EPA - REGION 9
GUIDELINES FOR CLOSURE
OF
SHALLOW DISPOSAL WELLS
1992
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TABLE OF CONTENTS
LIST OF FIGURES 2
LIST OF TABLES 2
I. INTRODUCTION 3
H. REQUIREMENTS FOR CONTRACTORS 5
m. LABORATORY SELECTION 6
IV. CLASS IV AND V WELL CLOSURE GUIDELINES 7
V. SAMPLING METHODS AND PROCEDURES 19
A. Sampling Equipment 19
B. Equipment Decontamination 20
C. Quality Assurance/Quality Control 20
1. Equipment Blanks 20
2. Field Blanks 21
3. Trip Blanks 21
4. Replicate Samples 21
5. Split Samples 21
6. Spiked Samples 22
D. Sample Analysis 22
E. Sample Labeling 23
F. Sample Collection - Liquid 23
1. Volatile Organics 23
2. Semi-Volatile Organics 24
3. Metals 24
4. Total Petroleum Hydrocarbons (TPH) -.- 24
5. Total Recoverable Petroleum Hydrocarbons (TRPH) 24
G. Sample Collection - Sediment 25
H. Sample Collection - Soil 25
I. Field Documentation 26
J. Sample Packaging and Shipping 26
K. Common Sampling Errors 29
L. Chain of Custody 29
REFERENCES 32
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LIST OF FIGURES
Figure A-l: Soil Sample Locations for a Septic System Receiving Both Industrial
and Sanitary Wastes - Plan View H
Figure A-2: Soil Sample Locations for a Septic System Receiving Both
Industrial and Sanitary Wastes - Side View 12
Figure B-l: Soil Sample Locations for a Septic System Receiving Only
Industrial Wastes - Plan View 13
Figure B-2: Soil Sample Locations for a Septic System Receiving Only
Industrial Wastes - Side View 14
Figure C-l: Drywell, Cesspool, or Drainage Well Receiving Both
Industrial and Sanitary Wastes or Only Industrial Wastes - Plan
View 15
Figure C-2: Drywell, Cesspool, or Drainage Well Receiving Both
Industrial and Sanitary Wastes or Only Industrial Wastes - Side
View 16
Figure D-l: Leachfield/Infiltration Gallery Receiving Both Industrial and
Sanitary Wastes or Only Industrial Wastes - Plan View 17
Figure D-2: Leachfield/Infiltration Gallery Receiving Both Industrial and
Sanitary Wastes or Only Industrial Wastes - Side View 18
Figure E - Chain-of-Custody Form 31
LIST OF TABLES
Table I - Sampling Methods 27
Table H - TCLP Sampling Methods 28
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I. INTRODUCTION
The Safe Drinking Water Act (SDWA) of 1974, as amended, requires the U. S.
Environmental Protection Agency (U.S. EPA) to establish a program which provides for
the safety of the nation's drinking water. The Underground Injection Control (UIC)
program was established under the SDWA to prevent contamination of underground
sources of drinking water from improper use of disposal wells.
Underground sources of drinking water vary in depth and quality from pristine
aquifers a few feet beneath the ground surface to aquifers that are thousands of feet
deep containing up to 10,000 parts per million of dissolved solids, usually in the form of
salts. Over 50% of the U.S. population relies on these aquifers for drinking water, and
the percentage is increasing every year.
Disposal wells covered by the UIC program include bored, driven or drilled shafts
or dug holes whose depth is greater than the largest surface dimension, where the
principal function of the shaft or hole is the emplacement of fluids. Under certain
conditions, sumps, septic tanks, cesspools and drainfields may also be considered disposal
wells. For the purposes of the UIC program, a fluid is any material or substance which
flows or moves, whether in a semisolid, liquid, sludge, gas or any other form or state.
Contaminants introduced into underground sources of drinking water through the use of
disposal wells include bacteria and viruses, minerals and nitrates, heavy metals, organic
chemicals and pesticides.
Most types of disposal wells are subject to construction, performance and
monitoring requirements designed to ensure that no contamination of underground
sources of drinking water occurs through their use. Wells that discharge fluids into or
above an underground source of drinking water are generally classified as shallow
disposal wells and are not always subject to these requirements. The disposal of
hazardous fluids into shallow wells (Class IV wells) is prohibited under the SDWA
However, many shallow wells (Class V) accept fluids that are not defined as hazardous,
but still have a potential to contaminate underground sources of drinking water. EPA
Region 9 is requesting closure of such wells.
This guidance is designed to aid in the proper closure of shallow disposal wells.
In addition to providing guidelines for the closure of these wells, general information is
included concerning sampling equipment, methods and procedures for collecting liquid,
sediment and soil samples; required methods of sample analysis; contractor and
laboratory requirements; and sample chain of custody requirements.
»««****«»««»*
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It is important to note that this guidance is designed to aid in the closure of wells.
The owner or operator of a facility is ultimately responsible for proper closure of the wells
and is also responsible for complying with other federal regulations such as RCRA and
CERCLA, and with state and local regulations. The owner or operator must ensure that
facility practices do not contribute to the contamination of ground water.
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II. REQUIREMENTS FOR CONTRACTORS
Activities involving site assessment and well closure require a professional level of
expertise. In addition to knowledge regarding the correct procedures and methods used
in collecting samples, some investigations may require a knowledge of the mechanisms of
contaminant transport; federal, state and local regulations and ordinances relating to
waste management; and actions needed to remediate a contaminated site.
To ensure that the contractor has the qualifications — through a combination of
education and experience — to perform sampling and site assessment requirements, EPA
Region 9 requires that:
1. The contractor submit an acceptable sampling plan which addresses:
a. types of sampling containers and their preparation
b. sample preservation methods
c. sampling equipment and method of sample retrieval
d. familiarity with specified sampling methods
e. quality assurance/quality control measures
f. certified lab to which samples will be sent
g. chain of custody
2. The individual signing any report related to a workplan for closure of a well or a
sampling plan must be a registered geologist or professional engineer registered
with the state. This individual shall be responsible for the content, validity and
completeness of the report. All reports related to well closure activities shall
include the following certification:
/ certify under penalty of law that this document and all attachments
were prepared under my direction or supervision in accordance with a
system designed to assure that qualified personnel properly gather and
evaluate the information submitted. Based on my inquiry of the person
or persons who manage the system, or those persons directly responsible
for gathering the information, I certify that the information submitted
is, to the best of my knowledge and belief, true, accurate, and
complete. I am aware that there are significant penalties for submitting
false information, including the possibility of fine and imprisonment for
knowing violations.
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III. LABORATORY SELECTION
Either state-certified laboratories or those associated with EPA's Contract Lab
Program must be used for sample analyses. If the distance to the nearest laboratory is
such that hand-delivery is not possible, samples should be express/overnight delivered.
All laboratories involved in the analysis of samples must retain their calibration logs for
two years, laboratory data logs for three years, and sampling labels or information from
the labels for three years. All analytical tests must be performed in accordance with
methods acceptable under quality assurance guidelines. A quality assurance plan must
be submitted with the sampling plan. For more information regarding laboratory
selection, see the reference section of this document.
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IV. CLASS IV AND V WELL CLOSURE GUIDELINES
When any Class IV or Class V well threatens to violate a primary drinking water
regulation or otherwise causes conditions that may adversely affect public health, EPA
Region 9, upon learning of such violation or conditions, will require closure of the well.
Closure must then be accomplished in such a manner as to ensure that no movement of
fluid containing any contaminant will move into underground sources of drinking water
(USDWs). As an element of proper well closure, Region 9 may require cleanup of soil
and/or groundwater in and around the Class IV or V well.
To meet EPA requirements, well closure should, at a minimum, include the
elements of the following guidelines:
1. Provide an acceptable alternative to well discharge for disposal of waste fluids.
The alternative must comply with all regulations such that no violation or future
violation of primary drinking water standards will result. EPA requests the use of
management practices that reduce the amount of contaminants released into the
environment through product changes, unproved operating practices, reuse of materials,
onsite closed-loop recycling, on and off-site reclamation, and water conservation.
2. Identify the locations of all drams, drain lines, drywells, and cesspools or septic
systems at the facility.
3. Contact EPA at least seven (7) days in advance of any site operations relating to
closure activities.
4. Take representative samples from the liquid and/or sludge phase present in the
drain(s) and the well(s) or septic tank(s) in accordance with the procedures described in
"Sampling Methods and Procedures" under "Sample Collection". Have the samples
analyzed for volatile organics, metals, total petroleum hydrocarbons and oil and grease in
accordance with the methods described under "Sample Analysis" and, when necessary,
prepared in accordance with the methods for the Toxicity Characteristic Leaching
Procedure (TCLP) in 40 C.F.R. Part 261 Appendix H as amended June 29, 1990. Copies
of sampling and analysis results, and results of all quality control samples, must be
submitted to EPA.
5. Remove the contents from the drains and drain lines and the well(s) or septic
tank(s) and determine appropriate disposal methods based on the results of the sample
analyses. The owner/operator is ultimately responsible for proper disposal of all wastes,
and should carefully review all arrangements for disposal to ensure compliance with
federal, state and local regulatory requirements.
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6. Disconnect the drain lines from the well, pressure wash the drains and lines, fill
them with grout or cement, and permanently seal them. All waste associated with
cleaning the drains and lines should be disposed of in accordance with federal, state, and
local regulations.
7. Observe the following closure requirements for septic tanks and wells:
Case A: Septic system accepting industrial and sanitary wastewater into a common
septic tank and drainfield or leachfield.
The septic tank should have the contents removed and disposed of appropriately. If a
visual inspection of the tank indicates cracks or leaks, the tank and any visibly or
potentially contaminated soil in the vicinity should be removed and disposed of
appropriately. Soil samples should be taken below the bottom of the tank excavation in
the manner described in "Sampling Methods and Procedures" under "Sample Collection"
and analyzed by a certified analytical laboratory. If the tank does not have any cracks or
leaks, soil samples may be taken at either end of the tank at a depth that is at least as
deep as the bottom of the tank. The tank may then be used for sanitary waste only, and
the drain pipes leading from the restrooms need not be disconnected. Soil samples must
also be taken along every twenty feet of drainfield or leachfield and sent to a certified
laboratory for analysis. It is recommended that soil samples be taken at other locations
where there is a potential for a high degree of contamination (worst-case locations) such
as elbows and joints in pipe lines, floor drains and clarifiers. All soil samples should be
analyzed according to the methods in "Sampling Methods and Procedures" under
"Sample Analysis". In addition, at least two soil samples, taken at the worst-case location
around either the tank or drainfield, must be both analyzed for total concentrations and
prepared in accordance with the methods for the Toaadty Characteristic Leaching Procedure
(TCLP) in 40 C.F.R. Part 261 Appendix II as amended June 29, 1990. See Figures A-l
and A-2 for required and recommended soil sample locations.
Case B: Septic system accepting only industrial wastewater into a septic tank and
drainfield or leachfield.
The septic tank and the contents should be removed and disposed of appropriately. Any
visibly or potentially contaminated soil in the vicinity of the tank should be removed and
disposed of appropriately. Soil samples should be taken below the bottom of the tank
excavation in the manner described in "Sampling Methods and Procedures" under
"Sample Collection" and analyzed by a certified analytical laboratory. Soil samples must
also be taken along every twenty feet of drainfield or leachfield. It is recommended that
soil samples be taken at other suspected worst-case locations such as elbows and joints in
pipe lines, floor drains and clarifiers. All soil samples should be analyzed according to
the methods in "Sampling Methods and Procedures". In addition, at least two soil
samples, taken at the worst-case location around either the tank or drainfield, must be both
analyzed for total concentrations and prepared in accordance with the methods for the
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Toxidty Characteristic Leaching Procedure (TCLP) in 40 C.FJL Part 261 Appendix II as
amended June 29, 1990. The excavated area should then be backfilled with clean
suitable fill material. See Figures B-l and B-2 for required and recommended soil
sample locations.
Case C: Drywells, cesspools or drainage wells accepting industrial and sanitary
wastewaters, or only industrial wastewaters.
The contents of the drywell, cesspool or drainage well (identified hereafter as Veil")
should be removed and disposed of appropriately. It is required that the well casing be
removed if it is practicable. Any visibly or potentially contaminated soil underlying the
contents of the well should be removed. Soil samples should be taken in the center of
the bottom of the well in the manner described in "Sampling Methods and Procedures"
under "Sample Collection" and analyzed by a certified analytical laboratory. If taking
samples from the bottom of the well is not feasible, samples should be taken on opposite
sides of the well, at a distance not to exceed one foot away from the borehole, and
starting at a depth that is equivalent to the depth of the bottom of the well. It is
recommended that soil samples be taken at other suspected worst-case locations such as
elbows and joints in pipe lines, floor drains and clarifiers. All soil samples should be
analyzed according to the methods in "Sampling Methods and Procedures". In addition,
at least two soil samples, taken at the worst-case location, must be both analyzed for total
concentrations and prepared in accordance with the methods for the Toxidty Characteristic
Leaching Procedure (TCLP) in 40 C.F.R. Part 261 Appendix II as amended June 29,1990.
The remaining hole where the well has been removed should then be filled with grout
and sealed with asphalt or cement. See Figures C-l and C-2 for required and
recommended soil sample locations.
Case D: Leachfield/infiltration gallery accepting sanitary and industrial
wastewaters, or only industrial wastewaters.
The practice of disposing sanitary and/or industrial wastewaters directly to a
leachfield/filtration gallery without the use of a septic tank is unacceptable. The
leachfield should be excavated, and all visibly or potentially contaminated soils removed
and disposed of appropriately. Soil samples must be taken along every twenty feet of
drainfield or leachfield in the manner described in "Sampling Methods and Procedures"
under "Sample Collection" and sent to a certified laboratory for analysis. It is
recommended that soil samples be taken at other suspected worst-case locations such as
elbows and joints in pipe lines, floor drains and clarifiers. All soil samples should be
analyzed according to the methods in "Sampling Methods and Procedures". In addition,
at least two soil samples, taken at the worst-case locations in the drainfield or leachfield,
must be both analyzed for total concentrations and prepared in accordance with the methods
for the Toxidty Characteristic Leaching Procedure (TCLP) in 40 CF.R. Part 261 Appendix
II as amended June 29,1990. The area should be regraded using clean fill. See Figures
D-l and D-2 for required and recommended soil sample locations.
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8. Contact state and local agencies and incorporate their requirements into the well
closure plans.
9. Submit a report, upon completion of well closure activities, that includes the
following items:
A plot plan showing locations of disposal or drainage well(s), sampling
points, buildings and adjacent streets. Indicate the north direction by an
arrow.
Copies of all fluid, sludge and soil sample analysis results, and results of all
quality control samples.
Copies of manifests or other documentation pertaining to proper disposal
of all removed liquid, sludge and soil.
A description of the extent of site contamination. Should site remediation
appear necessary, recommendations from a registered geologist or
professional engineer, with sufficient experience in soils, should be included
to address the problem.
10. Include, on all reports submitted to EPA that relate to well closure activities, the
certification given in "Requirements for Contractors".
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These guidelines do not constitute a remediation plan. It is the responsibility of the
owner or operator to ensure that further site evaluation be conducted if analytical results of
the soil samples indicate the presence of contamination.
All submittals are to be sent to:
Groundwater Pollution Control Section
U.S. Environmental Protection Agency
75 Hawthorne Street, W-6-2
San Francisco, CA 94105
Contact: (415) 744-1832
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Case A: Soil Sample Locations for a Septic System Receiving
Both Industrial and Sanitary Wastes
XYZ Industries
Drains
O
Rest
Rooms
sample every 20'
O
O
Septic Tank
Dralnfleld
• Required Sampling Location
O Recommended Sampling Location
Figure A-1: Plan View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
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Case A: Soil Sample Locations for a Septic System Receiving
Both Industrial and Sanitary Wastes
XfZ Industries
• Required Sampling Location
O Recommended Sampling Location
* Additional samples should be taken
every 5' until 5' below the last
suspected contamination.
Septic Tank
Dralnfleld
r-2f
- -1..
--o
--o
r-2'
-- o
i'-2f
y •
r~2'
5' •
sample every 20'
Figure A-2: Side View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
12
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Case B: Soil Sample Locations for a Septic System Receiving
Only Industrial Wastes
XYZ Industries
O
Drains
O
sample every 20'
Septic Tank
Dralnfleld
• Required Sampling Location
O Recommended Sampling Location
Figure B-1: Plan View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
13
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Case B: Soil Sample Locations for a Septic System Receiving
Only Industrial Wastes
XYZ Industries
\
• Required Sampling Location
O Recommended Sampling Location
* Additional samples should be taken
every 5' until 5* below the last
suspected contamination.
Septic Tank
Dralnfleld
r-r
5f*
o
O
3'*
O
O
r-2'
5' •
r-21
51 *
sample every 20*
Figure B-2: Side View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
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Case C: Drywell, Cesspool, or Drainage Well Receiving Both
Industrial and Sanitary Wastes or Only Industrial Wastes
XYZ Industries
O
Drains
Rest
Rooms
O
O
•o
Drywell,
Cesspool, or
Drainage Well
• Required Sampling Location
A Alternate Required Sampling Locations
O Recommended Sampling Location
Figure C-1: Plan View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
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Case C: Drywell, Cesspool, or Drainage Well Receiving Both
Industrial and Sanitary Wastes or Only Industrial Wastes
WZ Industries
s.
^
• Required Sampling Location
A Alternate Required Sampling Locations
O Recommended Sampling Location
* Additional samples should be taken
every 5' until 5' below the last
suspected contamination.
1'-2f
sf*
--O
r-y
S'*
-- o
Figure C-2: Side View
A
A
A
A
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
1G
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Case D: Leachfield/lnfiltration Gallery Receiving Both Industrial
and Sanitary Wastes or Only Industrial Wastes
XYZ Industries
Drains
O
Rest
Rooms
sample every 20'
O
O
Leachfleld/
Infiltration Gallery
• Required Sampling Location
O Recommended Sampling Location
Figure D-1: Plan View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
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Case D: Leachfield/lnfiltration Gallery Receiving Both Industrial
and Sanitary Wastes or Only Industrial Wastes
XYZ Industries
\
9'*
• Required Sampling Location
o Recommended Sampling Location
* Additional samples should be taken
every 5' until 5' below the last
suspected contamination.
Leachfield/lnfiltration Gallery
-o
LO
11 M
S1*
i
- o
L o
*
• -
* -
r-r r-y
S1 • 5' *
1
,i
«
j
sample every 20'
Figure D-2: Side View
Note: The soil sample locations shown above meet the minimum requirements of the EPA UIC Program. However, the owner
and/or operator of the well Is also responsible for meeting the requirements of all other applicable federal, state, and local
laws, and for adequately assessing the extent of any soil or ground water contamination.
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V. SAMPLING METHODS AND PROCEDURES
A. Sampling Equipmpnt
Various types of equipment may be used to collect grab samples from shallow
well systems. Typical sampling equipment includes pond samplers, weighted bottles, and
bailers. The equipment is usually made of stainless steel, glass or Teflon. Other
equipment may be used when the situation warrants.
The pond sampler is used when the system is easily accessible and when the
sampling point is deeper than arm's length. This sampling device consists of a
telescoping aluminum rod to which a stainless steel or nalgene beaker is attached using
an adjustable stainless steel C-clamp. The size of the beaker is determined by the
volume and number of samples to be collected.
Weighted bottles or similar devices may be utilized to sample fluid at a depth
below an oil/water interface. Such devices must be lowered below the floating product
phase before opening. Fluid from below the interface may then be retrieved.
The bailer is useful for sampling from small diameter wells, septic tanks, and
other areas where openings are too small to permit use of the pond sampler. A bailer is
lowered into the fluid with a rope and retrieved with a sample of the fluid.
Often sediment samples from the bottom of a sump are collected using a beaker
attached to a pond sampler. A stainless steel lab scoop is generally used to transfer the
sediment from the beaker to the required container. Trowels and drive samplers are
also used to collect samples.
In addition to the sampling equipment typically used to obtain samples, nalgene
bottles for liquid sample transfer; certified organic-free, metal-free water for quality
assurance blank samples; and instruments for measurement of fluid pH and temperature
are used.
It is important to avoid using equipment or containers that may alter the sample
through the introduction of foreign matter. Contaminated sampling equipment can
result in leaching or paniculate fallout, volatilization or adsorption of the sample.
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B. Equipment Decontamination
~~^^~.^a^jEar^-gA^j**********1**^**
All sampling equipment must be decontaminated before and after each sampling
event. All quality control equipment blank samples must be obtained after equipment
has been thoroughly decontaminated, prior to collecting fluid, sediment or soil samples.
Decontamination procedures should be as follows:
^«* uccu uiurougniy decontaminated, prior to coll<
Decontamination procedures should be as follows:
1. Disassemble equipment
2. Wash with non-phosphate detergent (alconox) and tap water
3. Rinse with tap water
4. Rinse with isopropyl alcohol (use a squirt bottle)
5. Triple rinse with deionized or distilled water
6. Rinse with acid
7. Rinse with certified organic free (HPLC grade) water
C. Quality Assurance/Quality Control
Quality assurance (QA) is the process of assuring that data obtained are
technically sound and properly documented. Quality control (QC) procedures are
employed to measure the degree to which quality assurance objectives are met. The
laboratory is not informed of the existence of field QC samples.
This document is intended to provide guidelines on some of the minimum
requirements necessary to ensure the quality of the data produced during
sampling/analysis activities. The regulated facilities are responsible for the quality of the
data produced, and are expected to provide data of known, documented, and verifiable
quality.
Following is a list of some of the quality control samples which can be employed.
Blanks are a check for cross-contamination during sample collection and shipment and in
the laboratory. Use analytically-certified organic-free (HPLC grade) water for organic
parameters and metal-free (deionized-distilled) water for inorganic parameters. In
general, at least one replicate sample, and one type of blank must be obtained for every
ten field samples. If there are less than ten field sampling points, at least one replicate
sample and one type of blank must be obtained.
1. Equipment Blanks
Quality control (QC) equipment blanks are used to assess the caliber of field
decontamination procedures. After the sampling equipment has undergone
decontamination procedures, the appropriate (certified metal-free or organic-free) water
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is poured into the sampling equipment and from there into sampling containers. These
containers are preserved, documented and analyzed in exactly the same manner as those
containers holding samples of waste fluid.
2. Field Blanks
This type of sample should be collected when equipment decontamination is
unnecessary and when a sample collection vessel will not be used. The field sample
should be taken at the sampling point. The sample consists of the appropriate (certified
metal-free or organic-free) water to which the same quantity of preservative is added as
is added to the field samples. These samples provide a check on any contamination of
chemical preservatives.
3. Trip Blanks
Trip blanks are used to detect contamination or cross-contamination which may
have occurred during sample handling and transportation. These blanks must be
prepared prior to the sampling effort and will accompany sample containers used during
sampling and in the transport cooler. The trip blanks consist of certified metal-free,
organic-free water and will be analyzed by a certified laboratory at the time the other
samples are analyzed.
4. Replicate Samples
Replicate sampling is used to determine consistency in both sampling procedures
and analytical methods. In general, replicate samples must be obtained at one out of
every ten sampling points, and at least one replicate sample must be obtained if there
are less than ten sampling points. To collect these samples, fluid is obtained from a
sampling point and split between two identical containers. Both containers undergo the
same method of analysis at the laboratory.
In addition, split samples and spiked samples are used for QA/QC purposes.
These can be briefly described as follows:
5. Split Samples
A split sample is divided into two containers for analysis by separate laboratories.
The purpose of this type of sample is to independently confirm laboratory results.
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6. Spiked Samples
A spiked sample is produced by adding a known quantity of analyte(s) of interest
to the sample. Spiked samples are used to check the accuracy of analytical procedures.
D. Sample Analysis
Region 9 requires that all samples associated with well closure activities be
analyzed for the compounds listed below using the indicated methods. Analysis for semi-
volatile organic compounds is only necessary when such compounds are suspected of
being in the waste stream.
1. Volatile Organics: EPA Method 8240 (Volatile Organics); EPA Method
8260 (Volatile Organics by Capillary Column); or a combination of EPA
Methods 8010 (Halogenated Volatile Organics), 8015 (Nonhalogenated
Volatile Organics) and 8020 (Aromatic Volatile Organics).
2. Semi-Volatile Organics: EPA Method 8270 (Semi-volatile Organics) is
recommended when the presence of semi-volatile organics is suspected in
the waste stream.
3. Metals: Appropriate EPA Methods for all metals on the Toxicity
Characteristics (TC) list (arsenic, barium, cadmium, chromium, lead,
mercury, selenium, and silver).
4. Total Petroleum Hydrocarbons (TPH): EPA Methods 5030/8015 and
5030/8020 to analyze for gasoline in liquid or soil, EPA Method 3510/8015
for diesel in liquid, and EPA Method 3540/8015 for diesel in soil.
5. Total Recoverable Petroleum Hydrocarbons (TRPH): EPA Methods
9070A/418.1 for liquid and EPA Methods 9071A/418.1 for soil. As of
10/1/92 EPA Methods 9071A/418.1 will be replaced by EPA Methods -1
3560/8440. For information on these methods, contact:
Quality Assurance Management Section
U.S. Environmental Protection Agency
75 Hawthorne Street, P-3-2
San Francisco, CA 94105
(415) 744-1492
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Note: Some waste streams may contain additional constituents not covered by these
methods. In those cases, additional EPA analytical methods must be
employed to determine whether other constituents are present at concentrations
which violate the primary drinking water standards or may otherwise adversely
affect the health of persons. For literature regarding appropriate methods, see
the reference section at the end of this document.
E. Sample Labeling
All samples should be tagged with an identification number; the date and time of
sample collection; type of sample (water, sediment, soil etc.); signature of the sampler;
whether the sample is preserved or unpreserved; the general types of analyses to be
conducted; and, if the sample is known or thought to be hazardous, the tag should be so
marked with information on the nature of the hazard (e.g. corrosive, flammable,
poisonous).
F. Sample Collection - Liquid
1. Volatile Organics
Samples for volatile organics are generally taken first to minimize the disturbance
of the fluid and resulting loss of volatiles.
An oil/water interface probe should be utilized to define the base of any free
floating product encountered while sampling. If no floating liquid phase is present, a
sampling device can be lowered into the fluid -- as deeply as possible without disturbing
the sediment - and extracted with a representative grab sample of fluid. The fluid can
then be transferred to pre-chilled, pre-labeled 40-ml volatile organic analysis (VOA) vials
with Teflon septa. The sample should be preserved by adding hydrochloric acid (HC1) to
a pH of less than 2. Two 40-ml vials should be obtained for each VOA sample. When
analyzing using the Toricity Characteristic Leaching Procedure (TCLP), bear in mind
that the volume of sample to be collected is dependent on the solids content of the
sample. Sufficient sample volume is needed to allow for each physical phase to be
analyzed separately. Sample bottles should be filled as completely as possible so that no
head space remains. Do not add HC1 to samples that will be prepared using the TCLP.
If a separate floating phase is encountered while sampling, a sampling device that
collects fluid from beneath the floating phase should be used. This device is operated by
gently lowering it in the closed position to a depth below the oil/water interface,
carefully opening and filling it with sampling fluid, and then closing and retrieving the
sample.
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When transferring the sampling fluid from the sampling container to a VOA vial,
the fluid must be poured slowly and smoothly to produce a meniscus over the lip of the
vial. The screw-top lid with the Teflon septum is then tightened onto the vial, and the
vial turned upside down and gently tapped to check for the presence of air bubbles. If
air is trapped in the vial, i.e. head space is present, the sample must be retaken. VOA
samples should not be taken near any exhaust systems which may cause contamination of
the sample.
The sample should tagged and chilled to approximately 4°C in a cooler and sent
to a certified analytical laboratory.
2. Semi-Volatile Organics
Samples for semi-volatile organics should be collected after those for volatile
organics. The method of collection is the same as that described for volatiles. After the
fluid is collected, it should be transferred to a pre-labeled, one-liter amber glass bottle
with a Teflon septum. The sample must be tagged and chilled to approximately 4°C for
shipping to the analytical laboratory.
3. Metals
Samples for total metals should be taken after those for volatile and semi-volatile
organics. After collection, the sample is transferred to a one-liter, polyethylene, certified
metal-free bottle and the unfiltered sample is acidified with 1:1 redistilled HNOj to a pH
of less than 2 at the time of collection. Do not add HNQj to samples that will be
analyzed for mercury or those that will be prepared using the TCLP.
4. Total Petroleum Hydrocarbons (TPH)
Use collection methods described for sampling for volatile organics. If sampling
for TPH as gasoline, the fluid should be transferred to two pre-labeled 40-ml vials with
Teflon septa (as described for volatile organics). If sampling for TPH as Diesel, the
fluid should be transferred using a funnel to a pre-labeled, one-liter glass bottle with a
Teflon septum. Preserve the sample by adding hydrochloric acid (HC1) to a pH of less
than 2. The sample must be tagged and chilled to 4°C for shipping to the analytical
laboratory.
5. Total Recoverable Petroleum Hydrocarbons (TRPH)
Use the collection methods described for volatile organics. The fluid should be
24
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transferred to a one-liter glass bottle with a Teflon septum. The sample must then be
preserved, tagged and chilled as above.
G. Sample Collection - Sediment
Often sediment samples from the bottom of a sump are collected using a beaker
attached to a pond sampler. A stainless steel lab scoop is generally used to transfer the
sediment from the beaker to the required container. Sediment samples should be placed
in an 8-oz. wide-mouthed glass jar. The jar should be completely filled so that no
headspace is present. After being taped and labeled, the sample should be placed
immediately in an ice chest and kept cold (4°C) for delivery to the laboratory. Care
should be taken throughout to avoid contamination of both the inside and outside of the
jar and its contents.
H. Sample Collection - Soil
The bore hole can be made with a continuous flight or hollow stem auger, rotary
corejirill or other drilling method. It is recommended that core sampling equipment
avoid the use of drilling fluids since these greatly increase the potential for sample
contamination. Soil sampling kits are commercially available that can be used at
relatively shallow depths to both drill the bore hole and collect a soil core. These units
contain augers, coring tubes and sufficient drill rod extensions to sample up to depths of
twenty-five feet.
The most common procedures for collecting soil samples use a thin-wall steel tube
(core barrel), fitted with a brass liner, which is forced into the undisturbed soil at the
bottom of the bore hole. This is sometimes referred to as drive sampling. Core barrels
are generally from one inch to three inches in diameter and 12 to 24 inches long. When
the core barrel is retrieved, friction will usually retain the sample inside the barrel in
most unsaturated materials.
Samples should be taken at locations where the potential for a high degree of
contamination easts (suspected worst-case locations) such as elbows, joints in pipe lines,
darifiers, floor drains, tanks and welts. Several depth borings should be planned to be
sampled for chemical analysis. Sample intervals will vary, but in general should be taken
between one and two feet beneath the excavation or the bottom of the septic tank, cesspool,
wen, pipe Une or floor drain surface, and then every five feet to the water table, or until five
feet past the last suspected contamination.
Upon retrieval from the borehole, the sample liners should be removed and
placed on clean plastic. Using cuttings or corings, the borehole should be logged to the
full depth by an on-site geologist according to the Unified Soil Classification System.
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After logging, the exposed ends of the liner should be covered. Typically, Teflon sheets
and plastic end caps are used and secured with silicone-based tape. After each use,
sampling equipment must be decontaminated.
Sample labels should be written or attached securely to the end caps and should
contain the following information: boring number, sample location, sample number,
sample depth, date and time of sampling, name of sampler, and required analytical
method. Sealed and labeled samples must be placed in cooled ice chests and shipped to
the analytical laboratory.
I. Field Documentation
Field information about sampling efforts should include sample identification
numbers; date and time of sample collection; description of the location of the
collection; the collection method; the rationale for selecting the sample and
representativeness of the sample; and a description of any deviations from standard
protocols.
J. Sample Packaging and Shipping
Samples should be packaged to prevent breakage. The shipping container should
be sealed or locked so that any evidence of tampering may be readily detected.
Packaging, labeling and shipping of samples must follow the Department of
Transportation (DOT) regulations. Samples that meet DOTs hazardous materials
criteria must be packed and labeled according to the requirements set forth in 49 CFR
172.101.
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TABLE I
SAMPLING METHODS
Recommended Sampling Containers0, Preservation
Techniques, and Holding Times
Analysis Method
Volatile Organic*
-EPA 8240,
-EPA 8260. or
-EPA 8010 and 8020
Semi-volatile Organic*:
-EPA Method 8270
Metals:
Appropriate EPA methods for
arsenic, barium, cadmium,
chromium, lead, selenium, and
silver
Mercury:
Appropriate EPA method
Total Petroleum Hydrocarbons-
Qasollne:
-EPA 5030/8015 and
5030/8020 (liquid)
-EPA 5030/8015 and
5030/8020 (soil)
Diesel:
-EPA 3510/8015 (liquid)
-EPA 3540/8015 (soil)
Total Recoverable Petroleum
Hydrocarbons:
-EPA9070A/418.1 (liquid)
-EPA 9071A/418.1* (soil)
Fluid
Two 40-ml volatile organic analysis vials
fitted with Teflon septa (VGA vials)
One 1 -liter amber glass bottle with Teflon
septum
One 1 -liter polyethylene bottle
One 1 -liter polyethylene bottle
Two 40-ml VOA vials (gasoline) or one 1-
liter glass bottle with Teflon septum
(diesel)
One 1 -liter glass bottle with Teflon
septum
Sediment and Son
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
One 8-oz. wide mouth glass jar, or
two 4-oz. wide mouth glass jars
One 8-oz. wide mouth glass jar, or
brass tube
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
Preservation
Chill to 4°C
For liquid samples, add HCI to
pH<2
Chill to 4'C+
Chill to 4'C
For liquid samples, add HNOg to
pH<2
Chill to 4° C
Chill to 4° C
For liquid samples, add HO to
pH<2
Chill to 4'C
For liquid samples, add HO to
pH<2
• i— i-fi——
noning
Time
14 days
7 days
180 days
28 days
14 days
14 days
Notes: ® Additional sample volume may be needed for quality control samples.
* As of October 1, 1992, use EPA Methods 3560/8440 for soil samples. Copies of these methods can be obtained from the USEPA Region IX Quality Assurance
Management Section at (415) 744-1492.
+ Check wtth the laboratory to see If any additional preservatives are needed for chemicals of concern.
27
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TABLE II
TCLP SAMPLING METHODS*
Recommended Sampling Containers4, Preservation
Techniques, and Holding Times
Analysis Method
Volatile Organic*:
-Appropriate TCLP methods
Semi-volatile Organic*:
-Appropriate TCLP methods
TCLP metals
-Arsenic: 7060
-Barium: 6010
-Cadmium: 6010
-Chromium: 6010
-Lead: 7421
-Selenium: 7740
-Silver: 6010
Mercury. 7470
Fluid
Two 40-ml volatile organic analysis vials
fitted with Teflon septa (VOA vials) and
two 1 -liter amber glass bottles with Teflon
septa
One 1 -liter amber glass bottle with Teflon
septum
One 1 -liter polyethylene bottle
One 1 -liter polyethylene bottle
Sediment and Soil
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
One 8-oz. wide mouth glass jar with
Teflon septum
One 8-oz. wide mouth glass jar with
Teflon septum, brass tube, or
stainless steel tube
Preservation
Chill to 4'C
Chill to 4°C
Chill to 4°C
Chill to 4'C
Holding
Time
14 days
7 days
180 days
28 days
Notes: * The TCLP cannot be used with analytical methods for total petroleum hydrocarbons (TPH) and total recoverable petroleum hydrocarbons (TRPH).
+ Additional sample volume may be needed for quality control samples and for each physical phase to be analyzed separately.
28
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K. Common Sampling Errors
The following are common errors made during sampling that lead to inconsistent
analytical results:
Failure to calibrate instruments
Lack of equipment maintenance
Use of inappropriate sample containers
Lack of QA samples to assure precision of sampling methods and
laboratory analysis.
Sample loss or leakage during shipping or handling due to improper
packaging
Mislabelling
Poor field records
L. Chain of Custody
The purpose of chain of custody procedures is to be able to trace possession of a
sample from the time it is collected until the analytical results are obtained by the
laboratory. Chain of custody procedures are important when analytical results are
introduced as evidence in a legal proceeding.
A sample is in "custody" if:
It is actually in one's physical possession
It is in one's view
It was in one's possession and it was secured so that it could not be
tampered with.
It is kept in a secured area with access restricted to authorized personnel
only.
It is placed in a container that is sealed with an official seal that will be
broken when the container is opened.
Chain of custody documentation includes, but is not limited to, the entries in the
sampler's field notebook, the official seals on the sampling containers and the chain of
custody record. The inspector needs to assure that the relationship between the physical
sample and the related documentation is clear, complete, and accurate. The sample
number, date and time of sampling, location and sample type, preservative used, analysis
required, and sampler's initials should appear on all documents.
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When transferring the samples, the individual relinquishing and the individual
receiving the sample must sign and record the date and time on the chain of custody
record. Every person who takes custody must fill in the appropriate section of the chain
of custody record. For a sample of a chain of custody record see Figure E. When the
samples are sent by mail, the package must be registered with return receipt requested.
30
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ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
CHAIN OF CUSTODY RECORD
REGION 9
75 Hawthorne Street
San Francisco, California 94105-3901
PROJ. NO.
PROJECT NAME
SAMPLERS: (Signature)
STA. NO.
DATE
TIME
STATION LOCATION
NO.
OF
CON-
TAINERS
REMARKS
Relinquished by: (Signature)
Date /Time
Received by: (Signature)
Relinquished by: (Signature)
Date /Time
Received by: (SignatureI
Relinquished by: (Signature)
Date /Time
Received by: (Signature)
Relinquished by: (Signature)
Date /Time
Received by: (Signature)
Relinquished by: (Signature)
Date /Time
Received for Laboratory by:
(Signature)
Date /Time
Distribution: Original Accompanies Shipment; Copy to Coordinator Field Files
Remarks
31
n 1 c /!
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REFERENCES
Carlin, Jayne and Tom, Laura, December 1986. EPA Region 9 Underground
Injection Control Direct Implementation Quality Assurance Project Plan.
County of Kern, Department of Environmental Health Services, July 1990. Site
Characterization and Remediation.
Engineering Enterprises, Inc, March 1986. Sampling Document for USEPA
Region IX Direct Implementation Program.
Engineering Enterprises, April 1988. Generic Plan for Injectate and Sediment
Sampling at Class V Facilities in Region DC.
Engineering Enterprises, February 1989. Standard Operating Procedures for
Injectate and Sediment Sampling at Class V Facilities in Region n.
Kern County Health Department and Kern County Fire Department.
Requirements for Permanent Closure of Underground Hazardous Substance Storage
Tanks.
Santa Clara Valley Water District, June 1989. Standards for the Construction and
Destruction of Wells and other Deep Excavations in Santa Clara County.
Stanislaus County Underground Tank Program, September 1989. Stanislaus
County Guidelines for Sampling and Site Investigations.
State of California, Leaking Underground Fuel Tank Task Force, December 1987.
Leaking Underground Fuel Tank Field Manual: Guidelines for Site Assessment,
Cleanup and Underground Storage Tank Closure.
State of California, Water Resources Control Board, August 1991. California
Underground Storage Tank Regulations and Related Health and Safety Code Sections.
USEPA Region 9 Quality Assurance Management Section, October 1989.
Preparation of a USEPA Region 9 Sampling and Analysis Plan for Private and State-
Lead Superfund Projects (9QA -06-89).
USEPA Region 9 Quality Assurance Management Section, September 1989.
USEPA Region 9 Guidance for Preparing Quality Assurance Project Plans for Superfund
Remedial Projects (9QA-03-89).
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USEPA, Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
(SW-846), available from Government Printing Office (202) 783-3238 (Doc. No. 955-001-
00000-1).
USEPA, Methods for Chemical Analysis of Water and Wastes, Doc. No. EPA
600/4-79-020.
USEPA, Methods for Organic Chemical Analysis of Municipal and Industrial
Wastewater, Doc. No. EPA 600/4-82-057.
USEPA, Methods for the Determination of Organic Compounds in Drinking
Water, Doc. No. EPA 600/4-88-039.
USEPA, Region 9 Quality Assurance Management Section, January, 1990,
Laboratory Documentation Requirements for Data Validation, Doc. No. 9QA-07-90.
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