2.
It is recommended that the DPO be notified of all problems and
requirements for a case at one time. If there is an urgent require-
ment, the OPO may be contacted by phone to expedite corrective action.
A data validation report with the ORDA form as a cover page must be
submitted to the DPO to provide documentation of the data review, and
for resolution of inter—regional problems.
2.5 The Data V 1jdation Report
. Objective
The findings of the review are distributed to readers
for three distinct applications: site assessment,
oversight of Contract Laboratory Program (CLP) laboratory
and method performance, and oversight of the data review
contractors performance. For individuals involved in
site-related decisions, it is imperative that the data
validation report present a clear explanation of those
issues affecting the application of the data to the site
investigation. The report must provide the data users
with an overview of data quality, but should also explain
the qualitative confidence and quantitative error
associated with all individual results. In addition, the
date users require a condensed form of the analytical
results which includes all positive sample results,
detection limits, and associated qualifier codes.
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On the other hand, the EPA individuals responsible for
management and oversight of CLP laboratory and method
performance require a presentation of issues related to
laboratory non-compliance, poor laboratory practice not
regulated in the SOW, and any unusual method or
analytical problems.
For both contractual issues and problems affecting the
usability of the data for site assessment, support
documentation must be sufficient to allow EPA to perfox-m
a full—scale review of the data validation in order to
substantiate the report’s conclusions.
B. Requirements
In order to meet the needs of the data users, a four-part
data validation report and an Inorganic Regional Data
Assessment form are the required data validation
del iverables.
1. DQO Sumnarv Form
The DQO Summary Form submitted with the one-month
pro)ections must be included in the data validation
report. An example of a blank form and a completed
form is contained in Appendix D, Figure 6 and
Appendix C, respectively.
2. Memo
This should briefly identify the scope of the
analytical effort, provide a general overview of data
quality, and list and interpret specific problem
areas that affect the usability of the data.
All memos must be addressed to the RSCC and the
Region I DPO must be copied.
The following parameters must be covered in the memo:
— A brief summary of the type and number of samples
analyzed, the case and SDG numbers, the site, the
laboratory that performed the analysis, the type
of analysis performed, whether routine or
non—routine protocols were followed, the
parameters evaluated, and the type and number of
field QC samples included in the sample set.
— A balanced perspective of the data quality must be
provided by summarizing the usable aspects of the data
and areas of compliant laboratory performance, as well
as qualifying problems as having either a major or
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minor inpact on data usability.
For each result which has been qualified, the
enio must identify the associated analytical
problem or quality control criterion which was
not set, and explain the resultant effect on the
data. The e o must clearly differentiate
problems affecting the confidence concerning the
presence of a compound versus those involving
quantitative error. The message to the user
should be conveyed in simple, concise language
that an individual without an extensive
background in analytical chemistry could
understand. The narrative should also list or
reference all changes that the reviewer has made
to the laboratory’s reported data, whetber due
to misidentification or errors in transcription
or calculation. Lastly, the narrative should
identify support documentation attachments and
should include the reviewer’s name and signature.
The for at of the enc, and a brief explanation
of how it is to be conpleted follows:
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MEMO PORMAT
Regional Sample Control Custodian
U.S. Environmental Protection Agency
90 Canal Street
Boston, Massachusetts 02114
Re: Contract/Work Assignment *
Case *, SDG*
Lab Name:
Site Name:
Metals: Isamples/matrices
Cyanide: Isampies/matrices
Dear ______________
A validation was performed on the inorganic analytical data fro’-
I ( matrix ) samples collected by ( contractor ) at the ( name ) site.
The data were evaluated based on the following parameters:
* — data completeness
* — holding times
* — calibration verification
— laboratory and field blank analyses
* — ICP interference check sample results
— matrix spike recoveries
* — laboratory and field duplicates
- laboratory control sample results
* - furnace atomic absorption results
* — serial dilution results
* - detection limit results
* - sample results
* All criteria were met for this parameter.
Table I sumsnari es the validation recommendations which were based
on the following information :
Every parameter that is not starred (*) must have a paragraph
written in the order that they are listed, which explains the
problems encountered, resulting qualifications of data, and impact
on data usability. The following formats must be utilized in the
body of the memo to identify problems with blank contamination and
matrix spike recoveries.
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Flanks
Element Maximum Conc./LJr)jts Action Level
Name xx ugh 5 times xx
Name xy ug/l S times xy
Value > IDL and < Action Level — Report value U
Value > IDL and > Action Level Report value unqualified
Matrix Spike Recoveries
List the percent recoveries of the matrix spikes which did not meet
specified criteria. Only these recoveries need to be included in
the table
TR:s Analyte Percent Recovery
xxxxxx
xxx x xy
A brief paragraph summarizing the actions taken and their
affects on the data usability must be included after each table.
Both the reviewer and the senior reviewer must sign the me o,
and the DPO must be copied (cc:) at the end of the memo.
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Tabl I. Recommendation Summary must summarize all the recommenda-
tions made in the memo that actually affect the sample results, ar
must be geared toward the end user. Where appropriate, the
reviewer must indicate the bias of the result. The followm ng
format is required for the table:
sit. $ams
Cass •
Ta bls I. Rsco msr datiom mary
Aluminum Magnesium
Antimony Manganese
Arsenic Mercury T , P 1
Barium Nickel
Berylium Potassium
Cadr um Selenium
Calcium Silver
Chron ium Am Sodium
Cobalt Thalllum
Copper Vanadium
Iron Zinc
Lead cyanm e
Acceptable flags for use in this table are A, 3, and R. If the
field is left blank the qualifier is A. These flags should be
superscripted to identify problems with individual parameters.
For example:
A - Accept all data.
A’ — Accept data, raise the sample detection limit(s) due to
blank contamination.
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—, Estimate (J) positive values due to poor laboratory
precision.
33 — Estimate (J) positive values and detection limits (UJ) due
to low matrix spike recoveries. These estimated results
would be minimum values.
Estimate (3) all positive values due to holding time
Violations. These estimated values would be minimum Values.
Reject non—detected values due to major holding time
Violations.
In all instances, the worst case supercedes any other qualifica-
tions in the table. For example, if an entire element is rejected
due to holding time violations, the only qualifier that needs to
appear on the table is R, even though other problems may exist with
the calibration, etc. Two qualifiers may be necessary when
positive values are flagged differently than non-detects or when
gi.aalifiers only apply to certain samples. An example of a
completed memo can be found in Appendix c.
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3. Data Summary
Separate tables in Lotus 1,2,3 have been developed
for soil and water analyses and for organies and
inorganics analyses. These tables must include all
positive sample results, IDLs and CRDLs and associ-
ated qualifier codes. Traffic report numbers, sample
locations/descriptions, matrix, concentration units,
site name, case number, and SDG number should be
clearly identified. Examples of the data summary
tables are provided in Appendix D, Figure ? and
Appendix C. Only codes defined by this document are
permitted to qualify data. Should it be necessary
to include other codes, prior approval must be
obtained through the ?egion I DPO. If approval is
given, complete definitions must be supplied in the
key for data summary tables. The glossary of Stan-
dard codes for use in qualifying data as per this
SOP is located in Glossary A.
4. Standard Worksheets
These worksheets must be utilized to perform the data
review. Examples of blank and completed worksheets
can be found in Appendix D, Figure 8 and Appendix C,
respectively.
5. Inorganic Recional Data Assessment Form (IRDA )
The IRDA delineates those issues relating to laboratory
non—compliance, poor laboratory practice, and any
unusual method or analytical problems resulting in
unacceptable or qualified data. The form contains a
checklist of areas verified during the review w .th
notations on data qualification in each area. DPO
Action items must be detailed and documented, with
notations indicating which issues require special
attention or follow-up action. Specific recommended
actions should be noted on the IRDA. An exampie of a
blank form and a completed form is contained in Appendix
D, Figure 9 and Appendix E, respectively. Appendix E
also contains guidance for completing the IRDA.
6. Sumoort Documentation
AIX problems identified either in the narrative report
or on the IR.DA should be documented by the attachment
of laboratory forms, raw data, or reviewer-prepared
tabulations that substantiate the findings and conclu-
sions presented in the text. (On the other hand, it is
15
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not necessary to attach support documentation to
substantiate compliant laboratory performance in cases
where there is no problem with data usability.) It is
recommended that support documentation attachments be
numbered or labeled and referenced accordingly in the
text of the narrative report and on the IRDA. In
addition, it is helpful if the reviewer circles the
specific items of concern located on these attachments.
C. Procedure
Sections 2, 3 and 4 of this document specify the proce-
dures for the preparation of all sections of the data
validation report. As a final step in this process, it
is important that a senior data reviewer check all
outgoing reports for accuracy and completeness, due to
the complexity of the data validation and the importance
of an accurate final assessment of data quality.
D. Distribution
1. A. One copy of the complete four-part validation
report (DQO Summary Form, Memo, Luminary Tables,
and Standard Worksheets) is distributed to:
— the Region I RSCC
— the Region I DPO
B. One copy of the Inorganic Regional Data Assess-
ment For-rn with memo and Support Documentation is
distributed to each of the following:
— the Region I DPO (without memo);
— the DPO for the laboratory that performed the
analysis;
— the EPA HQ Quality Assurance officer; and
— the designated recipient at EMSL—L,v.
(Names and addresses will be forwarded to the
reviewer and periodically updated by the Region I
DPO.)
2. The cognizant EPA contract manager may require the
data reviewer to send a preliminary copy of the
completed data summary, glossary, and sample location
map to the EPA site project officer immediately upon
completion of the reviewer’s evaluation (but prior
to typing and submission of the narrative with the
rest of the sampling investigation report).
16
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E. Actior
EPA will review and co ent upon contractor-prepared data
vaJ idation reports. Resubmission of data validation
reports ay be required in cases where the required
format and procedures were not followed, or when
clarifications or corrections are needed.
17
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2.0 PR.ELIMINARY REVIEW
2.1 The Data Summary
A. Objective
The purpose of the data summary is to provide a simple,
condensed form of the analytical results to the user,
which enables a quick evaluation and comparison of the
constituents identified at the various sampling boa-
tions.
B. Requirements
Requirements have been addressed above under Section 1.5.
C. Procedure
Transcribe the results from the Form Is Onto the data
summary tables (for samples of data summary sheets see
Appendix D, Figure 7). Do not transcribe the qualifi—
cation codes used by the laboratory (eg. N, *, or B). The
reviewer will fill in the usability qualifiers which have
been determined through the validation process.
C. Action
As appropriate, information will be added to or deleted
from the data summary during the course of data valida-
tion.
2.2 Usage of Qua ifjer Codes on the Data Summary
A. Objective
The data qualifier codes presented in Glossary A identify
the degree of confidence concerning the presence (or
absence) of reported analytes and identify results that
are considered to be quantitatively inaccurate. These
codes have been regionally standardized to insure that
contractors throughout the region all employ the same set
of simple, concise definitions that are understandable
to personnel within the various EPA branches.
B. Requirements
1. Only codes defined in Glossary A are permitted to
qualify data. Should it be necessary to include
other codes, prior approval must be obtained through
the Region I DPO.
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2. In general, only one qualifier code is permitted with
each reported result. The following hierarchy has
been developed to insure that only the most important
code is used in situations where more than one
quality control problem is associated with an
analytical result:
a. Codes relating to identification take precedence
ever codes related to quantitation. Thus,
whenever a positive result is qualified with an
R, the 3 code will not be used. Also, whenever
a not-detected result is qualified with an P , the
code U3 will not be used. The qualifier R should
reolace any numerical value that the laboratory
reported.
b. Within each of the two categories of codes, the
code that indicates a more serious problem with the
data takes precedence.
3. The above restriction on the use of multiple
qualifiers for a single result is applicable only to
the data summary and not to the narrative report.
(The narrative should mention major, as well as
minor, problems associated with individual results,
using appropriate emphasis.)
4. Positive sample results <2xIDL and 2XIDL
and
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3.0: INORGANIC DATA VALIDATION PROCEDURE
The requirements to be checked irt validation are listed below
(“CCS” indicates that the contractual requirements for these itens
will also be checked by CCS; CCS requ rements are not always the
same as the data review criteria.)
I. Data Completeness
II. Holding Times (CCS checks Lab holding times only)
III. Calibration
— Initial (CCS)
- Continuing (CCS)
IV. Blanks (CCS)
V. ICP Interference Check Sample (CCS)
VI. Matrix Spike Sample Analysis (CCS)
VII. Laboratory Duplicates Sample Analysis (CCS)
VIII. Field Duplicate Sample Analysis
Ix. Laboratory Control Sample Analysis (CCS)
X. Furnace Atomic Absorption Analysis (CCS)
XI. ICP Serial Dilution Analysis (CCS)
XII. Detection Limits (CCS)
XIII. Sample Result Verification (CCS 10%)
XIV. Overall Assessment of Data for a Case
20
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1. D iTA COMPLZTENE88
Check that the data package is complete and Contains all the
required deliverables listed in SOW 7/87.
If any of the required data are missing, contact the laboratory
to regi. est the information and prepare a Telephone Record Log.
Review CCS results to see if a request was made for missing
information and find out the expected delivery date.
II. BOLDX) G TIXZB
A. Objective
he objective Is to ascertain the validity of results based
on the holding time of samples from tii e of collection to
time of analysis or sample preparation, as appropriate.
B. Criteria
Technical requirements for sample holding times (} T) have
only been established for water matrices. The holding times
for soils are currently under investigation. Until the
results are available, the holding times for water matrices
should be applied to soil matrices. The following holding
time and preservative requirements were established under
40 CFR 136 1:Clean Water Act) and are found in Volume 49.
Number 209 of the Federal Register, page 43260, issued
October 26, 1984. Preservation refers to waters only.
METALS: 6 months; preserved at pH<2
MERCURY: 28 days; preserved at pH<2
CYANIDE: 14 days; preserved at pH l2
C. Evaluation Procedure
Actual holding times are established by comparing the san-
pling date on the EPA Sample Traffic Report with the dates
of analysis, these dates can be found in the laboratory raw
data. Examine the sample records to determine if samples
were properly preserved.
METALS: HT (Days)— Analysis Date — Sampling Date
MERCURY: liT (Days) — Analysis Date - Sampling Date
CYANIDE: WI’ (Days) — Analysis Date — Sampling Date
NOTE: folding times for Cyanide are calculated based on
the date of analysis and not on distillation date.
If the samples were distilled within holding times
and analyzed a couple days later it may be accept-
21
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able to use the data unqualified. However, if
several days pass between distillation and
analysis, the data may be questionable and need to
be qualified. Professional udgement must be used.
D. Action
1. If 40 CFR 136 criteria for holding times and preser-
vation are not met, qualify all positive results as
estimated (J) and results below the Instrument
Detection limit (IDL) as estimated (UJ).
2. If } olding times are grossly exceeded, the reviewer
must use professional udgement to determine the
reliablity of the data and the effects of additional
storage on the sample results. The reviewer may
determine that non—detect data are unusable (R).
III. CALXDR TION
A. Objective
Cornpi.i nce requirements for satisfactory instrument
calibration are established to ensure that the instrument
is capable of producing acceptable quantitative data.
Initial calibration demonstrates that the instrument is
capable of acceptable performance at the beginning of the
analysis run, and continuing calibration verification docu-
ments that the initial calibration is still valid.
B. Criteria
1. Initial Calibration
Instruments must be calibrated daily, and each time
the instrument is set up.
a. IC? Analysis
A blank and at least one standard must be used in
establishing the analytical curve.
b. Atomic Absorption Analysis (AA)
A blank and at least three standards, one of which
must be at the Contract Required Detection Limit
(CRDL), must be used in establishing the calibra-
tion curve.
The correlation coefficient must be 0.995.
22
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c. Mercury Analysis
A blank and at least four standards must be used
in establishing the analytical curve.
The correlation coefficient must be O.995.
d. Cyanide Analysis
A blank and at least three standards must be used
in establishing the analytical curve.
A correlation coefficient O.995 is required for
photometric determination.
At least one mid-point standard must be distilled
before analysis.
2. Initial and Continuing Calibration Verification
a. An EPA certified standard must be used for the
Initial Calibration Verification (ICV) and must
be analyzed for each wavelength used for analy-
sis.
b. Analysis results must fall within the control
limits of 90-llO%R of the true value for all
analytes except mercury and cyanide.
c. Analysis results for mercury must fall within the
control limits of 80-120%R.
d. Analysis results for cyanide must fall within the
control limits of 85—l15%R.
e. A CCV must be analyzed every ten samples or every
2 hours whichever is more frequent.
f. o verify linearity near the CRDL for ICP analy-
sis, the contractor must analyze a standard at 2
times the CRDL or 2 times the IDL. whichever is
greater. There are no specific acceptance criteria
for the standard at the present time. Professional
judgement must be used in qualifying the data.
C. Evaluation Procedure
I.. Verify that the instrument was calibrated daily and
each time the instrument was set up using the correct
nunber of standards and a blank.
23
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2. Verify that a standard at the CRDL. was used in the kk
calibration curve or that a standard at the CRDL was
analyzed at the beginning of the analysis run.
3. Verify the correlation coefficient is 0.995 for all
hA, Hg, and CN analyses.
4. Check the distillation log to verify that a u id-range
standard was distilled for cyanide analysis.
5. Verify that an EPA certified standard was used for the
Icy for all analyses.
6. Verify that all ICy and CCV recoveries fall within the
required windows.
7. Check the raw data to verify that the calibrat .on
standard values were transcribed correctly on to Forr
I I . Recalculate one or more of the ICy and CCV per-
cent recoveries (%R) using the following equation and
verify that the recalculated value agrees with the
laboratory reported values on Form hA. Due to
possible rounding discrepancies, allow results to fall
within 1% of the contract windows.
Found X 100
True
Where,
Found concentration (in ug/L) of each ana].yte meas-
ured in the analysis of the ICV or CCV
solution.
True concentration (in ug/L) of each analyte in the
ICV or CCV source.
8. Verify that a CCV was analyzed every 10 samples or
every 2 hours.
9. Verify that a standard at 2xCRDL or 2xIDL, whichever
is greater, was analyzed to verify linearity near the
IDL for IC? analysis.
D. Action
1. If the appropriate number of standards were not used
for the initial calibration or if the instriment was
not calibrated daily and each time the instrument was
setup, professional judgement must be used to qualify
the data. It may be necessary to qualify the data as
unusable (R).
24
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2. If a standard at the CRDL was not used in establish-
ing the calibration curve for AA, positive results up
to 2xCRDL and non-detected results may have to be
estimated. Exa ine the recoveries of any low level
standards analyzed during the analysis scheme in order
to make judgements on the accuracy of the calibration
curve at the low end.
3. If the correlation coefficient is cO995 for AA, Hg,
or CN, qualify results >IDL as estimated (a), and non-
detected results as estimated (U3).
4. If a mid range standard for cyanide was not distilled
before analysis or did not meet the 10% criteria, use
professional judgement to qualify the date. It may be
necessary to estimate results if it appears the
distillation procedure has a significant impact on
sample results.
5. If an EPA standard was not used for the ICV, check the
source of the standard used. The ICy must be fror a
different source than the CCV or the data is ques-
tionable.
6. If the ICy or CCV %R falls outside the acceptance win-
dows, use professional judgement to qualify all
associated data. The following guidelines are recon-
mended:
a. If the ICy or CCV %R falls outside the acceptance
windows but within the ranges of 75-89%, or 111-
125% (CM, 70—84% or 116—130%; Hg, 65—79% or 121—
135%), qualify results >IDL as estimated (fl.
b. If the ICy or CCV %R fall outside the acceptance
windows but is within the range of 111-125% (C1 ,
116—130%; Hg, 121—135%), non-detected results are
not qualified.
C. If the ICy or CCV %R is 75%—89% (CM, 70—84%; Hg,
65-79%), qualify non—detected results as estimated
(UJ).
d. If the ICy or CCV %R falls outside the range
of 75—125% (CH,70—130%; Hg, 65—135%), qualify all
associated results as unusable (R).
7. It the CCV was not analyzed at the required intervals,
use professional judgement to qualify the data. The
data may be unaffected.
25
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8. If the 2xCRDL standard for ICR a s not within ±20% of
the true value, results near the CRDL are questionable.
Estimate (.7) positive results less than 3xCRDL and (U3)
non—detected results.
IV. BLJJ S
The assessment of blank analysis results is to determine the
existence and magnitude of contamination problems. The cr1-
teria for evaluation of blanks applies to any blank associated
with the samples. If problems with y blank exist,(ie. prep
blank, calibration blank, equipment blank, or trip blank) all
data associated with the Case must be carefully evaluated to
determine whether or not there is an inherent variability in the
data for the Case, or if the problem is an isolated occurrence
not affecting the data.
B. Criteria
1. } o contaminants should be detected in the blanks.
2. A preparation blank must be analyzed for each matrix,
for every 20 samples digested, or for each batch
digested, whichever is more frequent.
3. A calibration blank (CCB) must be analyzed after every
ten samples or every 2 hours, whichever is more
frequent.
C. Evaluation Procedure
1. Review the results reported on the Blank Summary (FonT
III) as well as the raw data (IC? printouts, strip
charts, printer tapes, bench sheets, etc.) for all
blanks and verify that the results were accurately
reported.
2. Verify that the calibration blanks and prep blanks were
analyzed at the proper frequency.
3. Report results >IDL for any trip blanks or equipment
blanks taken with the Case.
D. Action
1. Action in the case of unsuitable blank results depends
on the circumstances and origin of the blank. Any
blank with a value below the negative IDL must be
carefully evaluated to determine it’s effect on the
sample data. Blanks that are >2x the negative IDL
26
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indicate instrumental problems. The possibility of
false negatives exist , therefore the associated data
must be qualified.
2. In instances where more than one blank is associated
with a given sample, qualification should be based upon
a comparison with the associated blank having the
highest concentration of a contaminant. The result
must fl be corrected by subtracting any blank value.
Action levels should be calculated that are 5 times the
maximum concentration of each contaminant detected in
any blank. ) o positive sample results should be
reported unless the concentration of the analyte in
the sample exceeds 5 times the amount detected in any
blank.
NOTE: The reviewer should note that the blank analyses may
not involve the same weights, volumes, or dilution factors
as the associated samples. In particular, soil sample
results reported on Form I will not be on the same basis
(units, dilutions) as the calibration blank data reported
on Form III or the aqueous field blank. Sample weights,
volumes, and dilution factors must be taken into considera-
tion when applying the Sx criteria. The reviewer may find
it easier to work from the raw data when applying the 5x
criteria to soil sample data/calibration blank data.
Sample results should be reported as follows:
a. If an analyte is detected in the blank but not in
the sample no action is taken.
b. Positive results less than the action level shall
be reported with a U.
c. Positive results greater than the action level
shall be reported unqualified.
4. The following are examples of applying the blank
qualification guidelines. Certain circumstances may
warrant deviations from these guidelines. However. DPO
approval for any deviation is required.
EXAMPLE 1:
Blank Result 7
IDL 5
Action Level 35
Sample Result 22
Qualified Sample Result 22 U
27
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The sample result is > DL but c the Action Level. Positive
results less than 35 are qualified as non—detects.
EXAiIPLE 2:
Blank Result 10
IDL 8
Action Level 50
Sample Result 70
Qualified Sample Result 70
The sample result is greater than the IDL and the Action
Level so no qualifiers are necessary.
V. CP ]NrE7ER NCZ CBEC7 SAMPLE
A. Objective
The ICP Interference Check Sample (ICS) Analysis is
performed to verify the contract laboratory’s interelenent
and background correction factors.
B. Criteria
1. An 1CS must be run at the beginning and end of each
sample analysis run or a minimum of twice per 8 hour
working shift, whichever is more frequent.
2. Results for the ICS solution AB analysis must fall
within the control limits of ± 20% of the true value.
C. Evaluation Procedure
1. Verify the ICS was analyzed at the proper frequency.
2. Verify the %R for the ICS is 80-120%.
. Recalculate from the raw data one or more recoveries
using the following equation and verify that their
calculated value agrees with the laboratory reported
values on Form IV.
ICS %R Found Solution AB X 100
True Solution AB
Where,
Found Solution AB concentration (in ug/L) of each
analyte measured in the analysis
of solution AB.
28
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True Solution AB concentration (in ug/L) of each
analyte in solution AB.
NOTE: The ICS solution ay be diluted to bring the
levels of the interferents (Ca, Mg, Fe, Al) within the
linear range of the instrument. Dilutions may not be
used for quentitation of any other elements.
4. Check ICS raw d ta for results with an absolute value
>IDL for those analytes which are not present in the
ICS A solution. Results greater than twice the
absolute value of the IDL indicate either a positive
or negative interference and must be qualified.
D. Action
1. If the ICS was not analyzed at the proper frequency the
data may be affected. Use professional judgement to
qualify the data.
2. For samples with concentrations of Al, Ca, Mg, and Fe
which are 50% or more than their respective levels in
the Interference Check Sample, the following actions
are recomnended:
a. If the ICS recovery for an element is >120% and
the reported sample results are non—detected, data
are acceptable for use.
b. If the ICS recovery for an element is >120% and
the reported sample results are >IDL, qualify the
affected data as estimated (J). Results may be
biased high.
c. If the ICS recovery for an element falls between
50 and 79% and reportable quantities of the
analyte were detected, qualify the affected data
as estimated ( ). Results may be biased low.
d. If an analyte is not detected in the sample, and
the ICS recovery for that ana].yte falls within the
range of 50-79%, the possiblity of false negatives
may exist. Qualify the data for these samples as
estimated (U3).
e. If ICS recovery results for an element are cSO%,
qualify the data as unusable (R).
3. If results >IDL are observed for elements which are
not present in the EPA provided solution, the
possibility of false positives exists. An evaluation
29
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of the associated sample data for the affected elements
should be made. Sample results > 2xIDL with levels
of interferents that are 50% or more of the levels
found in the ICS solution should be qualified as es-
timated (3). Certain circumstances may warrant rejec-
tion of the data (R) if it is impossible to determine
whether the sample result is due entirely to inter-
ferences or not.
4. If negative results with absolute values >2xIDL are
observed for elements which are not present in the EPA
ICS solutions, the possibility of false negatives in
the samples may exist. An evaluation of associated
sample data should be made. For samples with levels
of interferents that are 50% or more than the levels
found in the ICS solution all results for the affected
analytes which are reported as non—detected should be
qualified as (U3).
5. In general, the sample data can be accepted if the
concentrations of Al, Ca, Mg, and Fe in the samples
are found to be <50% of their respective concentrations
in the ICS. } owever, if other elements are present in
the sample at >10 mg/L, the reviewer should investigate
the possibility of other inter— ference etfects by
using Table 2 given on page D-22 of the 7/87 SOW.
These analyte concentration equivalents presented in
the references should be considered only as estimated
values, since the exact value of any analytical systert
is laboratory specific. Therefore, estimate the
concentration produced by an interfering element. If
the estimate is >2X CRDL. and also greater than 10% of
the reported concentration of the affected element,
qualify the affected results as estimated (3).
The following are examples of estimating interferences and
qualifying affected data.
EXAMPLE 1:
A positive result of 1050 ug/L was detected for Antimony in
the ICS solution although there should not be any Antimony
present in the solution. A review of sample concentrations
indicate the levels of interferents in the samples are at
least 50% of those found in the ICS solution (300,000 ug/L
Aluminum and 150,000 ug/l Iron). Positive results for
Antimony must be estimated (3) since they may be due to
interferences from Iron or Aluminum.
30
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Aluminum Result 300,000
Iron Result iso,ooo
Antimony Result 700
Qualified Antimony Result 700 3
EXAMPLE 2:
Samples contain 30,000 ug/L Vanadium. Table 2 on page D-
22 of SOW 7/87 indicates the iriterelement interference
factor for Vanadium on Beryllium is 0.05 mg/L Beryllium for
every 100 mg/L of Vanadium. Estimating the concentration
of Beryllium which is due to Vanadium yields a result of:
30,000 ug/L X 0.05 m /L — 15 ug/L. Beryllium.
100 mg/L
Vanadium Result 30,000
Reported Beryllium Result 70
Estimated Interference 15
Qualified Sample Result 70 3
The estimated concentration of Beryllium signal due to the
interference of Vanadium is >2xCRDL and >10% of the
reported concentration therefore the reported value is
estimated (3).
VI. MATRIX SPIKE SAMPLE ANALYSIS
A. Objective
The matrix spike sample analysis is designed to provide
information about the effect of the sample matr x on the
digestion and measurement methodology.
B. Criteria
1. Samples identified as field blanks cannot be used for
spiked sample analysis.
2. Spike recovery (%R) must be within the limits of 75-
125%. However, spike recovery limits do not apply when
sample concentration exceeds the spike concentration
by a factor of 4 or more.
3. 1! the matrix spike recovery does not meet criteria,
a post—digestion spike is required and reported on Form
VB for ICP, Flame, Mercury and Cyanide. (Post
digestion spikes are also required for all furnace
analyses but recoveries are reported on the raw data.)
31
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In some cases post digestion spike data ay aid in
evaluating matrix interferences. This information must
be included in the DPO report.
C. !valuation Procedure
1. Review Form V and verify that results fall within the
specified limits.
2. Check raw data and recalculate one or more %R using
the following equation to verify that results were
correctly reported on Form V.
( SSR—SR ’ X 100
SA
There,
SSR = Spiked Sample ?esult
SR = Sample Result
SA = Spike Added
3. verify that the field blank was not used for spike
analysis.
4. Verify that a matrix spike was prepared at the proper
frequency.
5. Ver .fy that a post—digestion spike was performed for
all aralytes th unacceptable pre—digestion spike
recovery.
D. Action -
1. If the spike recovery is >125% and the reported sample
results are non-detected, the data are acceptable for
use.
2. If the spike recovery is >125% or <75% and the reported
sample levels are >IDL, qualify the data as estimated
(3).
3. If the spike recovery falls within the range of 30-74%
and the sa ip1e results are non-detected, qualify the
data for these samples as estimated (UJ).
4. If spike recovery results fall <30% and the sample
results are non-detected, qualify the data as unusable
(R).
5. If the field blank was used for matrix spike analysis,
all, other QC data must be carefully checked and
32
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professional judgement exercised when evaluating the
data.
NOTE: Amy action taken applies to J, samples of the same
matrix.
VII. DUPLICATE BAXPI2 (ALYaIB
A. Objective
Duplicate analyses are indicators of the precision of the
sample results.
B. Criteria
1. Samples identified as field blanks cannot be used for
duplicate sample analysis.
2. A control limit of ± 20% (35% for soil) for the Rela-
tive Percent Difference (RPD) shall be used for sa ple
values > 5 times the CRDL.
3. A control limit of ± CRDL (± 2xCRDL for soil) shall be
used for sample values less than 5 times the CRDL,
including the case when only sample value is <5x
CRDL or when one sample is above the IDL. and one s
non-detected.
4. A duplicate sample must be prepared and analyzed for
every 20 samples, for every batch digested, or for
every matrix, whichever is more frequent.
C. Evaluation Procedure
1. Review Form VI and verify that results fall within
the control limits.
2. Check the raw data and recalculate one or more RPD
using the following equation to verify that results
have been correctly reported on Form VI.
RPD S-D X 100
(S+D)/2
Where,
S Original Sample Value
Duplicate Sample Value
33
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3. Verify that the field blank was not used for duplicate
analysis.
4. Verify that duplicates were prepared at the required
frequency.
D. Action
1. If duplicate analysis results for a particular analyte
fall outside the appropriate control windows, qualify
results > IDL for that analyte in all samples of the
same matrix as estimated (1).
2. If the field blank was used for duplicate analysis,
all other QC data must be carefully checked and
professional judgement exercised when evaluating the
data.
VIII. FIELD DUPLICATES
A. Objective
Field duplicate samples may be taken and analyzed as an
indication of overall precision. These analyses measure
both field and lab precision: therefore, the results may
have more variability than lab duplicates which measure only
lab performance. It is also expected that soil duplicate
results will have greater variance than water matrices due
to thfficulties associated with collecting identical field
sanpies.
B. Criteria
A control limit of +30% (50% for soil) for the RPD shall be
used for sample \‘alues >5xCRDL.
A control limit of ±2XCRDL (4XCRDL for soil) shall be used
for sample values < 5xCRDL.
C. Evaluation Procedures
Samples which are field duplicates should be identified us-
ing EPA Sample Traffic Reports or sample field sheets. The
reviewer should compare the results reported for each sample
and calculate the Relative Percent Difference (RPD), if
appropriate.
NOTE: The appropriate person should be contacted to
determine whether field duplicates were taken during
sampling.
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D. Action
If field duplicate analysis results for a particular analyte
fall outside the appropriate control windows, qualify
results >IDL for that analyte in all samples of the sane
matrix as estimated (J).
IX. LABORATORY CONTROL 8MPL! JIALYBIB (LCB)
A. Objective
The laboratory control sa ple analysis is designed to serve
as a monitor of the efficiency of the digestion procedure.
B. Criteria
1. All aqueous LCS results must fall within the control
limits of 80-120%R. According to SOW 7/87 Antimony and
Silver are excluded from this criteria. For validation
purposes the ±20% limit will be applied to both
Antimony and Silver.
2. All solid LCS results must fall within the contrc’2
limits established by the EPA. The 80-120% criteria
is not applied to the soil LCS.
3. An LCS must be prepared and analyzed for each matrix,
for each batch of samples digested, or for every twenty
samples, whichever is more frequent.
C. Evaluation Procedure
1. Review Form VII and verify that results fall within
the control limits.
2. Check the raw data to verify reported results on Form
VII. Recalculate one or more of the recoveries using
the following equation.
LCS %R — L.CS Found X 100
ISCS True
Where,
LCS Found concentration (in ug/L for aqueous, mg/kg
for solid) of each analyte measured in the
analysis of the LCS solution.
35
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LCS True — concentration (in ug/L for aqueous,
mg/kg for solid) of each analyte in the
LCS source.
3. Verify that an LCS was prepared and analyzed at the
proper frequency.
D. Action
1. Aqueous LCS
a. If the LCS recovery for any analyte (including Sb
or Ag) falls within the range of 50—79% or >120%,
qualify results >IDL as estimated (3).
b. If results are non-detected and the IJCS recovery
is greater than 120%, the data are acceptable for
use.
c. If results are non-detected and the LCS recovery
falls within the range of 5Q 9%, qualify the data
for these samples as estimated (UJ).
c i. If L .CS recovery results fall <50%, qualify all data
as unusable (R).
e. If an LCS was not analyzed at the proper frequen-
cy, professional judgement must be used to qualify
the data. ) atrix spike recovery may also indicate
digestion efficiency. Provide explanations in the
memo for all actions taken.
2. Solid LCS
a. If the solid LCS recovery for any analyte falls
outside the EPA control limits, qualify all
results I L as estimated (J).
b. If the L CS results are higher than the control
limits and the samples are non—detected, no
qualifiers are necessary.
c. If the LCS results are lower than the control
limits, qualify all non—detected results as
estimated (U). Results may be biased low.
3. If an LCS was not analyzed at the proper frequency,
evaluate the affect on the sample data and qualify
accordingly.
36
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Z. Ft7RNACE ATOMIC ABSORPTION AN LY8IS
A. Objective
Duplicate injections and furnace post—digestion spikes es-
tablish the precision and accuracy of the individual
analytical deter inations.
B. Criteria
1. For sample concentrations >CRDL, duplicate injections
must agree within ± 20% Relative Standard Deviation
(RSD), or Coefficient of Variation (CV), otherwise the
sample must be rerun once (two additional injections).
2. Spike recovery must be 85% and j. .]15%.
3. If post—digestion spike recovery is not within 85-
115% and sample absorbance is ‘ 50% of spike absor-
bance, the Method of Standard Addition is required.
The sample must be spiked with standards at 50, 100 and
150% of the sample absorbance.
C. Evaluation Procedure
1. Check raw data to verify that duplicate injections
were performed and agree within ± 20 % R.SD (or CV) for
sample concentrations >CRDL.
2. Review Furnace AA raw data to verify that the Furnace
Atomic Absorption Scheme, as described in SOW, p.E-15,
has been followed.
3. Verify the ..percent recoveries were calculated cor-
rectly *
4. Verify that all required ?ISA results are reported on
Form VIII and check that the correlation coefficients
and sample results are calculated correctly.
D. Action
1. If duplicate injections are outside the required
criteria and the sample has not been rerun once as
required, qualify positve results as estimated (J).
2. If the rerun sample results do not agree within ± 20%
RSD or CV, qualify the positive results as estimated
(.7).
37
-------
3. If sample absorbance is <50% of the post—digestion
spike absorbance then:
a. For sample results >IDL, if the furnace post-
digestion spike recovery is n within 85-
115%, qualify the sample results as estimated (J).
b. For non-detected results, if the furnace post-
digestion spike recovery is >10% but <85%, qualify
the sample result as estimated (U3).
c. If post—digestion spike recovery <10%, qualify
positive results and non—detected results as
unusable (R).
4. If Method of Standard Addition (MSA) is required but
has not been done, qualify the positive results as
estimated (3).
5. If any of the samples run by MSA have not been spiked
at the appropriate levels, qualify positive results as
estimated (3).
6. If the MSA correlation coefficient is <0.995, qualify
the positive results as estimated (3).
XI. ICP SERIAL DILeTION ANALYSIS
A. Objective
Serial dilution analysis determines whether significant
physical or chemical interferences exist due to sample
matrix.
B. Criteria
1. If the analyte concentration is sufficiently high (con-
centration in the original sample is minimally a factor
of 50 above the IDL) the laboratory is required to
report the results of a five fold dilution. Results
that do not agree within 10% of the original results
are flagged with “E” by the laboratory. For validation
purposes, the criteria for action is 15%.
2. A serial dilution is required for each matrix analyzed.
3. 11 the sample used for the serial dilution had to be
diluted for any elements in order to bring the result
within the linear range of the instru ent, an addition-
38
-------
al five fold dilution is required for evaluating matrix
interferences for that particular element.
C. Evaluation Procedures
1. Verify that reported results for the serial dilution
meet required criteria of ± l0%D.
2. Check the raw data and recalculate the %D using the
following equation to verify that the dilution
analysis results agree with inItial sample results
reported on Form IX.
X 100
I
Where,
I Initial Sample Result
S Serial Dilution Result (Instrument Reading X 5)
3. Check the ra data for evidence of negative inter-
ference, i.e. results of the undiluted samples are
significantly higher than the original sample.
D. Action
1. If the percent difference between results is 15%, and
the result of the diluted sample is greater than that
of the undiluted sample qualify positive results (3)
and non-detetced results as estimated (UJ). A
supression due to sample matrix has resulted in the
reported results being biased low.
2. If evidenc& of negative interference is found, use
professional judgement to qualify the data. Positive
results only need be estimated (3).
XII. DETECTION LIKITB
A. Objective
Instrument Detection Limits reported on Form XI are used for
reporting the detection limit for all sample analyses. Any
value less than the IDL is considered non—detected.
B. Criteria
1. IDLs must be less than the CRDL for all elements.
39
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2. ICP or other methods may be used that do not have IDI.,s
that are less than the CRDLs n y if all sample results
are greater than 5xIDL, for that instrument.
3. IDLs must be multiplied by dilution factors and prep
factors before being reported on Form I and the data
sum mary tables.
C. Evaluation
1. Verify the instrument detection limits are present on
Form XI for all elements and are less than the CRDLs.
2. Verify that results for all parameters are reported
down to the IDL not CRDL on Form I.
3. Verify that any sample weights, volumes, and dilutions
are taken into account when reporting the detecticn
limit for all samples.
4. Verify that sample results are >5XIDL if IC? analysis
results are used for As, Ti, Se, or Pb.
NOTE: When the laboratory provides both ICP and CFA.A results
for an analyte in a sample and the concentration is >ICP IDL,
the results can assist in identifying quantitatjo problems.
D. Action
1. If the IDL is not less than the CRDL notify the DPO
that the laboratory is not meeting contractual
requirements. Use the laboratory’s IDL as the
detection limit on the data summary tables.
2. Change any, results on the data summary tables for
samples on Form I that are not reported down to the IDL
or do not use proper dilution/prep factors.
3. Estimate (J) or Reject (R) any positive results or non-
detected results for As, Ti, Se, or Pb that are
analyzed by IC? but are not greater than 5xIDL.
XIII. BAJIPLE P.ISØLT VERIFICATION
A. Objective
The objective is to ensure that the reported quantitation
results are accurate.
40
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B. Criteria
Analyte guantitation must be calculated according to the
appropriate SOW.
C. Z valuation Procedure
The raw data should be examined to verify the correct
calculation of sample results reported by the laboratory.
Digest on and distil etion logs, instrument printouts, strip
charts, etc. should be compared to the reported results on
Form I.
l. Examine the raw data for anomalies (ie., baseline
shifts, negative absorbances, omissions, legibility,
etc.).
2. Verify that there are no transcription or reduction
errors (eg.,. dilutions, percent solids, sample
weights).
3. Verify that results fall within the linear range of
the C? (Fox-rn XIII) and within the calibrated range
for the non-IC? parameters.
4. The following guidelines should be applied in deterrnin-
ing the minimum level of data validation reguired to
assure the acceptability of the data package.
a. Choose at least two furnace A.A parameters and check
all related calculations and transcriptions.
b. Choose at least two IC ? parameters for complete
validation. If any errors are identified, then
evaluate an additional two parameters. If errors
are still encountered, then all remaining ICP
parameters must be evaluated.
c. Data for Cyanide and Mercury must be validated
100 percent.
D. Action
1. If there are any discrepancies found, the laboratory
must be contacted by the designated representative to
resolve any discrepancies.
2. If a discrepancy remains unresolved, the reviewer may
determine qualification of the data is warranted.
41
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X IV. O tPJ LL ).SBZBBXZNT 07 DATA ?O A CABE
It is appropriate for the data reviewer to sake professional
judge ents and express concerns and comments on the validity
of the overall data for a Case. This is particularly appro-
priate when there are several QC criteria out of specification.
The additive nature of QC factors out of specification is
difficult to assess in an objective tanner. Bowever, the
reviewer has a responsiblity to inform the user concerning data
quality and data limitations in order to assist that user in
avoiding inappropriate use of the data, while not precluding any
consideration of the data at all. The data reviewer would be
greatly assisted in this endeavor if the data quality objectives
were provided.
42
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GLO&SkRY A
Data Qualiflir Definitions
For the purposes of this document the following code letters and
associated definitions are provided.
U - The aterial was analyzed for, but was not detected ab ’.e
the level of the associatied value. The associated value
is either the sample q antitation limit or the sarple
detection limit.
3 - The associated value is an estimated quantity.
R - The data are unusable. (Note: Analyte ay or may not be
present)
1 ) 3 — The material was analyzed fore but was not detected. The
associated value is an estimate and may be inaccurate or
imprecise.
-------
GLOBBARY B
dditienal Thrms
AA Atomic Absorption
Case A finite, usually predetermined number of
samples collected in a given time period for
a particular site. A Case consists of one or
more Sample Delivery Groups.
CCS Contract Compliance Screening — process in
which SIlO inspects analytical data for
contractual compliance and provides EMSL/LV,
1aboratories and the Regions with their
findings.
CL? Contract Laboratory Program
CCB Continuing Calibration Blank — a deionized
water sample run every ten samples designed to
detect any carryover contamination.
CCV Continuing Calibration Verification — a
standard run every ten samples designed to test
instrument performance.
CRDL Contract Required Detection Limit
CV Coefficient of Variation
OPO Deputy Pro)ect Officer
EMSL/LV Environmental Ilonitoring System Laboratory/
Las Vegas
Equipment b ank Equipment blanks consist of water used to
decontaminate sampling equipment as a sample
check for cross-contamination from inadequate
decontamination.
}iolding Time The time from sample collection to laboratory
digestion, distillat .on, or analysis, whichever
is appropriate.
ICP Inductively Coupled Plasma
ICS Interference Check Sample
-------
Ini€ial Calibration The establishment of a calibration curve with
the appropriate number of standards and
concentration range. The celibra— tion curve
plots absorbance or emission versus
concentration of standards.
ICB Initial Calibration Blank — first blan)c
standard run to confirm the calibration curve.
icy Initial Calibration Verification - first
standard run to confirm the calibration curve.
LCS Laboratory Control Standard — A standard that
has gone through digestion and is designed to
measure digestion efficiency The solid is
suppplied by the EPA.
Matrix Spike — introduction of a knc.n
concentration of analyte into a sample to
provide information about the effect of the
sample matrix on the digestion and measureme- t
methodology.
MD Matrix Duplicate - a laboratory split sar le
to measure instrument precision.
MSA Method of Standard Addition
NPO National Program Office
PE Sample Performance Eva].uation Sample
PD Project Officer
Preparation blank Laboratory blank water which has gone through
digestion or distillation and analysis with
each SOC.
Quality Assurance — total program for assuring
reliability of data.
-------
QAC Quality Assurance Coordinator
QC Quality Control — routine application of
procedures for controlling the n onitoring
process.
RPD Relative Percent Difference
RSD Relative Standard Deviation
RSCc Regional Sample Control Center
Serial Dilution A sample run at a specific dilution to
determine whether any signicant chemical or
physical interferences exist due to sample
matrix effects. (ICP only)
S OC Sample Delivery Group - defined by one of the
following, whichever occurs first:
— Case of field samples
— each twenty field samples in a
Case
- each 14 day calendar period which
field samples in a Case are received,
beginning with receipt of the first
sample in the SDG.
Sample Management Office
SOP Standard Operating Procedure
TCL Target Compound List
Trip Blank A trip blank consists of bottled water that
accompanies sample bottles into the field and
to the laboratory as a sample check for
contamination along the trip.
-------
APPENDIX A
Cor.tract Cor.piiance Screening Procedures
for RAS 1norgar c Data Packages
-------
STANDARD OPERATING PROCEDURE
FOR
CONTRACT COMPLIANCE SCREENTh C (Ca)
OF
ROUTINE ANALYTiCAL SERVICES ANALYSES
OF
!NORGANI DATA
UNDER SOW NO. Th7
-------
TebI, of Coateet.
I trodwthon
A. Cover Pile
B. Data Shect (Fori I)
CA. Initial and Continuin. C Jbrstion (Form IIA)
CD. CRDL Stands.rd (or AA sod %CP (Form lID)
D. snk3 (Form 111)
E. ln*erferencc Check Simple (Form IV)
FA. Spiked Simple A iiyszs (P .Diieston/
Pre-Dll*IiooXForm VA)
ED. Spike Sample Analy u (Post-Digestion/
Post-DistilhatonXForm VB)
Ci Duplicsie Simple Aniiysu (Form VI)
It Laboratory Control Simple (Form VII)
L Method of Stat dird AdditioD (Form VIII)
J. Seriil Dilution (Form I X)
KA. Mercury HoId ng Time (Form X)
KB. Cyanide Holding Time (Form X)
L. ln.strumeot Detection Limit (Form XI)
M_ Interelement Correction Facton (Form XII A & B)
N. Linear Ran*e Aniiyss (Form XIIT)
L Rsw Data
1. Trifflc Reporta
AppeDdil
2
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Introdi.ict,on
The foltowin 1 is the Standard Operating Procedure (SOP) under which Contract Compliance
recning (Ca) screeru routine inorgarnc data (RAS) under SOW 717.
çcz asesses the delivcrsbes in terms of completeness icid technical comphance.
Discrepancies ore reported uider the relcwant screening criteria as hated in the Table or
Contents The screening results are sunimanzed en a summary form. The problems are
described in detail in the comments section of Worksheets A sod B. Worksheet A for ICP
datx and Worksheet B for AA, mercuq and cyanide data. Loch problem proceeded by the
e for the relevant Cfi*elDD. if there as more than one problem under a single code,
uertiiai numbering is used to differezittate between problems (i.e.. B 1 , B , B 3 ... etc.) For
eech action, the affected nmpks are ideotified by placing the problem code on the bottom
line of the commenu sectioS across from the corrospooding ample.
Tb. summ ary form consists of a matrix that lists the uazples in the left wgin. arid the
criteria in the top row. Loch box in the matrix represents a sample arid $ Criterion. An
sciioci code in a box means that there is a problem or to ambiguity In a iampte for the
re .ated criterion. More than one action code may apply to a single box. The actiori codes are
explained at the bottom of the summary page.
R • a requirement or deliverable is incomplete or detective arid must be
resu bm iued.
S • a deliverible is missing a.nd must be submitled.
N • a deliverible as iechrncaJly noocomplia.ot.
E • so ambiguity exists that requires to expli *to in order that a decision ca
be made.
Comments listed with No Action’ on Worksheet A or B do not appea’ on the summary sheet.
but need to be addressed in order so avoid future complications.
To ensure better uodersta.odiog of terms used throughout thu SOP. some of the terms are
defiried as (oltow
o A case may consist of one or more Sample Delivery Group(s).
o A Sample Delivery Group (SDG) is derined by the following, whichever is most
frequenc
• each case of Field Samples received. OR
- eecb 20 Field Samples within a case. OR
- each U caleodir day period during which Field Samples in a se are
rec ved.
o All samples must initially be run undiluted. When sri analyle concentrition
exceeds the calibrated or linear range, appropriate dilution and reanalysis of the
prepared sample is vequred, The diiutinn should be minimal and should not
dilute the sample below the instrument detection limit.
o An analytical sample is defined as any euvette in the auto sampler. excluding
sLandardiutiori. ICy. ICR. CCV and CCB. The )C . CR!. L nesr Range
Standard. LCS. Ariulytical Spikes (post digest/post distillatiori spikes) and
preparation blanks are all considered analytical sajnples
3
-------
A. Cover Page
Screen na Proced re
a. Check to see that the Cover Page is present.
b. Ensure that iii required information u filled in:
(I) Laboratory name, laboratory code, contract ao., a, y,
LAS. (where applicable), SOW a. and EPA umple
alphan erk order.
(2) All Sample 1 in data package cor pontheg with Form I and
TraffiC Repoil.
(3) Ensure that the SDG number ha s been properly s.ssigDed
(4) Lab managers signature and date
(5) Statement concerning interelemeni irid background correctioni
c. Check to s that the Cover Page u in EPA format
2. A
a. if the Cover Page is not present, it must be submitted (S)
b. If the Cover Page is not properly completed, ii must be resubmitted
(R) IF the SLX number is incorrectly assigned the cover pqe as well
as all affected forms and nv’ data must be resubmined (R).
c. If the Cover Page format is difrerent from that specified in EAibst B,
it must be resubmitted (R).
B. FormI-DsLaSbects
Screen ris Procedure
L Check to see that each sample in the data package has a Form I
responding to the l sl on the Cover Page and the Traffic Reports
S. Check to see that a]! r ured information is filled in.
I) EPA sample a and Laboratory Sample ID must be the same
as they appear on the Cover Page Laboratory name, Lab code,
case a, SDO a, SAS a, sad laboratory receipt date must be
present.
2) Spot check the results versus the raw data.
3) Ensure that the correct number of significant rigures and the
proper rounding nites (or reporting results on Form I have beers
followed 2 aig r g must be reported if the result < tO and 3
hg fig if the result ID For Hg report rtsult as fotlowt
0 2 ugJL, 0.2 U, between 02 and JO ugIL , one decimal, above
10 ugIL, whole numbers
4
-------
4) Units must be UC/L for waIers arid MG/KG (dry 1) lo g
solids
3) Solid samples require a value for % iclids (reported to one
decimal place) Water Dmples must have ‘O reported (or %
solids.
6) Ensure that iou results reported to the instrument detection
limit ire corrected for % solids.
7) D criptocs of coloration. clarity, texture and anifscts in sam-
ple axe required before and ifter sample digestion/distillation
For water samples report color and clarity, for soil samples
report color, texture and artifacts, as r mmecded in SOW $7,
B- 16
c. Ensure thai any required thu flags resulting from re uirernents let
Forms V - 1X (N. M, 5. , W, and L) have been entered on Form I
as appropriate.
d Ensure that values are reported properly Form I includes r lds ro
three types or uli qualrfier These qualifiers must be completed as
folIo
o C (co centrit.iofl) qualiflera Enter W if the reported vajue is
less than CRDL but greater than IDL. U the anai ’te was
analyzed for but not detected, a ‘U’ must be entered Samples
must not be diluted below the detection limit of the instrumecL
The laboratory must use the to est dilution factor ne.c -ary to
bring each analyse within the valid linear range sod report the
highest valid value for each arialyte.
o Q (Quality Control) qualifiers Specif ed cOtries and their
mea.niegs s ic as (oUow
E- The reported value is estimated because of the presence
of interference(s)
M - Duplicate injection precision cot met for GFA.A.
N - Spike sample recovery not within control limits
S - The reported value was determined by the method of
standard additions (MSA).
W - Post digestion spike for furnace AA analysis is out of
control limits
• — Duplicate analysis not within control limits
+ - Correlation coefficient for the MSA is less than 0995
5
-------
o M (Method) quskf ers - speciried ectr aed the,r eanngs
ate
P - ICP
A - FIa,ceAA
F - Furnace AA
CV - Minusj Cold Vipor AA
AV - Automated Cold Vapor AA
AS - Semi-Automated Spectrophotometne
C - Ma.cuai Spectrophotometric
T — Titrimetrk
NR - If the iniJyte is not required to be tnalyzed
e All dilutions not required by the SOW (and affecting [ DL) must be
noted on in a.naJyle by a.n*iyie basis in the comment section
f. Ensure that the z ul reported pertain to the s aiysu requested If
cyanide a.zalysis is Dot requested Form I should state NR, under the
method column
. Check to see that toy inalyte vaJue reported by icy method that has iu
IDL > CRDL is it ea.st a IDL.
2 Action
a. A missing Form 1 must be submitted. (5)
b ,c. ,d. ,e. Ac incomplete Form I must be resubmitted (R)
if transcription erroii, improper flagging or incorrect unU ire found,
Form I must be resubmitted (R)
Ifs simple ts dituied below the IDL the sample must be re.an*iyaed
using the appropriate dilution (actor lcd the dats submitted (5)
1. If a required u Jy i wu not reported, ressalu must be iubmitte4 (5)
undet C crnerioc R, as well is C criterion A, B, K.
g If an an lyte was determined by a method for whkh IDL > CRDL.
samples with analyte results below 5z IDL should be mvked
oricomplaant (N) under CriteriOn 1.
6
-------
CA. Form HA hl l.I ..d C..tl..t.g C.llbrat$ou
Screenini ?rcedurt
s. Easure that ill required ioformation OD Form H hu been completed,
Laboratory name, ab code 1 Css.e , SDG .. SAS., Units (u&/L),
In it ial & C ti ui Calibration Iourc and Ana$yiicat Methods used
b. Check the Form hA’s versus the raw data to verity that , u)ts for all
caiibrsuons brackeun relevtnt umples m the ae have been recorded
c. Vetify that 2-point (for ICP). d-poiot plu* blank (for Hj) and 3-point
plus blank ((or AA and cyanide) caflbrslioris have been performed If
the instrument b *0* .pable of perlormicij the required calibration the
iu.ndardz must be run mmediately after the instrument calibration
squen . The r u1ts must airee within j 5% or the ue value
(e ceptio CRDL cajibratioc standard).
d Instruments must be calibrated daily or once every 24 hours and each
time the insu ’umenc set up. The instrument ca brtion dale ar d time
must be I uded in the raw
e. Spot check the calibration results versus the raw data sod ensure proper
rouDding of resuJta was followed.
1. Ensure that the SiR caiculations are correct and are within the control
limits (90-110% for a n metsis. except aO-120% for Hg and 85-1 )5%
for CN) Ensure that the SiRs are calculated from the results reported
on Form (LA. Higher precision or unrounded vpjue cannot be used to
determine SiR..
g Verify that the proper calibration standajds have been used. and that
the same continuing calibration sra.nd .asd was used throughout the
analysis run for a case of samples received Verify that the reported
ee v*Ju (or )CVs a.nd CCVs are correct using EPA true values or
values submitied by the laboretor,es.
h Verify that the ICV has been run mmedistely sfter instrument
calibration and within the control Limits (90-110%)
I. Verify that the 10% continuing calibration frequency requirement has
been met No more tha.n ten analytical samples may be rue between
the ICY, rust ‘V or subsequent CCV’s (this includes the l , L ,
CR1, Linear Range, analytical ipike and prepo.r%Iion blanks) Ensure
that every a aiytiosi sample is between two sets or ICV/ICBs or
CCV/CCB’s that have met ill calibration requirements.
j. Verify that a CCV has been performed every 2 hours or at a 10%
frequency whichever is more frequent.
h Five full MSA’s may be performed between consecutive CCV/CCB
(whether single or duplicate injections were used) CCVI’CCB vsiues
may also be determined by MSA if the instrument ’s mode cannot be
changed white MSA is being performed.
I, Ensure that for alt AA (except for Hg) and cyande analyses one
cahbratiob standard is at CRDL
7
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2 Action
a. If any reQuired mformation is usrng from a Form It. the form mun
be resubmitted (R)
b. II any libraiion erir tioe pertinent to the Dmple.s has not beer,
reported. a Form H with the appropriate data a usi be submitted (S)
c. If the in stru ment tibration does Dot meet the reQuired crkerjs (2-
point (for IC?), 4 point ptus blank (for Hg). 3-point plus blank (for
AA and cyanide). or jS% Criteria) mark all teLated ptes
aoncompliint (N).
d. 11 Jibratioo raw data an eat present, they escat be subniined CS)
under C cr,terion CA.
e ,f. If the %R for the c*librsdon result (rounded to the n rest whole
number using EPA rounding rules) is outside the control lim the
in.sirurnent must be re hbrated, the previous ten samples re-inalyzed
for the iffected snalytes and the data submitted CS) If the %R
icutations Ire incorrect, a corrected form mmt be resubmitted (R)
g If improper Jibrstion standards have been used. miik the associated
samp t es u noocompliant (N). If the csJibration wurces hive oct been
idectiried, Form II must be resubmitted CR) whi, the required
information..
h If the IC’V is not run Immediately after iDstru.ment Jibr tioc and/or i.
not within the co tol limits ma.rk all affected samples noncompliant
(N)
iJ,k. if the 10% continuing librition frequency reQuirement ha& ot been
met, or if the 2 hour CCV ha., been violated, mark the preceding
naples (to previous compliant CCV or ICY) noncomplia.nt (N).
L If one of the libration standards for all AA (czcept Hg) a.nd cyanide
azialyaes-is not at CRDL. sit samples wiU be considered nonnomptiant
(N).
$
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CB. Forea IIB - CRDL Sia.dard for AA med ICP
Screeratne Procedure
a. Ensure that all required information on Form L 1B has been comptet
b Vezify that a itzodatd ii the CRDL ha, been analyzed for each ar 1 ’
by AA (eacept Hg). Verify that a itandard at 2s CRDL or 2x IDL,
whichever u greater, has been arta!yzad for each anaiyt.e by ICP but
not for Al. $a. Cs. Fe, Mg, Na or K.
c. Ensure that a CRDL acandud has been performed at the beginning and
cad of each IC? run (but not before the ICV/)CB or after the tanat
CCV/CCB at the end of the )CP run).
d. Verify that the 1 hour CRDL. re uiremeat was atisf cd for IC ?
analysis.
2. Action
a. If any re . uired information u missing from a Form 118, the form mu 1
be resubmitted (R) A missing Form 118 must be submitted (S)
b. U the true waives of the CRDL standard are nor at the appropriate
levels the anaiysis for &J samples must be marked oncompliact (N)
c If the CRDL itandard for ICP has been i-un before the ICV/)CB or
alter the fin .sJ CCV/CCB the analysis for sit aa.mples must be marked
noricomplia .nt (N)
d. If the CR.DL t j is not reaMJyzed within I hours for ICP
analysis, ena.rk ii! samples in the run as nonccmpliint (N) If analysis
times are not provided, the laboratory must subm.ar them (S) under CCZ
CrileriGO R..
9
-------
D. Fore ill - Blacks
Scretnint Pzoc du 1
I. E .surc that all raquued ,aforrnation on Form III has been completed
b Ensure that all viluei rot all required blanks were reported on F r
Ill
C. Spot c heck the results ‘enw the raw data.
d All blank results must be reported, pos’live aelative Or zero.
e. The values for the prepirstion blank must be rec rde4 in UG/L for
water samples and MG/MG for soil .mples. The values of )CB,’CCB
must be recorded in UG/L.
f. Ect.sure that the proper con niratior, flag .If is sppbed for an absolute
value below IDL ‘ B• for an sbsclute value greater than the IDL but
below the CRDL
i Ensure that the bLank values are within control limits
b Check the raw dau to ver (y that $ libraL on blank has been uuiyeed
immedaitely after each calibration vcrirtcston, at the beginning and
after the Last arsaiyticsi sample, every 2 hours. and at 10% frequency
I Ensure that a preparation blank has been analyzed for each b p f
san pTes (up to 20) For Hg the preparation blank is the same as the
calibration blank, in accordance with the mercury method 11 must be
l be lied for both uses n the raw data.
2. Action
i if Form D l is incomplete, it must be resubmitted (R).
b. It reQu.ue4 blanks s.re not documented, a Form Ill with the appropriate
data must be submitted (S)
c. If the absolute value of the blank ( ICB/CCB) resultt exceeds the CR.DL
for an element, mark the prec tog samples (to the previous compliu.n
)CB/CCB) as non-compliant (N) The instrument must be recalibrated
and the samples re-analyzed for the &ffected analyte. If an element is
determined on an instrument whose ID !.. uc eds the CR.DL. mark the
assothted umples as noncornpliant (N) if the calibration blank as
greater than the ID ! . ..
d If the 2 hour or 10% frequency has not been met, mark the preceding
samples (up to the last complaant ICB/CCB) as noncompliant (N).
e.g lithe ibsoluic value for any irtalyte ConcentrstiOn ira the prep blank as
above the CRDL. the lowest concentr ation of that analyte in the
as . oc ated samples must be lOx the blank concentration Otherwise. all
samples must be codagesled and reanalyzed for th,t araalyte and the d aa
submatied (S).
10
-------
U src improp rIy rsnscr,bed or the vnit3 Ire ncorTe . Form Ill
rn t be r ubm nod (R)
d t* . needed, code this i.s ubc it (S) unde CC Clitetion R
II
-------
L. Fore I V - tsIerl,r,,t, Cbeck Sa.pte
creenint Procedure
a. Check to see that all information r ured on Form I V has been
umpleted, incIudin. ) aourcc and ICP ID number.
b. Verify that an l analysu run hu been performed at the begi
(but not befott the ICY and ICR), sod end of cb IC? run (but not
slier the (inaJ CCV/CCB).
c. Ensure that p . 11 JC results are documented on Form IV . The Inalysis
with the lowest dilution factor within the how range for all element
must be reported.
d. l the 1C was Contractor prepved, verity that ii otsini all elements
it the kvel spec fled in Table 2 (SOW 717 £4) and that a mean and
standard deviation are Jcul.ite4 lot each sn.alytc based upon at k.ast
measurements.
e. Spot check the IC results venus the raw data E iure that the %R
.lcutztions are correct and are within the ‘Dtro) Ii its (&O-120)
except for Al, Ca. Fe, Mg Recoveries must tie eslcutited versus the
1.rue value if EPA solutions are wed or a mean value when a
contractor prepared solution is used.
1. Ensure that the %Ri s.re Jculated from the values reported on Form
IV. Hither precision or untouOded values are not permitted to be i.ued
to detera ne %R...
Verify that the $ hour lC requirement was r.atisrjed.
2. Action
L If any information on Form IV has not been completed, it must be
resubmirted (R).
b If the IC is run before the ICY/ICR or after the final CCV/CCR ms.rk
iii samples in the run as noncomptiant (N) If )C raw d*ra have not
been submitted for both the beginning and end of s.n ICP run, then the
data must be submitted (5) under C criterion R..
c. If any require4 ICS value has not been documented on a Form IV, it
must be submitted (S).
d If Form IV lacks the true values for JCF clements, except for those not
cnt.ained4n an EPA solution, it must be resubcnined (R) .
e. If any )C recovery (except for inlerferent.f such as At. Ca, Mg and
Fe) is outside the control limit, mark all samples in that IC ? run as
noncompliant (N) Results lot all elements must be within the linear
range or a diluted value must be submitted (S) from the diluted ICS
f. lithe %R.s are catculated from values other Char those reported on
Form IV the form must be resubmitted (R)
-------
If the CS ii bO re.IDaty2ed w,thiD I hours. i:k .M samples in the rur
i noncompli.nt (N) tf ans?ysu for tCP sic ptO dt , the
Laborstory must submit (S) them under C S CfiItlOfl R
13
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FA. Form VA SpIked Sa.pte Asityili (PIe.Dl 5 slO$/rfl.DtI(fllI lOD)
Screenint Pxoc’edure
a. Ensure thu all tntormstson required oe Form VA has beta compt ied
b. Verify that at kast one upked sample uniiysu has been performed on
each group of samples of $ similar mstr z type (i.e.. witer, soil) an
cr ce trati (i.e., low, medium), or for ch Sample Delivery Group
(SDG). whichever is aore frequent If two ntethods (ICP, GFAA) ur
wed rot an element, spike samples must be run and reported for each
method The isalu (or reporting spike sample results will be ideoti i
to those used for reporting sample results in Form I (i.e., UG/L. for
aqueous and MG/KG dry weight basis for solids).
Spike nceotntonJ should corJorn i to those ui Table 3 (SOW 787 E-
JO) Results must be in consistent units. IDL is tite minimum
reportable level
c. Ensure that SRi use reported for every spike performed and spot
check the results venu s the raw data and SR lculations. n
3cularing SR. use sample result (SR)—O for values IDL. If the
ipike i s performed on the rample that is used for the dup!i te salysis
ensure that the SRi arc kulated versu.s the results de.signated as the
origina sample. The duplioate results or the average of the duplicate
and sample results .nnot be used Ensure that the SRi are calculated
from the values reported on Form VA. Higher precision or unrounded
values rinot be used to determine SRi. SR must be reported.
whether it is negative, positive, Or zero.
d Under control Limit %R’, ‘75-125’ must be entered if the ipike added
(SA) value wa greater than or equai to one-fourth of the sample result
value Results outside the otrol limits must be flagged with ‘N’
This does not apply when SR (sample result) 4 a SA (spike added).
e. if there is more than one spike (per matrix, level, and method) and
only one requires the e riq, all samples of that mstri.x and level
done by the i& e method, must be flagged.
f. An identified field blank ca.nooi be used for mutri.z spike analysis
Except when it is the only sample of that con ntratjon and matrix for
that SDG.
g. Check the traffic reports to see it a specific sample is requested for the
spike analysis
2 Action
a A Form VA missing any required information must be resubmitted (R)
b. If matrix spikes have not been performed at the required frequency.
the data must be submitted (S) If required matrix spkes have not
been documented on Form VA, they must be submitted (S) If spike
COncentricions do riot conform to those in Table 3, the pikr analyses
((or affected elements) must be redone at the appropriale leveLs and
submitted (S) If incortshtens unitS have been used, Form VA must be
corrected and resubmitted (R).
14
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c. if the method of oak tatog the R is incorreci. Form VA must be
r,ected and r bmittt’d (R) If the %Rs are calcuisted from v ih es
other than ihose reported on Form VA, the form must be resubmitted
(R).
d.c if e %R esquires an ‘N’ lb& on Form VA and does not have ii, Form
VA must be r ubmiited (R), Form I must siso be resubmitted (R) as
appropriate.
1. II an ide*tified field blank bat been used for the matrix ipike analysts,
• matrix spike s.nsiyiis on $ field sample must be submitted (S).
(Except when the field blank is the only aquecus sample in a case of
soil samples.)
g. If the sample d&jnated to be sued for the spike analysts has DO’ been
used then the proper sampk must be ipiked and the resuib submitted
(S).
13
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lB. rora YB - Spike S pie A..1ytL (Po t-D1 1 tIos/P,it .Dtitillitio )
Screenint Procedure
a. Ensure that iii required intor stoe oe Form YB his been completed
b. For flime AA. IC ?. Hz, sod CN analyses, whee the pre-digent oo/pre-
dãstillstion ipike recovery (sib outside the control limits sod the
sample result does sot esceed 4* the spike sdded. (i.e. in at alyte thai
has bte fla ed ‘N’), s -digesboofpost-distilLst os ipike must be
performed for those elemests that do sot meet the apeoWied criteria
(escept Ag). The un.spiked ibquot of the sample must be spiked at 2*
C DL. or 2* the isdigesous level, whichever is greater. The usits for
reportiog spike sample results will be UG/L
c. S o check the resuits versus raw data sad check %R esiculatioas.
d. Eruure that the proper reportiog and esicuLatioc methodologies are
followed.
2. Action
a. if Form VB is mis.skg any required information it tr ,u.tt be resubmitted
(R).
b. If $ post dgestiosfpost distillation spike has sot been done is required
then the analysis must be performed and the dat.a submitted (S) If the
sample b.as been s rrecLJy spiked thee the s .nsjysis must be redone it
the appropriate spike level and the data submir ed (5)
c,d. if the results are improperly reported or ceiculated Form VB must be
resubmitted (R).
16
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C. Form VI - Dvpllcatt Sa ptt Anil ls
Screenins Procedurt
a Ensure that sit informsuon required on Form VI hij been covipie
b. Verify that at least cite duplicate sample analysis has been perfo
on each group of samples of a similar matrix type (i.e.. witty, i iI)
coocentritio (i.e., low, medium), for each whichever is most
frequent. It two eihods (ICP. GFAA) are used for in element,
duplicate samples must be run and reported for each method. Reslj! 13
must be in consistent units; IDL as the minimum reportable level. The
sample arid duplicate results cannot be averaged (or reporting values on
Form I. Duplicate analyses are required for % solids nlue.s and for ii)
tulyte results. Check for appropriate units (UGfL. foe water and
MGf) G dry weight for soil).
c. Spot check the results versu.s raw data arid the RPD calculati rij.
d If both umple and duplicate values are Si CRDL a control limit of
t 20 % RPD is applied If either the sa.znple or duplicate results are
below Si CRDL. a control limit of tCRDL is applied The ±CRDL
value mu.st be entered under conuol limit’ to applicable anaiytes. If
both sa.mple values are ( IDL the RPD is not to be caiculted arid
NC must be entered under the method column Values outside the
cootrol limits must be flagged with ‘. If theme is more than one
duplicate sample (per matrix, level, and method), and only one as
outside the control limits, a.1l samples of that mauix and level, done by
the sa me method, must be flagged
e. The RPD values must be calculated from the values reported on Form
VI Higher precision or unrounded vsi ies cannot be used to determine
the RYD.
1. Duplicate u.rriple .nuiysis may not be performed on u.n identified field
blank, except wbe it i.e the oniy sample of that c cenuilioo arid
matru for that SC .
g Check iriffic reports to see ii a specific sample is to be used for the
duplicate analysis.
2 Acton
a. If any required information is missing from Form V I, it must be
resubmitted (R),
b. If duplicate analyses hive not been performed at the required
frequency, these analyses must be performed, and the data must be
submitted (S).
11 requred duplicate analyses were performed, but were not docu-
mented on Form VI, these data must be submitted (S).
If inconsistent units were used, Form Vt must be corrected and re-
submitted (R)
Ii
-------
. It the P.PD cakutitioru ire inc.ortect, Form VI must be tebm ed
(R)
d,e. If the ineorreci contr& Ii iU hive been applied or the *CRDL COctr
limit Li ot entered when required, or if the flai&n n le M e beer
applied incorrectly Form VI must be coutcied m d resubmitLed (R)
If the snalytes hive aot been correctly fla&ged on Form I, the Form r
must be resubmitted (P.) unde, criterion 8.
1. If in identified field blank has been used for the duplicate a.naiy a
duplicate LezalysLi on I r ;d sample must be submitted (S).
. If the umpte desjnated to be used (or the duplicate analysu his not
been used then the proper *nrple must be used (or the duplicate
azslysis and the results submitted (S)
18
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H. Fore ‘U L..borsCor Co.troI Sa pte
j. çreenint Procedure
•. Verify that sit informilion required on Form V i i has been completed
Ettaure that the proper reporting methodology has been folloi ed.
b. Verify that it least one Form Vii. with aqueous ted/or solid tiborstory
control samples, his been submitted for each group of aqueous and/or
solid samples in each SDG or each batch at sample d geated. An
aqueous LCZ is not requimed for Hg a.nd CN analysis. If an s.nalyte is
determined by more than one method a eparate L must be na lysed
by each method.
C. Spot check resulu versus raw data and %R tona.
d. Ensure that the solid i.nd aqueous LCS results ire within specified
control limits (80-120% for the aqueous LC and wiihi the apecifie4
onc.entraton windows for the sohd L.a) it either aqueous or solid
LC is out of control the siajysis must be terminated, the problem
corrected. and the samples asociated with that LC redigested and
r esnatyz.e4.
2 Acti n
a.. It any re uIre4 information is mIssing from Form VII . it mu.st be
resubniitte4 (R)
b if the requred number of LC a sJyses has not been performed, these
i.naiyses must be performed and the data must be submined (S) If a
re .quire4 LCS s.nsJy is hat not been documented on a Form VII. it must
be submitted (S)
c,d If a.ny aqueous or sobd L-CS results are outside the control 1imit ($0-
120% (or aqueous or c.onc.e uition window for solids) (escept Ag and
Sb in the aqueous LC ), mark iii related samples as noncompliant (N)
19
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Fervn V III - Method .1 St..sd d Addillos ssd Fwr sce AIo•Ic Abiorptleo (AA) QC
Aoslyi s
3 ç reenini Piocedure
s. Ensure that Form Viii has been compielely md correcUy lined in arid
resulu flagged is appropriate r .
b Determine which elementi have been analyzed by Furnace AA. Find
the raw data sad verify that the pioper &naiyticai aequence bss been
followed. Full MSA must be performed withia the conteat at a regular
arislytiesi run, i.e., 3-point bration plus blank between conaecutive
ICV/ ICB and CCV/CCB wth no more than five futi MSA ’s. During
full MSA. single snjeclions for blanks sad , .e4a.rds are permissible. if
duplic*te iDj ectioDs are used thiring MSA. theL average vtiue muit be
wed to plot the M.SA curve.
c. If mpe coocentrstioni are greater than the CR.DL, ensure that the
duplicete readings agree to within 20% retative standard deviation
(RSD). If they do not agree within 20% R.SD after one rtrvn, the
result on Form I musi be flagge4 with in M’.
d Review the wiytical spike recoveres sad .mple and spike absorbance
(or c ncentntoo) to ensure that the MSA decision trot (Ftgure I:
SOW 787 E-lS) has been followed If the spiked umple requires
dilution, the unspiked sample must be rerun at the same dilution
factor. Arlalytic3J spikes are required on the LC and prep blank,
MSA is not to be performed on the L.CS or prtptrstion blank,
regaidles.s of spike recovery results. U MSA performed twice on one
p mple as required by the MSA decision tree and both MSAS have a
correlation coefficient <0 995, ensure that the result rtportod on Form
I for that aDalyte was from the MSA with the best correlation
coefricienL An a.naiyti 1 spike is not required on the pre-digestion
spike sa.mp le when the spike sample recovery within the 75%-1 5%
control Limit or when SR 4z SA.
A quick cheek for MSA.
%R for anaiyti J spikes
<40% - Dilute (5 to lOx) sample and rerun o U suit 40% the
results must be flagged with an ‘F.
) 40%
(I) Sample absorba rice or concentration is < 50% of the
spike, the sample mini be quanth3ted from the curve
and report dowri to the IDL. If the spike recovery is
kss than 15% or greater than 115%, the results must be
flagged with a W.
(2) Sample absorbance or concentration is 50% of the
Ip ke arid the spat recovery is between 85% and 315%.
the results must be Quantitated from the curve and
report down to the IDL ..
20
-------
(3) Sample abiorbance or concenir 00 18 50% of the
spike and spike recovery is greaser than 115% or less
than 15%, the sample must be qus.ntiuted by MSA.
a. %R must be calculated using .nipl result, SR.’O for values c 1DL.
Values between IDL and CRDL must be used in JcuLating the
analytical spike recovery.
If MSA’s have been performed ensure that ill MSA reaulta have been
reported correctly on Form VIZI and in the a. data. R lcutate
sevtriJ flow regressions. Ensure that the curve as plotted with
concentration added (x.sxu) vs. absorbance (y.u.is) sod that the y
intercept, slope, sod correlation coefficient sit rtported on Form V i ii
or in the w data s.s required. Also make itu all flags (5,., W) s.re
entered on Form rs as appropriate.
If the preparation bb.nk sJytical spike recotery is out of control (!S-
115%), the spiking solution must be verified by respiking sod
rerunning the preparation blank once If the preparation blank
analytical Spike recovery is still out of control, the problem must be
corrected and reanalysis of all analytical samples associated with that
blank is required.
2. A ti n
i. If Form VII ! is not present, it must be submitted (S) If the proper
data flags (E, S, ., W and M) have not been written on Form I, then
Form I must be resubmitted (P.). An incomplete or incorrectly
submitted Form VIII must be resubmitted (P.).
b. If the proper snalytical sequence has not been followed. mark the
affected samples s.s concorripliant (N).
c. It the % R.SD between a sample and its duplicate exceeds 20% and the
sample has not been rerun, mark the sample as noccompisazit (N).
d If the proper decision tree process has not been followed for a sample,
mark it as noncompliant (N) Examples are (1) noricontract specified
dilution of a samnpk before the first analysis, or (2) spiking at > 2 a
CRDL. then diluting the spiked sample to bring the spike to 2 a CRDL
or (3) rerunning a sample instead of diluting or performing MS.A. U
the ipiked sample was not run it the same dilution factor as the
unspiked sample, it is non-compliant (N).
e. If the %R is improperly calculated, the calculation must be corrected
and the data must be resubmitted (P.) if MSA is required, the
analyses must be performed and the data iubm ine4 (S) If the slope,
y-intercept arid correlation coefficient are not present in the raw data
they must be submitted (S)
If the preparation blank anilytical spike recovery is out of control and
it was rerun but remained out of control mark all affected samples as
rioncompliant (N).
21
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J. Serisi DIhIIIOD (Fore LX - IC ? Oii )
Screenint Procedure
•. Verify that Form LX has been submitted for each required serial
dilution and that all iDfOrTnatioa required on Form IX has beets
tom pIe ted
b. Ensure that at least one serial dilutiots has been performed on each
group of samples of a similar nssiris type (I e., wstei, soil) and
concentration (i.e. . low,, medium), for each SDG. whschever is most
frequent. II *0 samples in the case COrs in snal rtez at kasi ten Umes
(lOx) the IDL. in the original (undiluted) analysis, theo sinai ditutio is
not required (NR) The initial sample value must be eotere4 on Fortxs
LX sod (NR) entered under the method 1umo if the original mpie ss
below IDa IDL.
c. Check to see that s s-fold dilution that does ’ not agree within 7.0% of
the initial value has been flagged E’ br that snaiyte ott Form IX and
*11 associated Form Is II there is more than one serial dilutiou per
SDG. but *1 least one is DOt within the 10% limit for a specific arsa!yte,
flag al l s mpies of the same matrix acid concentration with E ’ flags for
that arialyte
d Ensure that identified field blank.s havi not been used for serial
dilution artatysi.s
e A 5x dilution is required (one part of sample mixed with four parts
distilled ater)
f. Spot check the resultt on Form IX against the raw data arid recalculate
the % Difference for a few elemeola.
g. Ensure that the proper concentration flags have been reported on Form
IX -
2 Action
a. If Form IX i s not present, ft must be submitted (S) An incomplete
Form IX must be resubmitted (R)
b. If no, or too few serial dilution •nalys.e have been performed
(provided that analyte concen lrations are sufflcientty high), these data
must be subrnuied (S).
c. If E flags are required, but are riot entered on Form IX, the form
must be resubmined (PS) The affected Form 74 must also be re-
submitted (R) under CCS criterion B
d. Lb an identified field blank has been used for serial dilutiott analysis.
an anaIy i on a field tample must be submitted (S)
e. If $ dilution factor other than x is used, the analysis is noncompliaric
(N)
22
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I II the rt3u U o Form LX do not rreipond 10 the tiw d*t, or the %
D f(erenct br my ekc eo1 incorTect. he form must be r ubc itted
(R)
$ If Form IX ii improperly completed it must be , ubminod CR).
23
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LAKB. HoIdi.g flts - Fare X
Screenint Procedure
Cyst de (CN) - 14 days
Mercury (Hi) - 26 days
Other me Js - 6 months
* Ensure that Form X has been submitted and comp’eted properly.
b. For C purpos the holding time is defined as the oumber of days
from the date of sample receipt at the Laboratory to the date of sample
Preparation (digestion or dutiUstio ). Comptre these i so dates for
each irtalyte and sample to see if holdtng times hsve beers ciceeded
Holding time s prep date - laborstory receipt date.
c. Ensure that the holding Lime has been properly calculated The dates
oa Form X must correspond to the dates on the distiflatio (or
digestion) log and the TraiIc Reports.
2 Action
a if Form X is not present. it must be submitted (S)
b If informaLion to determine holding times is not contained in the data
package, it must be submitted (S). If the ho)di g time for in snaiyte
in a sample has beers eiceeded, mark that ,.a.mpte .s noocompliant (N)
and report the number of days in excess on the C summary sheet
c. If the holding time calcu!at orss on Form X are incorrect, Form X must
be resubmitted (R).
24
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L.. Form X i- bstni.e.t DeIecdes U&
&menina Pr *dure
a. Verify that it least cac Fore Xi baa beco rubmJned.
b An TDL usi be reported for each wavelength used i the .mple
analysis (no lt)1. is required for CN). Verify that the IDL. sie not
greater than the CRDL for ch ,. aiyte. If an a ai)1e has been
determined by in La.nru ent whose IDL ea ds the CRDL. for that
element, check to see that the conce nDition La the sample ciceeds the
CRDL by it least a (actor of S.
c. Venfy that the IDL’s reported ire for the current quarter. (i.e no more
then 3 months old). If multiple instrumeo are used for the analysis
of an arialyle within an SDG, the highest IDL for the iastru eot niusi
be used for reporting concentration values fo that SDO
d Verify that ill information is recorded on Form X I including
Instrument ID.
2 Action
a it a reouired Form XI is missing it must be submitted CS)
b if an IDL is not reported for an analyte it mtist be submitted (S) if
the IDI. for art srta!yte esceeds the CRDI_, mark all samp’es
noncomp iant (N) and notify the laboratories Project Officer (P.O )
(Except i.heri the sample result is greater thin Si’s the IDL)
c It the case is submitted using out of date IDL’s, the new IDL’s must be
subritied (S) and all affected Forms 1-IX resubmitted (R) If the
inatyte ha.s been determined by more ths.n one instrument and the
highest IDL is not reported then all affected Forms i- TX must be
resubmitted (R)
d An Incomptele or ambiguous Form Xl (unclear a.s to which IDL.
corresponds to which instrument) must be resubmiued (R)
-------
U. Ferns )W A £ $ 1.ter.ka,.t Coemtiea Factors
Scretnios Procedure
a. Verify that *11 re ubed formstoo is recorded co Foru a X I I A a a
b. Verify that $ curreDi Fora X I I has been subu ii1ad with every
pa ks e. ET*SUTC that correction fscton for Al, Cs, F. sad M
been deter oed. Also ensure that the date of the correction f&ctorj
mot uceed the ICP snijysis date or precede the a alysis date by
than 12 booths.
2. Action
I. An incomplete form must be resubmitted (R).
b 31 interelement correction factors ha’ e not been determined for At, Ca,
Fe sod Mg mark alt uc ptes noncomphant ( ) It a Form XII 1.5
musing, it must be submitted (S). under criterion M.
26
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N. Fore Ofl - ICP LIsc.az Rsigrs
Screenina Piocethn -t
a I zure that ill roguired i for stion us recorded on Foru X1IJ
b Verify that a cunent Form XW ha.s been aubuuried (or ei b JCp
instrument used in determining ari Jyte results Ensure that the date of
3CP analysis does Dot eaceed the Linear Range determination by
than 3 months.
c. Make sure chat all the results obtained from each ICP insu ment to;
each snsiyte i. d wa e1eegth tsU below its established bne.a.r rs.nge for
that instrument For AA, CN and Hg the Iine.Lr range of the
in.strument is the vslue of the hghest standard used to ealibrate that
instrument
2 Action
a If Form XIII is improperly completed or incomplete ii must be
resubmtted (R)
b A mjssing Form XIfl must be submitted (S) If the l,near r.n e(s) are
out of date then the current ticear range.s mu.st be submitted (S)
c if arty vatue obtained from an instrument fiJis aboc its establLshed
linear rar ge of that in.strument the s ample houtd be marked as
non:omphartt ( I c)
27
-------
L .DsIa
1. Lb
•. Verily that 1e ble data ( IC ?, Flame #.A, Hj, CM. Dileabon irid
Distiilaton Lop, md % solids) UICIU6LD I ias eat tndoula and
indicston of pH 2 or ’ 12. ,.s spplicable. have a ivbmiried to
support *31 ple *naiyaes and QC operations reported in the aae.
b. Ensure that the raw data ire properly labelled nsia EPA Sample
numbers mad codes sod co tor sttictly to the ccauics requirements
(See Table I: SOW 717 -$).
c. Ensure that the raw data are in the correct order (IC ?, flame AA,
Furnace AA. Hg. CN. digestion sad Distillation Logs, sad % solids).
d Verity that proper bsckgrou d correction tad multiple izijec-
t,onfexposure re u rements have been fuliill d The Cover Page state.
menc on background correction app1 es only to ICP.
e Erasure that the time irid date of each analysis ba.s beect given irid the
run sequence i.s clear and follows the contract re4uiremenu.
1. Ensure thai Do QA/QC samples ire improperly run. If the first run of
s QA/QC sample u outside of its specified coot,ol li uts, the inalysis
viuSt be terminate4 , the problem(s) corrected, the nstrumenc
recalibrated, and alt affected samples reanalyzed
En .sure that s.ny crossouts made to the raw data are initialed and dated
by lab personnel
2 ActiOn
$ If the n data for soy sample or QC operation are missing they must
be subiriitted (S) If the data are illegible they must be re.submstted
(R)
b If the raw data are not properly labelled or do not strictly conform to
the contract requirements, the data rnsut be resubmitted (R).
c If the raw data are not in the correct order, note it on the worksheet as
a NQ Action item lithe problem persists, report it to the
laboratory ’s Project Officer.
d If background corrections have not been applied so Furnace AA, ICP,
or Flame AA measurements below 3S0 rim, mark all samples a.s
noricompliant (N) If duplicate injections/exposures for Furnace IC?
or AA (except MSA) have not been performed, mark the iffected
samples as noncompliant (N)
e It time and dtes or iach analysis are not given in the raw data, the
data must be resubmitted (R) If the raw data is not cle.ar (i.e too
marty crOtsOutS. inconsistency between actual raw data and summary
sheets, ambiguous explanations, dc .) the data must be resubmitted
(R)
28
-------
f ( QA/QC r%ru bCCU) the rlflt *X 1JyIU %3 OU de of
spoci(ied Li J for ths QA/QC nap e the i iaiytia! Rmpi
wit.b Iha piZbCubj QA/QC iii be wked
oDoou pIia.o1 (N) uDder the QA/QC tr terio ft per ins to.
it cro souu Lo the nw data ye DOt iciiiiied and daled, the raw
must be r uiltied (R) with the appropnate inithis and dates.
29
-------
1. S&wpl. Traffic leporli
1. Scçeeriini h diare
. Verily that iii mples Li sted oD the Cove, Pije ied havi & i Form 1,
also have $ m.rrK Report copy I a lb . da g*ckale.
b. Ecaure that the m.rrsc Report phol py is kgibie v to ae
umple number. uxnpte type, required analysis, receipt date and
iigD$tUrt. The Trtffic Reports shall be aJraDged is iZCretsi g EPA
ia ple oumber order, consderisg both alpha and numeric d i*natjo ,
c. Q eck to see that iii analyses requested o eb. mIrc Report hive
bec carried out. (Note If ‘filtered U entered on the Traffic report
$ ‘dissolved etal analysis as not automatically requested The specific
irtaiysia requested usi be under the proper cotu n in KCIIOS C RAS
ANALYSIS’ of the traffic report).
d Check to see if a.ny of the samples are Labeled as a field blank or a
Ii n.sa t e
2 Action
a If * Traffic Report photocopy as mszin . it must be submitted (S) if
there is a Tr*ffi Report photocopy but no Form I or raw dau, the
problem should b .c coded as ciplain (E)
b Ii the Triffic Report photocopy is illegibIe ii must be resubmitted (R)
c If requested snaiy es hive not been performed, the data for that
analysts and all required forms must be submitted (S)
d if an identified field blank or rinsate has been used for the dupiicatt,
spike or seral dilution analysis (nc.ept if the samp’e is the only sample
of that co entration and matris in that SDG) the *nalysis must be
submitted (5) on an appropriate sample, under the proper criterion
30
-------
App,,dI
31
-------
cON IAC COflPtIAMC? C V?HINC ,UP, A•Y ?QP !NOUSAHIC
taUt AT PU.1L OS
t&fl N& 1 CONTPACVt
c PIJ (I CAT! P(CflYt t
•
I *rcpt
wo.
5 A I B $
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$Pa; I wtE1I
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ICWCCV CRDLIeLN I
t I VA YR I
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ICOR..I UN.I
IPAcr I1A I5
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r.c R(Yp, COO Y • IxP( AD4. U • U! UBp tT I • UL PITT, H • t flh1 L.1A)4V
-------
COHttaCT CO PLIANC1 C !tNJMc ON !MORIAIIICI
c*ftI C fl?AC1i
LIJ k*M i
R IO
I I4IIT A - ICP
oAyr sc,rIp1ro.
ICO IRNID OTt
PA I l i
I SAMPU IC,IIISAIIPI OATt I QC A$ALT3!S I pg a
I t . I I WT.I P!CL ANAl.. 1
I I I I I I I
I I I I I I p
I I I I I
I I I I I I I _____________________
I I I I I I
r i i s i i i p
I I I I I I I I
I I I I I I I
I I I I I I I I
I I I I I I I I F
I I I I I I I I
I I I I I I I I I
I I I I I I I I I
I I I I I I I I P
I I I I I I I I I I
I I I I I
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P I I I I I I P
I I I I I I I
I I I I I I I I s
I I P I I I I I
I I I I I I I I
I I I P $ I I I
I I I I I I I I p
I I I I I I I I I
i.—.—i
1 I I I I I 1 P I
I I I P I I I I I
I I I I I I I I I
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I I I I I I I I I
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I .. I I I I P I I I I
I p I I i i
I I I I P I I I
I I I I I I I I
P I I I I I I I
I I I I I I
-------
CONtRACT COflPLIAKC ,C.t WINS POR XNOR ANJC RWUt -hAap OI
pAn,
CAfl. fTlAC,,
ue i *iir,
I I I I I I I I I I I I I lip
I I I I I I I i I i
I I I I I I I I I I I I I 1 I I
I I I I I I I I I I I I I I I
I I I I I t I I I I I I I I Ii
I I I I I I I I I I I I I I I I
I I I I I I P I I I I I I I t
I I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I I
I I I I I I P I I I I I I I I I
I I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I
I I I I II I I I I I I I I II I
I I I I I I I I 1 I I I I I I
I I I I I I I I I I I I I I I I
P I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I I ____________________
I I I I I I I I I I I I I I I I —
I I I I I I I I I I I I I I I I
I I I I I ‘ I I I I I I I I I I
I I I I I I I I I P I I I I I I
I I I I I I I I I I I I I I I I ____________________ I
I I I I I I I I I I I I I _I I I
.1 I I I I I P I I I I I I I 1 I
I I I I I I I I I I I I I I I I
I I I I I I I I $ I I I I I I I
I I I I I I I I I I I I I I I I ___________________
I I I $ I I I I I I $ I I I I I
I I I I I I I I 1 I I I I I I
I I I I I I I I I I I I I I I
I I I I I P I I I I I I I I I $
I I I I I I I 1 I I P I I I I I ____________________ p
I I I I I I I I I I I I I I I I
I I I I I I I P I I I I I I I
I I I I I I I I I I I I I I I I
I P I I I I I I I I I I I I I I
I I I I I I I I $ I I I I I I I ____________________
I I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I I
I I I I I I I I I I I I I I I I
I I I 1 I I I I I I i i i i i i ___________________
I I u . u , I i I I I P I I
I
I
I
— I
-------
Apper dL C
I$0RC flC TA.Rcrr A.MA1.Y11 LIST (VJ..)
Cntr ct R.qulr.d
Vet.etiort LL tt (1,7)
*i *1yte (ug/1.)
A1 inu 200
Mtthony 60
Arsinic 10
200
ery11iu
Csd. fu 5
C 1c1w 5000
10
Cobalt 50
Ccppe 25
1 on 100
S
?‘ae j 5000
‘ar in se 15
? crc ry 0 7
cke]
5000
Se1ir1u. 5
Sllvrr 10
5000
10
SO
Z nc 70
Cyan e 10
C.’
-------
.p erdLx V
TAZL.! 2. fl L .T2 ..D T A D AA 7 £1.L
1 Z1JEPD C C’i4
‘ L M. CONCUZTRATION$
C ( SA PLI
UStD FOR 3CP
* ilytes
( gJ .)
1n erferents
( &Jl)
Ag
1.0
Al
500
3 a
0.5
Ca
500
5 ,
0.5
Fe
200
Cd
10
Co
05
C
0.5
Cu
0.5
) i
Pb
.0
.
‘7
05
Zr
10
E. . /E;
-------
Appendix !
7A. U 3. S?1K1 C LFVELS 1
FOP , SPiXI 5A PLZ AMLYSIS
For lcP/U
For
FUrDace id
Other 2
(U!JL)
(u JL)
(u ,JL)
E1ID r:
Soil
Vater
SoU
A1u inu
2,000 *
J,:i n)’
500 500
100
100
Arsen c
2.000 2.000
40
.•
Zariuz
2,000 2 ,000
£ery11iu
50 50
50 50
5
5
CaIc -
•
200 200
Cooi) .
500 503
Ccppe
250 250
!r
1.000
Lead
500 500
20
20
‘ eS J
n r ese
$00 503
I
c c _y
? c te1
500 500
Po:a s: z
$e1er..
2 000 7.000
10
10
Silve
50 50
Sod t t
ThaIl
2000 2,030
50
50
Vi a :
500 500
Zthc
500 500
Cyan e
IOC
) 07E fle er.ts thout sp e levels and not des r ated vith an
asterisk. s: be spiked at •ppropr ate leve1
1 The levels sno.n jn cate concentratfor s in the i r al di&estste of the
£pi nec sazpl, (200 L final voh mr)
2 Sp .k1rg leve) rrpcted is for both atel and so /sed o ent atr ces
P o p ke reçu ed
t 10 7f
-------
Appendix I
TIj r. 1.
Tt7 J ACt A7O C A3$O&rnoN AMLYSIS $ tDt
PS t PARE AND ANALYZE
MMPLE AND ONE P AE __________________________
U x CRDt,)
CDcubk r jtC1JDlU qiired)
ANALYSE4 TPOJ _____________________
________________________________ DILUTE SAMP l
GALIa A HCE NO AND P1 E
YE3
RECOVERY or pj J If NO. Rrpc i O e
CRLA LR THAN SQ%
H St U NO [ FLAG A7A
17H Ab
YL
_________ __________ TO1 .
CRLATLR _____ TMAr
SAMPLE AeO fA E PIAE RECOY RY
OF SPiJ L A z ______________
AOR ANCE L 3S THA ’
_____________ _______________ __________________ RLP 7
TO TD:.
LAC
YES
.PDE ECOvLRY
IMAN 3 AND —
LESS THAN I ) CAL)B .
CU E
[
QUA TITATC ‘r 5A 3
Pi cU At 6 1 )0% _____________________________
-
or SA tPtt ABSOReANCE
IO’ 5rn 1 fr Ir Ct o t tcd)
I CORRELATION COEFFICIENT
CR(ATER THAN 0 _______
— I! t NO
rLAc OATA WITH
5p .b ’ ’l’(c I.n d (a o t.an ol ph .a np d (abb.n c V . iam Jr
L 1) 7/V
-------
PQpCo Z C
I.IXPLZ DY LIVUT UP (SDO)
TR .TTIC RZPOI? (TI) OOVLP. IWW T
Lab )(a e: ___________________________ Contract )Io.: 68-01 -
lab Code: ___________ Case Mo.: __________ LAS Mo.: _______
y ii sa.*ple Analysis Price in Contract: $_________
SDG Mo./First Sa p1e in SDG: ____________ Sa. ple Receipt Date: __________
(Lovest EPA Saraple )4u er (MM/DD/YY)
in first ship ertt of
sa p1e.s received under SDG)
Last Sa ..ple in SDG: ____________ Sa pIe Receipt Date: __________
(Highest EP? Sample Number . V /DD/YY)
in last shiprient of
samples received under SDG)
EPA S rple umber$ in the SDC (listed in alphanumeric order):
I
2 ________________________________________ 12
3 ______________________________________ 1)
4
5—
6
7 _____________________________________________ 17 _____________________________________
9 ____________________________________ I c
I D
Note: There are a tnaximulr of 20 1 1eld samples in an SDG.
Attach Traffic Reports to this 1or in alphanuLeriC order
(i.e., the order )isted on this lore).
SAmpic Custodian
-------
Appendix l
SUCCLS1ID U4STIWMEP T SLQUE CES (SOW $7)
The foHowin8 iuUested I,JC KQuCDCe$ ire based tipon a 20 p1e SDQ (Sa p1e
Delivery Cro p). The eun ple &znple 1l)s ar d resp cuve eDIJ1tionj ire Iuie below
Also note the abbrev atioas key supplied for raw data
Sainole ID Sarnole T iDe Abbreviations Key
)tZZOO I ILW
MZZOQ2 ILW ILW — lnorgaric Low Water
MZZOO3 ILW 1MW • I rganic Medium Water
MZZOO4 LLW 11_S — Inorganic L03 Soil
MZZOO5 TLW IMS — Inorganic Medium Soil
M2.Z006 tM A XXXXXX • Sample
M.ZZOQ7 IM V XXXX)(XD - Duphcate
M 1 1008 1MW XXXXXXS • Matr Spike (Predigest /Predistill)
MZZOO9 1MW XXXXXXL • Sertal Dilution
MZZO IO 1MW XXXXXXA • Analytical Spike (Posidigest /Postd still)
MZZOII 11_S
M120 12 lu
MZZO I3 ILS
MZZO I4 11_S
M2 1015 11_S
MZZOI6 IMS
IMS
M12018 IMS
MZ.Z0 19 IMS
MZZOO IMS
-------
ICP (DvptIc*(e Ixposur,i eq 1ied)
1) Blank 16) CCV I ’ 33) MZZOOZ 46) MZZ..016D
2) SidI 37) CCB I ’ 32) MZZOO9 47) MZZOI6S
3) Std7 1$) MZZOOID 33) MZZOIO 4$) MZZOI7
4) ICV 39) MZZ.OOIS 34) MZZOIOL. 49) Mll0I8
5) ICB ’ 20) MZZOO2 35 M720 1 1 50) MZZOI9
6) IcSAb 21) M22003 36) MZZO IID SI) MZZOO2O
7) 1 ABb 22) P 1ZZ004 37) MZZ01lS 52) CCV4 ’
8) CRIIC 23) MZZOOS 38) MZZOI2 53) CCB4
9) PB! (1L\ ) 24) MZZOO5L 39) ? 11Z0I3 34) MZZO2OL
30) PB2 (IM\ ) 25) M11006 40) CCV3a 55) ICSA
31) PB3 (ILS) 26) MZZOO6D 4!) CCB3 ’ 56) ICSABb
32) FB4 (IM.S) 27) MZZ00 S 42) MZZOI4 57) CRIF<
13) LCSW 2 ) CCV2a 43) MZZOIS 5$) CCV5
14) LCSS 29) CC82 2 44) MZZO 1$L 59) CCBS ’
15) MZZOOI 30) MZZ00 45) MZZOI6
I An ICV/CCV and )CB/CCB must be performed at )0 frequency or every 7 hours.
whichever is more freQuent —
b The inuial and final analyses of the ICSA and ICSAB solutions muss be performed within 8
hours of each other
c The init è1 and final analyses or the CR3 standards must be performed wiih n $ hours of
each other
2
-------
FURNACE AA (Di p3Ici e 3 jtcI3ob Required)
I) Blank 27) MZZOO2 53) CCV4 79) MZZOI7
2) SIdI 21) MZZ.002A 54) CCB4 $0) MZZOI7A
5) Std2 29) CCV2 55) MZZOII $1) MZZOO I$
4) S%d3 (CRA) 30) CCB2 56) MZZOIIA $2) MZZOIL’.
5) ICY 3)) MZZOO3 57) MZZOIID $3) MZZ0 9
6) IC? 32) MZZOO3A S I) MZZOIIDA 14) MZZOI9A
7) PB) (ILW) 33) MZ2004 59) MZZOIJS $5) MZZO2O
8) PBIA (ILV ) 34) MZZOO4A 60) MZZO ) 1SA $6) MZZO2OA
9) PB2 1M\) 35) MZZOO5 61) MZZOI2 $7) MZZOOI.0’
30) PB2A (1MW) 36) MZZOO5A 62) MZZOI2A U) MZZ00I+t0’
I I) PB3 (ILS) 37) MZZOO6 63) MZZOI3 $9) MZZOOI.20’
12) PB3A (ILS) 38) MZZOO6A 64) ?vtZZOl3A 90) M1100k30’
13) PB4 (IMS) 39) MZZOO6D 65) CCVS 91) CCV?
14) PB4A (JMS) 40) MZZOO6DA 66) CCBS 92) CC?7
15) L W 41) CCV) 67) MZZOI4
36) LCS’ A 42) CCB3 68) MZZOI4A
17) CCVI 4)) MZZOO6S 69) MZ.Z0l$ •MSA sngle inject’or.
38) CCBI 44) MZZOO6SA 70) MZZOISA
39) L S 4$) MZZOO7 71) MZZOI6
20) LcSSA 46) MZZOO7A 72) MZZO)6A
2)) MZZOOI 47) MZZOOS ‘73) MZZO I6D
22) MZZOOIA 48) MZZOO8A 74) MZZOI6DA
23) MZZOOID 49) MZZOO9 75) MZZOt6S
24) MZZOOIDA 50) MZZOO9A 76) MZZOI6SA
25) MZZOOIS 53) MZ10 )0 77) CCV6
26) MZZOOISA 52) MZZOIOA 7$) CCB6
3
-------
FL&P iE (S1agI Ffpolure Reqtilrrd)
I) Blank 26) MZ 0O*
2) SidI 27) MZ 0O9
3) Std2 28) MZZOiO
1) Std3 (CRA) 29) CCV2
5) JCV 30) CCE7
6) JCB 31) MZZOii
7) P81 (ILW) 32) MZl0I ID
8) P82 (ILW) 33) MZZOI IS
9) P83 (ILS) 34) MZZOI2
JO) P84 (IMS) 3$) MZZOI3
II) L W 36) MZZOI4
12) LCSS 37) MZZOI5
13) MZZOOI 38) MZZOI6
14) MZZOOJD 39) )1ZZ0 6D
15) MZZDOIS 40) MZZOI6S
16) MZZOO2 41) CCV3
17) CCvj 42) CCB3
38) CCBJ 43) MZZOI?
19) MZ.Z003 44) MZZOI8
20) MZZOO4 1$) MZZOI9
21) MiZOOS 46) MZZO2O
22) MZZOO6 47) CCV4
23) MZZOO6D 48) CCB4
24) MZZOOÔS
25) MZZOO7
4
-------
MERCURY (Sl &Ie Irpo rt Req itred)
1) Blank 26) MZZOO$
2) SidI 27) MZZOO9
3) Std2 2$) MZZOJO
4) Sid3 29) MZZOI1
5) Std4 3D) CCV2
6) ICY 31) CCB2
?) ICB 32) MZZOJID
8) P3 (ILW) 33) MZZOHS
9) PB2 (1MW) 34) MZZOI2
10) PB) ( 1MS) 35) MZZOI3
I I) PB4 (IMS) 36) MZZOI4
12) LCSS (IL.S, IMS) 37) MZZDI5
13) MZZOOI 38) MZZOI6
14) MZZOOiD 39) MZZO I6D
35) MZZOO IS 40) MZZOI6S
16) MZZOO2 d l) MZIOI7
37) MZZOO3 42) CCV3
18) CCVI 43) CCB3
19) CCBI 44) MZZOI$
20) MZZOO4 15) MZ1OI9
21) MZZOOS 46) MZZO2O
22) MZZDO6 17) CCV4
23) MZZDO6D 18) CCB4
24) MZZOO6S
25) MZZOO7
S
-------
APPENDIX B
Contract Co p1iance Screening
Listing of Defect Statements
-------
CONTRACT COMPLIANCE SCREENING
INORGANIC DEFECT STATEMENTS LISTING
Prepared for
An dy c ca) Operations Braach
Haz.ardou Site F ’aIu tjo Division
US EPA Ofhce of Emergency and Remedial Response
Viar & Company
under
Contract No 68-01-7235
Draft Version January 1989
-------
CONTRACT COMPLIANCE SCREENING
INORGANIC DEFECT STATEMENTS L iSTiNG
Conterin
CCS Error Statements for Forrn I throu&h 14 3
General and Header Criteria for all Forms 4
Criterion A. — Cover Pate. $
Criterion B. - Form 6
Criterion CA - Form 2A 7
Criterion CB. - Form 28
Criterion D - Form 3 9
Criterion E - Form 4 10
Criterion PA - Form SA I
Criterion FB — Form 58 12
Criterion C. - Form 6 13
Criterion H - Form 7 14
Criterion I - Form S
Criterion I - Form 9 16
Criteria KA and K8 - Form I and Form 14 17
Criterion L — Form 10 is
Criterion M - Form II 19
Criterion N. - Form 1, Form 12, and Form 14 20
Criterion P. — Form 13 21
Criterion R — Form 14 22
Criterion R — Raw Data 23
Criterion T. - Traffic Reports 24
2
-------
CCS DEFECT STATEMENTS FOR
RAS INORGANIC DELIVERABLES
The erTOf statea1en and SOW references d cnbed in this document are used for all
uoütication of detects identified during CC$ screening. Each statement is structured as
follows
Square brackets (3 enclose the list of possible items that may be associated with part of
a defeci statement. E.g., (slopefy.intercepVcorrelation coefficieM/x- intercept
(concentration)] (is/are] missng. Only applicable items altould be included for the
report statement.
Parentheses ( ) enclose the page reference to the Statement of Work on which
noILt3canon of noncompliance u based.
) enclose the element w ih which the defect is associated.
For example, statement R14.
) MSA fdata/slope/y-inierceptl (is/are] missing CE 14-17).
could be reported as
Pb MSA slope is missing (E14-17)
The following pages list the error statements to be used for uch type of defect, organixed by
the CCS criterion under which they should be reported. Note that the compliance of sample-
associated blanks, ipikes, and duplicates is partially assessed on the basis of their own
associated QC criteria
3
-------
Ge erg! aod fleader Crfterl. For Cover Page sad Forms Oae tbrougb Fouriua
3. tContrsct No.fLsb Code/Cue No./SAS No./SDQ No.] is/ire missiog or i corrtct o
Form ___.(B12).
2. Lab code i corroci oa Form ___. (812).
3. (Case No./SAS No.] is iocossisteat Do Forzns ____. (833).
4. EPA format is oot followed for Form ____. (A4).
3. Form suffix eot correctly incremented for records correspoDding to Form ____
(HS).
4
-------
CrigerloD A. Cower Ps e.
I. SOW No. u U3iDS or iocormct. (B 14).
2. EPA Sa p1e No. u (r . ot ID a1pha u erk order). (EU).
3. IQue tjoo one/Queujon two u Dot answered (B14). “B
4. Que.stjon Three zs (answered incorrectly/not left blank) (514). S’S..
5. Lab anager’s Signature b Dot pre3ent. (Bid).
6. Spike suffiz (S) is (mi ingfpanciat with an incorrect sa p1e). (B 14).
7. Duplicate suffi.z (D) is (miuiDg/$ssociated with an incorrect umpIej. (S14)
8. Cover page is issaog ( 514).
5
-------
Cr1 rJom B. Fore 1.
1. EPA Sa pTe No. b C s i ng /i icorrect . (B)3).
2. M C ssing/incorrectj. (B15).
3. Lab Sample fl). h inconsistent with the cover pqe. (B 14).
4. Level is ( issingfiacorreciJ. (B12).
3. Date received is ( gfinconsjstent with the traffic reportj. (BIS).
6. % Solids is (missing/inconsistent with the raw da (B 15).
7. Concentratjo units are (missing/inconsistent with the Sample Matrix] (BJS).
8. (Color/clarity C efore/atiery(exture/artif$cts) are (improperly entered/missing]
(B 16).
9. ( ) Concentration is ( .sing/inconsistent with the raw data] (B is).
10. ( ) Concentration flag in Form 3 column C is ssiti /incocjjsierjt with the raw
data] (BiS).
13. ( ) Form I Q qualifier is [ missing/incorrect) (B1S, Cl, D48, D69).
12 ( ) Form I M qualifier is [ missing/incorrectj (BIS)
13 ( ) Reported concentration is not to the required significant figures (Bl5).
14. ( ) Concentration is not corTected for % solids. (B5).
15. Form I is missing. (B5).
6
-------
CriterloD Ct. Fore 2A.
3. Initial 1ibritioe source n kt g . (816).
2. CoDtinuing 3ibrstioa source issicg. (836,17).
3. ()InltiaJ Jibration base ‘aJee is ( inconagtect with the source value].
(817).
4. fllnkial 1ibration found pi3ue is f owJstect with the source value).
(817).
3. Initial calibration SR i s g/incorrect/ncn reported to one decimal place].
(817).
6. flContinuing calibration true value is (mimingfinconsistent with the source value)
(817).
7. ()Cocticuing calibration (ound value is tmining/incorrect/not reponed to two
decimal places) (817).
$. flContinui g calibration SR is ( iming/bcorrect/not reported to one decimal
placej (918).
9. ()M column method is [ miszingfincorrect). (818).
10. ( ) (Inital calib on/continuing calibration] SR. is outside the specified control
hmits. (ES).
11, The &a e continuing calibration standard was not used throughout (or ().(ES)
32. Form 2A is missing (85)
7
-------
Crltedloi CB. Form 2B.
I. AA CRDL. s ndird source i missing. (B18).
2. JCP CRDL standard source missing. (Bi8).
3. ()CRDL. standard source for (AAIICP) u Imissing/not at the CRDL/ ot run at
two times the IDL when IDL is greater than the CR.DL/ not run it two times the
CRDL when the CRDZ. is greater than the 1D14 (B1$,E6).
4. ()CRDL standard (CR!) inilyzed in the middle of the run is (not reported/Dot
reported in the Final Found section of the Forv4 (B 19).
5. ()(CR.1/CRiJ is missing when more than one wavelength is used. (B19).
6. ()CRDL standard for AA true value is not reported to one decimal pLace. (B 18).
7. ()CR.DL standard for AA found value is not reported to two decimal places. (B 18).
8. ( ) CRDL. standard (or ICP (initial found/final foundj is not reported to two
deciznal plae . (BI9).
9. ( ) %R for (AAfICPJ is ( sing/incorrec fnot reported to one decimal place.
(B 18,19).
JO. Form 2B is missing. (B5).
8
-------
Crlteiiie D. Foi 3.
1. Prep* tio bla k caatrLz ist issin /repor e i rtect1yI. (B39).
2. Preptrstio traUo iini are ( iss ooasi teet with the stiiz3. (B 19).
3. ()finitial IibratioE bb.ck/a ueous preparatoo b nk/ooDUeui t Jibr*tio bla k3
I, ( issi g/ineoDjjste t with the nw data/ooi in ug/L/oot reported to oat decimal
plIce3. (B20).
4. ()ibsolate value of I /oo acini4ngj bmtlon blank ezcoeda the IEDL/CRDL.).
(El/Cl).
5. (} column C quilWier is j io /incorroctJ. (B20).
6. M qualifier is tm nifizicorrect). (B20).
7. ()Sa.mple vilue u below 10 times CRDL. and is reported incorrectly because the
preparation blank value is below the negative CRDL.. (17).
1. ()Sarnple value is less than 10 times the preparation blank rilue and the
preparation blank value ticeeds the CRDL. (El).
9. Form 3 is missing (B5).
9
-------
Cri*àr oa E. Fore 4.
1. iCY I D No. I missing. (B20).
2. ()tru. vajues f r fiolution A/solution AB] are (miuinj/inconectJso reported to
the nearest wbole number]. (B21).
3. ICS sour c ID (or Lot number) is missing. (B21).
4. ()f1nitia3f(j ,j found] [ Sol/A/Sol. AB] values ire ( uing/j consistent with the raw
thtafoot reported to the nearest whole number (or solution A/not reported to one
decirn,J place for solution AB]. (B21).
S. ()fNegative/aeroj found value (Or (solution A/solution AB] is
with the raw a J. (B2i).
6. ()Fou d values for (solution A/solution AB] are missing for the wavelength used.
(B21).
7. ( ) %R is Imissing/incorrect/not reported to one decimal place] for (initial found
value/final found value]. (B21).
S Form 4 is mis.sing (86).
tO
-------
-Criterion FA. Form SA.
3. Form SA ii tmis.sing/not performed for specified u.niplej. (B6IE9).
2. latriaflevel] ii (m ng/ine ns s,ent with the traffic repon . (812/822).
3. centrston is Imssszng/jnco (ent with the macri4 (822).
4. () ntroJ limits lYe Imss$thg/incoi-r1c1(not left empty when the U.mple is greater
than (our times the spike added]. (822). s’fi
S. ()sp lked san p1e result is [ i &fo with the raw data/aot in the
appropriate units]. (822).
6. ()(spiked un ple result/sample result) C qualifier h (missing/incorrect] (822).
7. ()sample result is with the raw data/incon jj en with Form
1] (822).
$. ( ) spike added is [ missingfincori.ect] (B22).
9. ()%R is C iDgfincorrec no reported to one decimal place]. (B22).
30. ( ) Q qualifier is (missingfincorrect whec the umpie is four times greater than the
spike added] (8221E9).
Ii. ( ) M qualifier is (missing/incorrect) (B23).
12.( ) (spiked ple resultf mpie result/spike added] is missing for the alternate
method used. (E9).
33. EPA Sample No. is missing suffix (813). •‘B
I I
-------
CriterloD TB. Form SB.
1. Form SB ts esiasing. (B6). B
2. [ Mstrix/Levefl is C issingfin nsistent with the traffic report). (B22/B23). ‘B’
3. ()fconvol Iindt/%RJQ field) u reported when ft should be blank. (B23). ‘B’
4. ()Sample result is C g/inconsisteni with Fore I/not reQuired/not reported to
two decimal places/not in ugfLJ. (B23).
S. (),piked u .mple result Is (utiuing/incon istern with the raw data/not reported to
two deithntl pisces/not reported in ug/L). (B23). B’
6. (Jspike added is [ missing except for Ag/incorrect/cot reported in ug/L/cot
reported to one decimal place/cot added at the greater of two times CR.DL or twice
the sample value) (823/E9). “B’
7. ()%R is (c issingfincorreci/cot lculated to one decimal place/not reported when
negative/not reported when zero). (B23). •‘B”
L ( ) Q qualifier is not left blank. (B23). “B’
9 ( ) M quahfier is ( issing/jncorrect) (B24) ‘B”
10 EPA Sample No is missing an A suffiz (B8). ‘B
12
-------
• CrItei Io C. FDnn 6.
L Fonc zs izsing/ ot submitted for specified u.mple]. (B6JEW.
2. (Mss rizfL.eve)j u s’ing /izcoc istent with the btWsc report). (824).
3. % soLids for (sa p2e/di pliste) u iiss&zg. (824).
4. Coccectratio are Im s z finco sizteot with the matzii). (824).
S. EPA Sample No is issrng the D suffli. (B13). e• 8 ee
6. ( ) co tro1 limit is (mimicj ir correctfcot corrected for origical sample weight/cot
corrected rot % solith/eot left empty whec sample or duplicate is greater than five
times CRDL). (824,27,Ell). “B’
7. ()umple va1ue is (mhsing/inconsisteat with Form lfinconsiste t with the raw
data). (824).
8. { ) Dupli te value is (miuiog/inconsisteot with the raw data) (824).
9. (CIM] ua1ifier is (missiag/socorrect). (B24,25).
10. ( ) Q quahf er is (missiog/iricorrect) (B24,25).
Ii. ( ) RPD is (missing/incorrect/not reported to one decimal pLace) (824.2$).
13
-------
CrIierku H. Fouu 7.
I. Form 7 is musing. (B6).
2. Solid/AqueousJ LC Source ID (or Lot number) is musing. (B25).
3. ()fAqueous/SolidJ true value u (mi sing,fincorrect]. (B23).
4. ( ) Aqueous found value is (missiD&fjn r)r,JiJtent with the liw dats/not reported to
Iwo decimal places). (B25,26/E32).
S. ( ) Solid found value is (missing/outside the control limits/inconsistent with the raw
data/not reported to one decimal pLace). (B25261E 12).
6. ( ) Aqueous %R is (missing/incorreci/not reported to one decimal place/outside
control limits] (B23,26).
7. ( ) Solid %R is (mi.uing(jncorrec(/no reported to one decimal place). (E25,26).
B’
8 ( ) C qualifier is rnissicg/incorrect]. (B25).
14
-------
Criterion I. For. I.
i. Form I is missing. (Be).
2. (EPA Sample No./ alytefdjJ jo 0 (actor) ii (missing/not in &phanumerjc
order/inconJ isient with the raw data) (B26).
3. Added ( ,D °fl/sb orb j is (mi 5$ing/inco istenl with the raw data).
(B26,27).
4. Final trsti is ssing/iz asj with the matriz/jnconsistent with the
raw data) for EPA Sample No. (B27).
S. MSA was incorrectly done on the LC . CE 14).
6. Final concentrat ion b (missing/not reported to one decimal/not reported as an
*b lute viiue/j not reported as less than the IDL] for EPA Sample No. (B27).
7. R value is (missing/not con.sistent with the raw data) for EPA Sample No (B27)
I. MS was not reported as required (E14-37) for EPA No.
9. Q Qualifier is (rnissing/incorrectJ (Ei4- 17)
‘5
-------
Crfterloa J. For 9.
I. Forn 9 j i ing. (B6).
2. [ MatrizfI v J3 u (c iuing /i consjste t with the tnITic report]. (B28).
3. ()I Jtj j Sa pJe result as 1 issingf consistent with Form 1]. (828).
4. ()serisj dilutiQD result as ( ing/incon jste t with the r*w diti/ ot ukip!ied by
33(828).
3 ()% dif(ere ce as [ iissingfincon . tj (828).
6. ()(lniiiaj Sample/Seriti dilution] result C qu&lifier is (missi g/incorrectj (B28).
7. ( ) Q qualifier is (m ing/j orrecl] (829).
8. ( ) M qualifier is [ missing/incorrect] (829). B
16
-------
CiiIuti &A B. Fore I sDd Fore 14.
1. (Mercy/C’yi.nide] hoIdi g time (cs. ot be deerrar ed/,zceed SOW specificationi.
(D4).
17
-------
Crft,rloa L. Fore 30.
3. Forna JO is missing (86).
2. Date is missing 830).
3. [ ICPfFlatne/Furnace) ID Number is missing. (B30).
4. ( ) Wavelength is (issingfnot reported to two decimal places] (B30).
S. ( ) Background code is [ g/incorrect] (B30).
6. ( ) IDI.. is (missing/not reported to one decmaj place] (B30).
7. ( ) M qualifier is (sing/incorrect] (B30).
Z Instrument (_ ) IDI..s were determined more than three monthi before the
date of analysis. (E14)
9 Sample values are invalid because the IDL exceeth the CRDL and reported values
are less than 5x IDL. (A2)
18
-------
CrIt.do M. Form 11.
I. Form Ii as iuing/ ot reported is required]. (B6).
2. Due as iuing. (B30).
3. IC? ID No. as issit g. (B3 1).
4. ( ) Wavelength as (missingfeot reported to two decitna3 places]. (B31).
5. tM/Ca/Fe/Mg] correction (actor is ( hsing/not reported when (z.ero/aegative).
(B3 1).
6. lrLztrunaent ( ) corteetion (actor(s) (was/were] determined more than one
year from date of analysis. (E16).
19
-------
CriverloD N. For 1, Fore Il, aad Fore 14.
1. Form 12 u missing. (832).
2. ICP ID No. is missing. (832).
3. Date ( iissing/i correctj. (832).
4. ()Integrsti time i i g/zaot in seconds/greater thu five spaces] (B32).
5. ()Concentratjon is (missing/not in ugfLj. (832).
6. (1 M qualifier is [ reported improperJy/mj jng (NR)J. (832).
7. ( ) linear range(s) (was/were] determined more than three months
before the date of analysis (E 16).
8 ( ) Concentration reported on Form I was obtained from a va’ue exceeding the
(Irnear/cal ibrac ion] range. (A3, 834).
20
-------
Crilirlee R. Form 13
I. Form 13 is (B35).
2. More thin 32 analys were reported on one Form 33.
3. Method of analysis is t iuingfnot an acceptable code]. (R35).
4. [ EPA sample no./dupli te/spjkejf [ ,prep blink] is [ missing/not in ascending
alpha numeric order/for fted inCOrrectly]. (B3$).
5. Reprepar j , of [ EPA U.mp e no.fduplic$te/spjke,q /p p blank) was
(missing/not in the order of increasing preparition date/formarted incorrectly]
(B35).
6. Preparation date is [ formatted incorrectlY/iflcOrTectly/rnj$$;flg/j , . I with respect
to the method used] (B35).
7. Under weight’, the wet weight is [ missing/not reported to two decimal places/not
ir grams/not the wet with regarth to the method to analysis) for
soil Samples (B35)
8 Weight as not bLa.nk for water samples. (B35)
9. The final volume is [ missing/not in mI/not to the nearest whole number) (B35)
21
-------
Crltei4oa R. Fore 14
I. Font 34 as maisiri;. (B36).
2. The followiog (field umple/QC sample (i.e. the calibration standards, ICVs, CCVs,
lCBs, CCBs, CR.M, CRIt, ICSs, LR.Ss , LCSs, PBs. duplicate, serial dilutions, pre-
digestion spikes, post digestion spikes, analytical spikes) MSA addition]. Issociated
with the SDG, (was/were] tot reported (or the following (AoalytesfMethod] on
Form 34. (B36).
3. More than 32 analysis were reported on one Form 34. (836).
4. Instrument ID number as (missing/greater than 12 spaces/not Uniquely den&ying
the instrument used to produce the data) (836).
5. Method code is (missing/greater than two characters).
(836).
6. rStart Date7End D te’)is (missing/formatted incorrectly/not when the analysis as
(done/ended) (B36).
7. Sample No. is not [ formatted properly/in temporal order) (B36)
S Dilution factor is (missing/not to two decimal places/incorrectly including the
inherent preparanort dilution) (837)
9 Time is [ not in the correct format/missing] (87) (837).
20. Percent recovery (or the furnace analytical spike(s) [ as/are) [ missingjincorrect).
(837).
I I. Data missing for ( ). (837)
22 Instrument calibration is not (performed/performed with proper number of
standards) for ( ) (E3).
13 Instrument calibration was not performed within 24 hours of analysis for { 3. (E3)
14. The two hour calibration time limit (or is violated for ( ) (ES).
15 The 10% calibration frequency is violated for ( } (ES, E6. E 14, E15)
16 (1c /CR1J (was/were) not analyzed twice within the 5 hour working hiIt for ( J.
(E6, ES)
17. The MSA tree was not followed correctly for ( ). (E 14)
18 [ ICS/CR1/ICVJ was not performed after calibration for ( ) (E6)
19 (ICB/CCBJ was not performed after (ICV/CCV) (or (3. (E6)
20. (ICS/CRI/CCV] was not performed at the end of the run for ( ). (E6)
21. Preparation blank anlyt cal spike recovery is out of SOW specified range for
(El?).
22 Sample was not run initially undiluted for ( ). (A3)
23 Serial dilution was not performed at Sx dilution for ( ) (E12)
22
-------
Crltetion L 8.aw Data
1. flCpffuuoefFlame/HSJCN] nw data are musin&. (B7).
2. SDG ckage is not numbered se uentia1ly. (84).
3. ()R.sw data is [ iUegible/deletod but not signed/unclear). (87).
4. SDG package not submitted with single-sided pages. (83).
3. SDG package forms are not in Ineres.sing EPA sample alphanumeric order. (8$).
6. 1nstrument readouts i.s strip charts/tapes/or hard cOpies are necessary. (86).
7. ( ) Raw data are submitted out of order. (86).
8. ( ) jw data are not labelled with (EPA umple number appropr*ale codes) (87).
9. ( ) Data for (calibration (standards/source/solution’preparation date/blanks)fs*mple
(volune/weight/dupl cate/spikes/seriaI dilution/analytical
spike/%R/CV/)/instrument usedfbackground correci on usedf) are missing (87)
tO. ( ) MSA [ data/slope/y-intercept] (u/are) missing (E14-l7).
I I. ( ) Integration limes are missing for AA analyses (87).
12 Digestion log(s) (is musing(uaiple/preparition blankfLcSfdate/volumefweight
used) (89)
13 AQueous pH is (less than 2/greater than 12/missing) (89)
14 ( ) Value is not reported uncorrected in the raw data (A3).
iS Dupitcate exposures are missing for ICP. (Dl).
16 { ) Furnace element did not have double Injections (except MSA) (E14)
17. (ICP/Furnace/Flarne/NG/CNJ standard curve is incomplete. (E4)
18 ( ICP/Furnace/flame/H3/CN) itandard at the CRDL is musiag for ( ) (E4)
19 EPA specified (lCP/FurnacefF1an e/Hg/CN) method was not used for ( ) (A2)
20 Furnace spike was added incorrectly for ( ). (ElO).
21. Percent solids data are (missing/incorrecl] (BPS. Eli)
22 The MSA tree was not followed correctly for ( ). (El4)
23. Post digest spiking volume exceeded 10% of the umple volume (E16)
24 Standardization solution concentrations are missing (B7)
25. ln.strument was not calibrated (daily/when it was set-up) (E3)
23
-------
• CrIierIoa T. Traffic Rrporti
I. Traffic report is iss ng. (B4).
2. SDO Group No. is tmissiog/improper,y assigned) on traffic report (B4).
3. SDC final saa ple iuing on uiffjc report (B4).
4. (Lab minager’s aignature/r ip( date/saple condjtjo on receipt] is missing on the
traffic report. (B4).
5. (Matrix spike/dupli te/urisi dilution) was run on a field blank. (E9,ll, 12).
24
-------
APPENDIX C
Cor p1eted Data Va1idat on Reports
-------
FIGURZ 6
000 SUMMAqY FORM
S TI
uaou
k 4 P O PtMO T ATTO J PHAII _______________
*J IP.* !I
I. MI I*
I JS riLD 1 I I
I VU / YI “
r r A ,1 I ‘
r 0 I O(I .)O
- . I,
i O$Jtct’vl E4Zo ‘OCLt4 -U tit 4ar pLed o det€A,Mnt t1
Mt p 6trL Z <‘ k€ ttL &e2L4 a d
Lc eL6 o cr ajvt n ot - 2e ob e Oil
‘i a .,fl cc o •a & tI CO4 RI M7 SFA.C1 )
IA A
cL Lt r
( T lPEIA *.L S,SIAlC.’4 -
________ Thji5PhQ iP $6I& C _______
I $L&I. 1Pt A
I $iTt IO b &TIQS
2OO X ?OO dtpi c 75 t_t
c,OJ,c IWkTtpfl
%OITYI’I$ G_ a! ti-d 3C ’z io1c 3o->7oo
Pk P
D * Il Pt $ C J 7 Qa 74
& LfTC& *T S P ALDA1A
Pt SI CW PtP (4 JYY
C O .C TMT L ._ ‘c tr, I
M
T .P
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SOW.
DPO-
7 7
ACTION
DATA ASSESSMENT SUMMA&Y
I. HOLDING TIMES — — 0 _____ _____
2. CALIBRATIONS — 0 0 ______
3. BLANKS X 0 ______
4. ic N 1 — _______ _______
S. LCS 0 0 ___
6. DUPLICATE ANALYSIS 0 — 0 ______
7. MATRIX SPIKE 0 0 ______
g. MSA ______ N 2 ______
9. SERIAL DILUTION — p ______ ______
10. SAMPLE VERIflCAT]ON ______ 0 - ______ ______
II. OTHERQC p _____ _____
12. OVERALL ASSESSMENT . — 0 _ — 0 _____ _____
0 • Data had no problems/or qualifled due to minor problems.
M • Dita qua.lified due to major problems.
Z • Data unacceptable.
X a Problems, but do not affect dati
ACTION ITEM.t —
AREAS OF CONCERN. - e c .inc ed a mp u, du to L co
. jtom ito,t. N 2 - Ve1 cJ o Lu, Ltó a t eAti cJ d thaJ2,.. .j’ du to to& ’
sp e ‘LecoveA.1 .e4.
NOTABLE PERFORMANCp .____________________________________________
INORGANIC PECIONAI. DATA ASSESS IENT
CASE NO _ 9764
LABORATORY XYZ Labcon .A
SITE _ 8C SL e
NO. OF SAMPLES,
MATRIX — 10 4Ou oLL8 —
REVIEWER (IF NOT ESD) Rog F. (‘JQ oto
REVIEWER’S NAME Ko &ot-Anne 0’ L a.’w
COMPLETiON DATE 11/7$/
IC ? AA Hg CYANIDE
___________ ___________ 0 ___________
__________ 0 __________
__________ 0 __________
___________ 0 ___________
__________ 0 __________
_________ _________ 0
_________ 0 __________
__________ 0 __________
-------
November 16, 1988
Dennis Gagne
Regional Sample Control Custodian
U.S. Environmental Protection Agency
90 Canal Street
Boston, Massachusetts 02114
Re: TID No. 01—8809—15
Case 9164, SDG235
XYZ Laboratories
ABC Site, Lexington, MA
Metals: 10/aqueous
Dear Mr. Gagne:
A validation was performed on the inorganic analytical data
from 10 aqueous samples collected by L1 0 at the ABC site. The data
here evaluated based on the following parameters:
* . data completeness
* • holding times
• calibration verification
• laboratory and field blank analyses
• ICP interference check sample results
• matrix spike recoveries
* • laboratory and field duplicates
• laboratory control sample results
• furnace atomic absorption results
• • 5erial dilution results
* • detection limit results
* • sample results
* All criteria were met for this parameter.
Table I summarizes the validation recommendations which were based
on the Z 1lowing information :
-------
) ovei ber 16, 1988
Mr. ;Dennis Gagne
Page 2
libration Verification
The 2xCRDL standard for Cadnium had a recovery of
Results near the CRDL nay be biased low. Estimate (. ) positive
results less than 3xCRDL and non—detected results (UJ).
Element axir um Conc,/Units Action Level
Antiriony 53.4 ugh 267 ug/l
Copper 12.1 ugh 60.5 ugh
Zinc 6.0 ugh 30 ug/l
Value > ZDL and < Action Level Report value V
Value IDL and > Action Level = Report value unq-ualified
1cp interference Check a.E p1s
Positive results were observed for Antimony in ICS A solution
although there is no Antinony present in the solution. The
positive results may be due to an interference fror iror .
Significant levels of iron are present in the sarples. It is
recormended to estimate all positive results for Antinony.
? (atr x 8 ike Recoveries’
TRts A na lvte Percent Recovery
MA.E236 Silver 72
MAE23G Lead 60
Positive and non-detected results shall be estimated for both
Silver and Lead.
J, .aboratortP puplicates
Laboratory duplicates did not meet required criteria for
Copper. Estimate (.1) positive results only.
Post—djgestion pjkes
The following samples analyied by graphite furnace had low
post digestion spike recoveries:
-------
.Mr. t ennis Gagne
Page / 3
)4ovember 26, 1988
MAE237, MAE247
MAE246
All except MAE24O and M) E247
affected samples are non—detected and shall be estimatei
(UJ)
Serial pilutiofl na1ysts
Serial dilution results did not ieet req .iired criteria for
Calcium. Estimate (J) all positive results.
No other prob1e s were encountered with this case.
joseph D. Mastone
Teait 1 anager
ESAT Region 1
Lie ne nt
Selenium
Lead
Thallium
All
Samples Affected
Very truly yours,
ROY 1. WESTON, INC.
Karol-Anne O’L.eary
Data Reviewer
Y AO/ k a o
Enlosures
cc. 0. Szaro
-------
BC Bit. )l& .
C&ss 93
Tabis . Reco mer 6atien Bu mary
Aluminum Magresium
Antimony A’ Manganese
Arsenic Mercury
Barium Nickel
Serylium Potassium
Cad ium Selenium
Calcium Silver
Chro r ium So um
Cobalt Thallium
Copper A’, J3 Vanadj
iron Zinc
Lead Cyanide
if the field is left blank the qualifier is A — Accept all data
— Accept data, raise the sample detection limit(s) due t
blank contar ination.
3) — Estimate (1 )3) non-detetced resuits due to poor linearity
near the CRDL. Detection limit is biased low.
— Estimate (3) positive values and detection linuts ( )J3)
due to low matrix spike recoveries. These estimated
results would be minimum values.
3’ — Estimate (3) all positive values due to duplicate
precision.
— Estimate (1)3) non-detected results due to low matrix
spike recoveries for Se (MAE237 and MAE247), and TI (al]
except MAE24O ard MAE247).
— Estimate (3) positive results due to a supression
observed through the serial dilution analysis. Estimated
results represent minimum values.
-------
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-------
REGION I
Data Re ’iew Worksheets
Site Name A3C S.te
Reference Number 01 - Haq- i
REGION 2 REVIEW OP INORGANIC
CONTRACT LABORATORY DATA PACKAGE
The hardcopied (laboratory name) XV? Lab n .a. o&ieA data package received
at Region I has been reviewed and the quality assurance and performance
data su ii arized. The data review Included:
9164
MAE 23
10
Sampling Date(s)
Shipping Date(s)
Date Re ’d by Lab
03/U/U
03/79/ U
Traffic Report Nos: MAf235 - MAE24O MAE245 - MAE247. MAU5
7rip Blank No.:
Equipnent Blank No.:
Yield Dup Nos:
SOW No. ? / 7 requires that specific analytical work be done and that
associated reports be provided by the laboratory to the Regions, EMSL-
LV, and SMO. The general criteria used to determine the performance were
based on an examination of:
-Data Completeness
-Holding Tines
—Cal ibrat.ions
-Blanks
—IC? Interference Check Results
- atrix Spike Recoveries
-Laboratory Duplicates
—Field Duplicates
—Lab Control Sample Results
-Furnace XA Results
—ICP Serial Dilution Results
—Detection Limit Results
-Sample Quantitation
Overall Comments: Tii da. pac c ‘ A c ” p e.Zc a.tid cc’pw wvte ci gc’cd
gu.a.U ‘1.
Definitions and Qualifiers:
A - Acceptable data.
.3 — Approximate data due to quality control criteria.
R — Reject data due to quality control criteria.
U — Analyte not detected.
Case No.
SOC. No.
No. of Samples
SAS No.______
) atrix
Reviewer: KaitcL -An O L oiui
Date: 11/7 /U
-------
REGION I
Data Review Worksheets
. ROL .DING TI S Complete table for all samples and Circle the
fractions which are not within criteria.
HG CYAN1DE OTHERS P t Ac ON
SAMPLE , DATE DATE DATE DATE
ID ‘ SAMPLED ANALYSIS ANALYSISANALYSIS
I, I I I
MA123 03/14/SS 03/27tH M 04/77/U 2 ____________
MAE236 03/74/H 03/27/fl NA 04117/U 2 _____________
i I
MAE237 03fl41fl 03/27JU __________ 04] 17]U . 2 ____________
13 I I I
MAE23 03’14/fl 03/27/ f l NA 04/ 77/U 7 _____________
1 13 I
MAE739 03/14’fl 03/271H WA 04/77Jfl . _____________
‘12
MAE2JO 03175!U 03/271U NA 04 117 /U 2 ____________
10
MAE24 ‘ Q3/77/fl 03/27/H MA 04177/H 2 ______________
‘70
MAE246 03177/H 03 /27/ f l NA t 0 4 /17 / f l c 2 _____________
M1E247 ‘ 3/UIU 0 3/27/fl ‘ MA 04 ’17JH 7 _____________
11
MA 25 031161U 03127JH NA 041 17/ H 7 _____________
I I
I I I
I ______ _____ I I
I I I
I I I I I I
I I I i I
I _____ I I I I 1
I _________ I I I I _______ I ___________
METALS — 180 DAYS FROM SAMPLE COLLECTION
MERCURY — 28 DAYS FROM SAMPLE COLLECTION
CYANIDE — 14 DAYS FROM SAMPLE COLLECTION
ACTION:
1. If holding times are exceeded all positive results are
estimated (i) and non—detects are est mated (Uj)).
2. If holding times are grossly exceeded, the reviewer m y
determine that non-detects are unusable (R).
-------
REGiON I
Data Review worksheets
I I I . INSTRUMENT CMJBR) 1 T10N (Section 1)
1. Recovery Criteria
List the analytes which did not meet the
for Initial or Continuing Calibration.
percent recovery (%R) criter
I cv/CcV !
Metals
Mercury
Cyanide
Estimate (J )
5-89%R, ill—125%R
65—79tR, 121—235%R
0-84%R, 116—130%R
Estimate (U. )
,5—89%R
6 —79%R
70-84%R
Reiect (R
c75%R, >125%R
<65tR, 135%R
130%R
Reiect (R )
<75tR, >125%R
<65tR, >135%R
(70%R >130%R
DATE
ACTION SAMPLES AFFEC
ACrIONS:
if any analyte does not meet the %R criteria follow the actions stated
below:
For Positive
Results:
? ccept
Metals 90—llC%R
Mercury 80- 120%R
Cyarude 85— 1 15%R
For Ncn—detected Results:
? ccept
9 0— 12!%R
8O-135%R
85- 13 0%R
AU c& c ZuL4 a MiMe met.
-------
REGION I
Data Review Worksheets
II B. INSTRUMENT CALIBR) 1 TION (Section 2)
2. Analytical Sequence
A. Did the laboratory use the proper number of
standards for calibration as described in the
SOW? Yes or No
B. Were calibrations performed at the beginning of
each analysis? Yes or No
C. Were calibration standards analyzed at the be-
ginning of sample analysis and at a minimum fre-
quency of ten percent or every two hours dunng
analysis, whichever is more frequent? Yes or No
D. Were the correlation coefficients for the cali-
bration curves for AA, Hg, and CN O.99 > Yes or No
E. Was a standard at 2xCRDL analyzed for all IC?
analyses? Yes or No
if No,
The data may be affected. Use professional udgenent to deterr ine
the severity of the effect and qualify the data accordingly. Discuss
any actions below and list the sa tples affected.
CRDL t’ da d Ac’ Cad,r w, h ad a ci i ci 6 . t r te a.U ‘a i
Ca ,’ .&wn 3 X CRVL C1 4JL). -
-------
REGION I
Data Review Worksheet
IV ,. BLXN NALYSI8 RESULTS (Sections 1—3)
AQU Q
Ac uU u.4
ANALYTE
Sb
Cu
MATRIX : Aqaeo .4
ONC. /UNITS
S3.4
12.1
6.0
2. Equipment/Trip Blanks
DATE EQUIP BLI
ANALYTE
CQP C. JUN ITS
3. Frequency Req rements
A. Was a preparation blank analyzed for each matrix
for every 20 samples and for each digestion
batch?
B. Was a calibration blank run every 10 samples or
every 2 hours whichever is more frequent?
11 No 1
;Or No
No
The data i ay be affected. Use professional judgement to determine
the severity of the effect and qualify the data accordingly. Discuss
any actions below 1 and list the samples affected.
A separate
List the blank contamination in Sections 1 2 below.
worksheet should be used for soil and water blanks.
1. Laboratory Blanks
DATE ICB/CCB! PREP BL _______
4113/H iCE ________ _________
4 17 31U __________ ________ _________
411 1’ ____________ __________ ____________
-------
RIGION I
Data Review Worksheets
LV B. BL.A}4X A.NALY8IB RESULTS (Section 4)
4. Blank Actions
The Action Levels for any analyte is equal to five tines the highest
concentration of that element’s contamination in any blank. The action
level for samples which have been concentrated or diluted should be
multiplied by the concentration/dilution factor. No positive sample
result should be reported unless the concentration of the anelyte in the
sample exceeds the Action Level (AL). Specific actions are as follovs:
1. when the concentration is greater than the IDL, but less than the
Action Level, report the sample concentration detected with a U.
2. When the sample concentration is greater than the Action Levels
report the sample concentration unqualified.
MATRIX: MATRIX: ____________
ELE ’ENT MAX. CONC. / ?.. .LL ELEPENT MAX. CONC.I
UNITS UNITS UNITS UNITS
Sb 53.4 2o7 u L _______ _____________ _________
Cu 12.? u IL _______ _____________ _________
Zn &.O 30 ugiL _______ _____________ _________
) OTE; Blanks analyzed during a soil case must be converted to mg/kg in
order to compare them with the sample results.
Conc. in ug/L X Volume diluted to (200ml ) X X l000qm X 1nL mg/kg
Weight digested (Igram ) l000mi 1kg l000ug
Multiplying this result by 5 to arrive at the action level gives a fina’
result in mg/kg which can then be compared to sample results.
-------
REGiON I
Data Review Worksheets
V. 1CP INTERFERENCE CHECK BA 4PLE (Sections 1 2)
1. Recovery Criteria
List any elements in the ICS AB solution which d d not r eet the criteria
for IR.
DATE ELEMENT ACTION SMPLES AFFECTED
ACTIONS:
If en element does not meet the %R criteria , follow the actions stated
below
PERCENT RECOVERY
<50% 50—79% >120%
Positive Sample Results R J
Non-detected Sample Results P UJ A
2. Freçuency Pe uirements.
Were Interference QC samples run at the beginning and
end of each sample analysis run or a minimum of twice
per 8 hour working shift, whichever is more frequent? Yes or No
If no,
The data may be affected. Use professional judgement to determine
the severity of the effect and qualify the data accordingly. Discuss
any actions below end list the samples affected.
.U acceptable.
-------
REG1ON I
Data Review % . or) sheets
V B. I P IN ERFER2NC! CRECX ØAMPLZ (Section 3)
3. Report the concentration of ny elements detected in the ICS A
solution > 2xIDL that should not be present.
ELEMENT CONC. DETECTED CONC. OF INTERFERENTS
IN ThE ICS IN THE ICS
AL CA FE pt
Sb 0 u /L 5O6 O 23OOO 711 OO S2JDO O
Estirate the concentration produced by the interfering element in all
affected sanpies. See gudelines for examples. List the sa-.ples
affected by interferences below:
SAMPLE ELEMENT SAM?LE SAMPLE INTERFERENT ESTIMATED
AFFECTED AFFECTED CONC. CONC. INTERF.
(ug/L) AL CA FE MG (ug/L)
MAE235 Sb ___________ — — 71Z.QOO_ 27
MAU3 Sb ____________ — — 9jjQO 24
MAE24O Sb t7 — — Lj .Q . OO 32
ACTIONS:
I. In general, the sample data can be accepted without qualification f
the sample concentrations of Al, Ca, Fe, and Mg are less than 50% of
their respective levels in the ICS solution.
2. Estimate (3) positive results for affected elements for samples with
levels of interferents 50% or more of that in the ICS solution.
3. Reject (R) positive results if the reported concentration is due
entirely to the interfering element.
4. Esticate (Ui) non-detected results for which false negatives are
suspect.
Give explanations for any actions taken below:
E t4J7 2e [ .1) pc .Ltu xc ” ar t.uno iy.
-------
REGION I
Oata Review Worksheets
VI. KkTRIX OPI7 .
TR 0 U4E 36
MATRIX: AQueo .o
1. Recovery Criteria
List the percent recoveries for artalytes
required criteria
S — e ount of spike added
SSR - spikes sample result
SR — sa p1e result
SSR SR S
S ’.2 ei.
36
4 .Ou
Lead
16
4,1
ACTIONS:
1. It the sarple concentration exceeds the spike concentration by a
factor of 4 or more, rio action is taken.
2. if any analyte does not meet the %R criterza follow the actions
stated below:
Positive Sample Results
Non-detected Results
2. Frequency Criteria
3
3
3
R
UJ
A
A. Was a matrix spike prepared at the required fre-
quency?
B. Was a post digestion spike analyzed for elements
that did not meet required criteria for r atrix
spike recovery?
No
No
Analyte
which did not meet the
Action
50
72
J!’1. UJ
20
60 U) N!
Matrix Spike Actions apply to all samples of the same matrix.
PERCENT RECOVERY
< 30% O%—74% ‘ 125%
A separate worksheet should be used for each matrix spike pair.
-------
REGIOI4 I
Data Review Worksheets
V I !. LXBORATORY D PL.ICATES
List the concentratiOns of any analyte not meeting the criteria for
duplicate precision. For soil duplicates, calculate the CRDL in mg/kg
using the sample weight, volume and percent solids data for the sample.
Indicate what criteria was used to evaluate precision by circling either
the RPD or CRDL for each element.
MATRIX: AQU OU .4
tle ent ____ ________
Aluminu.m ______ ____________
Antimony_
Arsenic_____ ______ ______________ ______________ _____ ________
Barium______ ______
Beryll ium _•• ____
Cadmium_____ ____ ______________ _____ ________
Calcium_____ ______________ _____ ________
Chromium
Cob a it______ ______________ _____ _________
Copper______
Iron________
Lead________ - _____ ________
Magnesium ._. 500 _____ _________
Nanganese_ S _____ _____
l4ercury____ . —
Nickel______ 40 ______ ______________ ______________ _____ ________
Potassium . ._. 0 .
Se1eni .Lm_ 5 ______
Silver______ 10 ______
Sodium_____ j j j
Thal liu.m 10 _____
Vanadui.im ______
Zinc_______ 0)
Cyanide____
1. Estimate (J) positive results for elements which have an RPD >20%
for waters and >35% for soils.
2. 11 sample results are less than 5x the CRDL., estimate ( . ) positive
results - a- -d--- ) ‘ ‘te-et d iIU1S for elements whose absolute
difference is >CRDL, (2xCRDL. for soils). If both samples are non-
detected, the RPD is not calculated (NC).
Sarole I
MAE 2 36
60. 5
Dur !llcatel Q Action
MAE 2 36
54.7
- u
3.0w
CR DL
water soil
“?$J -! . mg/kg
_ 2QL ____
60 ______
5000
10
J25)
37 u
3 Cu
2
NC
5 . Ou
NC
33400
4 0 !A
4.31.1
78.3
?.Ou
MC
S.Ou
NC
0.3
33500
4.Ou
4,31. 4
62.9
4. 2
142
5.2
)1 )
22.2
I ,
2000
NC
NC
2.8
NC
NC
23.2
70 u
0.71!
7810
1740
l
7 0
7.0
NC
4.0 i
4 .0w
NC
78900
18500
2. Cu
4 Its ,
4.01.!
596
4L3
Laboratory Duplicate Actions should
the same matrix type.
ACTiONS:
NC
NC
be applied to all other samples of
-------
REGiON I
Data Review Worksheets
VIII. TIELD DUPLICATES - nc C appL .cab e
List the concentrations of all analytes in the field duplicate pair.
For soil duplicates, calculate the CRDL in mg/kg using the sample weight,
volume and percent solids data for the sample. Indicate what criteria
was used to evalute the precision by circling either the RPD or CR01.. for
each elenent.
MATRIX: ____________
Element CRDJv _______
water soil _________
ug/L mg/kg
Aluminu m_ _200_
Ant jmony_’_GD_’
Arsenic____ _iO_
Barium______ _200
Bery l li um_ 5 ______ _____________ _____________ _____ ________
CadITIU ____ ____ ______
Calcium____ _5000_
Chrou iu. 10 ______ ______________ ______________ _____ ________
Cobalt_____ 50
Copper_____ ‘_25) ______ I
Iron________ _l00 _______ ______________ ______________ I
Lead_______ ____S ______ _____________ _____________ ________
Magnesiu .m_LS 0 00 _
Manganese_’ _l5_
Mercury____ _0.2_
Nickel______ ______ _____________ _____________ _____ ________
Potassium_ _5000_
Seleniu_. . ____ ______ _____________ _____________ _____ ________
Silver______ _10_
Sodium_____ S000_
Thalliu . 10 ______ ______________ _____________ _____ ________
Variadn. _ _50_’
Zinc________ ______ ______________ _____________ _____ ________
Cyanide_____
Field Duplicate Actions should be applied to all other samples of the
same matrix type.
ACTIONS:
1. Estimate (J) positive results for elements which have an RPD >30%
for waters and >50% for soils.
2. if sample results are less than 5x the CR01.., estimate (J) positive
results &, . è jU2) rt— - - t Pid iul- for elements whose absolute
difference is >2xCRDL., (4XCRDL. for soils). if both sample5 are non-
detected, the RPD is not calculated (NC).
Sample I
Duol icatel
Action
_________ i
1
1 I
_____________ I
-------
REGION I
Data Review Worksheets
I I. W BOR.1iTORY CONTROL BA1 PL3 a U accept ib e
L Aqueous L.CS
List any LCS recoveries not within the 80-120% criteria and the samples
affected.
DATE ELEMENT i.a ACTION SAJIPLES AFFECTED
2. Solid L.CS
List any analytes that were not within the control windows set by the
EPA for the solid LCS sample. The 80-120% criteria is not used to
evaluate solid LCS results.
EW’ENT LCS CO$C. CONTROL WINDOWS ACTION SAMPLES AFFECTED
ACTIONS:
Percent Recovery
AO1 EOUS tcs < 50% 52-79% > 120%
Positive Results R
Non-detected Results R A
SOLID LCS ( EPA Control Windows > EPA Control Windows
Positive Results J
Non-detected Results UJ A
3. Frequency Criteria
A. Was an LCS analyzed for every matrix, every
digestion batch, and every 20 samples? c or No
-------
REGIO$ I
Data Review Worksheets
Z . PN C TO1UC A 80RPTION A) ALY8I8
1. Duplicate Precision
Duplicate injections and one-point analytical spikes were per-
formed for all samples: duplicate injections agreed within +
20%.
Duplicate injections and/or spikes were not performed for the
following samples/elements:____________________________
Duplicate injections did not agree within ± 20% for samples/
elements: ___________________________________________________
2. Post Digestion Spike Recoveries
Spike recoveries met the 85—115% recovery criteria for all
samples.
Spike recoveries did not meet the 85-115% criter a but did
not require MSA for the following samples/elements:
S€ - M4E737. L kE247 Pb MAE?46
- all MJ E24 . MkE 41
MSA was used to quantitate analytical results when con-
tractually required.
, - Correlation coefficients 0.995, accept results.
_____ Correlation coefficients <0.995 for sample
nur bers/elements: _______________________________________
Method of Standard Addition (MSA) was not performed as re-
quired for samples/elements: _________________________________
ACTIOI S:
1. Estimate (3) positive results if duplicate injections are outside
± 20 % RSD or CV.
2. Il the sample absorbance Is <50% of post digestion spike absorbance
the following actions should be applied:
PERC } T RECOVER?
< 10% i1%—84% > 115%
Positive Sample Results 3 or R 3 3
non-detected Results R U3 A
3. Estimate (3) sample results if MSA was required end not performed.
4. Estimate (3) sample results if correlation coefficient was <0.995.
-------
REGION I
Data Rev*ew Worksheets
XI. I ( UCTIVELY COUPLED PL S?4A (ICP) 8ERIAL DILUTION J( LYB18
______ Serial Dilutions were performed for each matrix and results
of the diluted sample analysis agreed within ten percent of
the original undiluted analysis.
______ Serial Dilutions were not performed for the following:
Serial Dilutions were performed, but analytical results did
not agree within 10% for analyte concentrations greater than
50x the 1DL before dilution.
Report all results below that do not meet the required laboratory
criteria for ICP serial dilution analysis.
MATRIX:
ELEMENT IOL 5OxIDL
Aluminu . ______ ______ ______________ ______________ ________ ________
Eariu ______ ______ ______________ ______________ ________ ________
Beryll u.m ______ ______ ______________ ______________ _________ ________
Cadmiu.m_ ______ _____ ____________ ____________ _______ _______
Calcium ______ ______ _____________ _____________ ________ ________
Chro iu. _ ______ ______ _____________ _____________ ________ ________
Cobalt ______ ______ _____________ _____________ ________ ________
Copper ______ ______ _____________ _____________ ________ ________
Iron_____ ______ I ______ _____________ _____________ ________ ________
Lead______ _______ I I
Magnes iu ______ ______ _____________ _____________ ________ ________
Manganese ______ ______ _____________ _____________ ________ ________
Nickel ______ ______ _____________ ______________ ________ ________
Potass u _______ ______ ______________ ______________ _________ _________
Silver ______ ______ _____________ __________ ________ ________
Sodiur _____ _____ - _________ _______
Vanadium_ ______ ______ ____________ ____________ ________ ________
Zinc_____ ______ I ______ _____________ _____________ ________ ________
Actions apply to all samples of the same matrix.
ACTIONS:
S AMPLE
RESULT
SERIAL
Dl LUT1O1 i
1250
60.5
725 (1
700
76.
70 u
4050
33400
47000
5 00 24 ,2
100 102000
97000
25
2.0
14
8?
95
7360
3.0
ACTION
WR ___
22.g 37. )
WR _____
4,9 __________
WR _____
WR _____
wr ___
4050
300
4750
6 1000
- 1980
22
iflO
750
39.6
WR
1. Estin ate (J) positive results if %D )15.
-------
REGION I
Data Review Worksheets
XII. D!TECTION LIMIT RESULTB
1. Instrument Detection Limits
______ Instrument Detection Limit results were present and found to be
less than the Contract Required Detection Limits.
_______ IDLS were not included in the data package art Form Xl.
_______ IDLs were present, but the criteria was not met for the
following elements _________________________________________
2. Reporting Requirements
_______ Were sample results on Form I reported down to
the IDL not the CRDL for all analytes? o
_______ Were sample results that were anelyzed by ICP
for Se, Ti, As, or Pb at least 5x IDL. or No
_______ Were sample weights, volumes, and dilutions
taken into account when reporting detection
limits on Form I. )or No
It No,
The reported results may be inaccurate. ) ake the necessary changes
on the data summary tables and request that the laboratory resubmit the
corrected data.
-------
tEGIOH I
Data Review Wc,rksheets
XUI. EXI4PLE Qtl).NTITATION
Sample results fall within the linear range for ICP ond within
the calibrated range for all other parameters.
______ Sample results were beyond the linear range/ calibration range
of the instrument for the following samples/elements:
In the space below 1 please show a minlmu.m of one sample calculation
per method:
jç - R 4uU om &w e - 1.984 mg/i
984 X 7000 149 1980 ugiL
I 1 mg
FURNACE - 7r .w ar p r ca t n ug/L. P.tep ac. o’
RCURY - r ugh. P p £ac1ck 1
For soil samples, the following e uat1on may be necessary to convert
raw data values (usually reported in ug/L) to actual sample con-
centrat ions (mg/kg):
The lab is required to use 1 gram sample (wet weight) to 200 ml.
Wet weight concentration
digest conc. in X 200n1 X IL X l000qio X i mQ
L I gm 1000 ml 1kg l000ug kg
In add3tion the sample results are converted to dry weight using the
percent solids calculations:
Wet weight conc . X 100 — final concentration, dry weight (mg/kg)
%sol ids
-------
APPENDIX D
Figures
-------
FIGURE 1
Region I Data Vaixdatior
Roies and Respons bi1ities
-------
FIGURE 1
TA VALIDATION - ROLES AND RESPONSIBILITIES
3—PIONfl.i P OJtct:o.4
t-f m1 PQO.7tCT1OP
a o s i’ r crr
cc ii tL 5 LP I
7G CT CTO
P O( Z tCD
CP4 D
-------
fl PQcI4 o
1Q..D ‘QC C
LDC LOCATIOw
(r WITh
XCJC.iTA T I On
DX trrs y,
‘t, TA tnrsRn’
coøzn r47
-------
FIGURE 2
Overview of the Data Review Process
-------
PIGLr Z 2
OVERVIEW or TI-C DATA REVIEW PROCESS
t L T) C
roq I T QI
0
O’Co Cf6c P T C
rca
scv.p _ TO O-E O(
13 vrz
z ro - rz n15311
‘S. r
- ry -
J!CTI w7Th 1I fl/
I
IMC C r c ca
CAU. LA8 I C L it
A PH C L
cc,
-------
(
L ¶0
cc t c
c .Z?t L
I
V•’t
I :
— VILI. ! Tt
w:rw io
-CO 03
-
, 1 U v
—
PC
L a r
P o c LOG
PC
-------
FIGURE 3
Inorganic Traffic Report
-------
FIGURE JA
I sj t- S*J
,EPA ‘° “ “
Inorgsnlc Waffic Report I
P 4qq4 Q T3 SS 2
I - p iC o’ I — 2 i* 4
9 ..
I. T .-
£
2. O ound r
La i
r. .,....
4b
4. RJv di
6. SollS. ,isiI
4 ( )
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SI I
s_o Csp WP - .
-------
FIGURE 3fl
EPA
W d 1 n ö ..jji.j ?ç. y
IaJ 7
P0 I ’ S W. %3
46?
lno anlc IPeftic Report
a, ‘
k. 0 ’ v s
10/0!
t ‘ . 0 P p ICiIScS g
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5S Il I.. NS
3 Si b
Anolv?ical LoJ
100 tenter ..4e
Anykwn, CA ws
, ________
4 D . D ’ i,o.d A(.tm pj
II-’,’-88 Jo9e7 5’432,
Fed Lx
., ,4.,
O ‘ “* ‘ h
s’ .-
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2. Ovoiwid w
I
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S. SoII54d iII
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S. o (hsr(sAs) W
Drum
C Si ...
re e C l ! ’ 1 . OF ___
S .. Sc
05
C’,
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(5)
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LOC -‘
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JA 321
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LJ J f
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32g .
JA 325
JA
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M3z911
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MJZ.913_
MTL 91
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114/1030 JA . z9_
LM1Juoo JA33o
Jk% /II3o ,YA j
114/i7 .t j7A3 Z_
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114/12’1.5 JA 3
1Ii ,LL3o o JA 355_
114J133o JA3
114 [ i4ct JA3 7
114/IsL3p TA33B_
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LCC-20 II. S t Yic Xj ) :i14 3 .tJ
* P S?*4
P — • Qp,sis. SMO C - . , C * L C — • L C
-------
FIGURE 4
Chain of Custody Form
-------
‘I
R.cs,v .d I 01 Labolaloly by
J k F.d..& SuIIdI iij . Rni. 2203
o.io. M.... p..i,. 02203
OIl.c. .1 (&oIGsm q
CHAIN OF CUS
ODYRICOHO
REMARKS
STATION LOCATION —
C
by I$i.i ,, -
Osts/ Tim.
I
O.t. / Tim.
R’C.ivsd by IS.p.n...g RsIsnquish .dby s.,..... . .s - Oat. / Tim.
J
R.c.sv.d by. lS.p.. we
by ,$ a.i...,
Rsciw.d by fS pi .tiiv• R .linquiihid by lSp aeiw•i
Oats / Tim.
J
R.csavsd by
,
RsI’aqui .d by S.pws...I
Tim. -
Os SMIi1 O..A $Iw.m.ai. Copy ioCoo. ....ioi F..id
O.t. /TIIn. R.miiSs
1
1 2705
-------
FIGURE 5
Contract Laboratory Program
Telephone Record Log
-------
FIGURE 5
Contract Laboratory Program
REGIONAL/LABORATORY COMMUNICATION SYSTEM
Telephone Record Lo
Date of Call:
Laboratory Name:
Lab Contact:
Peg on:
Regional Contact:
Call lr a e By: — Laboralory Region
In referenCe to data !o the following 3ample njmber(s):
S irnmary of Que tiori /I$S eS D: cussed:
Summary of Resolution:
Signature
D 1 tnbution: (I) Lab Copy, (2) Region Copy, (3) SMO Copy
Date
-------
FIGURZ 6
DQO Summary Form
-------
F GURX 6
DOO SUMMARY FORM
‘ i s i s l ’ s
—
•. Pd 5 I)5AAfl
i
ec 1 -
W A
p j Cw T
i P (Y1C.AL DATA
Pc AI4 LffY ‘ &i 4AD
rv TS)( P . TQ TUT
LJJ GffY
P( 4’4
M1TsO ________________________________
&j &i v
I Pt C.ATI •‘ Pt* *J Aj ‘34 5AT
p i cvj sat o
CD,(TIACTOA
COW U DCO I
4.5
-------
FIGURE 7
Data Summary Tables
-------
SI it:
tW GANIC £ kJIGJS £ ALY $
CAM
LAL AI :
SML(
SHVIt L0CAII :
LA AI V J I:
Il p
urn p
MSIESII
MUGN(SL
IIC&(L
P0JASSIt
U I £NIt
% tLM
I
p
P
CV*.MlDt C
DSISCI I
UNITS
C I AC i
DIrECtION
I . lullS
AMAt IICAL I INOD
I — IUSNAC(
P • I(Pil&Ai LA
C V COtO VA
C cxicai iiit
NOTI: OJANUIATION IS APPROXIPILIE DUE It) LIPIIiAiItMS IDENII1ITD tu ill
QIMLIJI CtMIRO( R(VIIU (DAtA RLVItW).
I VALUE IS lEJICitO.
VALUE IS NON DEIICIED
5 0g .
c 1
0
p -P
‘I .
INOI lC LLt N1I
1I• ) ( 1LDELl
ALL Im. P 200
Mtl V P 60
ARSLNIC I JO
Uit t.M P 200
ILIV I L I IJI P 5
P 5
C.ALCJIJt P 5000
C$II1 ILIS P 10
C OSAI_1 P 50
II p 25
I00
S
5000
________ Is
0.2
40
S
i0
I0
so
to
P
p
c v
p
p
I
p
P
-------
Slit: I GANIC SOIt AWAtYSIS
CASt S0 •I ilk O
LA$ Ai0ST:
5M1 [ *.IISU:
WV&t I AVS :
t$ A1 Y J11:
10 C.lcut.l. (he s l• stect lt.(t.. dt lds The TOL solids. C IIMC1
Ott€Ctl0U DE ICCT ION
l IC ELE I1I LIMIII
( ,&p. )
ML l
11
MuNIC
P
MSTItlt P 1
CALC 1.JI 1000
I— Cs* I 01
h3 ALI P P0
1, ll P 20
g L(AO P
1000
P 3
IO*T CV 0.1
.ICUt P
POTASSIl P 1000
$ILINILM I
sauti P 2
1000
S 00 1t ( p
T 5ALLI* . I 10
VAMA0 1 1 P
P
CTAaPDt C
SiM IGS
*aALVIICAI. IIUNW NOlt: .1 0U*MII1* 1100 IS APPSOIIPI*1E tAil TO LIlTIlAIlOWS IDLNJITIIO IN 151
iuNu*t( 011*1.111 C(*IOIX HVICW (D*T NCVI 1V).
• JCPIIL’4 U I Vatlil IS i(JICI(t).
L V COlD WA VALIil IS sOtItCi(D
• c Aali lalC
-------
FIGURE 8
Standard Worksheets
-------
REGION I
Data Review Worksheets
Site Name___________________
Reference Number____________
REGION I REVIEW 07 INORGANIC
corrPAcT .J BOR.ATORY bATh PACRAGE
The hardcopled (laboratory rtame) _________________ data package received
at Region I has been reviewed an the quality assurance and performance
data su inarized. The data review included:
Case No.
SDG. No.
No. of Samples
______ LAS No._______ Sampling Date(s)
______ Matrix _______ Shipping Date(s)
______ Date Rec’d by Lab
Traffic Report Nos:
Trip Blank No.:
Eql.1iprnent Blank No.:
Field Dup Nos:
SOW No. _________ requires that specific analytical work be done and that
associated reports be provided by the laboratory to the Regions, EMSL-
LV, and SilO. The general criteria used to determine the performance ere
based on an examination of:
-Data Completeness
-Holding Times
—Cal ibrat ions
-Blanks
—ICP Interference Check Results
—Matrix Spike Recoveries
—Laboratory Duplicates
Overall Comnents: ___________________
-Field Duplicates
-Lab Control Sample Results
-Furnace AA Results
—ICP Serial Dilution Results
-Detection Limit Results
—Sample Quantitation
Definitions and Qualifiers:
A - Acceptable data.
J - Approximate data due to quality control criteria.
P — Reject data due to qi.iaiity control criteria.
U — Analyte not detected.
Reviewer:
Date:
-------
REGION I
Data Review Worksheets
I. DP Th CONPLETEN 8B
MISSING INFOR.MATIO DATE LAB CONTACTED DATE REC’D
-------
REGION I
Data Review Worksheets
II. BOLDING TIMES
Complete table for all samples and circle the
analysis date for samples not w thin criteria.
r HG ‘CYANIDE
SAMPLE DATE DATE DATE
ID SAMPLED 1 ANAL.YSIS’ANALYSIS
I I I
I I _____ _____ _____
I I I
C I I
I I
I I
I I
I I _____ _____
I I _____ _____
I __________ I
METALS - 180 DAYS FROM SAMPLE COLLECTION
MERCURY - 28 DAYS FROM SAMPLE COLLECTION
CYANIDE - I DAYS FROM SAMPLE COLLECTION
OTHERS
DATE
ANALYSIS
I
I
I
I
I
I
I
I
I
I
I ______
C I
I I
I I
__________ _________ I _____________ I
ACTION:
i. If hold ng times are exceeded all positive results are
estimated (3) and nor—detects are esti iated (UJ).
2. If holding times are grossly exceeded, the reviewer r ay
determine that non-detects are unusable (R)
pH
ACTION
-------
REGIOM I
Data Review worksheets
III A. I) STRUMENT CALIBR.ATIOW (Section 1)
1. Recovery Criteria
List the ena]ytes which did not meet the percent recovery (%R) criteria
for Initial or Continuing Calibration.
DkTE ICV1CCV
ANALYTE
‘B
ACTION SAMPLES AFFECTED
ACTIONS:
If any analyte does not r eet the
bel ow:
For Positive Results:
Accept
Metals 90—llO%R
Mercury 80-120%R
Cyanide 85-1 15%R
For Non—detected Results:
Accept
Metals 90- 125%R
Mercury 8O-135tR
Cyanide B5— 13 0%R
%R criteria follow the actions stated
Estii pte (J
Reiect
(R
75—89%R, lll—125tR
c 5%R,
>125%R
6579%R, 121—l)5%R
<65%R,
>135tP.
70-84%R, 1lG—130%R
<70%R,
>130%P
Estinate (TJJ
Relect
1R
75%R,
>125%R
75—89%R
65—79%R
<65%R,
>135%R
7O—84%R
< O%R,
>130%R
-------
REGION I
Data Review Worksheets
III 3. INBTRW1ENT CALIBRATION (Section 2)
2. Analytical Sequence
A. Did the laboratory use the proper number of
standards for calibration as described in the
SOW? Yes or No
B. Were calibrations performed at the beginning of
each analysis? Yes or No
C. Were calibration standards analyzed at the be-
ginning of sample analysis and at a minimum ire-
q-uency of ten percent or every two hours during
analysis, whichever is more frequent? Yes or ;c
D. Were the correlation coefficients for the cali-
bration curves for kA, Hg, and CN 0.995? Yes or ?.c
E. Was a standard at 2xCRDL. analyzed for all ICP
analyses? Yes or i.o
If No,
The data may be affected. Use professional judgement to deterr re
the severity of the effect and qualify the data accordingly. D sc ss
any actions below and list the samples affected.
-------
REGION I
Data Review Worksheet
V . BLMJX ).NALYSIS RESULTS (Sections 1-3)
List the blank contamination in Sections 1 2 below. A separate
worksheet should be used for soil end water blinks.
1. Laboratory Blanks MATRIX: ________
DATE ICBICCB# PREP BL ANAL.YTE CO 4C./ JNITS
2. Equipment/Trip Blanks
DATE EOUIP BLI A L?TE C NC .1UNITS
3. Frequency Requirements
A. Was a preparation blank analyzed for each matrix,
for every 20 sa p1es and for each digestion
batch? Yes or No
B. Was a calibration blank run every 10 samples or
every 2 hours whichever is more frequent? Yes or No
If Ho,
The data may be affected. Use professional judgement to deterrn e
the se’ ierity of the effect and qualify the data accordingly. Discuss
any actions below, and list the samples affected.
-------
REGION I
Data Review Worksheets
IV 8. 8LXN )..N LYSI8 RESULTS (Section 4)
4. Blank Actions
The Action Levels for any arialyte is equal to five times the highest
concentration of that element’s contamination in any blank. The action
level for samples which have been concentrated or diluted should be
multiplied by the concentration/dilution factor. Ne positive sample
result should be reported unless the concentration of the analyte in the
sample exceeds the Action Level (AL). Specific actions are as fdUo. s:
1. When the concentration Is greater than the IDL, but less than the
Action Level, report the sample concentration detected with a U.
2. When the sample concentration is greater than the Action Level,
report the sample concentration unqualified.
MATRIX: ___________ MATRIX:___________
ELEMENT X. CONCJ AL! ELEMENT MAX. C0Nc./ AL/
UNITS UN TS UNITS UNITS
NOTE: Blanks analyzed during a soil case must be converted to mg/kg in
order to compare them with the sample results.
Conc. in ug/L X Volume diluted to 1?O0ml X X lOOOq X g mg/kg
Weight digested (igram ) l000ml 1kg l000ug
Multiplying this result by 5 to arrive at the action level gives a final
result in mg/kg which can then be compared to sample results.
-------
REGION I
Data Review Worksheets
V . IC? INTERPERENCE CHECK 6 JIPLE (Sections 1 2)
1 Recovery Criteria
List any elements in the ICS AB solution which did not meet the criteria
for %R.
DATE ELEMENT ACTION SAMPLES AFFECTED
ACTIONS:
If an ele ent does not meet the %R criteria , follow the actions stated
bel o :
PERCENT RECOVERY
<50% 50—79% >120%
Positive Sa p1e Results R .
Non-detected Sanple Results R A
2. Frequency Requirements
were Interference QC samples run at the beginning and
end of each sample analysis run or a minimum of twice
per 8 hour working shift, whichever is more frequent? Yes or No
If no,
The data may be affected. Use professional judgement to determine
the severity of the effect and qualify the data accordingly. Discuss
any actions below and list the samples affected.
-------
REGION I
Data Review Worksheets
V B. IC? INTERFERENCE CKEC SAMPLE (SectIon 3)
3. Report the Concentration of any elements detected in the Ics A
solution > 2xIDL that should not be present.
ELEMENT CONC. DETECTED CONC. OF INTERFERENTS
IN TIlE ICS IN THE ICS
AL CA FE i . .c
Estittate the concentration produced by the interfering element in all
affected samples. See guidelines for examples. List the s rples
affected by interferences below:
SAMPLE ELEMENT SAMPLE SAMPLE INTERFERENT ESTIMATED
AFFECTED AFFECTED CONC. CONC. INTERT.
(ug/L) AL CA FE JIG (ug/L)
ACTIONS
1.. In general, the sample data can be accepted without qualification if
the sar ple concentrations of Al, Ca, Fe, and JIg are less than O% of
their respective levels in the ICS solution.
2. Estimate (J) positive results for affected elements for samples with
levels of interferents 50% or more of that in the ICS solution.
3. Reject (R) positive results it the reported concentration is due
entirely to the interfering element.
4. Estimate (UJ) non-detected results for which false negatives are
suspect.
Give explanations for any actions ta) en below:
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REGION I
Data Review
Worksheets
VI. XAT ’IX SPIKE
TR ___________
1. Recovery Criteria
MATRIX
List the percent recoveries for analytes which
required criteria.
S - amount of spike added
SSR - spikes sample result
SR — sample result
did not meet the
Analyte
SSR SR
$ SR
Act ion
1 atrix Spike Actions apply
ACTIONS:
to all samples of the same matrix.
1. if the sample concentration exceeds the
factor of 4 or mores no action is taken.
spike concentration by a
2. If any analyte does not meet the IR criteria follow the actions
stated below:
Positive Sample Results
Non-detected Results
2. Frequency Criteria
.,
3
3
R
V.3
A
A. was a matrix spike prepared at the required fre-
quen cy’
B. Was a post digestion spike analyzed for elements
that did not meet required criteria for matrix
spike recovery?
Yes or No
Yes or No
I I
—I I
I I I
< 30%
PERCENT RECOVERY
30 5—74%
‘ 125%
A separate worksheet should be used for each matrix spike pair.
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REGION I
Data Review Worksheets
VII. L OP. TORY DUPLICP TEB
List the concentrations of any analyte not meeting the criteria for
duplicate precision. For soil duplicates, calculate the CRDL in mg/kg
using the sample weight, volume and percent solids data for the sample.
Inthcate what cr teria was used to evaluate precision by circling either
the RPD or CRDL for each element.
MATRIX:
Element CRDL ________ __________ ______
soil _______ _________
ug/L mg/kg
Aluminum_ _2OO_ ______
Antimony_ _60_’
Arsenic____ ______
Barium______ _200_ _______ ______________ ______________ _____ _________
Beryllium_j _____________ _____________ ________
Cadmium____ I ____5_ ______ ____________ ____________ _____ ________
Calcium_____ I_5000_ _______ ______________ ______________ _____ _________
Chromiu.m 10 ______ _____________ _____________ _____ ________
Cobalt______ _50_ ______ ______________ _____________ _____ ________
Copper______ ______ ______________ _____________ _____ ________
Iron________ _l00 _______ ______________ ______________ _____ _________
Lead_______ ____5_ ______ ____________ ____________ _____ ________
MagnesiulD_ _5000_ ______ ______________ ______________ _____ _________
Manganese_ _15_ ______________ _____________ _____ ________
Mercury____ ______ _____________ _____________ _____ ________
Nickel_____ _40_ _____________ _____________ _____ _________
Fotassium_ _5000_ ______ ______________ ______________ _____ _________
Seleniu.m_ 5 ______ ______________ _____________ _____ ________
Silver______ _l0 ______ ______________ ______________ _____ _________
Sodium_____ 5000_ ______ _____________ _____________ _____ ________
Thallium ‘ 10 ______ _____________ _____________ _____ ________
Vanadium 50 _______ _______________ _______________ _____ _________
Zinc________ ______ _____________ _____________ _____ ________
Cyan de____ _l0 ______ ______________ _____________ _____ ________
Sam le I Dup licateI
Q Action
I
I I
I I
I I
I —I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
Laboratory Duplicate Actions should be applied to all other samples of
the same matrix type.
ACTIONS:
1. Estimate (3) positive results for elements which have an RPD >20%
for waters and >35% for soils.
2. If sample results are less than Sx the CRDL, estimate (3) positive
results for elements whose absolute difference is >CRDL, (2xCRDL for
soils). If both samples are non-detected, the RPD is not calculated
(NC)
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REGIOX I
Data Review Worksheets
VIII. I!LD UPLICPITE8
List the concentrations of all analytes in the field duplicate pair.
For soil duplicates, calculate the CROL in mg/kg using the sample Weight,
volume and percent solids data for the sample. Indicate what criteria
was used to evalute the precision by circling either the RPD or CRDL for
each elev ent.
MATRIX:___________
Element
A luininu
Antimony_’
Arsenic_____
Barium______
Beryl 1 iu _ ____
Cadmium____ ____
Calcium____
Chromium
Cobalt_____
Copper______
Iron________
Lead_______ ____ -
Magnesiu.m_ 5O00
Manganese_ _l5
Mercury____
?Jic)cel______
Potassium_ 5000
Seleniu.m 5
Silver______ _lO_
Sodium_____ _5 000_
Thallium 10
Vanad iu 50
Zinc_______
Cyanide____
ACTIONS:
I I
•1 __________ 1
I I
I I
SarlD].e 4
Du 1icate B.E.Q Action
CRDL
water soil
ug/L mg/kg
200
60 ______
10 ______
200 ______
5 ________
5 _______
5000 _______
10 _______
50 _______
25 ______
100 ______
5
‘ I
— I
i I
I I
I I
I I
___ ______ ______ __ I ____
___ ______ ______ __ I ____
___ ______ ______ __ I ____
___ ________ I
Field Duplicate Actions should be applied to all other samples of the
sane matrix type.
1. Estimate J) positive results for elements which have an RPD >30%
for waters and >50% for soils.
2. If sample results are less than 5x the CRDL. estimate (3) positive
results i (iPT) raa. .ha for elements whose absolute
difference is >2xCRDL, (4xCRDL for soils). If both samples are non-
detected, the RPD is not calculated (NC).
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REGION I
Data Review Worksheets
l x. LABORATORY CONTROL EANPLE
1. Ao eous L,CS
List any LCS recoveries not within the 80-120% criteria and the samples
affected.
DATE ELEMENT 3. ACTION SAMPLES AFFECTED
2. $ol d LCS
List any analytes that were not within the control vindovs set by the
EPA for the solid L,CS sample. The 80—120% criteria is not used to
evaluate solid LCS results.
ELEMENT LCS CONC CONTROL WINDOWS ACTION SAMPLES AFFECTED
ACTIONS:
Percent Recovery
AOUEO S LCS < 50% 51-79% > 120%
Positive Results R J
Non-detected Results R A
SOLID LCS cEP. Control W.jndow& > EPA Control Windows
Positive Results .1
Non-detected Results U3 A
3. Frequency Criteria
A. Was an LCS analyzed for every matrix, every
digestion batch, and every 20 samples? Yes or No
-------
REGIO)4 Z
Data Review Worksheets
x . 7URJUIC! IT0M1C ).BSORPTION A1 ALY8I8
i. Duplicate precision
Duplicate injections end one-point analytical spikes were per-
formed for all samples: duplicate injections agreed within ±
20%.
— Duplicate injections and/or spikes were not performed for the
following samples/elements:
Duplicate injections did not agree within ± 20% for samples!
elements:_____________________________________________________
2. Post Digestion Spike Recoveries
Spike recoveries net the 85-115% recovery criteria for all
samples.
Spike recoveries did not meet the 85-115% criteria but thd
not require MSA for the following samples/elements:
MSA was used to quantitate analytical results when con-
tractually required.
_____ Correlation coefficients 0.995, accept results.
_____ Correlation coeffIcients <0.995 for sample
numbers/elements: _________________________________________
Method of Standard Addition (MSA) was not performed as re-
quired for samples/elements:
ACTIONS:
1. Estimate (3) positive results if duplicate injections are outside
± 20 % RSD or CV.
2. If the sample absorbance is <50% of post digestion spike absorbance
the following actions should be applied:
PERCENT RECOVERY
< 10% ll%—84% ‘ 115%
Positive Sample Results 3 or R 3 3
Non-detected Results R 133 A
3. Estimate (3) sample results if MSA was required and not performed.
4. Estii ate (3) sample results If correlation coefficient was <0.9 5.
-------
REGION I
Data Review Worksheets
xI. IWDUCTIVELY COUPLED PLASM3i (ICP) $ER!AL DILUTION ANALYSIS
______ Serial Dilutions were performed for each matrix and results
of the diluted sar ple analysis agreed within ten percent of
the original undiluted analysis.
Serial Dilutions were not performed for the following:
______ Serial Dilutions were performed, but analytical results did
not agree within 10% for analyte concentrations greater than
SOx the IDL. before dilution.
Report all results below that do not meet the required laboratory
criteria for ICP serial dilution analysis.
M.kTR IX: ______________
ELEMENT IDL 5OXIDL SA 1?LE SERIAL ACTION
RESULT DiLUTION
A lu i nu.m _______ _______ ______________ _______________ _________ _________
Barium _______ _______ _______________ _______________ _________ _________
Berylilum ______ ______ _____________ _____________ ________ ________
Cad ium ______ ______ ______________ ______________ _________ _________
Cal cium ______ ______ _____________ _____________ ________ ________
Chronium ______ ______ _____________ _____________ ________ ________
Cobalt ______ ______ ____________ ____________ ________ ________
Copper_i
Iron_____ ______ ______ ______________ ______________ ________ _________
Lead______ _______ _______ ______________ _______________ _________ _________
Magnesium ______ ______ ______________ ______________ ________ _________
Manganese ______ ______ ______________ ______________ ________ _________
Nickel ______________ ______________ ________ ________
Potassium ______ ______ ______________ ______________ ________ _________
Silver ______________ ______________ ________ ________
Sodium ______ ______ _____________ _____________ ________ ________
Vanadium_ ______ ______ ______________ ______________ ________ ________
ZLnc_____ ______ ______ ______________ ______________ ________ ________
ctions apply to all sanpies of the sane matrix.
ACTIONS:
1. Estimate (J) positive results if 1D >15.
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REGION I
Data Review Worksheets
X II. E TECT1ON LIMIT R RULT
I. Instrument Detection Limits
______ Instrument Detection Limit results were present and found to be
less than the Contract Required Detection Limits.
______ IDLS were not included in the data package on Form XI.
_______ IDLS were present, but the criteria was not met for the
following elements:_________________________________________
2. Reporting Requirements
_______ Were sample results on Form I reported down to
the IDL not the CRDL for all analytes? Yes or No
_______ Were sample results that were analyzed by IC?
for Se, TI, As, or Pb at least 5x IDL. Yes or I ’o
_______ Were sarrple weights, volumes, and thiutions
taken into account when reporting detection
limits on Fo r m I. Yes or o
If No,
The reported results may be inaccurate. Make the necessary changes
on the data sunnary tables and request that the laboratory resubmit the
corrected data.
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REGION I
Data Rev2ew Worksheets
XII1. B MFLE QUX} TITMION
_____ Sample results fall within the linear range for IC? and within
the calibrated range for all other parameters.
______ Sample results were beyond the linear range/ calibration range
of the instrument for the following samples/elements:
In the space below, please show a minimum of one sample calculation
per method:
FURNA CE
MERCURY
CThN IDE
For soil samples, the following equation may be necessary to convert
raw data values (usually reported in ug/L) to actual sar ple con-
centrations (mg/kg):
The lab is required to use 1 gram sample (wet weight) to 200 ml.
Wet weight concentration
digest conc. in X 200m1 X IL X l0O0 m X lm
L 1 gm 1000 ml 1kg l000ug kg
In addition the sample results are converted to dry weight using the
percent solids calculations:
Wet wejg t conc . X 100 — final concentration, dry weight (mg/kg)
tsolidg
-------
FIGURE 9
Inorgarxc Regional Data Assessment Forn
-------
FIGURE 9
INORC ANIC REC1ONAL DATA ASSESSMENT
CASENO. _____________________ SITE _____________
LABORATORY_ NO OF SAMPLES/
MATRIX ______________________
SDG.___________________________ REVIEWER (IF NOT ESD) _____________
Sow.__________________________ REVIEWERS NAME _______________
DPO ACTION _____ FYI __________ COMPLETION DATE ______________
DATA ASSESSMENT SUMMAR Y
IC ? AA Hg CYANIDE
I. HOLDING TIMES _____ _____ _____ _____
2. CALIBRATIONS
3. BLANKS
4, IGS
. ic
6. DUPLiCATE ANALYSIS ______ ______ _____ _____
7. MATRIX SPIKE ______ ______ _____ ______
$. MSA
9. SERIAL DILUTION ______ ______ ______ ______
tO. SAMPLE VEREFICATION _____ _____ _____ _____
I L OT1IERQC
12. OVERALL ASSESSMENT _____ _____
0 • D ts hsd oo probtem fo QuIIIfled due ic n i or probIerr .
M • Data tht iDd due o major piobIe s .
2. • Da s UD)CCepUbk.
X — PsobIe t.3. bul do ot etfec deti.
ACTION ITEM S ;
AREAS OF CONCERNS —
NOTABLE PERFORMANCE
-------
APPENDIX £
Completed inorganic Regior a1
Data Assessment Form (IRDA) and
Guidance for Cornpletn g the RDA
P* ted o” Recyclea Pape;
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Table of Conte
Page
Introduction,....
I . folding Times. . . . . . . . . . . . . . . . .4
II. Calibrations . . . . . . . . . . . . . . .4
III. Blanks. . . . . . . , . . , .5
IV. ICS . . . . . . . . . . . . . . . . . . . . . . . . . .5
V. L.CS. •........ . . • .. 5 liii.. .6
VI . Duplicate Analysis. . . . . . .7
VI I. Matrix Spike . . . • • B
VIII. MSA.
IX. Serial Dilution .•.... . ...... 9
X. Sample Result Verification 10
XI . Other QC 10
XII. OverallAssessment 10
Inorganic Regional Data Assessment Tore 12
2
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GuidsliDss for tvaluating Validatiou )(ssos amd Cospl.ti g
the inorqazio R.giosal Data kssssPssDt ion
XBtrodu ottOn
This document is de5igned to offer guidance in evaluating
validation meios and completing the Inorganic Regional Data
Assessment (IRDA) Form.
The document is designed to define and clarify the areas
evaluated and the resulting actions for the Inorganic Regional Data
Assessment Form. The procedure must be performed by a qualified
data reviewer, since technical expertise is utilized in completing
the form. An IRDA Form must be completed for each data package
reviewed and validated for Region 1.
3
P -L7u d on Rer c1ea Pape
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BOLDI1IQ TI) 3B
A. Definition or Zxplanation
The holding time of the sample can be defined as the time
from sample collection to the time of analysis or sample
preparation, as appropriate.
). Actions
If all th. sample holding time criteria were met, the
category will be qualified with “0’, data had no
problems/or qualified due to minor problems.
If the sample holding times were exceeded and all the
positive results and detection limits are estimated, the
Inorganic Regional Data Assessment Form (IRDA) will be
qualified with ‘0’, data had no problems/or qualified due
to minor problems.
If the holding times were grossly exceeded and all the
positive results are estimated and non-detected results
are rejected, the IRDA form will be qualified with “Ma,
data qualified due to major problems.
If the holding times were grossly exceeded and all
positive and non—detected results are rejected, the IRDA
form will be qualified with “Z”, data i.macceptable.
II. CALIBP) TION8
A. Definition or Explamation
Calibrations refer to the instrument’s initial and
continuing calibrations and demonstrate the instru-
ment’s ability to produce acceptable quantitative data.
E. Actions
If all the calibration criteria are within
specifications, and met the frequency requirements the
IRDA form will be qualified with ‘0’, data had no
problems/or qualified due to minor problems.
If the %R for the ICy or CCV is between 75-89 or 111—125,
(or the respective ranges for CH and Hg) and the positive
results have been estimated the IRD.A form will be
qualified with 94”, data qualified due to major problems.
If the %R is outside the 75-125% limits, (or the
respective ranges for CW and Hg) and the positive results
and non-detected results are rejected, the IRDA will be
qualified with “Z 0 , data unacceptable.
If other problems related to calibrations exist that do
4
-------
not affect the data (eg. standards were not run at the
proper frequency) , the IRDA will be qualified with ax’,
problees but do not affect data.
flI.
A. Definition or E]rpls.tation
The blanks consist of preparation blanks, calibration
blanks, and equipment or trip blanks. The blanks ar.
r.view.d to detarein. the existence and eagnitud. of
contawinetien problens. The problea .s associated with
one blank apply to all the associated sa pl.s . Blanks
are reported per eatrix, and for •ach digestion batch.
1. Actions
If no contanination is present, and the proper number of
blanks were analyzed, the IRDA fore will require
data had no problens/or qualified due to ninor problems.
If low levels of contaninants are present, and the
detection limit is raised, the IRDA fore will be
qualified with “X”, problees, but do not affect the
data.
If contaninants were found in the laboratory blanks at
levels greater than the CRDL, the associated samples eust
be reanalyzed or redigested depending on the source of
contaninatlon. if the samples are not reanalyzed, the
IRDA qualifier will be Z 0 , data unacceptable.
If high levels of contaminants are detected in the
equipment blanks, the IRDA shall be qualified with “M”,
data qualified due to ea or problems.
It blanks wer.e not analyzed at the proper frequency but
do not affect the date, the IRDA will be qualified with
IX”, problems but do not affect the data.
IV. Z) ZR7EP.ENCE CXECR BAflPLE (ICS )
A. Definition or Zxplanation
The ICP Interference Check Sample is analyzed at the
beginning and end of each s .mple analysis run to verify
the contract laboratory’s interelement and background
correction factors.
B. Actions
5
P* ed i Rxyc4Iea Pope.
-------
If all the recoveries for the ICS meet criteria and an
ICS was analyzed at the proper frequency, the IRDA
qualifier will be NO”, data had no problems/or qualified
due to minor problems.
If the ICS recovery does not meet criteria but the
levels of intarferente in the samples are not 50% or more
of thos, found in the ICS solution, the qualifier will
be problems, but do not affect the data.
If ICS recoveries are 50—79% or >120%, and levels of
interferents are 50% or more of that found in the ICS
solution, the IRDA will be qualified with 0R, data had
no problems or qualified due to minor problems.
If results >2x IDL are detected for elements not present
in the EPA solution and the samples have levels otinter-
ferents that are 50% or more of those found in the ICS
solution, the IRDA qualifier will be J4, data qualified
due to major problems.
If sample results are rejected due to major inter-
ferences, the IRDA form will be qualified with ZN, data
unacceptable.
If the ICS recovery falls <50 %, the IRDA qualifier
will be UZN, data unacceptable.
If the ICS was not analyzed at the proper frequency but
the data are not affected, qualify the IRDA with “Xe,
problems, but do not atfect the data.
V. LBQP.ATORY CO) TR0L BAXPLI
. .tinition or Explanatiom
The laboratory control sa p1e analysis is designed to
serve as a monitor of the efficiency of the digestion
procedure. Reported results may be biased either high
or low for elements with LCS recoveries outside required
criteria.
). Jctioni
If the aqueous LCS recovery falls within the range of
50—150%, or the solid LCS falls within the control
windows and LeSs were analyzed at the required frequency
the IRDA qualifier will be “0”, data had no problems or
qualified due to minor problems.
If the aqueous LCS recovery >150%, or soil LCS results
6
-------
are > control windows and results are >IDL the IRDA
qualifier will be MW, date qualified du. to major
problems.
If the aqueous LCS recovery >150%, or soil LCS results
are ‘ control windows and results are non—detected, the
IRDA qualifier will b. •X , problems but do not affect
the data.
If the aqueous LCS recovery is cSO% or th. solid L.CS
falls below the control windows th. qualifier should be
data unacceptable.
If an tICS was not analyzed at the proper frequency but
the data are not effected, the qualifier shall be MX ”,
problems, but do not affect data.
DIJPLICMZ M LY9I8
A. Description or Ziplamation
Duplicate analyzes are indicators of the precision of
the sample results. Laboratory duplicates give an
indication of the precison of the laboratory analysis.
Field duplicates are indicators of field precision as
well as laboratory precision. Laborator-y duplicates are
required per matrix and per digestion batch. Qualifiers
apply to all samples of a similar matrix.
B. Actions
If samples have an R.PD for lab or field duplicates that
<50% for waters, <75 % for soils and were analyzed at
the required frequency, the IRDA qualifier will be “0”,
data had no problems/or qualified due to minor problems,
For samples that are <5xCRDL , if the difference between
the results is ± 2xCRDL for laboratory duplicates or ±
4xCRDL for field duplicates and were analyzed at the
required frequency, the IRDA qualifier will be “0”, data
had no problems or qualified due to minor problems.
If the RPD is >50% for waters and 75 % for soils, for
either laboratory or field duplicates for samples that
are >SXCRDL, the qualifier should be “M’, data qualified
due to major problems.
If the absolute difference between samples is > ±2xCRDL
for laboratory duplicates and >± 4xCR .DL for field
duplicates for samples less than SxCRDL, the qualifier
7
I’thued i Recyclea Pope.
-------
should be data qualified due to sajor problems.
If duplicate, were not analyzed at the proper frequency
but the data are not affected, qualify the IRDA with •X ,
problems, but do not affect the date.
VII.
. D.fiBttio or *rplLDatio
The matrix spike sampl. analysis is designed to provide
information about the effect of the sampie matrix on the
digestion and measurement methodology. A matrix spike
is required for each matrix analyzed and qualifiers apply
to all samples of similar matrix.
B. If all the matrix spik. recoveries ar. within the
specified criteria, and were enlayzed at the required
frequency, the IRDA form will be qualified with “0., data
had no problems/or qualified due to minor problems.
If the matrix spike recovery is >125% and the reported
results are non-detected, the qualifier should be “X ”,
problems, but do not affect the data.
If the matrix spike recovery is between 50-150%, and the
results are >IDL, the qualifier shall be “0”, data had
no problems/or qualified due to minor problems.
If the matrix spike recovery is >150% and positive
results are estimated, qualify the IRD with “M ”, data
qualified due to major problems.
If the matrix spike recovery is between 30% and 50%, for
non-detected results or <50% for results >IDL, the
qualifier shall be 14 ”, data qualified due to major
problems.
If the spike recovery results fall below 30% and the
sample results are non-detected 1 the IRL A form should be
qualified with 2”, data unacceptable.
it a matrix spike was not analyzed at the proper
frequency, or a post—digestion spike was not analyzed as
required, but the data are not affected, quality the IRDA
with IX”, problems, but do not affect the data.
8
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V I I I. METhOD 07 BTM DARD P.DDITIOM (NSA )
2. D.sariptiom or Ixplarsation
The Method of Standard Addition (NSA) is required when
th. furnac. post digestion spike r.cov.ry is not within
85-115%, and the sample ebsorbance is >50% of spike
absorbance. This section of the IRDA is used to qualify
problems with post-digestion spik. r.cov.ry as v.11 as
)ISAa.
B. 2ctie a
If duplicate injections were performed as required arid
the %RSD or CV <40, qualify the IRDA with data had
no problems/or qualified due to minor problems.
If the %P.SD or CV >40, qualify the IRDA with ‘M”, data
qualified due to major problems.
If post digestion spike recoveries were within 75-125%
and were analyzed for every sample, the 1RDA will be
qualif led with “0”, data had no problems/or qualified due
to minor problems.
If post digestion spike recoveries were >125% but samples
were non-detected, qualify the IRDA with “X ”, problems
but do not affect the data.
If post digestion spike recoveries 11—75%, (or >125% for
positive results) the IRDA qualifer will be “M”, data
qualified due to major problems.
If post digestion spike recoveries were i l0%, qualify the
IRDA with “Z”, data unacceptabl•.
If MSAs were performed as required and the correlation
coefficient is >0.995, the IRDA form will be qualified
with “0”, data had no problems/or qualified due to minor
problems.
If the correlation coefficient is <0.995 for both NSA
analyses, the form shall be flagged with “N”, data
qualified due to major problems.
I X. SERIAL DIL TIQ$
A. Description or Explanation
Serial dilution analysis determines whether significant
physical or chemical interferences exist due to sample
9
v Reqc1e Pape
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matrix.
B. Actio a
If the %D is <30%, the IRDA shall be flogged with 0,
data had no problems/or qualified du. to minor problems.
If the %D ii >30%, the IPDA shall be flagg.d with ‘,
data qualified du. to major problems.
If a serial dilution was not performed as required, the
IRDA form shall be flagged with ‘Xe, problems, but do
not affect the data.
X. BA)1PL! RXBVL? VERIFICATION
A. Ds.criptioz or Explamation
The objective is to ensure that the reported quantitation
results are accurate.
B. Actioms
If transcription, calculation, linear range, or raw
instrument data discrepancies are found and are resolved
after contacting the laboratory, the IRDA foz-m shall be
qualified with “0”, data had no problems/or qualified due
to minor problems.
If transcription, calculation, linear range, or raw
instrument data discrepancies cannot be resolved, qualify
the form with “14”, data qualified due to major problems.
II. OTR!R OC
A. Description or !xpla.mation
Other problems with quality control parameters pertaining
to the Case may be qualified using professional judge-
ment. (ie. detection limits, post digestion spikes,
etc.)
XII. QY ERALL AE6814Z T
A. D.scriptiom or Erplamatiom
The data reviewer makes professional judgements and
expresses concerns and comments on the validity of the
overall data package for a Case. The additive nature of
10
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QC parameters out of specification ii difficult to assess
in an objective manner. Th. data quality objectives will
aid in making the decicien of the overall validity ef the
data.
I. otiens
If there are no significant problems associated vith the
Case, the IRDA will be qualified with data had no
problems/or qualified due to minor problems.
If there were small problems with the data package or
contractual violations but the data could be utilized,
qualify the form with XR, problems, but do not affect
the data.
If there was a significant problem which interfered with
use of the data, the category will be qualified, “1”,
data unacceptable.
11
on ecyciea Pq e
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INORCANIC REGIONAL DATA ASSESSMENT
Cq’ SE NO 9164 SITE ABC S 1e
LABORATORY * ‘Z L f’( 4 4 P lO OF SAMPLES/
MATRIX JO 4Q tOu .
$DO. MAE235 REVIEWER (IF NOT ESD) Rag F.
sow. 7$7 PEVIEWERS NAME K ’LOLAr t( O’Le.ciu ’
DPO ACTION _____ FY i __________ COMPLETION DATE 1 7/RI/U
DATA ASSESSMENT SUMMARY
JCP AA CYANiDE
I. HOLDING TIMES _____ 0 0
2. CALIBRATIONS 0 0 0
3. BLANKS X 0 0
4. K S M 7 ______ ______
5. Lc C 0 ___
6 DUPL)CATE ANALYSIS _____ a ______
J. MATRtX SPIKE C C 0
I. MSA _____ U 2 ______
9. SERIAL DILUT]ON C ______ ______
10 SAMPLE VERrFJCAT ON ______ 0 0
Ii OTHERQC _____ 0 0
22. OVERALL ASSESSMENT 0 0 _____
0 • D t* hd o problemi/oi qu* ifled due to oor piobIuo
M • Dira 4ulWied due to ge ajo; pTobIe a
Z • Data uDaccepLabIe.
X • Pr bIe , but do ot arreci d&
ACTiON ITEMS _______________________________
ARE&S OF CONCERN - R W e e j’ cd c’ j r• i th e $ r .b
j .&c, . - V 1t .t4.O Lur ..Z.o o e2t’J’ ed o’ kLLw th1C Zo to
po4 -d4e 8tit r 4pi e kOV C . .
NOTABLE PERFORMANCE.
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