OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 1 of 41
,^EDST^
United States Environmental Protection Agency
Region 3
Sample Submission Procedures
for the
Office of Analytical Services and
Quality Assurance (OASQA)
Laboratory Branch
Revision 13
January 29, 2014
Environmental Science Center
701 Mapes Road
Fort Meade, Maryland 20755-5350
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OASQA Sample Submission Procedures Rev, 13.0
Januarv 29. 2014
Page 2 of 41
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OASQA Sample Submission Procedures Rev. 13.0
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TABLE OF CONTENTS
1.0 Introduction 5
2.0 Project Planning and Analytical Request Preparation and Scheduling 5
3.0 Sampling 5
3.1 Collection Types/Techniques 6
3.1.1 Grab sample 6
3.1.2 Composite sample 6
3.2 Sample Types 6
3.2.1 Duplicate sample 6
3.2.2 QC sample 6
i) Matrix Spike (MS) 6
ii) Matrix Spike Duplicate (MSD) 6
3.3 Blanks 6
3.3.1 Sample Matrix "Field" Blank 7
3.3.2 Trip Blank 7
3.3.3 Rinsate or Equipment Blank 7
3.3.4 Temperature Blank 7
3.4 Dissolved Analysis 8
3.5 Dechlorination 8
4.0 Holding Times 8
5.0 OASQA Laboratory Sampling Requirements 9
6.0 Laboratory Quality Control Requirements 9
7.0 Paperwork Requirements 9
7.1 Chain of Custody (COC ) 9
7.2 Sample Tag 10
7.3 Exposure Data Sheet 10
7.4 Letter to File 10
8.0 Shipping Requirements 10
8.1 Shipment of Dangerous Goods 11
8.2 Shipment of Environmental Laboratory Samples 11
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TABLE OF CONTENTS (com.)
9.0 Shipping Notification 13
10.0 Pollution Prevention (P2) and Environmental Management System (EMS) 13
11.0 References 15
Table 1 Aqueous Sample Requirements 16
Table 2 Non-Aqueous Sample Requirements 21
Table 3 SDWA Program Special Requirements 25
Table 1, 2, and 3 Footnotes 26
Appendix 1 - Quality Control (QC) Sampling Requirements 28
Appendix 2 - Metals Quantitation Limits (QLs) 29
Appendix 3 - Pesticide/PCBs Quantitation Limits (QLs) 30
Appendix 4 - Semivolatiles (SVOCs) Quantitation Limits (QLs) 31
Appendix 5 - Volatiles (VOCs) Quantitation Limits (QLs) 34
Appendix 6 - Nitroaromatics/Nitramines/Expiosives Quantitation Limits (QLs) 37
Appendix 7 - Sample Tag Example 37
Appendix 8 - Chain of Custody Example 38
Appendix 9 - Hazard and Risk Exposure Data Sheet 39
Appendix 10 - OASQA Sample Acceptance Policy 40
Appendix 11 - Region 111 5035A Fact Sheet 41
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1.0 Introduction
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
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This document specifies the procedures that are to be followed when submitting samples to the
Office of Analytical Services and Quality Assurance (OASQA) Laboratory Branch located at
Ft. Meade, Maryland. These procedures will help ensure that the field and laboratory aspects of
the sampling event are linked in a way to produce reliable data of known quality.
2.0 Project Planning and Analytical Request Preparation and Scheduling
The Quality Assurance Project Plan (QAPP) and Sampling Analysis Plan (SAP) are documents
that identify the purpose of a project along with the sampling and analytical requirements.
Approved plans should be in place at least 2 weeks before project scheduling. For information,
please contact a member of the Quality Assurance staff in OASQA's Technical Services Branch
(TSB), listed below.
Mike Mahoney: 410-305-2631 (ph), 410-305-3095 (fax) mahonev.mike@epa.gov
Brandon McDonald: 410-305-2607 (ph), 410-305-3095 (fax) mcdonald.brandon@epa.gov
Jay Burman: 410-305-2743 (ph), 410-305-3095 (fax) burman.iarmael@epa.gov
EdMesser: 410-305-2744 (ph), 410-305-3095 (fax) messer.ed@epa.gov
The Analytical Request Form (ARF) is a request for analytical work that is offered to the
OASQA laboratory. All requests are scheduled through the OASQA Technical Services Branch
using the contacts listed below.
John Kwedar: 410-305-3021 (ph), 410-305-3095 (fax) kwedar.iohn@epa.gov
Dan Slizys: 410-305-2734 (ph), 410-305-3095 (fax) slizys.dan@epa.gov
NOTE: Instructions on preparing and submitting Analytical Request Forms (ARF), accessing
the paper versions of the Chain of Custody (COC ) form. Sample tags, Custody Seals, and other
documentation requirements are available by contacting the Technical Services Branch or at the
following website:
http://www2.epa.gov/aboiitepa/about-region-3s-laboratory-and-field-services-epas-environniental-science-center
3.0 Sampling
Proper collection, identification of samples, documentation of the collection event, and submittal
of required paperwork are all essential parts of a successful sampling event. When samples are
not properly collected, preserved, documented, or shipped, the quality of the data may be
compromised. If this occurs, the requestor is notified and (1) given the opportunity to resample
or (2) receives qualified data. Refer to the OASQA Sample Acceptance Policy. (Appendix 10)
NOTE: In some cases it may be possible for the laboratory to complete the analysis with some
adjustments (i.e., if there is insufficient sample volume, the data may have to be reported with
increased quantitation limits or the analyst may be asked to prioritize analyses).
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3.1 Collection Types/Techniques
The two collection types/techniques, Grab and Composite, are normally used when
collecting samples.
3.1.1 Grab sample - An individual sample collected over a period of time generally not
exceeding 15 minutes. A grab sample is normally associated with water or wastewater
sampling. However, liquid hazardous waste samples and non-aqueous samples (soil,
solid, oil, and sediment) may also be considered grab samples.
3.1.2 Composite sample - A sample containing discrete aliquots (1) collected over a
defined time period at equal time intervals (time composite), (2) collected in volumes
proportional to the flow rate (flow proportional composite), or (3) composited from
individual grab samples collected on an area or cross-sectional basis (area composite).
3.2 Sample Types
A sample is defined as a discrete portion of material to be analyzed that is contained in
single or multiple containers, and identified by a unique sample number. A sample includes
duplicates and QC samples.
3.2.1 Duplicate sample - It is a second aliquot of the same sample to determine the
precision of the method, to check the accuracy and precision of analyses.
3.2.2 QC sample - An additional volume of an existing sample used to detect contamination
or error.
i) Matrix Spike (MS) - It is an aliquot of a sample (water or soil ) that is fortified
(spiked ) with known quantities of a specific compound and subjected to the
entire analytical procedure.
ii) Matrix Spike Duplicate (MSP) - It is a second aliquot of the same matrix as the
Matrix Spike (MS) that is spiked to determine the precision of the method.
3.3 Blanks
Blank samples are used to identify potential sources of contamination during sampling,
shipping, storage and analysis. Blanks should be specified as part of every Quality
Assurance Project Plan (QAPP) or Sampling Analysis Plan (SAP). It is highly
recommended that field blanks accompany all sample sets. Each blank is assigned its own
unique sample number. A blank includes trip blanks, rinse blanks, equipment blanks, etc,
NOTE: All water used for blanks must be deionized lab pure water, free of the parameter* s) of
interest. The water may have to be tested prior to use. Commercially available I IPLC water is
not acceptable for most blank uses. I IPLC water is not certified as "organic-free" and/or "metal-
free", and therefore, may contain compounds of interest. Blanks that are preserved must be
prepared with the same stock and same volume of the preservative that was used with the
samples.
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3.3.1 Sample Matrix ("Field") Blank - The field blank is used to determine whether
contamination has been introduced during sample collection, storage and shipment, as
well as, sample handling in the analytical laboratory. Field blanks are prepared by
transferring demonstrated analyte-free water to the appropriate sample containers
during the time when site-specific samples are collected. These blanks are transported
to the field and exposed to the same conditions as site-specific samples including
removal of the container caps and addition of any appropriate preservatives. Field
blanks should be collected whenever aqueous samples are collected and at a frequency
of one per 20 samples. This sample should be analyzed for the same parameters as
those associated with site-specific samples collected from potentially contaminated
media.
3.3.2 Trip Blank - The trip blank is only used for Volatile Organic Compounds (VOCs) to
determine whether contamination has been introduced to aqueous samples through
cross-contamination during shipment and storage of sample containers. Trip blanks
should be prepared, and include preservatives prior to the sampling event, and are not
exposed to field conditions. They may be furnished by the analytical laboratory and
will consist of certified analyte-free water provided in the appropriate container (i.e.,
40 ml teflon-lined glass vial). Trip blanks should be collected at a frequency of
i) One per each cooler used to store/transport site-specific samples designated for
VOC analyses, or
ii) One for each day that VOCs are collected.
NOTE: Trip Blanks are not required for VOCs in Air.
3.3.3 Rinsate or Equipment Blank - The rinsate blank is used to determine whether the
sampling equipment decontamination procedure has been adequately performed,
thereby assuring that no "carryover" contamination has been introduced before (or
during) sample collection. Rinsate blanks are prepared in the field by pouring
demonstrated analyte-free water through/over the sampling equipment (including
filters) and collecting rinsate in the appropriate sample containers and adding
appropriate preservatives. Rinsate blanks should be collected at a frequency of one
per 20 samples per matrix per sampling equipment type (or one per day per matrix per
equipment type). This sample should be analyzed for the same parameters as those
associated with site-specific samples collected from potentially contaminated media.
NOTE: The sampler will provide both the sample containers and sample preservation when
sampling. The Field Blank and the Rinsate Blank should both use the same lot of sample
containers and preservatives that are used for the samples.
3.3.4 Temperature Blank - The temperature blank is used only to determine whether site-
specific samples have been adequately cooled during shipment and storage.
Temperature blanks can be prepared any time before or during field sampling
activities by adding water to an appropriate sample container such as a VOA vial.
Temperature blanks should be collected at a frequency of one per each cooler used to
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store/transport site-specific samples. The temperature blank will be measured upon
receipt by the analytical laboratory.
NOTE: The Temperature blank is not analyzed and it will not be combined with a sample that
is intended to be analyzed.
3.4 Dissolved Analysis
Samples collected for analysis of dissolved components must be filtered in the field. A
filtered Field Blank must also be collected for each new lot of filters. These are considered
separate samples from the unfiltered aliquot, so a separate sample number will be needed on
the Chain of Custody form.
3.5 Dechlorination
Only those samples which actually contain chlorine should be dechlorinated. Chlorine
presence may be determined using a color wheel or Flach kit.
NOTE: If the sampling requirements (for preservation, sample containers, etc,) are exactly the
same, then one sample can be taken for several parameters in a single container if the volume
will accommodate all analysis (Section 10.0 Pollution Prevention (P2) and Environmental
Management System EMS). It is especially important to consolidate parameters when
collecting solid samples because of the difficulty in disposing of the excess sample. Solids
should be collected in a single 8 oz. container for either the organic or inorganic parameters. If a
parameter cannot be combined with other parameters, it is noted in the table.
Holding Time
Samplers must be aware of the holding times for all analyses requested and ship samples to the
OASQA laboratory as quickly as possible. Holding time is the elapsed time from the date/time
of collection of the sample until the date/time of its analysis. This is not the date/time of receipt
at the lab. To ensure that OASQA can meet the required holding time, it may be necessary to
ship samples at the end of each collection day.
Data from sample!s) analyzed past the holding time(s) must be carefully examined by the data
user. These values may be biased low due to possible loss of the parameter* s) of interest, and
they will be flagged by the laboratory. (Tables 1, 2, and 3)
NOTE: Planning should be done so that samples are collected, shipped and analyzed within
holding times. Sample shipments will not be accepted before or after normal business hours
(07:30 - 16:30 Eastern), on weekends or Federal Holidays. This excludes Emergency sampling
events.
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5.0 OASQA Laboratory Sampling Requirements
Tables 1, 2, and 3 lists Parameter/Analyte. Analysis Technique, Collection Technique,
Container Type, Temperature/Preservation, Holding Time(s), Minimum Volumes/Weights,
Analytical Method* s), and Quantitation (QLs) for Aqueous and Non-Aqueous samples submitted
to OASQA laboratory.
IMPORTANT: Critical information is provided in the Tables 1, 2, and 3 Footnotes. It is
essential to comply with these requirements so that reliable data meets the needs of the project
are produced. The listed QLs are optimum levels and may be raised due to matrix interferences
and necessary dilutions.
6.0 Laboratory Quality Control Requirements
In addition to the minimum volumes or weights needed to perform a single analysis for each
parameter listed in Tables 1, 2, and 3 it is essential that the sampler collect enough sample to
allow the laboratory to analyze samples for Quality Control (QC) purposes. For every 10
inorganic parameter samples or for every 20 organic parameter samples, a QC sample is required
for each batch of samples. If there are more than 10 (inorganic ) or 20 (organic ) samples per
batch, another QC sample should be collected for each group. (Appendix 1)
NOTE: It is extremely important that sufficient volume be collected for quality control analysis.
Please do not collect any more volume than necessary; it is expensive to properly dispose of
excess volume and is inefficient for both the sampler and laboratory. (Section 10.0 Pollution
Prevention (P2) and Environmental Management System EMS)
7.0 Paperwork Requirements
The following documents must accompany the sample shipment for accurate identification and
safety information. Each document must be legibly written with indelible (waterproof) ink. No
erasures or white outs are allowed. Any writing errors made on a document must be corrected by
a single line through the error, initialed, dated, and rewritten.
7.1 Chain of Custody (COO - The COC is a legal document that must be complete, accurate,
and show an unbroken trail of accountability that insures the physical security of sample! s),
data, and records. A COC must accompany each sample shipment. The COC must be sealed
in a water proof zip-locked bag and taped on the inside of the ice chest lid with the samples.
The original COC record must accompany the shipment and a copy retained by the sampler.
Each distinct sample must appear on a separate line. It is NOT necessary to have a separate
line for each container (or each sample tag/label ). A sample shipment without a COC may
be rejected by the laboratory. (Appendix 8)
NOTE: Samples collected for dissolved constituents are considered distinct from the unfiltered
aliquot and should be placed on a separate line.
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Chain of Custody documentation must include:
a) Site name that is recorded on the Analytical Request Form (Project Name)
b) Analytical Request number (Project Number)
c) Sampler's name/signature
d) Sample ID (Station Number)
e) Date and Time of collection (recorded in 24 hour clock time)
f) Type of sample (grab or composite)
g) Sample description (Station Location)
h ) Accurate number of containers
i) Parameters requested
j) Preservation of sample
k) Sample tag/label numbers
1) Sample remarks (i.e. filtered for dissolved components, or if it is a field duplicate)
m) Date, Time and Signatures for sample receipt and transfer
7.2 Sample Tag - Each sample must have a sample tag tied to the container or some type of
adhesive label with identifying information. The information that is written on the sample
label must match the information on the COC. (Appendix 7)
NOTE: Ensure each sample tag/label is secured to each container since they might loosen and
fall off if the containers get cold or wet. For the safety of lab staff, indicate on each sample
tag/label any preservative used for the samples.
7.3 Exposure Data Sheet - Each time samples are collected, the sampler must complete a
Hazard and Risk Exposure Data Sheet. This information helps ensure the safety of the lab
staff receiving the samples so that proper precautions are taken whenever potentially
hazardous samples are encountered. This sheet is a vital part of the OASQA safety program
and must be attached to the OUTSIDE of at least one shipping container so that it is
available for review by the sample managers before opening any coolers or chests.
(Attachment 9)
7.4 Letter to File - The Letter to File is an official document (hard copy with an original
signature of the Remedial Project Manager (RPM) or the sampler, that provides corrective
actions for incorrect, unclear, incomplete, or inconsistent information found with any of the
sample documentation or problems were detected with the physical condition of the
sample!s) upon arrival at the laboratory.
Shipping Requirements
Prior to shipment, samples collected during field investigations or in response to a hazardous
materials incident must be classified as either environmental or hazardous materials samples. In
general, environmental samples include drinking water, most groundwater and ambient surface
water, soil, sediment, treated municipal and industrial wastewater effluent, biological specimens,
or any samples not expected to be contaminated with high levels of hazardous materials.
Samplers are expected to be aware of all State, Federal, Department of Transportation (DOT),
and International Air Transport Association (I ATA) regulations governing environmental and
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hazardous sample packaging. The sample shipping personnel is responsible for being in
compliance with applicable packaging, labeling, and shipping requirements.
Samples collected from process wastewater streams, drums, bulk storage tanks, soil, sediment, or
aqueous samples from areas suspected of being highly contaminated may require shipment as
dangerous goods. Regulations for packing, marking, labeling, and shipping of dangerous goods
by air transport are promulgated by the IATA, which is equivalent to United Nations
International Civil Aviation Organization (UN/ICAO). Transportation of hazardous materials
(dangerous goods) by EPA personnel is covered by EPA Order 1000. 18.
8.1 Shipment of Dangerous Goods
8.1.1 The project manager and/or sampler is responsible for determining if samples
collected during a specific field investigation meet the definitions for dangerous
goods. If a sample is collected of a material that is listed in the Dangerous Goods List
(Section 4.2, IATA), that sample must be identified, packaged, marked, labeled, and
shipped according to the instructions given for that material.
NOTE: The loaded cooler must not be heavier than 50 pounds to allow for safe handling. Only
certified personnel are allowed to ship the containers, according to the Dangerous Goods
Regulations promulgated by the International Air Transport Authority (IATA). At least one
member of the sampling team should be aware of the Department of Transportation (DOT) and
IATA legal requirements for shipping these types of materials.
8.1.2 The sample may not be shipped by air transport if the composition of the collected
sample(s) is unknown, and the project leader knows or suspects that it is a regulated
material (dangerous goods). If the composition and properties of the collected sample
is suspected of being highly contaminated, the sample may not be shipped by air
transport. Contact DOT and the IATA for shipping requirements and restrictions.
8.1.3 In addition, the shipment of pre-preserved sample containers or bottles of
preservatives (e.g., NaOI I pellets, I ICL, etc.) which are designated as dangerous goods
by IATA is regulated. Shipment of nitric acid is forbidden on all aircraft. Dangerous
goods must not be shipped by air transport without contacting the Division's
dangerous goods shipment designee. The preservation for the metals analysis may be
added at the lab if safety precautions warrant.
8.2 Shipment of Environmental Laboratory Samples
8.2.1 The OASQA laboratory will not accept any samples shipped with any particulate
(dusty) type packing material, especially vermiculite.
8.2.2 Guidance for the shipment of environmental laboratory samples by personnel is
provided in a memorandum dated March 6, 1981, subject "Final National Guidance
Package for Compliance with Department of Transportation Regulations in the
Shipment of Laboratory Samples" (3). By this memorandum, the shipment of the
following unpreserved samples is not regulated:
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a) Drinking water
b) Treated effluent
c) Biological specimens
d) Sediment
e) Water treatment plant sludge
8.2.3 In addition, the shipment of the following preserved samples is not regulated, provided
the amount of preservative used does not exceed the amounts found in 40 CFR 136.3.
It is the shippers' (individual signing the airway bill ) responsibility to ensure that
proper amounts of preservative are used:
a) Drinking water
b) Ambient water
c) Treated effluent
d) Biological specimens
e) Sediment
f) Wastewater treatment plant sludge
8.2.4 Samples determined by the project manager to be in these categories are to be shipped
using the following protocol, developed jointly between EPA, OSI IA, and DOT. This
procedure is documented in the "Final National Guidance Package for Compliance
with Department of Transportation Regulations in the Shipment of Environmental
Laboratory Samples".
Environmental samples should be packed prior to shipment by air using the following
procedures:
a) Allow sufficient head space in all bottles (except VOC containers with a septum
seal) to compensate for any pressure and temperature changes (approximately 10
percent of the volume of the container ).
b) Be sure the lids on all bottles are tight (will not leak).
c) Place bottles in separate and appropriately sized polyethylene bags and seal the
bags with tape (preferably plastic electrical tape). Up to three VOC bottles may be
packed in one Whirl-Pak container. (We recommend using plastic bags to double-
bag glass containers to prevent leakage, then wrapping each container in bubble
wrap to prevent breakage).
d) Select a sturdy cooler in good condition. Secure and tape the drain plug with fiber
or duct tape. Department of Transportation (DOT) and/or Federal Express/UPS
approved shipping containers must be used. To further assure that any leakage will
be contained, the cooler should be lined with a large heavy duty plastic bag.
e) Put ice (that has been "double bagged" in heavy duty polyethylene bags and
properly sealed to contain the melted water) on top of and/or between the samples.
This will ensure uniform cooling of the samples.
f) Samples preserved by chilling must be shipped with sufficient ice to remain
cool, < 6°C (without allowing the sample to become frozen), while in transit. A
temperature blank must be included in the shipment to allow the laboratory to
verify the temperature upon receipt.
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NOTE: The loaded cooler must not be heavier than 50 pounds to allow for safe handling.
g) Securely fasten the top of the large garbage bag with tape.
h) Place the Chain-of-Custody Record and all other applicable documents into a
plastic bag, and tape the bag to the inner side of the cooler lid.
i) Close the cooler and securely tape, with strapping tape, the top of the cooler shut.
Custody seals should be affixed to the top and sides of the cooler within the
securing tape so that the cooler cannot be opened without breaking the seal.
j) Shipping containers must be marked "THIS END UP", and arrow labels which
indicate the proper upward position of the container should be affixed to the
container.
k) A label containing the name and address of the shipper should be placed on the
outside of the container. Labels used in the shipment of hazardous materials (e.g..
Cargo Only Air Craft, Flammable Solids, etc,) are not permitted to be on the
outside of containers used to transport environmental samples.
IMPORTANT: Return of the cooler( s) should be scheduled by the sampler, prior to sending
the samples in for analysis. All return shipping documentation should be sealed in a water proof
zip-locked bag and taped on the inside of the cooler(s) lid with the samples.
9.0 Shipment Notification
The OASQA Sample Scheduling Coordinator should be notified as soon as possible when (1)
samples have been shipped, (2) a scheduled shipment has been ch anged/can eel ed, or (3) there
are changes in the number or types of samples. Notification should be via e-mailed and/or faxed,
and followed up by a phone call BEFORE the expected shipping date.
Sample Scheduling Coordinator (SSC)
Kevin Martin: 410-305-3032 (ph), 410-305-3095 (fax), martin.kevin@epa.gov
Secondary Contacts
John Curry: 410-305-2608 (ph), 410-305-3093 (fax), curry.iohn@epa.gov
Mailing Address
U.S. EPA, Region III, OASQA
Environmental Science Center
701 Mapes Road
Fort Meade, Maryland 20755-5350
10.0 Pollution Prevention (P2) and Environmental Management System (EMS)
It is the Environmental Science Center's policy to integrate environmental stewardship into our
operations and we have therefore instituted an Environmental Management System (EMS). This
means that we manage our organizations and our programs in a manner that protects the
environment, the safety of our employees, and the public health. In support of this policy, the
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OASQA lab is committed to the promotion of Pollution Prevention (P2) awareness and the
Agency's waste reduction strategies. To support our Pollution Prevention (P2) goals, the lab
requests that samplers take a common sense approach to the collection of samples with respect to
how much volume is collected. Of course, the most important consideration must be the need for
enough volume to constitute a representative sample, and to accommodate the analysis
requested. Many parameters can be combined together to avoid excess volumes. Since the
laboratory must pay to dispose of the material after analyses, if at all possible, please combine
samples for all analytes requiring the same container and preservative in a minimum number of
containers.
Examples of parameters for aqueous samples which are commonly combined are:
(A) Metals + Mercury + Hardness —» 250 ml. container; or
(B) Ammonia + TOC + TP + TKN —» 200 mL container.
Parameters for solid samples have few preservative requirements; therefore, most inorganic or
organic parameters can be combined in one container. It is especially important to consolidate
parameters when collecting solid samples because of the difficulty in disposing of the excess
sample. Solids should be collected in a single 8 oz. container for either the organic or inorganic
parameters. For additional guidance on combining samples, please contact the Sample
Scheduling Coordinator (SSC).
IMPORTANT: If any of part of this document is unclear or if you want to verify the requirements,
please contact the Sample Scheduling Coordinator (SSC ) for clarification.
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11.0 References
The current versions of the following guidance documents are referenced.
11.1 EPA Region 3, Users' Guide for Acquiring Analytical Services.
http://www.epa.gov/region3/esc/pdf/6users_guide_rev.pdf
11.2 EPA Region 3, Analytical Request Form Instructions.
http://www.epa.gov/region3/esc/instruct.htni
11.3 EPA Region 3, Laboratory Quality Manual, revision 9.
11.4 International Air Transport Authority (TATA), Dangerous Goods Regulations.
http://www.iata.org
11.5 US Environmental Protection Agency (US EPA) Order 1000.18-Transportation of
Hazardous Materials, February 16, 1979.
11.6 Contract Laboratory Program (CLP) Guidance for Field Samplers, OSWER 9240.0-47,
EPA540-R-09-003, January 2011.
11.7 National Environmental Laboratory Accreditation Conference (NET.AC) Standards.
http://www.nelac-institute.org
11.8 Federal Register/Vol. 72, No. 47/Monday, March 12, 2007/Rules and Regulations.
11.9 40 Code of Federal Regulations (CFR), Part 136 - Guidelines Establishing Test
Procedures for the Analysis of Pollutants, Section 136.3 Identification of test procedures.
Table IA— ID and Table II.
11.10 40 Code of Federal Regulations (CFR ), Part 141 - National Primary Drinking Water
Regulations.
11.11 49 Code of Federal Regulations (CFR ), Subtitle B - Other Regulations Relating to
Transportation, Pt. 171 180.
11.12 Manual for the Certification of Laboratories Analyzing Drinking Water,
EPA 815-R-05-004, January 2005.
11.13 Supplement 1 to the Fifth Edition of the Manual for the Certification of Laboratories
Analyzing Drinking Water, EPA 815-F-08-006, June 2008.
11.14 EPA Region 3 Analytical Request Form, Revision 11.09.
http://www.epa.gov/region3/esc/doc/analytical_request_forni.doc
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Table 1 Aqueous Sample Requirements
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Alcohols
Ethanol
Methanol
1-Propanol
1-Butanol
Sec-Butanol
GC-FID
G, C
V
cool, < 6 °C (5)
7 days
10 mL
SW8015D
10 mg/L
10 mg/L
10 mg/L
10 mg/L
10 mg/L
Alkalinity (Total)
Bicarbonate
Carbonate
P-Alkalinity
Titration
G, C
P
cool, < 6 °C (5)
14 days
500 mL
SM 2320B
20 mg/L
20 mg/L
20 mg/L
20 mg/L
Anions
Bromide
Chloride
Fluoride
Sulfate
Nitrite (9)
Nitrate (9)
Orthophosphate (9,36)
Ion
Chromatography
G, C
GL, P
cool, < 6 °C (5)
28 days
48 hrs (9)
200 mL
EPA 300.0
0.50 mg/L
0.25 mg/L
0.10 mg/L
0.50 mg/L
0.05 mg/L
0.15 mg/L
0.5 mg/L
Ammonia (not distilled)
(Total)
Automated
Colorimetric
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
200 mL
SM 4500-NH3 BG
0.04 mg/L
Biochemical Oxygen Demand (BOD5)
Carbonaceous (CBOD)
DO probe
G, C
GL, P
cool, < 6 °C (5)
48 hrs
500 mL
SM 5210B
4 mg/L
Chemical Oxygen Demand (COD)
Spectrophotometric
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
200 mL
HACH 8000
10 mg/L
Corrosivity
(pH for > 20% water)
Electrometric
G, C
P
None
ASAP
500 mL
SW 9040C
NA
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 17 of41
Table 1 Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Cyanide
(Total)
Distillation,
Automated
G
GL, P
cool, < 6 °C (5)
Dechlorinate (30k) then
NaOH to pH>10
14 days
200 mL
EPA 335.4
0.02 mg/L
Glycols
2-Butoxyethanol
Diethylene Glycol
Triethylene Glycol
Tetraethylene Glycol
HPLC/MS/MS
G, C
V
cool, < 6 °C (5)
14 days
40 mL
SW 8321 mod
ASTM D7731-11 mod
25 Hg/L
25 Hg/L
25 Hg/L
25 Hg/L
Hardness (calculation)
ICR + calculation
G, C
GL, P
HN03 to pH<2 (8)
6 months
200 mL
Both EPA 200.7 and
SM 2340B
3300 ng/L
Hexavalent Chromium
Ion
Chromatography
G
P
cool, < 6 °C (5)
pH of 9.3 - 9.7 with
(nh4)2so4
28 days
200 mL (14)
EPA 218.6
10 ng/L (26)
or
1.0 pg/L (27)
Ignitability
Pensky-Martens,
closed cup
G
SWJ
None
ASAP
250 mL
SW1010A
NA
Infrared (IR) screen
FTIR, GC-FTIR,
GC/MS
G, C
GL, P
cool, < 6 °C (5)
ASAP
100 mL
IR identification scan
NA
Lab pH
(for > 20% water)
Electronic
G
P
None
ASAP
500 mL
SW 9040C
NA
Mercury
(Dissolved (14) and Total)
Cold Vapor
Spectrometry
G, C
GL, P
HN03 to pH<2 (8)
28 days
250 mL
EPA 245.1,
SW 7470A,
CLP Equivalent
0.2 Mg/L
Mercury - TCLP
TCLP; Cold Vapor
Spectrometry
G, C
GL, P
cool, < 6 °C (7)
28 days
1000 mL
SW 1311,
SW 7470A
0.2 mg/L
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 18 of 41
Table 1 Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
EPA 200.7,
EPA 200.8,
SW 6010B,
SW 6020A,
CLP Equivalent
Metals
(Dissolved (14) and Total)
ICR, ICP/MS
G, C
GL, P (24)
HN03 to pH<2 (8)
6 months
250 mL
Refer to
Appendix 2
Metals-TCLP
TCLP; ICR
G, C
GL, P
cool, < 6 °C (7)
180 days
1000 mL
SW 1311,
SW 6010B
Refer to
Appendix 2
Total Kjeldahl Nitrogen (TKN)
Automated
colorimetric
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
200 mL
EPA 351.2
0.1 mg/L
Nitrite + Nitrate
Automated
colorimetric
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
250 mL
EPA 353.2
(Use if EPA 300
isn't an option)
0.05 mg/L
Nitrogen (TN) - digested
(Total)
Automated
colorimetric
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
250 mL
EPA 353.2
1 mg/L
Nitroaromatics, Nitramines, and
Explosives
HPLC/PDA
G, C
AGL
cool, <6°C (5'30h)
7 days
1000 mL (4)
SW 8330
Refer to
Appendix 6
Oil & Grease
Solid phase
extraction
G
WGL
cool, < 6 °C (5)
HCI to pH<2
28 days
2x1000 mL
per sample14'
EPA 1664A
5 mg/L
Perchlorate
IC Conductivity
or
LC/MS
G, C
GL, P
cool, < 6 "C (6)
with headspace
28 days
100 mL
EPA 314.0 (IC)
or
SW 6850 (LC/MS)
1 Mg/L (IC)
or
0.5 [ig/L (LC/MS)
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 19 of 41
Table 1 Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Percent water
Wet Chemistry
G, C
P
None
ASAP
200 mL
SW 9001
NA
PCB Congeners
Cont L/L extraction;
GC/MS
G
AGL
cool, < 6 "C (5,30h)
1 year
1000 mL (4)
EPA 1668C
20 pg/L
Pesticides
Cont L/L extraction;
GC/MS
G
AGL
cool, <6°C (5'30h)
7 days
1000 mL (4)
EPA 608,
SW 808IB,
SW3520C
Refer to
Appendix 3
PCBs
Cont L/L extraction;
GC/MS
G
AGL
cool, <6°C (5'30h)
7 days
1000 mL (4)
EPA 608,
SW 8082A,
SW3520C
Refer to
Appendix 3
Pesticides - TCLP
Cont L/L extraction;
GC/MS
G
AGL
cool, < 6 °C (7)
14 days
1000 mL
EPA 608,
SW 8081B,
SW3520C
Refer to
Appendix 3
Phenol
(Total)
Colorimetric -
automated
G
AGL
cool, < 6 °C (5)
Dechlorinate (30i) then
H,S04 to pH<2
28 days
1000 mL
EPA 420.1/420.4
20 [ig/l
Phosphorus (TP)
(Total)
Colorimetric -
automated
G, C
GL, P
cool, < 6 °C (5)
HCI to pH<2
28 days
200 mL
EPA 365.4
0.05 mg/L
Polyaromatic Hydrocarbons
(PAH-SIM)
Cont L/L extraction;
GC/MS
G
AGL
cool, < 6 ° C (5,30h)
7 days
1000 mL (4)
SW 3520C,
SW8270D
Refer to
Appendix 4
Semivolatiles (SVOCs)(12)
Cont L/L extraction;
GC/MS
G
AGL
cool, < 6 °C (5,30h)
7 days
1000 mL (4)
EPA 625,
SW 8270D,
SW 3520C,
CLP Equivalent
Refer to
Appendix 4
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 20 of 41
Table 1 Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Semivolatiles (SVOCs)(12) - TCLP
TCLP; GC/MS
G
AGL
cool, < 6 "C (5,7)
14 days
1000 mL
SW 1311,
SW 8270D
Refer to
Appendix 4
Total Solids (TS)
Gravimetric
G, C
GL, P
cool, < 6 °C (5)
7 days
500 mL
SM 2540B
10 mg/L (11)
Total Dissolved Solids (TDS)
Gravimetric
G, C
GL, P
cool, < 6 °C (5)
7 days
500 mL
SM 2540C
10 mg/L (11)
Total Organic Carbon (TOC)
Dissolved Organic Carbon (DOC)(14)
Combustion,
Oxidation
G, C
GL, P
cool, < 6 °C (5)
H,S04 to pH<2
28 days
100 mL
SM 5310B
3 mg/L
Total Suspended Solids (TSS)
Gravimetric
G, C
GL, P
cool, < 6 °C (5)
7 days
500 mL
SM 2540D
10 mg/L (11)
Total Toxic Organics (TTO)
Follow the same requirements for PCB/Pesticides, SVOCs, and VOCs
Refer to
Appendix 3, 4, 5
Volatiles (VOCs)(12)
Purge & Trap
extraction, GC/MS
G
V
cool, < 6 °C (5)
Dechlorinate (30h) then
1:1 HCI to pH<2pi)
7 days (20)
14 days (21)
120 mL (33)
EPA 624,
SW 5030C,
SW 8260C,
CLP Equivalent
Refer to
Appendix 5
Volatiles (VOCs) - TCLP/ZHE
Purge & Trap
extraction, GC/MS
G
V
cool, < 6 °C (5)
14 days
160 mL (32)
SW 1311,
SW 5030C,
SW 8260C
Refer to
Appendix 5
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 21 of 41
Table 2 Non-Aqueous Sample Requirements
mmmmmmmmiihiiiiiiiiiiiiiiiiiii"^^^^™ ¦———————-————iiiiiiiiiiiiiiiiiiiiiiWui iiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiirnrnrnrnrnrnrriiiiiiiiiiiiiiiiiiiiiirnrnr
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Weight (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Anions
Bromide
Chloride
Fluoride
Sulfate
Nitrite
Nitrate
Orthophosphate
Ion
Chromatography
G, C
GL
cool, < 6 °C
None
50 g
EPA 300.0
0.1 mg/kg
0.1 mg/kg
0.1 mg/kg
0.1 mg/kg
0.1 mg/kg
0.1 mg/kg
0.1 mg/kg
Benthic Invertebrate Taxonomy
Micro
G
GL
70% Ethanol
None
NA
Benthic
NA
Chemical Oxygen Demand (COD)
Spectrophotometric
G, C
GL
cool, < 6 °C
28 days
50 g
HACH 8000
10 mg/L
Cyanide
(Total)
Distillation,
Automated
G
GL
cool, < 6 °C
28 days
100 g
EPA 335.4
1 mg/kg
Grainsize
Gravimetric
G
SWJ
cool, < 6 °C
None
50 g
EMAP Estuaries,
Plumb 1981
Report as %silt,
%sand, and
%clay
Hexavalent Chromium
Ion
Chromatography
G
GL
cool, < 6 °C
pH of 9 ± 0.5 with
NH4OH
30 days
50 g
EPA 218.6
10 mg/L
Ignitability
Pensky-Martens,
closed cup
G
SWJ
cool, < 6 °C
ASAP
50 g
SW 1030
NA
Infrared (IR) screen
FTIR, GC-FTIR,
GC/MS
G, C
GL
cool, < 6 °C
ASAP
50 g
IR identification scan
NA
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 22 of 41
Table 2 Non-Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique (1)
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Weight (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Lab pH
Electronic
G
GL
None
ASAP
200 g
SW 9045D
NA
Mercury
(Solids)
Cold Vapor
Spectrometry
G, C
GL
cool, < 6 °C
28 days
50 g
EPA 245.5,
SW 7471A,
CLP Equivalent
0.1 Hg/g
Mercury-TCLP
(Solids)
TCLP; Cold Vapor
Spectrometry
G, C
SWJ
cool, < 6 °C
28 days
200 g
SW 1311,
SW7470A
0.2 mg/L
Metals
(Solids)
ICP, ICP/MS
G, C
GL
cool, < 6 °C
6 months
50 g
EPA 200.7,
EPA 200.8,
SW 6010B,
SW 6020A,
CLP Equivalent
Refer to
Appendix 2
Metals-TCLP
(Solids)
TCLP; ICP
G, C
SWJ
cool, < 6 °C
180 days
200 g
SW 1311,
SW 6010B
Refer to
Appendix 2
Nitroaromatics, Nitramines, and
Explosives
HPLC/PDA
G, C
AWJ
cool, < 6 °C
14 days
50 g
SW 8330
Refer to
Appendix 6
Perchlorate
IC Conductivity,
LC/MS
G, C
GL
cool, < 6 °C
28 days
50 g
EPA 314.0 (IC)
or
SW 6850 (LC/MS)
0.005 mg/kg
Percent Dry Weight
Gravimetric
G, C
GL
None
None
100 g
USGS-PD105
NA
Percent Moisture
Gravimetric
G, C
AWJ
cool, < 6 °C
None
50 g
ASTM D2216-98
NA
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 23 of 41
Table 2 Non-Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Weight (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
PCB Congeners
Soxhlet extraction;
GC/MS
G, C
AWJ
cool, < 6 °C
1 year
100 g
EPA 1668C
10 pg/g
PCB
(Solids/Tissue/Petroleum/Wipes)
ASE,
Waste dilution;
GC/ECD
G, C
AWJ
cool, < 6 °C
1 year
100 g
10 g (15)
SW 8082A,
SW 3545A,
SW 3580A
Refer to
Appendix 3
Pesticides
(Solids/Tissue)
ASE; GC/ECD
G, C
AWJ
cool, < 6 °C
14 days
100 g
SW 8081B,
SW 3545A
Refer to
Appendix 3
Pesticides - TCLP
Cont L/L extraction;
GC/ECD
G, C
AWJ
cool, < 6 °C
7 days
250 g
SW 8081B,
SW3520C
Refer to
Appendix 3
Phenol
(Total)
Colorimetric -
automated
G, C
GL
cool, < 6 °C
28 days
50 g
EPA 420.1/420.4
10 mg/kg
Phosphorus (TP)
(Total)
Colorimetric -
automated
G, C
GL
cool, < 6 °C
28 days
50 g
EPA 365.4
0.050 mg/L
Polyaromatic Hydrocarbons
(PAH-SIM)
Soxhlet extraction;
GC/MS
G, C
AWJ
cool, < 6 °C
14 days
50 g
SW 8270D,
SW3520C
Refer to
Appendix 4
Semivolatiles (SVOCs)(12)
(Solids/Petroleum)
Soxhlet extraction;
GC/MS
G, C
AWJ
cool, < 6 °C
10 days (17)
14 days (16)
100 g
SW 8270D,
SW 3540C (solids),
SW 3580A (petroleum)
Refer to
Appendix 4
Semivolatiles (SVOCs)(12) - TCLP
TCLP; GC/MS
G, C
AWJ
cool, < 6 °C
14 days
200 g
SW 1311,
SW8270D
Refer to
Appendix 4
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 24 of 41
Table 2 Non-Aqueous Sample Requirements (cont.)
Parameter
(Analyte)
Analysis
Technique
Collection
Technique 111
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Weight (min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Total Organic Carbon (TOC)
Combustion,
Oxidation
G
SWJ
cool, < 6 °C
None
50 g
SM 5310B
100 mg/kg
Volatiles (VOCs)(12)
(Solids/Petroleum)
Purge & Trap
extraction, GC/MS
G
Refer to
Appendix 11
Refer to
Appendix 11
14 days (15)
48 hrs (29)
Refer to
Appendix 11
SW 5035A,
SW 5030C,
SW 8260C
Refer to
Appendix 5
Volatiles (VOCs)(12)
(Air/Vapor)
Purge & Trap
extraction, GC/MS
G, C
S
None
30 days
6 L
TO-15
Refer to
Appendix 5
Volatiles (VOCs) - TCLP/ZHE
Purge & Trap
extraction, GC/MS
G
V
cool, < 6 °C
14 days
160 g (32)
SW 1311,
SW 5030C,
SW 8260C
Refer to
Appendix 5
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 25 of 41
Table 3 SDWA Program Special Requirements
— vmmmmmmmmmmmmmvBaiaiaiaiaiasihMiiMj. — J— mm&Mmmm
Parameter
(Analyte)
Analysis
Technique
Collection
Technique (1)
Container
Type 121
Temperature
and
Preservation
Holding
Time(s)
Sample
Volume
(min)
Method(s)131
Optimum
Quantitation
Limits (QLs)
Coliforms
(Total and Fecal)
Micro
G
gl(23), pl(23)
cool, < lcrc (5'30k)
8 hrs,
30 hrs (18)
120 mL (22)
SM 9221 B (Total)
SM 9221B,E (Fecal)
2 MPN/100 mLs
E. coli
Enzyme Substrate
G
PL®23'
cool, < lcrc(5,30k)
8 hrs,
30 hrs (18)
120 mL (22)
SM 9223 Colilert QT
1 MPN/100 mL
E. Coli and Total Coliforms
Micro
G
PL®23'
cool, <10 °C (5,30k)
30 hrs
120 mL (22)
SM 9223 Colisure
Report only
Presence/Absence
Heterotrophic Bacteria
Heterotrophic
Plate Count
G
GL®23', PL®23'
cool, < lcrc(5,30k)
8 hrs
120 mL (22)
SM 9215B
1 cfu/1 mL
Nitrate (N03-N)
Automated
colorimetric
G
GL, P
cool, <6°C (5)
14 days (34)
48 hrs (35)
200 mL
EPA 300.0
0.15 mg/L
Pesticides (Chlorinated)
Endrin
gamma-BHC (Lindane)
Heptachlor epoxide
Solid phase
extraction
G
AGL
cool, < 6 "C (5)
Dechlorinate (30i) then
6N HCI to pH<2
14 days
2000 mL (4)
EPA 508.1
0.02 ng/L
0.02 ng/L
0.02 Mg/L
Total Trihalomethanes (TTHMs)
Purge & Trap
extraction, GC/MS
G
V
cool, < 6 "C (5)
Dechlorinate (30h) then
1:1 HCI to pH<2
14 days
120 mL (33)
EPA 524.2
0.5 Mg/L
Regulated Volatiles (VOCs)
Purge & Trap
extraction, GC/MS
G
V
cool, < 6 "C (5)
Dechlorinate (30h) then
1:1 HCI to pH<2
14 days
24 hrs (18)
120 mL (33)
EPA 524.2
Refer to
Appendix 5
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 26 of 41
Table 1„ 2 and 3 Footnotes
1
C
Composite only (sampling period must have a Start and Ending time)
G,C
Grab or Composite
G
Grab only for:
i) Volatile (i.e. VOCs, Cyanide and Sulfide - may vary in volatility with pH changes) or
ii) Highly biodegradable (i.e. Total Phenols) or
iii) Tend to adhere to surfaces (i.e. Oil&Grease, PCBs/Pesticides and SVOCs) or
iv) Reactive (i.e. Hexavalent Chromium)
2
The analytical procedure! s) to be used for sample analysis often requires the use of a particular type
of sample container. The type of container also may depend on the sample matrix and analysis. It is
recommended that samplers use borosilicate glass containers, which are inert to most materials, when
sampling for pesticides and/or other organics. Conventional polyethylene is recommended when
sampling for metals because of the lower cost and absorption rate of metal ions.
GL
Glass
P
Polyethylene
PL
Plastic container*s) has been autoclaved prior to sampling
AGL
1 L amber glass bottle with Teflon lined cap
AS J
Amber, straight-sided, glass jar with Teflon lined screw cap
WGL
1 L clear, wide mouth, straight-sided, glass bottle with 89 mm Teflon lined screw cap
SWJ
8 oz short, wide mouth, straight-sided, glass jar with Teflon lined cap
AW J
8 oz short, wide mouth, straight-sided, amber glass jar with Teflon lined cap
V
40 nil. clear glass VOA vial
TGL
4 oz (120 nil . ) tall, wide mouth, straight-sided, glass jar
PB
Heavy plastic bag
S
Sum ma canisters (supplied by lab)
3
SM
Standard Methods
SW
SW 846 Method
EPA
EPA Method
4
Cannot combine with other parameters.
5
Do not allow the sample! s) to become frozen.
6
Avoid extreme temperatures.
7
Unless cooling causes precipitation of the waste.
8
The acid may be added at the Lab if safety precautions warrant.
9
Maximum holding time is 48 hrs for Nitrite, Nitrate and Orthophosphate.
10
Dechlorinate only those samples which actually contain chlorine with 50 mg Sodium Sulfite - Na2SO.i
-------
Table 1„ 2 and 3 Footnotes (corn.)
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 27 of 41
11
This QL is based on 100 ml. of sample.
12
TICs for organic analysis are available upon request.
13
For SDWA, unpreserved sample! s).
14
Filter in the field.
15
For petroleum sample(s) only.
16
For EPA 8270D sample(s) only.
17
For CLP sample!s) only.
18
For SDWA sample(s).
19
For NPDES sample! s).
20
Unpreserved.
21
Preserved.
22
One (1) inch air space in bottle.
23
Sterile container.
24
When requesting the analyte Boron, only use a plastic container
25
Filter in the field for NPDES sample! s).
26
On a 25 pL Sample Injection Loop size
27
On a 250(.iL Sample Injection Loop size
28
If water has been chlorinated, use 0.2 ml. of sterile 10% Na^O* per 250 ml. or less of sample.
29
To preserve or analyze for solid matrix only.
Dechlorinate only those samples which actually contain chlorine:
k) With Ascorbic Acid - C(TIsO(,
30
h) With Ascorbic acid - OTIsO(, (25 mg per 40 ml.); or Sodium Thiosulfate - Na2S:0<
(3 mg per 40 ml.)
j) With excess Ferrous Ammonium Sulfate - (NH4)2Fe(S04)2 * 6H20
31
RCRA and NPDES samole!s) must be submitted both preserved and unpreserved if 2-Chloroethvl.
Vinyl Ether is an analyte of interest. This is due to losses of 2-Chloroethyl Vinyl Ether in acidified
sample! s).
32
Four (4) glass 40 m I . VOA vials for 160 m 1. of sample filled with no headspace.
33
Three (3) glass 40 mI. VOA vials for 120 m 1. of sample filled with no headspace.
34
Chlorinated
35
Non-chlorinated
36
Filter in the field if for NPDES
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 28 of 41
Appendix 1: Quality Control (QC) Sampling Requirements
Parameter
Matrix
Additional Volume or Weight
required of that in
Tables 1-3
Biochemical Oxygen Demand (BODS)
Aqueous
500 mL (a)
Glycols
Aqueous
2x40 mL(a)
IR Identification
Aqueous
Solids
Wipes
Petroleum
40 mL ""
100 g (b)
1 blank wipe (b)
20 g of material(b)
Mercury
Aqueous
Wipes
25 mL ""
3 blank wipes (b)
Nitroaromatics, Nitramines, and Explosives
Aqueous
Soil
2x1000 mL(a)
100 g (b)
Oil & Grease
Aqueous
3x1000 mL(a)
PCB Congeners
Aqueous
4x1000 mL(a)
Perchlorate
Aqueous
Soil
2x100 mL(a)
100 g (b)
Phenol (Total)
Aqueous
1000 mL (a)
Pesticides (Chlorinated)
Aqueous
2x1000 mL(c)
Pesticides
Aqueous
Solids
2x1000 mL(a)
50 g ""
Pesticides/PCBs
Aqueous
4x1000 mL(a)
PCBs
Aqueous
Solids
Petroleum
Wipes
2x1000 mL(a)
60 g (b)
10 g of material(b)
1 blank; 2 duplicates(b)
Semi Volatiles (SVOCs)
Aqueous
Solids
2x1000 mL(a)
50 g l b l
Volatiles (VOCs)
Aqueous
6x40 mL(a,c)
Appendix 1 Footnotes
a
Refer to Table 1 Aqueous Sample Requirements
b
Refer to Table 2 Non-Aqueous Sample Requirements
c
Refer to Table 3 SDWA Program Special Requirements
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 29 of 41
Appendix 2: Metals Quantitation Limits (QLs)
Analyte(s)
CAS
Number
Aqueous
Solids
TCLP
ICR
ICR/MS
ICR
ICR/MS
ICR
Aluminum
7429-90-5
200 ng/L
30 Mg/L
20 Mg/g
3 Mg/g
NA
Antimony
7440-36-0
60 ng/L
2 Mg/L
6 Mg/g
0.2 Mg/g
NA
Arsenic
7440-38-2
200 ng/L
1 Mg/L
20 Mg/g
0.1 Mg/g
5 mg/L
Barium
7440-39-3
200 ng/L
10 Mg/L
20 Mg/g
iM-g/g
100 mg/L
Beryllium
7440-41-7
5 ng/L
1 Mg/L
0.5 Mg/g
0.1 Mg/g
NA
Boron
7440-42-8
50 ng/L
NA
5 Mg/g
NA
NA
Cadmium
7440-43-9
5 ng/L
1 Mg/L
0.5 Mg/g
0.1 Mg/g
1 mg/L
Calcium
7440-70-2
500 ng/L
NA
50 Mg/g
NA
NA
Chromium
7440-47-3
10 Mg/L
2 Mg/L
iM-g/g
0.2 Mg/g
5 mg/L
Cobalt
7440-48-4
50 Mg/L
1 Mg/L
5 Mg/g
0.1 Mg/g
NA
Copper
7440-50-8
25 ng/L
2 Mg/L
2.5 Mg/g
0.2 Mg/g
NA
Iron
7439-89-6
100 Mg/L
NA
10 Mg/g
NA
NA
Lead
7439-92-1
50 Mg/L
1 Mg/L
5 Mg/g
0.1 Mg/g
5 mg/L
Magnesium
7439-95-4
500 Mg/L
NA
50 Mg/g
NA
NA
Manganese
7439-96-5
15 Mg/L
1 Mg/L
1.5 Mg/g
0.1 Mg/g
NA
Nickel
7440-02-0
40 Mg/L
1 Mg/L
4 Mg/g
0.1 Mg/g
NA
Potassium
7740-09-7
2000 Mg/L
NA
200 Mg/g
NA
NA
Selenium
7782-49-2
200 Mg/L
5 Mg/L
20 Mg/g
0.5 Mg/g
1 mg/L
Silver
7440-22-4
10 Mg/L
1 Mg/L
iM-g/g
0.1 Mg/g
5 mg/L
Sodium
7440-23-5
1000 Mg/L
NA
100 Mg/g
NA
NA
Thallium
7440-28-0
200 Mg/L
1 Mg/L
20 Mg/g
0.1 Mg/g
NA
Tin
7440-31-5
200 Mg/L
NA
20 Mg/g
NA
NA
Titanium
7440-32-6
200 Mg/L
NA
20 Mg/g
NA
NA
Vanadium
7440-62-2
50 Mg/L
5 Mg/L
5 Mg/g
0.5 Mg/g
NA
Zinc
7440-66-6
20 Mg/L
2 Mg/L
2 Mg/g
0.2 Mg/g
NA
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 30 of 41
Appendix 3: Pesticides/PCRs Quantitation Limits (QLs) (PCBs>sw 8082A, Pesticides >sw sosibi
Analyte(s)
CAS
Number
Aqueous
Solid/Tissue
Petroleum
Wipes
TCLP
EPA 608
SW 808IB,
SW 8082A,
SW 3520C
SW 808IB,
SW 8082A,
SW 3545A
SW 8082A,
SW 3580A
SW 8082A,
SW 3545A
EPA 608,
SW 808IB,
SW 3520C
4,4 -DDD
72-54-8
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
4,4'-DDE
72-55-9
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
4,4 -DDT
50-29-3
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
Aldrin
309-00-2
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
alpha-BHC
319-84-6
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
alpha-Chlordane
5103-71-9
NA
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
beta-BHC
319-85-7
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
Chlordane
57-74-9
1 Mg/L
1 Mg/L
0.033 mg/kg
NA
NA
5.0 Mg/L
delta-BHC
319-86-8
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
Dieldrin
60-57-1
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
Endosulfan 1
959-98-8
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
Endosulfan II
33213-65-9
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
Endosulfan sulfate
1031-07-8
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
Endrin
72-20-8
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
1.0 Mg/L
Endrin aldehyde
7421-93-4
0.1 Mg/L
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
Endrin ketone
53494-70-5
NA
0.1 Mg/L
0.0033 mg/kg
NA
NA
NA
gamma-BHC (Lindane)
58-89-9
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
0.5 Mg/L
gamma-Chlordane
5103-74-2
NA
0.05 Mg/L
0.00167 mg/kg
NA
NA
NA
Heptachlor
76-44-8
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
0.5 Mg/L
Heptachlor epoxide
1024-57-3
0.05 Mg/L
0.05 Mg/L
0.00167 mg/kg
NA
NA
0.5 Mg/L
Methoxychlor
72-43-5
NA
0.5 Mg/L
0.0167 mg/kg
NA
NA
5.0 Mg/L
Toxaphene
8001-35-2
5 Mg/L
5 Mg/L
0.167 mg/kg
NA
NA
25.0 Mg/L
Aroclor-1016
12674-11-2
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1221
1104-28-2
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1232
11141-16-5
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1242
53469-21-9
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1248
12672-29-6
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1254
11097-69-1
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1260
11096-82-5
1 Mg/L
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1262
37324-23-5
NA
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
Aroclor-1268
11100-14-4
NA
1 Mg/L
0.033 mg/kg
1 mg/kg
1 Mg/wipe
NA
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 31 of 41
Appendix 4: Semivolatiles (SVOCs) Quantitation Limits (QLs)
Analyte(s)
CAS
Aqueous
Solid
Petroleum
PAH-SIM
TCLP
Number
EPA 625,
SW 8270D,
SW 3520C
SW 8270 D,
SW 8270D,
SW 8270 D
SW 8270D
SW 1311,
SW 3540C
SW 3580A
(Aqueous)
(Solids)
SW 8270D
1,1-BiphenyI *
92-52-4
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
1,2,4,5-Tetrachlorobenzene *
95-94-3
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
2,3,4,6-Tetrachlorophenol *
58-90-2
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
2,4,5-Trichlorophenol *
95-95-4
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
2,4,6-Trichlorophenol
88-06-2
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
2,4-Dichlorophenol
120-83-2
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
2,4-Dimethylphenol *
105-67-9
5 ng/L
670 ng/kg
200 mg/kg
NA
NA
NA
2,4-Dinitrophenol
51-28-5
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
2,4-Dinitrotoluene
121-14-2
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
2,6-Dinitrotoluene
606-20-2
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
2-Chloronaphthalene
91-58-7
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
2-Chlorophenol
95-57-8
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
2-Methylnaphthalene *
91-57-6
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
2-Methylphenol *
95-48-7
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
2-Nitroaniline *
88-74-4
5 ng/L
670 ng/kg
200 mg/kg
NA
NA
NA
2-Nitrophenol
88-75-5
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
3,3 -Dichlorobenzidine
91-94-1
5 ng/L
670 ng/kg
200 mg/kg
NA
NA
NA
3-Methylphenol K
108-39-4
NA
NA
NA
NA
NA
0.1 mg/L
3-Nitroaniline *
99-09-2
5 ng/L
670 Mg/kg
200 mg/kg
NA
NA
NA
4,6-Dinitxo-2-methyIphenoI
534-52-1
10 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
4-Bromophenyl phenyl ether
101-55-3
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
4-Chloro-3-methylphenol
59-50-7
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
4-Chloroaniline *
106-47-8
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
4-Chlorophenyl phenyl
ether
7005-72-3
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
4-Methylphenol *A
106-44-5
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.1 mg/L
4-Nitroaniline *
100-01-6
5 ng/L
670 Mg/kg
200 mg/kg
NA
NA
NA
4-Nitrophenol
100-02-7
10 ng/L
670 Mg/kg
200 mg/kg
NA
NA
NA
Acenaphthene
83-32-9
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Acenaphthylene
208-96-8
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
* Not an EPA 625 compound
X
These compounds either coelute or cannot be separated during the analysis.
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 32 of 41
Appendix 4: Semivolatiles (SVOCs) Quantitation Limits (QLs) (cont.)
Analyte(s)
CAS
Number
Aqueous
Solid
Petroleum
PAH-SIM
TCLP
EPA 625,
SW 8270D,
SW 3520C
SW 8270 D,
SW 3540C
SW 8270D,
SW 3580A
SW 8270D
(Aqueous)
SW 8270D
(Solids)
SW 1311,
SW 8270D
Acetophenone *
98-86-2
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Anthracene
120-12-7
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Atrazine *
1912-24-9
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Benzaldehyde *
100-52-7
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Benzo(a)anthracene
56-55-3
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Benzo(a)pyrene
50-32-8
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Benzo(b)fIuoranthene
205-99-2
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Benzo(ghi)perylene
191-24-2
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Benzo(k)fIuoranthene
207-08-9
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Bis(2-chloroethoxy)methane
111-91-1
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Bis(2-chIoroethyI)ether
111-44-4
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Bis(2-chIoroisopropyI)ether
108-60-1
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Bis(2-ethylhexyl)phthalate
117-81-7
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Butyl benzyl phthalate
85-68-7
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Caprolactam *
105-60-2
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Carbazole *
86-74-8
5 ng/L
670 ng/kg
200 mg/kg
NA
NA
NA
Chrysene
218-01-9
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Dibenz(a,h)anthracene
53-70-3
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Dibenzofuran *
132-64-9
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Diethyl phthalate
84-66-2
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
Dimethyl phthalate
131-11-3
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Di-n-butyl phthalate
84-74-2
5 ng/L
670 Mg/kg
200 mg/kg
NA
NA
NA
Di-n-octyl phthalate
117-84-0
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Fluoranthene
206-44-0
5 ng/L
330 ng/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Fluorene
86-73-7
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Hexachlorobenzene
118-74-1
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
Hexachlorobutadiene
87-68-3
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
0.05 mg/L
Hexachlorocyclopentadiene
77-47-4
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
Hexachloroethane
67-72-1
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
lndeno(l,2,3-cd)pyrene
193-39-5
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Isophorone
78-59-1
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
* Not an EPA 625 compound
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 33 of 41
Appendix 4: Semivolatiles (SVOCs) Quantitation Limits (QLs) (cont.)
Analyte(s)
CAS
Number
Aqueous
Solid
Petroleum
PAH-SIM
TCLP
EPA 625,
SW 8270D,
SW 3520C
SW 8270 D,
SW 3540C
SW 8270D,
SW 3580A
SW 8270D
(Aqueous)
SW 8270D
(Solids)
SW 1311,
SW 8270D
Naphthalene
91-20-3
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Nitrobenzene
98-95-3
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
0.05 mg/L
N-Nitrosodimethylamine
62-75-9
5 ng/L
330 ng/kg
100 mg/kg
NA
NA
NA
N-Nitroso-di-n-propylamine
621-64-7
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
NA
N-Nitrosodiphenylamine
86-30-6
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
0.05 mg/L
Pentachlorophenol
87-86-5
5 ng/L
670 Mg/kg
200 mg/kg
NA
NA
NA
Phenanthrene
85-01-8
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Phenol
108-95-2
5 ng/L
330 Mg/kg
100 mg/kg
NA
NA
0.05 mg/L
Pyrene
129-00-0
5 ng/L
330 Mg/kg
100 mg/kg
0.1 ng/L
7 Mg/kg
NA
Pyridine r
110-86-1
NA
NA
NA
NA
NA
0.5 mg/L
1 Not an EPA 625 compound and TO P compounds only
-------
OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 34 of 41
Appendix 5: Volatile* (VOCs) Quantitation Limits (QLs)
Analyte(s)
CAS
Number
Aqueous
Solid
Air
Petroleum
TCLP
CLP
Equivalent
(Trace)
EPA 624,
SW 8260C,
SW 5030C
(Mid)
SW 8260C,
SW 5030C,
SW 5035A
TO-15
SW 8260C,
SW 5030C
SW 1311,
SW 8260C,
SW 5030C
1,1,1,2-Tetrachloroethane
630-20-6
0.5 ng/L
5 Mg/L
5 M-g/kg
NA
12.5 mg/kg
NA
1,1,1-Trichloroethane
71-55-6
0.5 ng/L
5 Mg/L
5 M-g/kg
0.5 ppbv
12.5 mg/kg
NA
1,1,2,2-Tetrachloroethane
79-34-5
0.5 ng/L
5 Mg/L
5 M-g/kg
0.5 ppbv
12.5 mg/kg
NA
1,1,2-Trichloroethane
79-00-5
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,1-Dichloroethane
75-34-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,1-Dichloroethene
75-35-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
1,1-Dichloropropene
563-58-6
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
1,2,3-Trichlorobenzene
87-61-6
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
1,2,3-Trichloropropane
96-18-4
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
1,2,4-Trichlorobenzene
120-82-1
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,2,4-Trimethylbenzene
95-63-6
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
l,2-Dibromo-3-chloropropane
96-12-8
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
1,2-Dibromoethane (EDB)
106-93-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,2-Dichlorobenzene
95-50-1
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,2-Dichloroethane
107-06-2
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
1,2-Dichloropropane
78-87-5
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,3,5-Trimethylbenzene
108-67-8
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,3-Butadiene
106-99-0
NA
NA
NA
0.5 ppbv
NA
NA
1,3-Dichlorobenzene
541-73-1
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
1,3-Dichloropropane
142-28-9
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
1,4-Dichlorobenzene
106-46-7
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
1,4-Dioxane
123-91-1
NA
NA
NA
0.5 ppbv
NA
NA
2,2-Dichloropropane
594-20-7
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
2-Butanone
78-93-3
2 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
2-Chloroethylvinyl ether
110-75-8
NA
NA
5 Mg/kg
NA
12.5 mg/kg
NA
2-Chlorotoluene
95-49-8
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
2-Hexanone
591-78-6
2 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
4-Chlorotoluene
106-43-4
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
4-Ethyltoluene
622-96-8
NA
NA
NA
0.5 ppbv
NA
NA
4-Methyl-2-pentanone
108-10-1
2 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
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January 29, 2014
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Appendix 5: Volatile* (VOCs) Quantitation Limits (QLs) (cont.)
Analyte(s)
CAS
Number
Aqueous
Solid
Air
Petroleum
TCLP
CLP
Equivalent
(Trace)
EPA 624,
SW 8260C,
SW 5030C
(Mid)
SW 8260C,
SW 5030C,
SW 5035A
TO-15
SW 8260C,
SW 5030C
SW 1311,
SW 8260C,
SW 5030C
Acetone
67-64-1
2 ng/L
5 Mg/L
10 ng/kg
0.5 ppbv
12.5 mg/kg
NA
Benzene
71-43-2
0.5 ng/L
5 Mg/L
5 M-g/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Benzyl chloride
100-44-7
NA
NA
NA
0.5 ppbv
NA
NA
Bromobenzene
108-86-1
0.5 ng/L
5 Mg/L
5 M-g/kg
NA
12.5 mg/kg
NA
Bromochloromethane
74-97-5
0.5 ng/L
5 Mg/L
5 M-g/kg
NA
12.5 mg/kg
NA
Bromodichloromethane
75-27-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Bromoform
75-25-2
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Bromomethane
74-83-9
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Carbon disulfide
75-15-0
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Carbon Tetrachloride
56-23-5
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Chlorobenzene
108-90-7
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Chlorodibromomethane
124-48-1
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Chloroethane
75-00-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Chloroform
67-66-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Chloromethane
74-87-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
cis-l,2-Dichloroethene
156-59-2
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
cis-l,3-Dichloropropene
10061-01-5
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Cyclohexane
110-82-7
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Dibromomethane
74-95-3
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Dibromochloromethane
124-48-1
NA
NA
NA
0.5 ppbv
NA
NA
Dichlorodifluoromethane
75-71-8
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Dichlorotetrafluoroethane
76-14-2
NA
NA
NA
0.5 ppbv
NA
NA
Ethanol
64-17-5
NA
NA
NA
0.5 ppbv
NA
NA
Ethyl Acetate
141-78-6
NA
NA
NA
0.5 ppbv
NA
NA
Ethylbenzene
100-41-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Freon 113
76-13-1
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Heptane
142-82-5
NA
NA
NA
0.5 ppbv
NA
NA
Hexachlorobutadiene
87-68-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Hexane
110-54-3
NA
NA
NA
0.5 ppbv
NA
NA
Isopropyl alcohol
67-63-0
NA
NA
NA
0.5 ppbv
NA
NA
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January 29, 2014
Page 36 of 41
Appendix 5: Volatile* (VOCs) Quantitation Limits (QLs) (cont.)
Analyte(s)
CAS
Number
Aqueous
Solid
Air
Petroleum
TCLP
CLP
Equivalent
(Trace)
EPA 624,
SW 8260C,
SW 5030C
(Mid)
SW 8260C,
SW 5030C,
SW 5035A
TO-15
SW 8260C,
SW 5030C
SW 1311,
SW 8260C,
SW 5030C
Isopropylbenzene
98-82-8
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Methyl Acetate
76-20-9
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Methylcyclohexane
108-87-2
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Methylene Chloride
75-09-2
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Methyl-tert-butyl ether
1634-04-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
m-Xylene
p-Xylene
108-38-3
106-42-3
1 Mg/L
10 Mg/L
10 Mg/kg
1 ppbv
25 mg/kg
NA
Naphthalene
91-20-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
n-Butylbenzene
104-51-8
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
n-Propylbenzene
103-65-1
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
o-Xylene
95-47-6
1 M-g/L
10 Mg/L
10 Mg/kg
0.5 ppbv
25 mg/kg
NA
p-lsopropyltoluene
99-87-6
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Propylene
115-07-1
NA
NA
NA
0.5 ppbv
NA
NA
sec-Butylbenzene
135-98-8
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Styrene
100-42-5
1 M-g/L
10 Mg/L
10 Mg/kg
0.5 ppbv
25 mg/kg
NA
tert-Butylbenzene
98-06-6
0.5 ng/L
5 Mg/L
5 Mg/kg
NA
12.5 mg/kg
NA
Tetrachloroethene
127-18-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Tetrahydrofuran
109-99-9
NA
NA
NA
0.5 ppbv
NA
NA
Toluene
108-88-3
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
trans- 1,2-DichIoroethene
156-60-5
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
trans- 1,3-Dichloropropene
10061-02-6
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Trichloroethene
79-01-6
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
Trichlorofluoromethane
75-69-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Vinyl acetate
108-05-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
NA
Vinyl chloride
75-01-4
0.5 ng/L
5 Mg/L
5 Mg/kg
0.5 ppbv
12.5 mg/kg
0.005 mg/L
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January 29, 2014
Page 37 of 41
Appendix 6: Nitroaromatics/Nitramines/Explosives Quantitation Limits (QLs)
Analyte(s)
CAS
Number
Aqueous
Soil
Octahydro-l,3,5,7-tetranitro-l,3,5,7-tetrazocine (HMX)
2691-41-0
0.075 |ig/L
0.04 mg/kg
Hexahydro-l,3,5-trinitro-l,3,5-triazine (RDX)
121-82-4
0.075 |ig/L
0.04 mg/kg
1,3,5-Trinitrobenzene (1,3,5-TNB)
99-35-4
0.075 ug/L
0.04 mg/kg
1,3-Dinitrobenzene (1,3-DNB)
99-65-0
0.075 ug/L
0.04 mg/kg
Methyl-2,4/6-trinitrophenylnitramine (tetryl)
479-45-8
0.075 ug/L
0.04 mg/kg
Nitrobenzene (NB)
98-95-3
0.075 ug/L
0.04 mg/kg
2,4,6-Trinitrotoluene (2,4,6-TNT)
118-96-7
0.075 ug/L
0.04 mg/kg
4-Amino-2,6-dinitrotoluene (4-Am-DNT)
1946-51-0
0.075 ug/L
0.04 mg/kg
2-Amino-4,6-dinitrotoluene (2-Am-DNT)
35572-78-2
0.075 ug/L*
0.04 mg/kg
2,4-Dinitrotoluene (2,4-DNT)
121-14-2
0.15 |jg/L*
0.08 mg/kg
2,6-Dinitrotoluene (2,6-DNT)
606-20-2
0.15 ug/L
0.08 mg/kg
2-Nitrotoluene (2-NT)
88-72-2
0.075 fig/L
0.04 mg/kg
3-Nitrotoluene (3-NT)
99-08-1
0.075 ug/L
0.04 mg/kg
4-Nitrotoluene (4-NT)
99-99-0
0.075 fig/L
0.04 mg/kg
Nitroglycerine (NG) (On Demand only)
55-63-0
_
-
1,2-Dinitrobenzene (surrogate standard)
528-29-0
-
-
* Reported as cocluting isomers
Appendix 7: Sample Tag Example
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 38 of 41
Appendix 8: Chain of Custody Example
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CHAIN Of- CUSTODY RECORD
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 39 of 41
Appendix 9: Hazard and Risk Exposure Data Sheet
Region III, Office of Analytical Services and Quality Assurance
Ft Meade, Maryland
HAZARD AND RISK-EX POSH RE DATA SHEET
LEVELS OF PERSONAL PROTECTION DURING SAMPLING
BACKGROUND
Under the authority Section 104 of the Comprehensive Environmental Response, Compensation, and Liability
Act (CERCLA or Superfund) of 1980, Section 311 of the Clean Water Act, and Subtitle I of the Resource
Conservation and Recovery Act (RCRA), EPA has been delegated the responsibility to undertake response
actions with respect to the release or potential release of oil, petroleum, or hazardous substances that pose a
substantial threat to human health or welfare, or the environment.
GENERAL
This form is to be used when collecting Environmental Samples (i.e. streams, farm ponds, wells, soils etc.) and
for Hazardous Sample (i.e. drums, storage tanks, lagoons, leachates, hazardous waste sites). This information
is intended for use as a guide for the safe handling of these laboratory samples in accordance with EPA and
OSHA regulations. The sample classification(s) and levels of personal protection used by the sampler in all
situations will enable the analyst to be better aware of potential exposure to substances in air, splashes of
liquids, or other direct contact with material due to work being done.
DEGREE OF PROTECTION
Level A: Highest level of respiratory, skin, and eye protection needed. Fully encapsulated suit, respirator
self-contained (Tank type).
Level B: Highest level of respiratory protection but lesser level of skin protection needed. Chemical suit,
respirator self-contained (Tank type).
Level C: Lesser level of respiratory protection than Level B. Skin protection criteria are similar to Level B.
Chemical suit, canister respirator/cartridge
Level D: Work uniform without any respirator or skin hazards. Lab coat, gloves etc.
CLASSIFIED FIELD SAMPLES
. Environmental Hazardous Comb. (Env. & Haz.) Radioactive
Site Name: Sampling Date:
Station No. , , , , ,
Field pH: , , , , ,
(must be taken prior to submission of aqueous samples)
Sampler: Work Phone Number:
Personal observations at time of sampling (surroundings):
Sample collection observations (physical sample, odors etc.):
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OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 40 of 41
Appendix 10: OASQA Sample Acceptance Policy
OASQA Sample Acceptance Policy
The following are those conditions which indicate that the integrity of the sample may have been
jeopardized, either during the actual sampling event or during its shipment to the lab. If one or more of these
conditions exist, the laboratory will consult with the requester to determine whether to reject the sample(s)
for analysis or to perform a qualified analysis. If the sample(s) is (are) rejected, the sampler will be given the
opportunity to resample. If the analysis is performed, the data will be reported with qualifiers explaining
why the data may have been compromised, and the potential impact on the data. In some cases it may be
possible for the laboratory to complete the analysis with some adjustments. For example, if there is
insufficient sample volume, the data may have to be reported with increased quantitation limits or the
requestor may be asked to prioritize analytical requests.
The condition of sample(s) and shipment will be documented on the OASQA Shipment Documentation
Form. The Sample Scheduling Coordinator may request a Letter-To-File from the sampler to document
additional critical details. Any actions taken because of the compromised condition of a sample will be
noted in the laboratory's information management database and in the report narrative sent to the requester.
Conditions which may jeopardize the integrity of the sample:
• Not collected in appropriate containers.
• If cooling is required for the requested analytes, samples are received at greater than 6 degrees C or
missing the temperature blank.
• Not properly preserved as outlined in Tables 1, 2, and/or 3 of the OASQA Sample Submission
Procedures.
• Received past the analytical holding time.
• Samples tampered with during shipment. (Example: custody seal has been broken)
• Insufficient sample to perform sample analysis or the quality control analysis.
• Sample identification incorrect, incomplete, or missing.
• Chain-of-custody documentation not available, inaccurate or incomplete.
• Samples inappropriate for requested analysis. (Example: decomposed condition)
• Leaking or broken container.
• Lack of a trip blank with samples collected for volatile analysis.
• Not completing the Hazard and Risk Exposure Data Sheet.
NOTE: One other condition which would cause samples to be rejected by OASQA is if the samples are
suspected to contain dioxin or radioactivity. At this time, this facility is not prepared to handle the potential
hazard of dioxin contamination.
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January 29, 2014
Page 41 of 41
Appendix 11: Region III 5035A Fact Sheet
Region III 5035A Fact Sheet
May 15, 2003, Revision No: 2
Field Samplers Guide to the Collection and Handling of Soil Samples for
Volatile Organic Analysis using SYV 846 Method 5035A, July 2002
Summary:
The purpose of this fact sheet is to specify procedures for the collection and handling by field samplers of
soil samples for volatile organic analysis (VOA) in Region III. SW-846 Method 5035A is the collection
method required for analysis of soil samples for VOA. This method incorporates chemical preservatives and
sample storage techniques to limit volatilization and biodegradation of organic compounds. Method 5035A
is applicable to both low/medium and high level soil samples.
Collection Procedures:
• Soil samples being analyzed for volatile organic compounds collected via Method 5035A should not be
chemically preserved in the field.
• Samples should be collected using the following collection options:
Option 1: For most Soil types
Number of samples: 4 EnCore (or similar closed-sampling vessel) samplers
4 QC EnCore samplers
1x40 ml. vial for moisture analysis
EnCore samplers (or similar sample collection device, refer to Section 6.5 of Method 5035 A)
Samples must be cool, < 6°C upon collection and during shipment and bagged individually upon collection.
Samples must arrive at the laboratory within 24 hours.
Samples must be analyzed or preserved by the lab within 48 hours of collection.
Option 2: For Non-Cohesive Granular Material (wet, rocky, sediments, etc,)
Number of samples: 4x40 ml. vials (sampler may use wide mouth jars if sample
not amenable to smaller vials)
2 QC 40 m 1. vials
1x40 ml. vial for moisture analysis
Samples must be cool, < 6°C upon collection and during shipment.
Samples must arrive at the laboratory within 24 hours.
Samples must be analyzed or preserved by the lab within 48 hours of collection.
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