OASQA Sample Submission Procedures Rev. 13.

0
January 29, 2014
Page 1 of 41

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
 OASQA Sample Submissio n Procedures Rev. I 3.0
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Sample Submission Procedures for OASQA Laboratory Branch

Issued hy the Office of Analytical Services & Quality Assurance

(OASQA)
Eftl!ctive Date: January 29,2014 Number: Revision 13

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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 (cont.)

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/Explosives 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 III 5035A Fact Sheet 41
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1.0 Introduction

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) [Link]@[Link]

Brandon McDonald: 410-305-2607 (ph), 410-305-3095 (fax) [Link]@[Link]
Jay Burman: 410-305-2743 (ph), 410-305-3095 (fax) [Link]@[Link]
Ed Messer: 410-305-2744 (ph), 410-305-3095 (fax) [Link]@[Link]

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) [Link]@[Link]

Dan Slizys: 410-305-2734 (ph), 410-305-3095 (fax) [Link]@[Link]

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:

[Link]

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 (MSD) - 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 HPLC water is
not acceptable for most blank uses. HPLC 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 Hach 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.

4.0 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 (COC) - 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
l) 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.

8.0 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 (IATA) 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., NaOH pellets, HCL, 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, OSHA, 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 headspace 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 changed/canceled, 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), [Link]@[Link]

Secondary Contacts
John Curry: 410-305-2608 (ph), 410-305-3093 (fax), [Link]@[Link]

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.

[Link]

11.2 EPA Region 3, Analytical Request Form Instructions.

[Link]

11.3 EPA Region 3, Laboratory Quality Manual, revision 9.

11.4 International Air Transport Authority (IATA), Dangerous Goods Regulations.

[Link]

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 (NELAC) Standards.

[Link]

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.

[Link]
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Table 1 Aqueous Sample Requirements
Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Volume (min)
Preservation Limits (QLs)

Alcohols
Ethanol 10 mg/L
Methanol (5) 10 mg/L
GC-FID G, C V cool, ≤ 6 °C 7 days 10 mL SW 8015D
1-Propanol 10 mg/L
1-Butanol 10 mg/L
Sec-Butanol 10 mg/L

Alkalinity (Total) 20 mg/L

Bicarbonate (5) 20 mg/L
Titration G, C P cool, ≤ 6 °C 14 days 500 mL SM 2320B
Carbonate 20 mg/L
P-Alkalinity 20 mg/L

Anions
Bromide 0.50 mg/L
Chloride 0.25 mg/L
Fluoride Ion 28 days 0.10 mg/L
G, C GL, P cool, ≤ 6 °C (5) 200 mL EPA 300.0
Sulfate Chromatography 48 hrs (9) 0.50 mg/L
Nitrite (9) 0.05 mg/L 1
Nitrate (9) 0.15 mg/L 1
Orthophosphate (9, 36) 0.5 mg/L1

Ammonia (not distilled) Automated cool, ≤ 6 °C (5)

G, C GL, P 28 days 200 mL SM 4500-NH3 BG 0.04 mg/L
(Total) Colorimetric H2SO4 to pH<2

Biochemical Oxygen Demand (BOD5)

DO probe G, C GL, P cool, ≤ 6 °C (5) 48 hrs 500 mL SM 5210B 4 mg/L
Carbonaceous (CBOD)

cool, ≤ 6 °C (5)
Chemical Oxygen Demand (COD) Spectrophotometric G, C GL, P 28 days 200 mL HACH 8000 10 mg/L
H2SO4 to pH<2

Corrosivity
Electrometric G, C P None ASAP 500 mL SW 9040C NA
(pH for ≥ 20% water)
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Table 1 Aqueous Sample Requirements (cont.)
Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Volume (min)
Preservation Limits (QLs)

cool, ≤ 6 °C (5)
Cyanide Distillation,
G GL, P Dechlorinate (30k) then 14 days 200 mL EPA 335.4 0.02 mg/L
(Total) Automated
NaOH to pH>10

Glycols
2-Butoxyethanol 25 μg/L
SW 8321 mod
Diethylene Glycol HPLC/MS/MS G, C V cool, < 6 °C (5) 14 days 40 mL 25 μg/L
ASTM D7731-11 mod
Triethylene Glycol 25 μg/L
Tetraethylene Glycol 25 μg/L

Both EPA 200.7 and

Hardness (calculation) ICP + calculation G, C GL, P HNO3 to pH<2 (8) 6 months 200 mL 3300 μg/L
SM 2340B

cool, ≤ 6 °C (5) 10 μg/L (26)

Ion (14)
Hexavalent Chromium G P pH of 9.3 - 9.7 with 28 days 200 mL EPA 218.6 or
Chromatography
(NH4)2SO4 1.0 μg/L (27)

Pensky-Martens,
Ignitability G SWJ None ASAP 250 mL SW 1010A NA
closed cup

FTIR, GC-FTIR,
Infrared (IR) screen G, C GL, P cool, ≤ 6 °C (5) ASAP 100 mL IR identification scan NA
GC/MS

Lab pH
Electronic G P None ASAP 500 mL SW 9040C NA
(for ≥ 20% water)

EPA 245.1,
Mercury Cold Vapor
G, C GL, P HNO3 to pH<2 (8) 28 days 250 mL SW 7470A, 0.2 μg/L
(Dissolved (14) and Total) Spectrometry
CLP Equivalent

TCLP; Cold Vapor SW 1311,

Mercury - TCLP G, C GL, P cool, ≤ 6 °C (7) 28 days 1000 mL 0.2 mg/L
Spectrometry SW 7470A
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Table 1 Aqueous Sample Requirements (cont.)
Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Volume (min)
Preservation Limits (QLs)

EPA 200.7,
EPA 200.8,
Metals Refer to
ICP, ICP/MS G, C GL, P (24) HNO3 to pH<2 (8) 6 months 250 mL SW 6010B,
(Dissolved (14) and Total) Appendix 2
SW 6020A,
CLP Equivalent

SW 1311, Refer to
Metals - TCLP TCLP; ICP G, C GL, P cool, ≤ 6 °C (7) 180 days 1000 mL
SW 6010B Appendix 2

Automated cool, ≤ 6 °C (5)

Total Kjeldahl Nitrogen (TKN) G, C GL, P 28 days 200 mL EPA 351.2 0.1 mg/L
colorimetric H2SO4 to pH<2

EPA 353.2
Automated cool, ≤ 6 °C (5)
Nitrite + Nitrate G, C GL, P 28 days 250 mL (Use if EPA 300 0.05 mg/L
colorimetric H2SO4 to pH<2
isn’t an option)

Nitrogen (TN) - digested Automated cool, ≤ 6 °C (5)

G, C GL, P 28 days 250 mL EPA 353.2 1 mg/L
(Total) colorimetric H2SO4 to pH<2

Nitroaromatics, Nitramines, and Refer to

HPLC/PDA G, C AGL cool, ≤ 6 °C (5, 30h) 7 days 1000 mL (4) SW 8330
Explosives Appendix 6

Solid phase cool, ≤ 6 °C (5) 2x1000 mL

Oil & Grease G WGL 28 days EPA 1664A 5 mg/L
extraction HCl to pH<2 per sample(4)

IC Conductivity EPA 314.0 (IC) 1 μg/L (IC)

cool, ≤ 6 °C (6)
Perchlorate or G, C GL, P 28 days 100 mL or or
with headspace
LC/MS SW 6850 (LC/MS) 0.5 μg/L (LC/MS)
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Table 1 Aqueous Sample Requirements (cont.)
Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Volume (min)
Preservation Limits (QLs)

Percent water Wet Chemistry G, C P None ASAP 200 mL SW 9001 NA

Cont L/L extraction;

PCB Congeners G AGL cool, ≤ 6 °C (5, 30h) 1 year 1000 mL (4) EPA 1668C 20 pg/L
GC/MS

EPA 608,
Cont L/L extraction; Refer to
Pesticides G AGL cool, ≤ 6 °C (5, 30h) 7 days 1000 mL (4) SW 8081B,
GC/MS Appendix 3
SW 3520C

EPA 608,
Cont L/L extraction; Refer to
PCBs G AGL cool, ≤ 6 °C (5, 30h) 7 days 1000 mL (4) SW 8082A,
GC/MS Appendix 3
SW 3520C

EPA 608,
Cont L/L extraction; Refer to
Pesticides - TCLP G AGL cool, ≤ 6 °C (7) 14 days 1000 mL SW 8081B,
GC/MS Appendix 3
SW 3520C

cool, ≤ 6 °C (5)
Phenol Colorimetric -
G AGL Dechlorinate (30j) then 28 days 1000 mL EPA 420.1/420.4 20 µg/L
(Total) automated
H2SO4 to pH<2

Phosphorus (TP) Colorimetric - cool, ≤ 6 °C (5)

G, C GL, P 28 days 200 mL EPA 365.4 0.05 mg/L
(Total) automated HCl to pH<2

Polyaromatic Hydrocarbons Cont L/L extraction; SW 3520C, Refer to

G AGL cool, ≤ 6 ° C (5, 30h) 7 days 1000 mL (4)
(PAH-SIM) GC/MS SW 8270D Appendix 4

EPA 625,
(12) Cont L/L extraction; (5, 30h) (4) SW 8270D, Refer to
Semivolatiles (SVOCs) G AGL cool, ≤ 6 °C 7 days 1000 mL
GC/MS SW 3520C, Appendix 4
CLP Equivalent
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Table 1 Aqueous Sample Requirements (cont.)
Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Volume (min)
Preservation Limits (QLs)

SW 1311, Refer to
Semivolatiles (SVOCs) (12) - TCLP TCLP; GC/MS G AGL cool, ≤ 6 °C (5, 7) 14 days 1000 mL
SW 8270D 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) Combustion, cool, ≤ 6 °C (5)

G, C GL, P 28 days 100 mL SM 5310B 3 mg/L
Dissolved Organic Carbon (DOC) (14) Oxidation H2SO4 to pH<2

Total Suspended Solids (TSS) Gravimetric G, C GL, P cool, ≤ 6 °C (5) 7 days 500 mL SM 2540D 10 mg/L (11)

Refer to
Total Toxic Organics (TTO) Follow the same requirements for PCB/Pesticides, SVOCs, and VOCs
Appendix 3, 4, 5

EPA 624,
cool, ≤ 6 °C (5)
(12) Purge & Trap 7 days (20) SW 5030C, Refer to
Volatiles (VOCs) G V Dechlorinate (30h) then 120 mL (33)
extraction, GC/MS 14 days (21) SW 8260C, Appendix 5
1:1 HCl to pH<2(31)
CLP Equivalent

SW 1311,
Purge & Trap Refer to
Volatiles (VOCs) - TCLP/ZHE G V cool, ≤ 6 °C (5) 14 days 160 mL (32) SW 5030C,
extraction, GC/MS Appendix 5
SW 8260C
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Table 2 Non-Aqueous Sample Requirements

Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Weight (min)
Preservation Limits (QLs)

Anions
Bromide 0.1 mg/kg
Chloride 0.1 mg/kg
Fluoride Ion 0.1 mg/kg
G, C GL cool, ≤ 6 °C None 50 g EPA 300.0
Sulfate Chromatography 0.1 mg/kg
Nitrite 0.1 mg/kg
Nitrate 0.1 mg/kg
Orthophosphate 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 Distillation,
G GL cool, ≤ 6 °C 28 days 100 g EPA 335.4 1 mg/kg
(Total) Automated

Report as %silt,
EMAP Estuaries,
Grainsize Gravimetric G SWJ cool, ≤ 6 °C None 50 g %sand, and
Plumb 1981
%clay

cool, ≤ 6 °C
Ion
Hexavalent Chromium G GL pH of 9 ± 0.5 with 30 days 50 g EPA 218.6 10 mg/L
Chromatography
NH4OH

Pensky-Martens,
Ignitability G SWJ cool, ≤ 6 °C ASAP 50 g SW 1030 NA
closed cup

FTIR, GC-FTIR,
Infrared (IR) screen G, C GL cool, ≤ 6 °C ASAP 50 g IR identification scan NA
GC/MS
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Table 2 Non-Aqueous Sample Requirements (cont.)

Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Weight (min)
Preservation Limits (QLs)

Lab pH Electronic G GL None ASAP 200 g SW 9045D NA

EPA 245.5,
Mercury Cold Vapor
G, C GL cool, ≤ 6 °C 28 days 50 g SW 7471A, 0.1 μg/g
(Solids) Spectrometry
CLP Equivalent

Mercury – TCLP TCLP; Cold Vapor SW 1311,

G, C SWJ cool, ≤ 6 °C 28 days 200 g 0.2 mg/L
(Solids) Spectrometry SW 7470A

EPA 200.7,
EPA 200.8,
Metals Refer to
ICP, ICP/MS G, C GL cool, ≤ 6 °C 6 months 50 g SW 6010B,
(Solids) Appendix 2
SW 6020A,
CLP Equivalent

Metals – TCLP SW 1311, Refer to

TCLP; ICP G, C SWJ cool, ≤ 6 °C 180 days 200 g
(Solids) SW 6010B Appendix 2

Nitroaromatics, Nitramines, and Refer to

HPLC/PDA G, C AWJ cool, ≤ 6 °C 14 days 50 g SW 8330
Explosives Appendix 6

EPA 314.0 (IC)

IC Conductivity,
Perchlorate G, C GL cool, ≤ 6 °C 28 days 50 g or 0.005 mg/kg
LC/MS
SW 6850 (LC/MS)

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
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Table 2 Non-Aqueous Sample Requirements (cont.)

Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Weight (min)
Preservation Limits (QLs)

Soxhlet extraction;
PCB Congeners G, C AWJ cool, ≤ 6 °C 1 year 100 g EPA 1668C 10 pg/g
GC/MS

ASE, SW 8082A,
PCB 100 g Refer to
Waste dilution; G, C AWJ cool, ≤ 6 °C 1 year SW 3545A,
(Solids/Tissue/Petroleum/Wipes) 10 g (15) Appendix 3
GC/ECD SW 3580A

Pesticides SW 8081B, Refer to

ASE; GC/ECD G, C AWJ cool, ≤ 6 °C 14 days 100 g
(Solids/Tissue) SW 3545A Appendix 3

Cont L/L extraction; SW 8081B, Refer to

Pesticides - TCLP G, C AWJ cool, ≤ 6 °C 7 days 250 g
GC/ECD SW 3520C Appendix 3

Phenol Colorimetric -
G, C GL cool, ≤ 6 °C 28 days 50 g EPA 420.1/420.4 10 mg/kg
(Total) automated

Phosphorus (TP) Colorimetric -

G, C GL cool, ≤ 6 °C 28 days 50 g EPA 365.4 0.050 mg/L
(Total) automated

Polyaromatic Hydrocarbons Soxhlet extraction; SW 8270D, Refer to

G, C AWJ cool, ≤ 6 °C 14 days 50 g
(PAH-SIM) GC/MS SW 3520C Appendix 4

SW 8270D,
Semivolatiles (SVOCs) (12) Soxhlet extraction; 10 days (17) Refer to
G, C AWJ cool, ≤ 6 °C 100 g SW 3540C (solids),
(Solids/Petroleum) GC/MS 14 days (16) Appendix 4
SW 3580A (petroleum)

SW 1311, Refer to
Semivolatiles (SVOCs) (12) - TCLP TCLP; GC/MS G, C AWJ cool, ≤ 6 °C 14 days 200 g
SW 8270D Appendix 4
 OASQA Sample Submission Procedures Rev. 13.0
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Table 2 Non-Aqueous Sample Requirements (cont.)

Temperature Optimum
Parameter Analysis Collection Container Holding Sample
and Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s) Weight (min)
Preservation Limits (QLs)

Combustion,
Total Organic Carbon (TOC) G SWJ cool, ≤ 6 °C None 50 g SM 5310B 100 mg/kg
Oxidation

SW 5035A,
Volatiles (VOCs) (12) Purge & Trap Refer to Refer to 14 days (15) Refer to Refer to
G SW 5030C,
(Solids/Petroleum) extraction, GC/MS Appendix 11 Appendix 11 48 hrs (29) Appendix 11 Appendix 5
SW 8260C

Volatiles (VOCs) (12) Purge & Trap Refer to

G, C S None 30 days 6L TO-15
(Air/Vapor) extraction, GC/MS Appendix 5

SW 1311,
Purge & Trap Refer to
Volatiles (VOCs) - TCLP/ZHE G V cool, ≤ 6 °C 14 days 160 g (32) SW 5030C,
extraction, GC/MS Appendix 5
SW 8260C
 OASQA Sample Submission Procedures Rev. 13.0
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Table 3 SDWA Program Special Requirements

Temperature Sample Optimum

Parameter Analysis Collection Container Holding
and Volume Method(s) (3) Quantitation
(Analyte) Technique Technique (1) Type (2) Time(s)
Preservation (min) Limits (QLs)

Coliforms 8 hrs, SM 9221 B (Total)

Micro G GL(23), PL(23) cool, < 10 °C (5, 30k) 120 mL (22) 2 MPN/100 mLs
(Total and Fecal) 30 hrs (18) SM 9221B,E (Fecal)

8 hrs,
E. coli Enzyme Substrate G PL(23) cool, < 10 °C (5, 30k) 120 mL (22) SM 9223 Colilert QT 1 MPN/100 mL
30 hrs (18)

Report only
E. Coli and Total Coliforms Micro G PL(23) cool, < 10 °C (5, 30k) 30 hrs 120 mL (22) SM 9223 Colisure
Presence/Absence

Heterotrophic
Heterotrophic Bacteria G GL(23), PL(23) cool, < 10 °C (5, 30k) 8 hrs 120 mL (22) SM 9215B 1 cfu/1 mL
Plate Count

Automated 14 days (34)

Nitrate (NO3-N) G GL, P cool, ≤ 6 °C (5) 200 mL EPA 300.0 0.15 mg/L
colorimetric 48 hrs (35)

Pesticides (Chlorinated)
Endrin cool, ≤ 6 °C (5) 0.02 μg/L
Solid phase
gamma-BHC (Lindane) G AGL Dechlorinate (30j) then 14 days 2000 mL (4) EPA 508.1 0.02 μg/L
extraction
Heptachlor epoxide 6N HCl to pH<2 0.02 μg/L

cool, ≤ 6 °C (5)
Purge & Trap
Total Trihalomethanes (TTHMs) G V Dechlorinate (30h) then 14 days 120 mL (33) EPA 524.2 0.5 μg/L
extraction, GC/MS
1:1 HCl to pH<2

cool, ≤ 6 °C (5)
Purge & Trap 14 days Refer to
Regulated Volatiles (VOCs) G V Dechlorinate (30h) then 120 mL (33) EPA 524.2
extraction, GC/MS 24 hrs (18) Appendix 5
1:1 HCl to pH<2
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Table 1, 2 and 3 Footnotes

C Composite only (sampling period must have a Start and Ending time)
G, C Grab or Composite
Grab only for:
G
1 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)
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
2
ASJ 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
AWJ 8 oz short, wide mouth, straight-sided, amber glass jar with Teflon lined cap
V 40 mL clear glass VOA vial
TGL 4 oz (120 mL) tall, wide mouth, straight-sided, glass jar
PB Heavy plastic bag
S Summa canisters (supplied by lab)
SM Standard Methods
3 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 - Na2SO4
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Table 1, 2 and 3 Footnotes (cont.)

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 25μL Sample Injection Loop size
27 On a 250μL Sample Injection Loop size
28 If water has been chlorinated, use 0.2 mL of sterile 10% Na2S2O3 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 – C6H8O6
30 h) With Ascorbic acid – C6H8O6 (25 mg per 40 mL); or Sodium Thiosulfate – Na2S2O3
(3 mg per 40 mL)
j) With excess Ferrous Ammonium Sulfate – (NH4)2Fe(SO4)2 * 6H2O
RCRA and NPDES sample(s) must be submitted both preserved and unpreserved if 2-Chloroethyl
31 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 mL VOA vials for 160 mL of sample filled with no headspace.
33 Three (3) glass 40 mL VOA vials for 120 mL of sample filled with no headspace.
34 Chlorinated
35 Non-chlorinated
36 Filter in the field if for NPDES
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Appendix 1: Quality Control (QC) Sampling Requirements

Additional Volume or Weight

Parameter Matrix required of that in
Tables 1 – 3
(a)
Biochemical Oxygen Demand (BOD5) Aqueous 500 mL
(a)
Glycols Aqueous 2x40 mL
(a)
Aqueous 40 mL
(b)
Solids 100 g
IR Identification (b)
Wipes 1 blank wipe
(b)
Petroleum 20 g of material
(a)
Aqueous 25 mL
Mercury (b)
Wipes 3 blank wipes
(a)
Aqueous 2x1000 mL
Nitroaromatics, Nitramines, and Explosives (b)
Soil 100 g
(a)
Oil & Grease Aqueous 3x1000 mL
(a)
PCB Congeners Aqueous 4x1000 mL
(a)
Aqueous 2x100 mL
Perchlorate (b)
Soil 100 g
(a)
Phenol (Total) Aqueous 1000 mL
(c)
Pesticides (Chlorinated) Aqueous 2x1000 mL
(a)
Aqueous 2x1000 mL
Pesticides (b)
Solids 60 g
(a)
Pesticides/PCBs Aqueous 4x1000 mL
(a)
Aqueous 2x1000 mL
(b)
Solids 60 g
PCBs (b)
Petroleum 10 g of material
(b)
Wipes 1 blank; 2 duplicates
(a)
Aqueous 2x1000 mL
Semi Volatiles (SVOCs) (b)
Solids 60 g
(a, c)
Volatiles (VOCs) Aqueous 6x40 mL

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
 OASQA Sample Submission Procedures Rev. 13.0
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Appendix 2: Metals Quantitation Limits (QLs)

CAS Aqueous Solids TCLP

Analyte(s)
Number
ICP ICP/MS ICP ICP/MS ICP

Aluminum 7429-90-5 200 μg/L 30 μg/L 20 μg/g 3 μg/g NA

Antimony 7440-36-0 60 μg/L 2 μg/L 6 μg/g 0.2 μg/g NA
Arsenic 7440-38-2 200 μg/L 1 μg/L 20 μg/g 0.1 μg/g 5 mg/L
Barium 7440-39-3 200 μg/L 10 μg/L 20 μg/g 1 μg/g 100 mg/L
Beryllium 7440-41-7 5 μg/L 1 μg/L 0.5 μg/g 0.1 μg/g NA
Boron 7440-42-8 50 μg/L NA 5 μg/g NA NA
Cadmium 7440-43-9 5 μg/L 1 μg/L 0.5 μg/g 0.1 μg/g 1 mg/L
Calcium 7440-70-2 500 μg/L NA 50 μg/g NA NA
Chromium 7440-47-3 10 μg/L 2 μg/L 1 μg/g 0.2 μg/g 5 mg/L
Cobalt 7440-48-4 50 μg/L 1 μg/L 5 μg/g 0.1 μg/g NA
Copper 7440-50-8 25 μg/L 2 μg/L 2.5 μg/g 0.2 μg/g NA
Iron 7439-89-6 100 μg/L NA 10 μg/g NA NA
Lead 7439-92-1 50 μg/L 1 μg/L 5 μg/g 0.1 μg/g 5 mg/L
Magnesium 7439-95-4 500 μg/L NA 50 μg/g NA NA
Manganese 7439-96-5 15 μg/L 1 μg/L 1.5 μg/g 0.1 μg/g NA
Nickel 7440-02-0 40 μg/L 1 μg/L 4 μg/g 0.1 μg/g NA
Potassium 7740-09-7 2000 μg/L NA 200 μg/g NA NA
Selenium 7782-49-2 200 μg/L 5 μg/L 20 μg/g 0.5 μg/g 1 mg/L
Silver 7440-22-4 10 μg/L 1 μg/L 1 μg/g 0.1 μg/g 5 mg/L
Sodium 7440-23-5 1000 μg/L NA 100 μg/g NA NA
Thallium 7440-28-0 200 μg/L 1 μg/L 20 μg/g 0.1 μg/g NA
Tin 7440-31-5 200 μg/L NA 20 μg/g NA NA
Titanium 7440-32-6 200 μg/L NA 20 μg/g NA NA
Vanadium 7440-62-2 50 μg/L 5 μg/L 5 μg/g 0.5 μg/g NA
Zinc 7440-66-6 20 μg/L 2 μg/L 2 μg/g 0.2 μg/g NA
 OASQA Sample Submission Procedures Rev. 13.0
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Appendix 3: Pesticides/PCBs Quantitation Limits (QLs) (PCBs→SW 8082A, Pesticides→SW 8081B)

Aqueous Solid/Tissue Petroleum Wipes TCLP

CAS
Analyte(s)
Number SW 8081B, SW 8081B, EPA 608,
SW 8082A, SW 8082A,
EPA 608 SW 8082A, SW 8082A, SW 8081B,
SW 3580A SW 3545A
SW 3520C SW 3545A SW 3520C
4,4´-DDD 72-54-8 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
4,4´-DDE 72-55-9 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
4,4´-DDT 50-29-3 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
Aldrin 309-00-2 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA NA
alpha-BHC 319-84-6 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA NA
alpha-Chlordane 5103-71-9 NA 0.05 μg/L 0.00167 mg/kg NA NA NA
beta-BHC 319-85-7 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA NA
Chlordane 57-74-9 1 μg/L 1 μg/L 0.033 mg/kg NA NA 5.0 μg/L
delta-BHC 319-86-8 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA NA
Dieldrin 60-57-1 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
Endosulfan I 959-98-8 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA NA
Endosulfan II 33213-65-9 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
Endosulfan sulfate 1031-07-8 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
Endrin 72-20-8 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA 1.0 μg/L
Endrin aldehyde 7421-93-4 0.1 μg/L 0.1 μg/L 0.0033 mg/kg NA NA NA
Endrin ketone 53494-70-5 NA 0.1 μg/L 0.0033 mg/kg NA NA NA
gamma-BHC (Lindane) 58-89-9 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA 0.5 μg/L
gamma-Chlordane 5103-74-2 NA 0.05 μg/L 0.00167 mg/kg NA NA NA
Heptachlor 76-44-8 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA 0.5 μg/L
Heptachlor epoxide 1024-57-3 0.05 μg/L 0.05 μg/L 0.00167 mg/kg NA NA 0.5 μg/L
Methoxychlor 72-43-5 NA 0.5 μg/L 0.0167 mg/kg NA NA 5.0 μg/L
Toxaphene 8001-35-2 5 μg/L 5 μg/L 0.167 mg/kg NA NA 25.0 μg/L
Aroclor-1016 12674-11-2 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1221 1104-28-2 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1232 11141-16-5 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1242 53469-21-9 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1248 12672-29-6 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1254 11097-69-1 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1260 11096-82-5 1 μg/L 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1262 37324-23-5 NA 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
Aroclor-1268 11100-14-4 NA 1 μg/L 0.033 mg/kg 1 mg/kg 1 μg/wipe NA
 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 31 of 41

Appendix 4: Semivolatiles (SVOCs) Quantitation Limits (QLs)

Aqueous Solid Petroleum PAH-SIM TCLP

CAS
Analyte(s)
Number EPA 625,
SW 8270D, SW 8270D, SW 8270D SW 8270D SW 1311,
SW 8270D,
SW 3540C SW 3580A (Aqueous) (Solids) SW 8270D
SW 3520C
1,1-Biphenyl * 92-52-4 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
1,2,4,5-Tetrachlorobenzene * 95-94-3 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2,3,4,6-Tetrachlorophenol * 58-90-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2,4,5-Trichlorophenol * 95-95-4 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
2,4,6-Trichlorophenol 88-06-2 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
2,4-Dichlorophenol 120-83-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2,4-Dimethylphenol * 105-67-9 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
2,4-Dinitrophenol 51-28-5 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2,4-Dinitrotoluene 121-14-2 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
2,6-Dinitrotoluene 606-20-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2-Chloronaphthalene 91-58-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2-Chlorophenol 95-57-8 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
2-Methylnaphthalene * 91-57-6 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
2-Methylphenol * 95-48-7 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
2-Nitroaniline * 88-74-4 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
2-Nitrophenol 88-75-5 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
3,3´-Dichlorobenzidine 91-94-1 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
λ
3-Methylphenol 108-39-4 NA NA NA NA NA 0.1 mg/L
3-Nitroaniline * 99-09-2 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
4,6-Dinitro-2-methylphenol 534-52-1 10 μg/L 330 μg/kg 100 mg/kg NA NA NA
4-Bromophenyl phenyl ether 101-55-3 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
4-Chloro-3-methylphenol 59-50-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
4-Chloroaniline * 106-47-8 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
4-Chlorophenyl phenyl
7005-72-3 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
ether
λ
4-Methylphenol * 106-44-5 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.1 mg/L
4-Nitroaniline * 100-01-6 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
4-Nitrophenol 100-02-7 10 μg/L 670 μg/kg 200 mg/kg NA NA NA
Acenaphthene 83-32-9 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Acenaphthylene 208-96-8 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA

* Not an EPA 625 compound

λ
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.)

Aqueous Solid Petroleum PAH-SIM TCLP

CAS
Analyte(s)
Number EPA 625,
SW 8270D, SW 8270D, SW 8270D SW 8270D SW 1311,
SW 8270D,
SW 3540C SW 3580A (Aqueous) (Solids) SW 8270D
SW 3520C
Acetophenone * 98-86-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Anthracene 120-12-7 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Atrazine * 1912-24-9 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Benzaldehyde * 100-52-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Benzo(a)anthracene 56-55-3 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Benzo(a)pyrene 50-32-8 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Benzo(b)fluoranthene 205-99-2 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Benzo(ghi)perylene 191-24-2 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Benzo(k)fluoranthene 207-08-9 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Bis(2-chloroethoxy)methane 111-91-1 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Bis(2-chloroethyl)ether 111-44-4 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Bis(2-chloroisopropyl)ether 108-60-1 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Bis(2-ethylhexyl)phthalate 117-81-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Butyl benzyl phthalate 85-68-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Caprolactam * 105-60-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Carbazole * 86-74-8 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
Chrysene 218-01-9 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Dibenz(a,h)anthracene 53-70-3 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Dibenzofuran * 132-64-9 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Diethyl phthalate 84-66-2 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Dimethyl phthalate 131-11-3 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Di-n-butyl phthalate 84-74-2 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
Di-n-octyl phthalate 117-84-0 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Fluoranthene 206-44-0 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Fluorene 86-73-7 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Hexachlorobenzene 118-74-1 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
Hexachlorobutadiene 87-68-3 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
Hexachlorocyclopentadiene 77-47-4 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
Hexachloroethane 67-72-1 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
Indeno(1,2,3-cd)pyrene 193-39-5 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Isophorone 78-59-1 5 μg/L 330 μg/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.)

Aqueous Solid Petroleum PAH-SIM TCLP

CAS
Analyte(s)
Number EPA 625,
SW 8270D, SW 8270D, SW 8270D SW 8270D SW 1311,
SW 8270D,
SW 3540C SW 3580A (Aqueous) (Solids) SW 8270D
SW 3520C
Naphthalene 91-20-3 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Nitrobenzene 98-95-3 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
N-Nitrosodimethylamine 62-75-9 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
N-Nitroso-di-n-propylamine 621-64-7 5 μg/L 330 μg/kg 100 mg/kg NA NA NA
N-Nitrosodiphenylamine 86-30-6 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
Pentachlorophenol 87-86-5 5 μg/L 670 μg/kg 200 mg/kg NA NA NA
Phenanthrene 85-01-8 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Phenol 108-95-2 5 μg/L 330 μg/kg 100 mg/kg NA NA 0.05 mg/L
Pyrene 129-00-0 5 μg/L 330 μg/kg 100 mg/kg 0.1 μg/L 7 μg/kg NA
Γ
Pyridine 110-86-1 NA NA NA NA NA 0.5 mg/L
Γ
Not an EPA 625 compound and TCLP compounds only
 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 34 of 41

Appendix 5: Volatiles (VOCs) Quantitation Limits (QLs)

Aqueous Solid Air Petroleum TCLP

CAS EPA 624,

Analyte(s) CLP SW 8260C, SW 1311,
Number SW 8260C, SW 8260C,
Equivalent SW 5030C, TO-15 SW 8260C,
SW 5030C SW 5030C
(Trace) SW 5035A SW 5030C
(Mid)
1,1,1,2-Tetrachloroethane 630-20-6 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,1,1-Trichloroethane 71-55-6 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,1,2,2-Tetrachloroethane 79-34-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,1,2-Trichloroethane 79-00-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,1-Dichloroethane 75-34-3 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,1-Dichloroethene 75-35-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
1,1-Dichloropropene 563-58-6 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,2,3-Trichlorobenzene 87-61-6 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,2,3-Trichloropropane 96-18-4 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,2,4-Trichlorobenzene 120-82-1 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,2,4-Trimethylbenzene 95-63-6 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,2-Dibromo-3-chloropropane 96-12-8 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,2-Dibromoethane (EDB) 106-93-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,2-Dichlorobenzene 95-50-1 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,2-Dichloroethane 107-06-2 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
1,2-Dichloropropane 78-87-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,3,5-Trimethylbenzene 108-67-8 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
1,3-Dichloropropane 142-28-9 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
1,4-Dichlorobenzene 106-46-7 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
2-Butanone 78-93-3 2 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
2-Chloroethylvinyl ether 110-75-8 NA NA 5 μg/kg NA 12.5 mg/kg NA
2-Chlorotoluene 95-49-8 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
2-Hexanone 591-78-6 2 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
4-Chlorotoluene 106-43-4 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 35 of 41

Appendix 5: Volatiles (VOCs) Quantitation Limits (QLs) (cont.)

Aqueous Solid Air Petroleum TCLP

CAS EPA 624,

Analyte(s) CLP SW 8260C, SW 1311,
Number SW 8260C, SW 8260C,
Equivalent SW 5030C, TO-15 SW 8260C,
SW 5030C SW 5030C
(Trace) SW 5035A SW 5030C
(Mid)
Acetone 67-64-1 2 μg/L 5 μg/L 10 μg/kg 0.5 ppbv 12.5 mg/kg NA
Benzene 71-43-2 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Bromochloromethane 74-97-5 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Bromodichloromethane 75-27-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Bromoform 75-25-2 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Bromomethane 74-83-9 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Carbon disulfide 75-15-0 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Carbon Tetrachloride 56-23-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
Chlorobenzene 108-90-7 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
Chlorodibromomethane 124-48-1 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Chloroethane 75-00-3 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Chloroform 67-66-3 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
Chloromethane 74-87-3 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
cis-1,2-Dichloroethene 156-59-2 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
cis-1,3-Dichloropropene 10061-01-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Cyclohexane 110-82-7 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Dibromomethane 74-95-3 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Freon 113 76-13-1 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/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
 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 36 of 41

Appendix 5: Volatiles (VOCs) Quantitation Limits (QLs) (cont.)

Aqueous Solid Air Petroleum TCLP

CAS EPA 624,

Analyte(s) CLP SW 8260C, SW 1311,
Number SW 8260C, SW 8260C,
Equivalent SW 5030C, TO-15 SW 8260C,
SW 5030C SW 5030C
(Trace) SW 5035A SW 5030C
(Mid)
Isopropylbenzene 98-82-8 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Methyl Acetate 76-20-9 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Methylcyclohexane 108-87-2 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Methylene Chloride 75-09-2 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Methyl-tert-butyl ether 1634-04-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
m-Xylene 108-38-3
1 μg/L 10 μg/L 10 μg/kg 1 ppbv 25 mg/kg NA
p-Xylene 106-42-3
Naphthalene 91-20-3 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
n-Butylbenzene 104-51-8 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
n-Propylbenzene 103-65-1 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
o-Xylene 95-47-6 1 μg/L 10 μg/L 10 μg/kg 0.5 ppbv 25 mg/kg NA
p-Isopropyltoluene 99-87-6 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Styrene 100-42-5 1 μg/L 10 μg/L 10 μg/kg 0.5 ppbv 25 mg/kg NA
tert-Butylbenzene 98-06-6 0.5 μg/L 5 μg/L 5 μg/kg NA 12.5 mg/kg NA
Tetrachloroethene 127-18-4 0.5 μg/L 5 μg/L 5 μg/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 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
trans-1,2-Dichloroethene 156-60-5 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
trans-1,3-Dichloropropene 10061-02-6 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Trichloroethene 79-01-6 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
Trichlorofluoromethane 75-69-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Vinyl acetate 108-05-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg NA
Vinyl chloride 75-01-4 0.5 μg/L 5 μg/L 5 μg/kg 0.5 ppbv 12.5 mg/kg 0.005 mg/L
 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 37 of 41

Appendix 6: Nitroaromatics/Nitramines/Explosives Quantitation Limits (QLs)

CAS
Analyte(s) Aqueous Soil
Number

Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) 2691-41-0 0.075 μg/L 0.04 mg/kg

Hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) 121-82-4 0.075 μg/L 0.04 mg/kg
1,3,5-Trinitrobenzene (1,3,5-TNB) 99-35-4 0.075 μg/L 0.04 mg/kg
1,3-Dinitrobenzene (1,3-DNB) 99-65-0 0.075 μg/L 0.04 mg/kg
Methyl-2,4,6-trinitrophenylnitramine (tetryl) 479-45-8 0.075 μg/L 0.04 mg/kg
Nitrobenzene (NB) 98-95-3 0.075 μg/L 0.04 mg/kg
2,4,6-Trinitrotoluene (2,4,6-TNT) 118-96-7 0.075 μg/L 0.04 mg/kg
4-Amino-2,6-dinitrotoluene (4-Am-DNT) 1946-51-0 0.075 μg/L 0.04 mg/kg
2-Amino-4,6-dinitrotoluene (2-Am-DNT) 35572-78-2 0.075 μg/L* 0.04 mg/kg
2,4-Dinitrotoluene (2,4-DNT) 121-14-2 0.15 μg/L* 0.08 mg/kg
2,6-Dinitrotoluene (2,6-DNT) 606-20-2 0.15 μg/L 0.08 mg/kg
2-Nitrotoluene (2-NT) 88-72-2 0.075 μg/L 0.04 mg/kg
3-Nitrotoluene (3-NT) 99-08-1 0.075 μg/L 0.04 mg/kg
4-Nitrotoluene (4-NT) 99-99-0 0.075 μg/L 0.04 mg/kg
Nitroglycerine (NG) (On Demand only) 55-63-0 − −
1,2-Dinitrobenzene (surrogate standard) 528-29-0 − −

* Reported as coeluting isomers

Appendix 7: Sample Tag Example

 OASQA Sample Submission Procedures Rev. 13.0
January 29, 2014
Page 38 of 41

Appendix 8: Chain of Custody Example

ENV IRONMENTAL PROTECTION AGENCY REGION 3

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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-EXPOSURE 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.):
 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.
 OASQA Sample Submission Procedures Rev. 13.0
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 SW 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 5035A)

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 mL 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.