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Site SpecificQuality ManagementPlan (SSQMP)
Operable Unit/Phase 1- Drum RemovalBlosenski Superfund SiteChester County, PennsylvaniaDACW45-89-C-0084
Department of the ArmyCorps of EngineersOmaha District
1989
OBRIENGGERE
8R000230
SITE SPECIFIC QUALITY MANAGEMENT PLAN (SSQMP)
Project Name: Operable Unit/Phase I - Drum RemovalBlosenski Superfund Site
Location: Chester County, Pennsylvania
Applicable Program: USEPA Superfund
Contracting Officer: John Barrett
Office Location: Omaha, Nebraska
QA Laboratory: Missouri River DivisionEnvironmental Division Laboratory(CEMRD-ED-L)
Points of Contact at To Be Determinedthe Design/ConstructionDistrict
Design/Construction To Be DeterminedDistrict
Design Division To Be DeterminedLaboratory (ifnecessary)
AR00023I
TABLE OF CONTENTS
.-.-•-.,» Ragei,. .... •!;••'.* -£.J)
SECTION 1 - PROJECT DESCRIPTION 1
SECTION 2 - PROJECT ORGANIZATION AND QMRESPONSIBILITIES 3
SECTION 3 - SAMPLING AND SAMPLE CUSTODYPROCEDURES 8
SECTION 4 - ANALYTICAL METHODS/PROCEDURES 24
SECTION 5 - ANALYTICAL/STATISTICAL CONTROLPARAMETERS 26
SECTION 6 - CALIBRATION PROCEDURES AND FREQUENCY 32
SECTION 7 - PREVENTATIVE MAINTENANCE 34
SECTION 8 - DATA ANALYSIS AND REPORTING 35
SECTION 9 - CONSTRUCTION CONTRACTOR DAILYQUALITY CONTROL REPORTS 36
SECTION 10 - PERFORMANCE AUDITS 38
TABLES
1 Analytical Parameters2 Distribution of Trench Samples
FIGURES
1 Location Map2 Location Plan3 Federal Express Airbill
ATTACHMENTS
1 "Sample Handling Protocol for Low, Medium, and High Concentrationof Samples of Hazardous Waste", USAGE, 10/86
2 USAGE QA/QC Requirements
flR000232
SECTION 1 - PROJECT DESCRIPTION
The Blosenski Landfill Site is located on 13.6 acres in West Cain
Township, Chester County, Pennsylvania (Figure 1). It is surrounded
by heavily wooded areas to the north and west, and by agricultural
areas to the east and northwest. Approximately 30 residents live within
a quarter mile radius of the site. Pennsylvania Department of Environ-
mental Resources (DER) estimates indicate that 600 residents live within
3 miles of the site. The closest dwelling to the site is a house trailer
located adjacent to the site on the southern perimeter.
Beginning in the 1950s, the site operated as a landfill by accepting
municipal and industrial wastes. In 1971, the site was purchased by Mr.
Joseph Blosenski, who operated the landfill until the early 1980s.
Wastes were randomly dumped on the surface during the operating
period. Wastes included solvents, waste water treatment sludges,
demolition and construction wastes, undercoating materials, and open
and leaking drums. Numerous citizen complaints of odors, smoke and
airborne debris led to petition and regulatory actions against Mr.
Blosenski. In 1982, the Environmental Protection Agency (EPA) con-
ducted a Site Inspection and found serious ground water contamination.
The primary contaminants of concern are volatile organic compounds
(VOCs) including benzene, toluene and trichloroethene (TCE), and
inorganics including lead, cadmium, chromium and mercury.
The current contract focuses on the removal of drums and soils in
immediate contact (within 18 inches) with the drums, and transport of
the excavated material to a Resource Conservation and Recovery Act
(RCRA) approved incinerator. These efforts are to be conducted in
1 flR000233
accordance with the EPA Record of Decision
dated September 1986). Removal actions will be directed to six
locations suspected to contain buried drums (Figure 2). These areas
were identified based on the results of test pits installed during the
site Remedial Investigation (conducted by the NUS Corporation and
published in February, 1986) as well as the results of a recent
magnetometer and geophysical survey conducted by O'Brien & Cere
Engineers, Inc. Presently, the actual number of drums that may be
buried at each of these locations and the contaminants contained within
the drums and associated soil are unknown. For this reason, additional
efforts will be directed to drum and soil sampling to determine proper
methods of disposal and transport of the material which meet applicable
Department of Transportation (DOT) and EPA requirements. Runoff
and wastewater generated during the Remedial Investigation and
predesign work are to be disposed of in a similar manner.
SECTION 2 - PROJECT ORGANIZATION AND QM RESPONSIBILITIES
The contract for this work will be administered by The U.S. Army
Corps of Engineers (USAGE), Omaha District. Quality Assurance (QA)
will be performed by the Missouri River Division Environmental Division
Laboratory (CEMRD-ED-L). Quality Management (QM) for this contract
involves the maintenance of field and laboratory practices/checks insur-
ing the scientific reliability, comparability, and legal defensibility of
chemical data. Quality Management during construction will be managed
by the North Atlantic District - Baltimore (NAB).
The Contractor will, at a minimum, provide the following informa-
tion:
(a) A project organization chart and an accompanying discussion
of corresponding Quality Control (QC) responsibilities.
Company project management and QC chains-of-command must
be mutually exclusive. The chart and discussion will also
include any Contractor/subcontractor interactions, such as
that between the Contractor and the contract laboratory.
(b) The qualifications of the assigned QC Officer with overall
responsibility for the design and successful implementation for
the project's Quality Control Plan. The QC Officer will be
independent of project management, reporting directly to a
senior company official. The QC Officer will interface with
the external USAGE QA laboratory (CEMRD-ED-L) and the
contract laboratory in matters of quality control. The QC
Officer must have demonstrated experience with chemical QC
and analyses of toxic/hazardous chemicals. The QC Officer
will provide a resume detailing his/her relevant education
(including continuing education) and years of experience in
the field.
(c) A list of all other Quality Management Personnel, by name,
involved in field sampling activities, and their respective
qualifications (education and experience) related to
handling/sampling toxic and hazardous waste materials.
Resumes for these individuals will be provided to the USAGE
for review. A Field Operations Manager will be included
among the Quality Management Personnel. This individual will
be responsible for day-to-day management of sampling activ-
ities. Other Quality Management Personnel will be identified
who are responsible for collecting samples, including a
sampling coordinator who will be responsible for maintaining
the project field notebook, field sample custody,
chain-of-custody records, and the proper packaging and
shipment of samples.
(d) Identification of the QA laboratory (CEMRD-ED-L), and a
description of its responsibilities. The CEMRD-ED-L rep-
resentative will provide technical staff support to the Con-
tracting Officer (CO) on QM issues and problems. The
CEMRD-ED-L representative is responsible for promptly
notifying the CO and the respective Design/Construction
Division in writing of any significant QM problems; and for
providing technical advice on recommended corrective actions.
CEMRD-ED-L shall promptly notify the CO upon failure to
receive: a) Quality Control Plan/Chemical Quality Control
88000236
Plan; b) request to inspect the contract laboratory before
samples are received; c) the Contractor's analytical results
for QA checks (replicates, splits, field blanks, reference
samples); or d) timely information on significant problems
encountered in QM.
(e) The contract laboratory shall be selected by the Contractor
and approved by the USAGE. In conformance with ER
1110-1-261, the CO and QA Laboratory representatives will
inspect the contract laboratory and prepare an inspection
report. The QA Laboratory will be responsible for prepara-
tion of the contract laboratory inspection report. The Con-
struction Division has approval authority for the contract
laboratory. If the inspection reveals correctable deficiencies,
the Contractor will be requested to rectify them. If neces-
sary, additional inspections at the Contractor's expense may
be required.
The Construction Division will base approval of the
contract laboratory upon review and recommendation of the
QA Laboratory and the Design Division, and consideration of
the QA Laboratory inspection report. The contract laboratory
must be approved before samples are furnished for analysis.
The contract laboratory shall have demonstrated experi-
ence with the EPA Contract Laboratory Program (CLP) and
SW-846 ("Test Methods for Evaluating Solid Wastes") proto-
cols. In describing the qualifications of the contract labo-
ratory, the Contractor will provide information relating to
physical laboratory facilities, instrumentation, participation in
AR000237
interlaboratory and performance audits, and familiarity with
EPA CLP and SW-846 protocols. Details of specific instrumen-
tation will include manufacturer, model types, accessories,
calibration, and year of purchase. Should information be
contained in the Contract Laboratory's "Standard Operating
Plan (SOP)", the Contractor may wish to include the SOP as
an attachment to the SSQMP.
Laboratories used for air analyses will either be Ameri-
can Industrial Hygienist Association (A1HA) certified for
appropriate tests (if applicable) or satisfactorily participating
in current National Institute of Occupational Safety and Health
(NIOSH) proficiency tests. Any history of chronic laboratory
contamination will be included in the SSQMP.
(f) Laboratory scientific personnel. Included will be a laboratory
organization chart and a discussion of the responsibilities of
key individuals (supervisors, chemists, technicians, QC
Manager). Resumes listing experience/education (including
continuing education) will be provided. One QC Manager will
be identified by the laboratory QC coordinator. This indi-
vidual will be responsible for overall management of QC
related to the project and interface with the Contactor and
the USAGE external QA laboratory. The minimum requirement
for the QC coordinator and bench chemists will be a Bachelor
of Science (B.S.) degree in chemistry and one (1) year of
appropriate experience in preparations, testing and analysis.
(g) A copy of the letter notifying the Contractor personnel re-
sponsible for QC about exact duties and responsibilities. The
W000238
letter should be signed by a responsible executive/manager of
the company.
(h) The Design Division will approve the Contractor laboratory
prior to the collection of any samples for this project phase.
3ROQ0239
SECTION 3 - SAMPLING AND SAMPLE CUSTODY PROCEDURES
The Contractor will provide a detailed description of sampling and
sample custody procedures which includes, at a minimum, the following
elements:
a. Sampling Locations
The Contractor will collect samples from the following: each
intact or partially intact drum containing residue material; soils in
immediate contact (within 18 inches) with the drum(s); and soil
remaining in trenches after the removal of drums and soil in
immediate contact with the drums. Field compatibility testing will
be performed on unmarked drum residues prior to compositing sam-
ples for off-site transport. It should be noted that the exact
sample collection frequency (e.g., the number of drums and soil
samples) is not known at the present time.
Soil Samples: The Contractor will collect soil samples for
analysis of EPA Target Compound List (TCL) volatiles, semivola-
tiles, metals, and pesticides/PCBs (Table 1) using CLP protocols.
The following soil samples will be analyzed for these parameters:
at least one composite sample per roll-off or bulk container holding
soils to be disposed off-site (5 locations within the roil-off or bulk
container equal one composite sample); and grab samples from soil
remaining in trenches after the removal of drums and soil in
immediate contact with the drums (see distribution of trench sam-
ples in Table 2). At least one additional composite sample will be
obtained from each roll-off or bulk container, and analyzed for the
following hazardous waste characteristics: Extraction Procedure
Toxicity (EP TOX), ignitability, corrosivity, reactivity, and total
sulfides according to the procedures outlined in SW-846 (1986). In
addition, any other analytical testing required by the off-site
incineration facility will be performed at this time.
Unmarked Drum Samples: The Contractor will perform a
series of compatibility tests on unmarked drum liquids to determine
their compatibility for compositing purposes. Compatibility testing
will be performed to separate unknown drummed materials into the
following classifications:
organics
organic peroxides
organic chlorides
oxidizers
inorganic acids
inorganic neutrals and bases
inorganic peroxides
The following compatibility tests will be performed:
water solubility
hexane solubility
peroxide test
oxidizer test
pH (inorganic liquids only)
cyanide test (inorganic neutrals and bases only)
sulfide test
organochlorine test
bench scale bulking test
At the discretion of the CO, similar field tests will be con-
ducted for compositing purposes on intact or partially intact drums
which are found to contain only solid residual material. Under
these circumstances, the residual material will be initially mixed
with water (solubility test) prior to performing the remaining
compatibility tests.
Based on the results of the field compatibility tests and the
quantity of material in the drums, 2-5 unmarked drums will be
composited as one sample. One sample will be collected from each
composite drum, and will be analyzed off-site at the Contractor's
laboratory. Each sample will be analyzed for the following hazard-
ous waste characteristics: EP TOX, ignitability, corrosivity, reac-
tivity with cyanides and sulfides, and total sulfides. In addition,
any other analytical testing required by the off-site incineration
facility will be performed at this time.
Marked Drum Samples: The Contractor will collect one sample
from each marked drum. This sample will be submitted to the
Contractor's laboratory for analysis of EPA TCL volatiles,
semi-volatiles, metals, and pesticides/PCBs (see listing in Table 1)
using CLP protocols. Each sample will also be analyzed for the
following hazardous waste characteristics: EP TOX, ignitability,
corrosivity, reactivity with cyanides and sulfides, and total
sulfides. In addition, any other analytical testing required by the
off-site incineration facility will be performed at this time.
10
Water Samples: Runoff from the area of waste excavation and
the Contamination Reduction Zone, as well as decontamination
wastewater, will be collected in two on-site storage tanks. Each
time a tank is full, a grab sample shall be collected and analyzed
for the purpose of characterization prior to off-site disposal. The
sample shall be sent to the Contractor's laboratory, and analyzed
for the following parameters: VOCs, semi-volatile organic com-
pounds (BNAs), heavy metals, and polychlorinated biphenyls
(PCBs). The following analytical methods will be used for the
indicated parameters: VOCs - EPA Methods 601 and 602; BNAs -
EPA Method 625; heavy metals (except mercury) - EPA Method
200.7; mercury - EPA Method 245.1; PCBs - EPA Method 608.
b. Sample Handling and Sampling Procedures
Samples will be handled in accordance with the USAGE "Sam-
ple Handling Protocols for Low, Medium and High Concentration
Samples of Hazardous Waste", 3/89. The Contractor will present
in the SSQMP detailed protocols for the collection of representative
samples. Sampling protocols will be based on EPA-recommended
procedures for the collection and handling of environmental sam-
ples. Appropriate source documents for environmental sampling
procedures include: "Methods for the Collection and Analysis of
Water and Waste Water" (EPA 600/4-79- 020); "Sampling and
Sampling Procedures for Hazardous Wastes Sources" (EPA
600/27-80-018), EPA Regional Standard Operating Procedures,
Guideline and Directives; and, "A Compendium of Superfund Field
Operations Methods" (EPA/540/P-87/001 ) . Included in the proto-
cols will be the container and preservative requirements, sample
11
collection, and compositing procedures. The protocols should be
prepared to serve as detailed field instruction sheets for field
sampling personnel.
Soil Sampling: It is anticipated that composite soil samples (5
locations equal one sample) will be obtained directly from the
roll-off or bulk containers using a stainless steel scoop or an
equivalent tool. In addition, grab samples will be collected from
soil remaining in trenches, using a stainless steel scoop or an
equivalent tool. At a minimum, the Contractor's sampling protocol
will include the following sequence:
(1) Complete the sample container label (date and time of
sampling, etc.).
(2) Insert the scoop or trowel, and remove the sample creating as
little disturbance of the sample as possible, to prevent the
loss of volatiles (volatile samples only).
(3) Fill and cap the volatile sample container, allowing minimal air
contact with the sample. The sample container should be
completely filled to eliminate headspace. A stainless-steel
bowl will be used for compositing roll-off or bulk container
samples to be analyzed for metals and semivolatiles.
(4) Transfer the sample to the appropriate sample container using
a stainless-steel lab spoon or equivalent.
(5) Cap and label the sample container.
(6) Record sampling information and observations in .. the bound
project notebook.
(7) Transfer sample custody to the sample coordinator.
12 /IR0002H
(8) Decontaminate sampling equipment as necessary. '
Drum Sampling: Drum sampling will be performed in accor-
dance with the "Characterization of Hazardous Waste Sites - A
Methods Manual: Volume II, Available Sampling Methods",
EPA-600/4-83-040, September 1983. Drum sampling will include the
following sequence:
(1) Formulate a drum identification and numbering system to allow
tracking of samples from individual drums.
(2) Log drum information (e.g, assigned number, location, appar-
ent physical condition, etc.).
(3) Extract liquid drum sample using a peristaltic pump,
glass-tube, Composite Liquid Waste Sampler (COLIWASA), or
other suitable device. For solid material, a stainless steel
scoop or trowel waste pile sampler, sample trier, or other
suitable device should be used to obtain the sample.
(4) Fill and cap the volatile sample container. For liquids, the
container should be filled completely to eliminate air bubbles.
For solids, the sample container should be filled completely to
eliminate headspace.
(5) Record sampling information and observations in the bound
project notebook.
(6) Transfer sample custody to the sample coordinator.
(7) Decontaminate sampling equipment as necessary.
(8) The CO will direct the Contractor in sampling those drums, if
any, which are under pressure (e.g., bulging), according to
accepted EPA guidelines. Detailed procedures for
closed-container sampling can be found in the following docu-
ments: "Drum Handling Practices at Hazardous Waste Sites",
EPA/600/2-86/103, Cincinnati, Ohio, January, 1986, and
"Guidance Document for Cleanup of Surface Tank and Drum
Sites", OSWER Directive 9380.0-3, (NTIS PB- 87-110672), 28
May 1985.
Water Sampling: A grab sample will be collected from the
runoff/decon water storage tank each time the tank is full. At a
minimum, the Contractor's sampling protocol will include the follow-
ing sequence:
(1) Complete the sample container label (e.g., date and time of
sampling).
(2) Obtain a sample using an appropriate device.
(3) Fill and cap the sample container (for VOC samples, the
container should be completely filled to eliminate air bubbles).
(4) Label the sample container.
(5) Record sampling information and observations in the bound
project notebook.
(6) Transfer sample custody to the sample coordinator.
Samples should be immediately placed in a cooler and main-
tained at 4 degrees Celsius.
c. Sample Containers
Sample containers will be obtained from the approved EPA
Superfund supplier (Eagle-Picher of Miami, OK), which are
pre-cleaned to EPA specifications (USEPA CLP Statement of Work,
8/87). The Contractor will provide a list of sampling container
1* AR0002lf6
requirements for each analytical method (see Minimum Requirement
4) and sample media (e.g., liquid and solid). Sample container
specifications will be consistent with USAGE "Sample Handling
Protocols for Low, Medium, and High Concentration Samples, 3/89
(see Appendix 1).
d. Cleaning and Decontamination of Sampling Equipment
The Contractor will prepare a protocol by which sampling
equipment will be decontaminated before each use. The decon-
tamination protocol will include the following steps:
1. Wash equipment thoroughly with a non-phosphate laboratory
detergent and hot water, scrubbing with a brush to remove
surface film and particulates.
2. Rinse with tap water.
{ 3. Rinse thoroughly with deionized water.
4. Rinse equipment with pesticide-grade isopropanol.
5. Rinse with deionized water.
6. Air dry.
7. Wrap in aluminum foil (shiny side out) for transport or stor-
age in the field.
e. Sample Preservation and Holding Times
The Contractor will provide a listing by analytical method
(see Minimum Requirement 4) of required sample containers (type,
size, etc.), preservatives, and holding times. Container and
preservative requirements and holding times will be consistent with
the USAGE "Sample Handling Protocol for Low, Medium and High
Concentration Samples of Hazardous Waste" (10/86).
AR00021*?
f. Documentation in Field Notebook
A bound project field notebook will be maintained by the
designated sampling coordinator to provide daily records of signifi-
cant events, observations, and measurements during field inves-
tigations. The field notebook will also provide a record of all
instrument maintenance and calibration activities. The field note-
book will be kept as a permanent record of all field sampling
activities. All sampling personnel are to use the field notebook.
To avoid contamination of the field notebook, observations and
measurements recorded in areas of contamination may be recorded
in a separately bound and numbered logbook before being trans-
ferred to the project field notebook. In such cases, the original
record must also be maintained, and the delayed entry must be
noted as such in the project field notebook.
At a minimum, sampling entries into the project field notebook
will include the following:
1. Purpose of sampling.
2. Rationale for sampling.
3. Description of sampled materials (e.g., excavated soil in
roll-off container).
4. Date and time of sample collection.
5. Location of sampling point.
6. Description of sampling point.
7. Type of sample taken (e.g., solid or liquid).
8. Suspected composition.
9. Number of samples taken.
10. Sampling methodology.
11. Sample identification number.
12. References such as maps or photographs of the sample lo-
cation or drum.
13. The disposition of all samples materials after excavation.
14. Field measurements.
15. Signature of personnel responsible for observations.
16. Signed record of sample(s) transfer between the field sampler
and the sampling coordinator, including date and time.
17. Sample distribution (laboratories) and method of shipment.
g. Sample Labeling, Packaging and Shipment Requirements
The Contractor will include the following minimum require-
ments for sample labeling, packaging, and shipment: (Note: This
guidance is for low level contaminants only, classified as "Environ-
mental Samples" for shipment purposes. Should it be determined
that the samples are medium or high concentration hazardous
wastes, the Contractor will prepare a protocol which meets EPA
and DOT requirements for the shipment of hazardous materials.
Guidance and information on the proper labeling, packaging and
shipping of Environmental and Hazardous Samples can be found in
"A Compendium of Superfund Field Operations Methods,"
EPA/540/P- 87/001, December, 1987, and the USAGE "Sample
Handling Protocol for Low, Medium, and High Concentration Sam-
ples of Hazardous Wastes" (included as Attachment 1).
1. Samples will be transported to the Contractor's and QA labo-
ratories in waterproof metal or equivalent strength plastic
coolers.
17
2. Before placing a sample in its container, the field sampler
write the following information in indelible ink on the contain-
er label:
a. date
b. time of collection
c. site name
d. brief description of contents
e. intended analytes
f. preservation used
Note: Labels which do not float or soak off must be used.
3. Discrete samples will be placed in clear plastic bags and
placed upright in the cooler for transport. The containers will
be segregated such that they cannot touch each other during
sample shipment.
4. On water samples, the volume will be marked with a grease
pencil.
5. Approximately three inches of vermiculite or peanut styrofoam
cushioning material will be placed in the bottom of the cooler.
6. Additional vermiculite or peanut styrofoam packing material
will be placed in the cooler to partially cover the sample
bottles (more than half way). Sufficient ice will then be
placed among and on top of the bottles to cool the samples to
4 degrees Celsius.
7. The cooler will then be filled with cushioning material.
8. The chain-of-custody record will be placed in a . waterproof
plastic bag and secured with masking tape to the inside of
the cooler lid.
9. The cooler drain will be taped shut.
is ftR000250
10. The lid will be secured with strapping tape by wrapping
completely in at least two locations. (Taping should not
obscure any labels place on the cooler).
11. The shipping label will be attached to the top of the cooler.
The label will contain the words "Environmental Samples".
12. "This Side Up" labels will be placed on all four sides of the
cooler. "Fragile" labels will be placed on at least two sides.
13. Numbered and signed custody seals will be affixed on the
right front and back of the cooler. These seals will be
covered with wide, clear tape.
14. Sample coolers will be shipped by overnight common carrier
service (e.g., Federal Express), or driven directly from the
site to the Contract Laboratory. An example of the standard
Federal Express airbill is shown'in Figure 3.
h. Chain-of-Custody Procedures
To document sample possession, the Contractor will maintain a
chain-of-custody (COG) record for each sample. A sample is
under custody if one or more of the following criteria are met:
The sample is in the sampler's possession
It is in the sampler's view after being in his possession
It was in the sampler's possession and then was locked up to
prevent tampering
It is in a designated secure area.
i. Field Custody
The Contractor will provide the names of individuals responsi-
ble for collecting samples in the field. As few people as possible
should handle samples. The contractor will also designate
19
AROQQ25
- .one sample coordinator. Each field sampler will be personally/-,•
responsible for the care and custody of the samples collected until
the samples are transferred to the sample coordinator. The sample
coordinator will maintain care and custody until the samples are
shipped to the contract or QA laboratory. The sample coordinator
will also be responsible for the proper packaging and shipment of
the samples, as described above (item g).
Transfer of Custody and Shipment
The Contractor will devise a transfer of custody protocol that
will meet or exceed the following minimum specifications: (Note:
It is assumed here that the samples contain low level contaminants
and will be classified as "Environmental Samples" for shipment
purposes. Should it be determined that the samples are high
concentration hazardous wastes, the Contractor will prepare a
protocol meeting EPA and DOT requirements for the shipment of
hazardous materials. Guidance and information on the proper
labeling, packaging and shipping of Environmental and Hazardous
Samples can be found in "A Compendium of Superfund Field Op-
erations Methods". Attachment 1 specifies the USAGE Sample
Handling Protocol for Low, Medium, and High Concentration Sam-
ples of Hazardous Waste".)
Each sample shipment (i.e., each cooler) to the contract or
QA laboratory will be accompanied by a separate COG form (see
Attachment 1) identifying the shipment's contents. The purpose of
the COC record is to document sample transfer from the field
custodian to the contract or QA laboratory. When transferring a
20 AROOQ252
sample shipment, the individuals relinquishing and receiving the
shipment will sign, date and note the time on the COC forms. The
original form accompanies the shipment; copies are retained by the
sample coordinator.
Samples will be shipped to the contract and QA laboratories
by overnight common courier (e.g., Federal Express). Air bills,
receipts, etc., will be maintained as part of the permanent docu-
mentation of the COC records. The method of shipment, courier
name(s), and other pertinent information (e.g., the laboratory
name) should be entered in the "Remarks" section of the COC
form.
The following procedures will be followed in using the COC
forms:
1. The sample coordinator will fill in all requested information
from the sample labels.
2. The sample coordinator will sign the COC at the "Relinquished
By" box and retain a copy.
3. The person receiving custody will check the information on
the sample labels against the COC form. He/she will also
check the condition of the samples and note anything unusual
in the "Remarks" section of the COC form. However, it is
not necessary that the agent acting for the common courier
sign the COC.
4. The person receiving custody of the sample shipment will sign
the "Received by" box and keep the original of the COC
form.
5. The Date/Time must be the same for both signatures since
custody must be transferred to another person.
21 HROQQ253
'••-,-'•>6. When custody is transferred to the contract or QA Laboratb- -'
ry, the last "Relinquished By" and Received By" boxes are
signed, and a line will be drawn through all unused signature
boxes.
7. In all cases, it must be evident that the same person who has
received the sample shipment has relinquished it to the next
custodian.
8. If samples are left unattended or a person refuses to sign the
COC, this will be documented and explained on the COC
form.
k. Laboratory Custody
The contract laboratory must have an adequate COC proce-
dure. If the contract laboratory is not in the EPA Contract
Laboratory Program, the Contractor must provide the laboratory's
custody procedures (Part of the Laboratories Standard Operating
Procedures).
At a minimum, the Contractor will specify an individual in the
contract laboratory who is responsible for sample custody. The
designated custodian of laboratory samples will accept custody of
shipped samples and verify that the information on the sample
labels matches that on the COC forms. The custodian will also
inspect the samples for any leakage and check that the sample seal
is intact. As appropriate, the custodian will enter pertinent
information on shipment, pickup, courier, and condition of samples
in the "Remarks" section of the COC forms. Any discrepancies
should be resolved before the sample is assigned for analysis.
The laboratory custodian will then assign a unique laboratory
22 AR0002514
CV;::-H-number to each sample, and transfer the samples to the appropn- '
ate analyst or secure them in a restricted access storage area.
Laboratory analysts will be responsible for the care and custody of
samples in their possession.
When sample analyses and necessary quality assurance checks
have been completed, the unused portion of the sample and the
sample containers must be properly disposed. All data sheets and
laboratory records will be retained as part of the permanent docu-
mentation.
23
AR000255
SECTION 4 - ANALYTICAL METHODS/PROCEDURES
Samples of soil and marked drum material will be analyzed for EPA
TCL VOCs, BNAs, metals and pesticides/PCBs. All chemical analyses
will be performed according to CLP and SW-846 methodologies. Parame-
ters to be analyzed, detection and control limits for CLP are listed in
Table 1.
Samples from marked drums and soil samples from roll-off or bulk
containers will also be analyzed for hazardous waste characteristics: EP
TOX, ignitability, corrosivity, flammability, sulphides, cyanides and
phenolics (listed in SW-846 [1986]). Further, any additional testing
required by the RCRA incineration facility will be performed at that
time.
One sample from each unmarked drum containing liquid material will
undergo compatibility testing (see listing of tests in Section 3[a]). In
addition, at the discretion of the CO, one sample from each unmarked
drum containing solid material may also undergo compatibility testing.
Upon completion of compatibility testing, 2-5 drums of liquid or solid
material (liquid material will not be composited with solid material) will
be composited into one drum. One sample will be collected and analyzed
for the hazardous waste characteristics listed above. At that time, any
additional testing required by the RCRA incineration facility will be
performed.
Water samples from the storage tanks containing runoff and decon-
tamination water will be analyzed for the following parameters: VOCs,
BNAs, heavy metals, and PCBs. The following analytical methods will
be used for the indicated parameters: VOCs - EPA Methods 601 and
24
602; BNAs - EPA Method 625; heavy metals (except mercury) - EPA '"l!
Method 200.7; mercury - EPA Method 245.1; PCBs - EPA Method 608.
Air quality will be analyzed with real-time and time-weighted
average measurements. The following real-time measurements will be
collected: organic vapors in the breathing zone in the area of exca-
vation and at the site perimeter, using portable photoionization detec-
tors or flame ionization detectors; explosive atmospheres in the area of
excavation using a combination explosimeter/oxygen meter; and inorgan-
ic particulates at the site perimeter using a Miniram or similar device.
The time-weighted samples which will be collected are organic
vapors at the site perimter and in the breathing zone for personnel in
the area of excavation. Samples will be collected with personal air
pumps and charcoal tubes, and will be analyzed by NIOSH Method 1003.
The Contractor will provide the names of chemical quality man-
agement personnel performing each method, and the instrumentation and
equipment to be employed in the analyses.
SR000257
SECTION 5 - ANALYTICAL/STATISTICAL CONTROL PARAMETERS
a. Accuracy
Accuracy is a measure of bias in a measurement system.
Sources of bias or error include the sampling process, field con-
tamination, preservation, sample matrix effects, sample preparation
and analytical techniques. Sampling accuracy may be assessed
through the use of field and trip blanks. Analytical accuracy may
be used through the use of known or unknown QC samples and
matrix and surrogate spikes.
Prior to initiation of construction activities, the contract
laboratory will be required to satisfactorily determine the concen-
trations of analytes in a performance audit sample submitted by the
Missouri River Division laboratory. Analytes will include all pri-
ority pollutant list compounds.
Routine assessment of accuracy will be accomplished through
the analysis of matrix spikes/matrix spike duplicates (MS/MSD),
surrogate spikes, as well as trip and field blanks. The recoveries
from spikes must be within the QC limits specified under EPA CLP
Statement of Work (8/87) or "Test Methods of Evaluating Solid
. Wastes" (SW-846, 1986), depending on the analytical methods
employed. The frequency of MS/MSD and surrogate spikes will, at
a minimum, meet the QC requirements of EPA CLP or SW-846,
depending on the analytical method employed.
b. Sensitivity
The Contractor will provide a listing of method detection
limits for priority pollutant compounds, based on QC requirements
26 flROOQ258
specified in either the EPA CLP Statement of Work (8/87) or "Test
Methods for Evaluating Solid Wastes" (SW-846, 1986).
c. Precision
Precision is a measure of the agreement between a set of
replicate results. Overall precision (sampling plus analytical
precision) will be assessed based on duplicate field samples (exca-
vation/construction area soil and drum samples) and matrix spike
duplicates. Analytical precision will be based on the analysis of
matrix spike/matrix spike duplicates. Regarding overall precision,
duplicates should agree at least qualitatively. For duplicate water
samples, the relative percent difference (RPD) should not exceed
25 percent. For soil duplicates, the RPD should not exceed 50
percent. Should any duplicate show disagreement (as to the
presence of a particular contaminant) between the contract labo-
ratory and the QA laboratory, corrective measures will be taken.
Regarding analytical precision, the RPD between matrix spikes and
matrix spike duplicates must be within the QC limits specified
under "EPA CLP Statement of Work for Organics and Inorganics"
(2/88, 8/87, respectively) or "Test Methods for Evaluating Solid
Wastes" (SW-846), depending on the EPA analytical methodology
employed.
d. Quantity/Frequency of Samples
The number of samples to be collected will depend on what is
encountered during excavation activities. Each intact or partially
intact drum is to be sampled (refer to Section 3). One set of
composite samples will be collected from each roll-off or bulk
container holding soils to be disposed off-site. A total of 58 soil
27 flR000259
samples .will be collected from the soil remaining in the trenches'
after drums and soil in immediate contact with drums (within 18
inches) are excavated. Also, one water sample will be collected
from each full storage tank holding runoff/decon water. Further,
four time-weighted air samples will be collected each week.
The Contractor will collect QC samples, at a minimum, in the
following relative frequencies:
Trip blanks - one per cooler of samples for volatiles analyses.
Field Blanks - 10% of the number of liquids samples collected
each week from marked drums.
Duplicate/Split - 10% of the number of samples collected each
week from soil and marked drums.
USAGE requirements for chemical QA/QC are provided in
Attachment 2.
e. Contractor Internal QC Checks
The Contractor will provide a description of the nature and
frequency of internal QC checks. At a minimum, these QC checks
will consist of the following elements.
Internal QC checks will involve the analysis of trip and field
blanks, field duplicates and splits. Additional QC checks will
include the analysis of surrogate spikes, matrix spikes and matrix
spike duplicates, method and instrument blanks, and the perfor-
mance of standard calibration according to QC requirements spec-
ified in the EPA "CLP Statement of Work" or "Test Methods for
Evaluating Solid Wastes" (SW- 846). The Contractor will explicitly
itemize the QC requirements (e.g., frequency of MS/MSD) stipulat-
ed by the EPA analytical methods to be employed.
28
Should internal laboratory QC results fall outside the EPA
specified QC limits, or should duplicates show disagreement on the
presence of a particular contaminant, corrective measures will be
taken. The Contractor will provide a description of potential
corrective actions to be implemented by the QC manager. These
options may include renewal of standards, recalibration, instrumen-
tation checks, resampling, recheck of instrument and method
blanks, accepting data with known levels of uncertainty, and
discarding the data. If a problem cannot be resolved, the QC
manager will consult with the QA laboratory. The Contractor will
provide to the USAGE the chain of communication and events
leading to the implementation of corrective action, and will provide
a list of corrective action options that will be considered.
f. External QA Samples
External QA samples will be taken at the same frequency as
the internal field QC samples, as specified above (Quantity Fre-
quency of Samples), for submittal to the USAGE Missouri River
Division Laboratory (CEMRD-ED-L). The contract laboratory will
promptly report analytical results for internal field QC samples to
the CO, and forward the results to the CEMRD-ED-L for compari-
son with the CEMRD-ED-L's results. Serious discrepancies be-
tween the two sets of data will be reported by CEMRD-ED-L to the
USAGE.
g. Representative Samples
The Contractor will describe the supportive rationale that
samples are representative of the matrix being analyzed or the site
location. The supportive rationale will include the use of
29 AR00026I
EPA-recommended procedures for the collection and handling of
environmental samples. Appropriate source documents for environ-
mental sampling procedures include: "Methods for the Collection
and Analysis of Water and Waste Water"(EPA 600/4-79-020);
"Sampling and Sampling Procedures for Hazardous Wastes Sources
(EPA 600/27-80-018), EPA Regional Standard Operating Proce-
dures, Guideline and Directives"; and, "Compendium of Superfund
Field Operations Methods" (EPA/540/P-87/001).
The objective of sampling in the excavation area is to identify
the contaminants present in the drums and soil in immediate con-
tact with the drums. Composite soil samples will be collected from
each roll-off or bulk container holding soil to be disposed off-site.
Grab samples will be collected from the soil remaining in the
trenches following excavation of drums and soil in immediate con-
tact with the drums. The number of sampling locations is dis-
tributed among the six areas of excavation, based on surface area.
No more than one sample will be collected in each trench. The
exact sampling locations will be randomly selected by the CO. In
addition, drummed materials and runoff/decon water will be
sampled in a manner which meets the objective of acquiring rep-
resentative samples.
In addition to identifying the nature of contamination, the
objective of sampling efforts will be to determine the material's and
soil's hazardous waste characteristics for subsequent transport to a
RCRA-approved incinerator. A representative indication of con-
tamination will, therefore, be obtained by analyzing one composite
30 flR000262
soil sample from each roll-off or bulk container, and one sample
from each excavated drum containing solid or liquid materials.
The USAGE CO will specify the number and locations of
individual samples from each of the excavated areas to meet dis-
posal requirements.
h. Data comparability
To ensure data comparability, analytical results must be re-
ported in consistent units. Concentrations of soil/solid drum
residue will be reported in units of ug/kg (ppb) dry weight.
Liquid samples will be reported in ug/L (ppb).
i. Performance and Audit Samples
An initial performance audit sample will be provided by the
Division Laboratory as a requirement for validation of the contract
laboratory, prior to initiation of excavation and removal activities.
One or more additional performance audit samples may be sent to
the contract laboratory if the quality of data is in question during
excavation and removal activities.
SECTION 6 - CALIBRATION PROCEDURES AND FREQUENCY
a. Each analytical instrument will be calibrated in a manner and
frequency consistent with the requirements for CLP routine .analytical
services (RAS) specified in the USEPA CLP Statements of Work for
Inorganics Analysis and Organics Analysis (7/87 and 2/88, respectively)
or with requirements specified in "Test Methods for Evaluating Solid
Wastes" (SW-846). EPA-CLP control limits and analytes are presented
in Table 1.
b. Field Instrument (HNu PI-101)
The HNu PI-101 is a portable, non-specific vapor/gas detector
employing the principle of photoionization to detect a variety of
chemical compounds. During excavation activities, the HNu (or
equivalent instrument) will be used to detect volatile contaminants
in the excavation areas and at the site perimeter.
The HNu PI-101 photoionization detector will be operated,
maintained, and calibrated in accordance with the manufacturer's
recommendations and instructions by one or two individuals trained
in the proper use of the HNu meter. (Training courses may be
given by the manufacturer, other commercial entities, or the EPA).
The Contractor will provide, as an exhibit to the USAGE, a de-
tailed and specific calibration and operation instruction sheet which
will accompany the PID in the field. Calibration procedures and
frequency will be in accordance with guidelines presented in "A
Compendium of Superfund Field Operations Methods"
(EPA/540/P-87/001). Documentation of instrument use, including
32
dates of use, instrument identification number, maintenance and
calibration functions, and instrument readings will be maintained in
the project field notebook.
3RQQ0265
SECTION 7 - PREVENTATIVE MAINTENANCE
a. Laboratory Maintenance
The Contractor will provide a copy of the Standard Operating
Procedures employed by the contract laboratory. Included in the
SOP will be a general description of preventative maintenance
activities and schedules for all analytical instruments and equip-
ment. The contract laboratory will be required to document all
maintenance activities by detailed entries into appropriate log
books.
b. Field Maintenance
The Contractor will provide detailed field sheets for routine
operation and maintenance of each field instrument which will
accompany the equipment in the field. At a minimum, a field sheet
will be prepared for the HNu PI-101 photoionization detector. The
Contractor will follow the manufacturer's recommendations and
instructions for the general operation of the HNu meter. The
schedule of maintenance and calibration activities for the HNu will,
at a minimum, be according to that outlined in "A Compendium of
Superfund field Operations Methods". All maintenance activities
will be documented in the project field notebook.
34 flR000266
SECTION 8 - DATA ANALYSIS AND REPORTING
The Contractor will describe the following for each analytical
method and major measurement parameter:
a. The data analysis scheme (including units and equations) required
to calculate concentrations or the value of the measured parameter.
b. The principle criteria used to assure data integrity during col-
lection and reporting.
c. Plans for treating outliers.
d. Description of the data management systems including, but not
limited to, the collection of raw data, data storage, and data
quality assurance documentation.
e. Identification of raw data, data storage, and data quality control
and quality assurance documentation.
f. Identification of individuals to be involved in the reporting se-
quence. The contract laboratory will utilize the reporting format
and provide the quality control documentation described in "Test
Methods for Evaluating Solid Wastes" (SW-846).
35
SR000267
SECTION 9. CONSTRUCTION CONTRACTOR DAILY
QUALITY CONTROL REPORTS
a. Construction Contractor Daily Quality Control Reports will be
prepared by the Contractor and submitted to the CO. Each report
will contain, at a minimum, the following: 1) location of work; 2)
weather conditions; 3) work performed; 4) specific inspections
performed and results; 5) QA/QC problems encountered; 6) cor-
rective actions, if any; 7) verbal or written instructions from
government personnel for re-analysis or re-sampling of materials;
8) types of measurement and analyses performed, samples collect-
ed, personnel involved, and the results of measurements and
analyses; 9) general remarks; 10) instrument maintenance and
calibration procedures; and, 11) Contractors certification.
b. Corrective Action Reports
The USAGE Omaha District will be notified by phone within 24
hours if any corrective action is determined to be necessary. All
corrective actions will be documented in a written report and sent
to the USAGE Omaha District. The report will describe in detail
the reason for corrective action, the nature of the corrective
action and the expected result. All relevant QA/QC will b^ provid-
ed for review, as indicated in ER 1110-1-263.
c. Summary Report
At the conclusion of excavation and construction activities,
the Contractor will submit a report to the USAGE outlining the QC
practices employed by the Contractor. The report will briefly
describe all quality control problems encountered, and all
5R000268
corrective actions taken during construction activities. The report
will contain a consolidation and summary of the Construction Con-
tractor Daily Quality Control Reports, all quality control documen-
tation generated by the Contract Laboratory, and a consolidation
of all chemical data.
37 &RQQQ269
SECTION 10 - PERFORMANCE AUDITS
The Contractor will submit samples to the external QA laboratory.
These samples will include duplicate samples as well as trip and field
blanks.
The QA lab will submit a performance audit sample to the contract
lab as part of the laboratory validation procedure. As identified by the
USAGE and contract QA/QC managers, additional performance audit
samples may be submitted to the contract lab by the QA lab to resolve
problems in the quality of data. Pre-cleaned containers available from
the EPA through the Missouri River Division Laboratory will be used for
performance audit samples.
38 5R000270
Tables
flR00027l
Table 1. Page 1 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
HSl TCL VOLATILES - MATRIX: AQUEOUS
QUANTITATIONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
chlororoethane 10 SEE BELOW** SEE BELOW** SEE BELOW**bromomethane 10 " " "vinyl chloride 10 " " * "chloroethane 10 " " "methylene chloride 5 " " "acetone 10 " " "carbon disulfide 5 " " "1,1-dichloroethene 5 " " "1,1-di chloroethane 5 " " »1,2-dichloroethene 5 » " »chloroform 5 " " "1,2-dichloroethane 5 " » "2-butanone 10 " " »1,1,1-trichloroethane 5 » » "carbon tetrachloride 5 " " "vinyl acetate 10 " " "bromodichloromethane 5 " " "1,2-dichloropropane 5 " " "c-1,3-dichloropropene 5trichloroethene 5dibromochloromethane 51, 1,2-trichloroethane 5benzene 5t-1,3-dichloropropene 5bronwform 54-nethyl-2-pentanone 102-hexanone 10tetrachloroethene 5toluene 51,1,2,2-tetrachloroethane 5ch I orobenzene 5ethyl benzene 5styrene 5xylenes (total) 5
+ Specific quantisation limits are highly matrix dependent. The quantisation limits listedhere are provided for guidance and may not always be achievable.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised: 1/87, 2/87, 7/87, 2/88. IFB-W802035 01, IFB W802036 01,IFB W802081 D1.
**Frequency tables are on the following page.
13 July 89
flR000272
Table 1. Page 2 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
HSL TCL VOLAT1LES - MATRIX: AQUEOUS
AUDITSurrogate Spike
MS/MSD
CalibrationContinuing
Method Blank
MS Tuning
CalibrationVerification
FREQUENCYAll samples and blank (includ-ing MS/MSD).
1 per case or 1 in 20 ofsimilar concentration/matrix.
Each 12 hours
1 in 20-provided by samplingcrew
Every 12 hours.
Once
CONTROL LIMITSRecovery limits within those of Table 4.2, Exhibit E
Recovery limits within those of Table 5.2, Exhibit E
Minimum RF 0.300; must be less than 25% difference for anycheck compound. Table 2.2, also E-15 to E-17, Sections2.6 - 2.7.Less than 5 times CRQL for methylene chloride, acetone,toluene, and 2-butanoneLess than CRQL for all other TCL compounds
BFB key ions and abundance criteria must be met forall 9 ions. Table 1.1, Exhibit E
Five concentrations - linear range volatiles 20 -200 mg/L. See Part 2, E-12 to E-15, Sections 2 - 2.5.
13 July 89
AR000273
Table 1. Page 3 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL VOLATILES - MATRIX: SOLIDS
QUANT I TAT I ONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
chloromethane 10 SEE BELOW** SEE BELOW** SEE BELOW**bromomethane 10 " " "vinyl chloride 10 " " "chloroethane 10 " " "methylene chloride 5 " " "acetone 10 " '• "carbon disulfide 5 " » "1,1-dichloroethene 5 » " "1,1-dichloroethane 5 " " »1,2-dichloroethene 5 " " "chloroform 5 " " "1,2-dichloroethane 5 » " "2-butanone 10 " " "1,1,1-trichloroethane 5 " " "carbon tetrachloride 5 " " »vinyl acetate 10 " " "bromodichloromethane 5 " " "1,2-dichloropropane 5 " " "c-1,3-dichloropropene 5 " " "trichloroethene 5 " " "dibromochloromethane 5 " » "1,1,2-trichloroethane 5 " " "benzene 5 » " "t-1,3-dichloropropene 5 " " "bromoform 5 " " "4-methyl-2-pentanone 10 " " "2-hexanone 10 " " "tetrachloroethene 5 " " "toluene 5 " " "1,1,2,2-tetrachloroethane 5 " " "chlorobenzene 5 " " "ethyl benzene 5 " " "styrene 5 " " "xylenes (total) 5 " " "
+ Specific quant i tat ion limits are highly matrix dependent. The quantisation limits listedhere are provided for guidance and may not always be achievable.
Medium Soil/Sediment Contract Required Quantitation Limits (CRQL) for VolatileCompounds are 125 times the individual Low Soil/Sediment CRQL. Quantitat ion limits listedfor soil/sediment are based on wet weight. The quantitation limits calculated by thelaboratory for soil/sediment, calculated on dry weight basis as required by the contract,will be higher.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised! 1/87, 2/87, 7/87, 2/88. IFB-W802035 01, IFB WS02036 01,IFB W802081 D1.
**Frequency table is on the following page.
13 July 89
Table 1. Page 4 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL VOLATILES - MATRIX: SOLIDS
AUDITSurrogate Spike
MS/MSD
CalibrationContinuing
Method Blank
MS Tuning
CalibrationVerification
FREQUENCYAll samples and blank (includ-ing MS/MSD).
1 per case or 1 in 20 ofsimilar concentration/matrix.
Each 12 hours
1 in 20-provided by samplingcrew
Every 12 hours.
Once
CONTROL LIMITSRecovery limits within those of Table 4.2, Exhibit E
Recovery limits within those of Table 5.2, Exhibit E
Minimum RF 0.300; must be less than 25% difference for anycheck compound. Table 2.2, also E-15 to E-17, Sections2.6 - 2.7.Less than 5 times CRQL for methylene chloride, acetone,toluene, and 2-butanoneLess than CRQL for all other TCL compounds
BFB key ions and abundance criteria must be met forall 9 ions. Table 1.1, Exhibit E
Five concentrations - linear range volatiles 20 -200 mg/L. See Part 2, E-12 to E-15, Sections 2 - 2.5.
13 July 89
AR000275
Table 1. Page 5 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL SEMI-VOLATILES - MATRIX: AQUEOUS
QUANT I TAT I ONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
phenol 10 SEE BELOW SEE BELOW SEE BELOWbis(2-chloroethyl) ether 10 « " »2-chlorophenol 10 " " "1,3-dichlorobenzene 10 " " "1,4-dichlorobenzene 10 " " "benzyl alcohol 10 " " "1,2-dichlorobenzene 10 " " "2-methylphenol 10 " " "bis(2-chloroisopropyl) ether 10 " " "4 -methyl phenol 10 " » "N-nitroso-di-n-propylamine 10 " " "hexachloroethane 10 " " "nitrobenzene 10 " " "isophorone 10 " " "2-nitrophenol 10 " " "2,4-dimethylphenol 10 " " »benzoic acid 50 " » "bis(2-chloroethoxy)methane 10 " " "2,4-dichlorophenol 10 " " "1,2,4-trichlorobenzene 10 " " "naphthalene 10 " " "4-chloroaniline 10 " " "hexachlorobutadiene 10 " " "4-chloro-3-methylphenol 10 " " »2-methylnaphtalene 10 " " "hexachlorocyclopentadiene 10 " " "2,4,6-trichlorophenol 10 " " "2,4,5-trichlorophenol 50 " " »2-chloronaphthalene 10 " " »2-nitroaniline 50 " " "dimethyl phthalate 10 " " "acenaphthylene 10 " " "2,6-dinitrotoluene 10 " " "3-nitroaniline 50 " " "acenaphthene 10 " " "2,4-dinitrophenol 50 " " »4-nitrophenol 50 " " "dibenzofuran 10 " " "2,4-dinitrotoluene 10 " " "di ethyl phthalate 10 " " "4-chlorophenyl phenyl ether 10 " « "fluorene 10 » " "4-nitroaniline 50 " " "4,6-dinitro-2-methylphenol 50 » " "N-nitrosodiphenylamine 104-bromophenyl phenyl ether 10hexachlorobenzene 10pentachlorophenol 50phenanthrene 10anthracene 10di-n-butylphthalate 10fluoranthene 10pyrene 10
13 July 89
WOOQ276
Table 1. Page 6 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL SEMI-VOLATILES - MATRIX: AQUEOUS
QUANTITAT IONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
butyl benzyl phthalate 10 SEE BELOW SEE BELOW SEE BELOW3,3'-dichlorobenzidine 20 " " "benzo(a)anthracene 10 " " "chrysene 10 " " "bis(2-ethylhexyl)phthalate 10 '< " "di-n-octyl phthalate 10 " " "benzo(b)fluoranthene 10 " " "benzo(k)fluoranthene 10 " " "benzo(a)pyrene 10 '• " "indeno(1,2,3-c,d)pyrene 10 » » "dibenzo(a,h)anthracene 10 " " "benzo(g,h,i)perylene 10 » » "
+ Specific quantisation limits are highly matrix dependent. The quantitat ion limits listedhere are provided for guidance and may not always be achievable.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised: 1/87, 2/87, 7/87, 2/88. IFB W802035 D1, IFB W802036 D1,IFB W802081 D1.WA87-K238.
AUDITSurrogate Spike
MS/MSD
CalibrationContinuing
MethodBlank
MS Tuning
CalibrationVerification
FREQUENCYAll samples and blank (includ-ing MS/MSD).
1 per case or 1 in 20 ofsimilar concentration/matrix.
Each 12 hours
1 per extraction group
Each 12 hours.
Once
CONTROL LIMITSRecovery limits within those of Table 4.2, Exhibit E
Recovery limits within those of Table 5.2, Exhibit E
Minimum RF 0.05; must be less than 25% difference for anycheck compound. Table 2.3, also #-32 to E-35, Sections2.6 - 2.7
Less than 5 times CRQL of the phthalate esters.Less than CRQL for all other TCL compounds.
DFTPP key ions & abundance criteria must be met for all 13 ionsTable 1.2, Exhibit E.
Five concentrations - linear range 20 - 160 ng.Four concentrations • nine compounds (See Section 2.1.1.)50 - 160 ng/L.See Part 2, E-30 to E-32, Sections 2 - 2.5.
13 July 89
flROOQ277
Table 1. Page 7 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL SEMI-VOLATILES - MATRIX: SOLIDS
QUANT I TAT I ONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
phenol 330 SEE BELOW SEE BELOW SEE BELOWbis(2-chloroethyl) ether 330 » » "2-chlorophenol 330 » " "1,3-dichlorobenzene 330 " » »1,4-dichlorobenzene 330 " " "benzyl alcohol 330 " » »1,2-dichlorobenzene 330 » » «2-methylphenol 330 " " '•bis(2-chloroisopropyl)ether 330 " " "4-methylphenol 330 " " «N-nitroso-di-n-propylamine 330 " " "hexachloroethane 330 " " "nitrobenzene 330 " " "isophorone 330 " " "2-nitrophenol 330 » " "2,4-dimethylphenol 330 " " "benzoic acid 600 " " "bis(2-chloroethoxy)methane 330 " " "2,4-dichlorophenol 330 " " "1,2,4-trichlorobenzene 330 " " "naphthalene 330 " " "4-chloroaniline 330 " " "hexachlorobutadiene 330 " " "4-chloro-3-methylphenol 330 " " "2-methylnaphtalene 330 " " "hexachlorocyclopentadiene 330 " " "2,4,6-trichlorophenol 330 " " "2,4,5-trichlorophenol 600 " " "2-chloronaphthalene 330 " « "2-nitroaniline 600 " " "dimethyl phthalate 330 " " "acenaphthylene 330 " " "2,6-dinitrotoluene 330 " " "3-nitroaniline 600 " " "acenaphthene 330 " " "2,4-dinitrophenol 600 " " "4-nitrophenol 600 " " "dibenzofuran 330 « » »2,4-dinitrotoluene 330 " " "diethyl phthalate 330 '• " "4-chlorophenyl phenyl ether 330 " " "fluorene 330 '4-nitroaniline 6004,6-dinitro-2-methylphenol 600N-nitrosodiphenylamine 3304-bromophenyl phenyl ether 330h exach I orobenzene 330pentachlorophenol 600 " " "phenanthrene 330 " " "anthracene 330 " " "di-n-butylphthalate 330 » " "fluoranthene 330 " " "pyrene 330 " " "
13 July 89
3ROQQ278
Table 1. Page 8 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL SEMI-VOLATILES - MATRIX: SOLIDS
QUANTI TAT IONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
butyl benzyl phthalate 330 SEE BELOW SEE BELOW SEE BELOW3,3'-dichlorobenzidine 660 " "benzo(a)anthracene 330 " "chrysene 330 " "bis(2-ethylhexyl)phthalate 330 » "di-n-octyl phthalate 330 " "benzo(b)fluoranthene 330 " "benzo(k)fluoranthene 330 " "benzo(a)pyrene 330 " "indeno(1,2,3-c,d)pyrene 330 " " "dibenzo(a,h)anthracene 330 " " "benzo(g,h,i)perylene 330 " " "
+ Specific quantisation limits are highly matrix dependent. The quantisation limits listedhere are provided for guidance and may not always be achievable.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised: 1/87, 2/87, 7/87, 2/88. IFB W812135D1, U80203601,IFB W802036 D1.
**Medium Soil/Sediment Contract required Quantitation Limits (CRQL) for Semi-volatileCompounds are 60 times the individual Low SoiI/Sediment CRQL.
Quantitation limits listed for soil/sediment are based on wet weight. The quantisationlimits calculated by the laboratory for soil/sediment, calculated on dry weight basis asrequired by the contract, will be higher.
AUDITSurrogate Spike
MS/MSD
CalibrationContinuing
MethodBlank
MS Tuning
CalibrationVerification
FREQUENCYAll samples and blank (includ-ing MS/MSO).
1 per case or 1 in 20 ofsimilar concentration/matrix.
Each 12 hours
1 per extraction group
Each 12 hours.
Once
CONTROL LIMITSRecovery limits within those of Table 4.2, Exhibit E
Recovery limits within those of Table 5.2, Exhibit E
Minimum RF 0.05; must be less than 25% difference for anycheck compound. Table 2.3, also #-32 to E-35, Sections2.6 - 2.7
Less than 5 times CRQL of the phthalate esters.Less than CRQL for all other TCL compounds.
DFTPP key ions & abundance criteria must be met for all 13 ionsTable 1.2, Exhibit E.
Five concentrations - linear range 20 - 160 ng.Four concentrations - nine compounds (See Section 2.1.1.)50 - 160 ng/L.See Part 2, E-30 to E-32, Sections 2 - 2.5.
13 July 89
flR000279
Table 1. Page 9 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP METALS - MATRIX: AQUEOUS
QUANTITATIONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
M9/Laluminum 200 SEE BELOW SEE BELOW SEE BELOWantimony 60 " " "arsenic 10 " " "barium 200 " » "beryllium 5 " " "cadmium 5 " " "calcium 5000 " " "chromium 10 " " "cobalt 50 " " "copper 25 " " "iron 100 " » "lead 3 n n »magnesium 5000 " " "manganese 15 " " "mercury 0.2 " " "nickel 40 " » "potassium 5000 " " "selenium 5 " " »silver 10 " "sodium 5000 " " "thallium 10 " " "vanadium 50 » " "zinc 20 " " "cyanide 10 " " '•
* U.S.EPA Contract Laboratory Program Statement of Work For Inorganics Analysis Multi-mediaMulti-concentration. SOW NO. 788. DP00205R1, D900206R1, D900207R1.
+ Subject to the Restrictions specified in the first page of Part 6, Section IV of ExhibitD (Alternate Methods - Catastrophic Failure) any analytical method specified in SOW ExhibitD may be utilized as long as the documented instrument or method detection limits meet theContract Required Detection Limit (CRDL) requirements. Higher detection limits may only beused in the following circumstances:
If the sample concentration exceeds 5 times the detection limit of the instrument ormethod in use, the value may be reported even though the instrument or method detectionlimit may not equal the Contract Required Detection Limit. This is illustrated in theexample below:
For lead:Method in use * ICPInstrument Detection Limit (IDL) = 40Sample concentration * 220Contract Required Detection Limit (CRDL) => 5
The value of 220 may be reported even though instrument detection limit is greater thanCRDL. The instrument or method detection limit must be documented as described in Exhibit E.
The CRDL are the instrument detection limits obtained in pure water that must be met usingthe procedure in Exhibit E. The detection limits for samples may be considerably higherdepending on the sample matrix.
13 July 89
Table 1. Page 10 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP METALS - MATRIX: AQUEOUS
AUDITCalibrationVerification
CalibrationBlank
PreparationBlank
Spiked SampleAnalysis
DuplicateSample Analysis
Lab ControlSample(aqueous)
FREQUENCYCalibrated daily and each timeinstrument is set up; verify atat a frequency of 10% or every2 hr, whichever is greater.
During calibration at a fre-quency of 10% during run andat end of run.
1 per batch of samples digestedor 1 in 20 whichever is greater
1 per group of similar concen-tration and matrix, 1 per caseof samples, or 1 in 20, which-ever is greater.
Same as spiked sample analysis.
1 for each procedure for eachcase of samples received; 1 in20 or 1 per batch digested,whichever is greater.
CONTROL LIMITSWithin ±10% of true value for all except tin and mercury(±20% of true value).
No more than CRDL.
No more than CRDL.
Within ±25% recovery unless SSR exceeds SR by a factorof 4 or more
±20% RPD for values 5X CRDL or more tCRDL for samplesless than 5X CRDL
Within 80-120% recovery
Dissolved Metals: Those constituents (metals) which will pass through a 0.45fi membrane filter.
Field Filtration Protocol;An aliquot of sample will be passed through a 0.45ft membrane filter by one of the following methods:1) Plastic syringe equipped with a filter holder (Swimex Filter Holder).2) Hand vacuum pump and a 500 ml side arm, glass filtration flask.3) Bench top (electric) filtration system.
•Standards and samples will be matrix-matched to the concentration of the mineral acid.
•Calibration curves, continuing calibration and corrective measures records will be documented.
•One medium range internal synthetic standard will be analyzed to verify calibration and will bewithin ±10% of true value
•Furnace work will require duplicate analysis of each sample to verify recovery of spiked material. If. recoveries are within ±10%, methods of addition will not be required. If outside this criterion, methods ofstandard addition will be required.
•For chromium analysis, a nitrous oxide flame will be used.
13 July 89
flR00028l
Table 1. Page 11 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP METALS - MATRIX: SOLIDS
QUANTITATIONCHEMICAL COMPOUND* LIMIT + AUDIT FREQUENCY CONTROL LIMITS
mg/kgaluminum 40. SEE BELOW SEE BELOW SEE BELOWantimony 12. » " "arsenic 2. " " "barium 40. " " '«beryllium 1.0 " " "cadmium 1. " " »calcium 1000. " " "chromium 2. " " "cobalt 10. " » »copper 5. " » "iron 20. " " »lead 0.6 " " »magnesium 1000. " " "manganese 3. " " "mercury 0.1 " " »nickel 8. " " »potassium 1000. " " "selenium 1. " " "silver 2. "sodium 1000. "thallium 2. "vanadium 10. "zinc 4. »cyanide 1. "
* U.S.EPA Contract Laboratory Program Statement of Work For Inorganics Analysis Multi-mediaMulti-concentration. SOW NO. 788. D900205R1, D900206R1, D900207R2.
**Subject to the Restrictions specified in the first page of Part G, Section IV of Exhibit D(Alternate Methods - Catastrophic Failure) any analytical method specified in SOW Exhibit Dmay be utilized as long as the documented instrument or method detection limits meet theContract Required Detection Limit (CRDL) requirements. Higher detection limits may only beused in the following circumstances:
If the sample concentration exceeds 5 times the detection limit of the instrument ormethod in use, the value may be reported even though the instrument or method detectionlimit may not equal the Contract Required Detection Limit. This is illustrated in theexample below:
For lead:Method in use * ICPInstrument Detection Limit (IDL) * 40Sample concentration = 220Contract Required Detection Limit (CROL) = 5
The value of 220 may be reported even though instrument detection limit is greater thanCRDL. The instrument or method detection limit must be documented as described in Exhibit E.
The CROL are the instrument detection limits obtained in pure water that must be met usingthe procedure in Exhibit E. The detection limits for samples may be considerably higherdepending on the sample matrix.
13 July 89
W000282
Table 1. Page 12 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP METALS - MATRIX: SOLIDS
AUDITCalibrationVerification
CalibrationBlank
PreparationBlank
Spiked SampleAnalysis
DuplicateSample Analysis
Lab ControlSample(soils)
FREQUENCYCalibrated daily and each timeinstrument is set up; verify atat a frequency of 10% or every2 hr, whichever is greater.
During calibration at a fre-quency of 10% during run andat end of run.
1 per batch of samples digestedor 1 in 20 whichever is greater
1 per group of similar concen-tration and matrix, 1 per caseof samples, or 1 in 20, which-ever is greater.
Same as spiked sample analysis.
Once a month for each of theprocedures (applied) to solidsample analysis.
CONTROL LIMITSWithin ±10% of true value for all except tin and mercury(±20% of true value).
No more than CRDL.
No more than CRDL.
Within ±25% recovery unless SSR exceeds SR by a factorof 4 or more
±20% RPD for values 5X CRDL or more ±CRDL for samplesless than 5X CRDL
Within recovery of ±35% or within established controllimits
•Standards and samples will be matrix-matched to the concentration of the mineral acid.
•Calibration curves, continuing calibration and corrective measures records will be documented.
•One medium range internal synthetic standard will be analyzed to verify calibration and will bewithin ±10% of true value
•Furnace work will require duplicate analysis of each sample to verify recovery of spiked material. Ifrecoveries are within ±10%, methods of addition will not be required. If outside this criterion, methods ofstandard addition will be required.
13 July 89 _ _ _ .
flROOb283
Table 1. Page 13 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL PESTICIDES/PCBS - MATRIX: AQUEOUS
QUANTITATIONCHEMICAL COMPOUND METHOD LIMIT AUDIT FREQUENCY CONTROL LIMITS
(CLP) ppb+a-BHC WA 87-K* 0.05 SEE BELOW SEE BELOW SEE BELOW0-BHC WA 87-K* 0.05 " " "5-BHC WA 87-K* 0.05 " " "r-BHC (lindane) WA 87-K* 0.05 » " "heptachlor WA 87-K* 0.05 '• " »aldrin WA 87-K* 0.05 » " "heptachlor epoxide WA 87-K* 0.05 " "endosulfan I WA 87-K* 0.05 " "dieldrin WA 87-K* 0.10 » »4,4'-DDE WA 87-K* 0.10 " "endrin WA 87-K* 0.1 " «endosulfan II WA 87-K* 0.1 » "4,4'-ODD WA 87-K* 0.10 » "endosulfan sulfate WA 87-K* 0.1 " "4,4'-DDT WA 87-K* 0.10 » "methoxychlor WA 87-K* 0.5 " "endrin ketone WA 87-K* 0.1 » "ot-ehlordane WA 87-K* 0.5 " »T-chtordane WA 87-K* 0.5 » "toxaphene WA 87-K* 1.0 " "Aroclor 1016 WA 87-K* 0.5 " "Aroclor 1221 WA 87-K* 0.5 " '<Aroclor 1232 WA 87-K* 0.5 " »Aroclor 1242 WA 87-K* 0.5 » »Aroclor 1248 WA 87-K* 0.5 " "Aroclor 1254 WA 87-K* 1.0 " "Aroclor 1260 WA 87-K* 1.0 " "
+ Specific quantisation limits are highly matrix dependent. The quantisation limits listed hereare provided for guidance and may not always be achievable.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised: 1/87, 2/87, 7/87. IFB-WA-87K236, IFB WA-87K237,IFB WA-87K238.
AUDITRetentionTime Windows
EvaluationMixturesA,B, & C
ColumnBreakthrough
Standard Mix
ConfirmationAnalysis
Reagent Blank
Surrogate Spike
MS/MSD
13 July 89
FREQUENCYOnce per 24 hours
Once per 72 hours.
Once per 72 hours.
Once per 72 hours then inter-mittently throughout analysis
Once per 72 hours.
1 per case or 5% of sampleshipment.
All samples and blank (includ-ing MS/MSO).
1 per case or 1 in 20 ofsimilar concentration/matrix.
CONTROL LIMITS4,4'-DDT must have retention time greater than or equal to 12minutes on packed column, less than 2% shift on packed and .3%for capillary column.
X RSO for aldrin, endrin, and heptachlor epoxide must beless than or equal to 10%.
Must not exceed 20% - if greater remedial action is required.
Calculated factors must not exceed 15% difference for the quan-titation run nor 20% difference for confirmation run during 12-hr period. Deviation greater than or equal to 15% requiresreanalysis.
Separation should be greater than or equal to 25% resolutionbetween peaks.
Less than 5x CRDL for solvents, less than CRDL for all others.
Recovery limits within those of Table 4.2, Exhibit EWA 87-J001 (10/86).
Must fall within limits of Table 5.2, Exhibit EWA 87-J001 (10/86).
Table 1. Page 14 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL PESTICIDES/PC8S+ - MATRIX: SOLIDS
QUANTITATIONCHEMICAL COMPOUND METHOD LIMIT AUDIT FREQUENCY CONTROL LIMITS
(CLP) ppb**a-BHC WA 87-K* 8.0 SEE BELOW++ SEE BELOW** SEE BELOW++0-BHC WA 87-K* 8.0 " '5-BHC WA 87-K* 8.0 "T-BHC (lindane) WA 87-K* 8.0 "heptachlor WA 87-K* 8.0 "aldrin WA 87-K* 8.0 "heptachlor epoxide WA 87-K* 8.0 "endosulfan I WA 87-K* 8.0 »dieldrin WA 87-K* 16.0 »4,4'-ODE WA 87-K* 16.0 "endrin WA 87-K* 16.0 »endosulfan II WA 87-K* 16.0 »4,4'-ODD WA 87-K* 16.0 »endosulfan sulfate WA 87-K* 16.0 "4,4'-DOT WA 87-K* 16.0 »methoxychlor WA 87-K* 80.0 "endrin ketone WA 87-K* 16.0 "a-chlordane WA 87-K* 80.0 »T-chlordane WA 87-K* 80.0 »toxaphene WA 87-K* 160.0 "Aroclor 1016 WA 87-K* 80.0 »Aroclor 1221 WA 87-K* 80.0 »Aroclor 1232 WA 87-K* 80.0 »Aroclor 1242 WA 87-K* 80.0 "Aroclor 1248 WA 87-K* 80.0 »Aroclor 1254 WA 87-K* 160.0 "Aroclor 1260 WA 87-K* 160.0 " " "
+ Specific quantitation limits are highly matrix dependent. The quantisation limits listed hereare provided for guidance and may not always be achievable.
++See next page.
* U.S.EPA Contract Laboratory Program Statement of Work For Organics Analysis Multi-mediaMulti-concentration. 10/86. Revised: 1/87, 2/87, 7/87. IFB-WA-87K236, IFB WA-87K237,IFB WA-87K238.
**Mediun Soil/Sediment Contract Required Quantitation Limits (CRQL) for Pesticide/PCB TCLcompounds are 15 tinws the individual Low Soil/Sediment CRQL.Quantitation limits listed for soiI/sediment are based on wet weight. The quantitation limitscalculated by the laboratory for soil/sediment, calculated on dry weight basis as requiredby the contract, will be higher.
13 July 89
Table 1. Page 15 of 15ANALYTICAL METHODS AND DATA QUALITY REQUIREMENTS
CLP TCL PESTICIDES/PCBS+ - MATRIX: SOLIDS
AUDITRetentionTime Windows
EvaluationMixturesA,B, & C
ColumnBreakdown
Standard Mix
ConfirmationAnalysis
Reagent Blank
Surrogate Spike
MS/MSD
FREQUENCYOnce per 24 hours
Once per 72 hours.
Initially after approx. 18 hrand every 10 samples thereafter
Initially, then alternatestandard mixes A and B every10 samples.
After every positive result oninitial column
1 per case or 5% of samplesh i pment.
All samples and blank (includ-ing MS/MSD).
1 per case or 1 in 20 ofsimilar concentration/matrix.
CONTROL LIMITS4,4"-DOT must have retention time greater than or equal to 12minutes on packed column, less than 2% shift on packed and .3%for capillary column.
% RSD for aldrin, endrin, and heptachlor epoxide must beless than or equal to 10%.
Must not exceed 20% - if greater remedial action is required.
Calculated factors must not exceed 15% difference for the quan-titation run nor 20% difference for confirmation run during 12-hr period. Deviation greater than or equal to 15% requiresreanalysis.
Separation should be greater than or equal to 25% resolutionbetween peaks.
Less than 5x CRDL for solvents, less than CRDL for all others.
Recovery limits within those of Table 4.2, Exhibit EWA 87-J001 (10/86).
Must fall within limits of Table 5.2, Exhibit EWA 87-J001 (10/86).
13 July 89 , - .
flftO'00286
TABLE 2
DISTRIBUTION OF TRENCH SAMPLES
Excavation Number ofArea Samples
I 1II 2
III 1IV 11V 26VI 17
Figures
AR000288
FIGURE 1
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IF ACCEPTABLE FOR PASSENGER AIRCRAFT. THIS SHIPMENT CONTAINS RADIOACTIVE MATERIAL INTENDED FOR USE IN, ORINCIDENT TO. RESEARCH, MEDICAL DIAGNOSIS OR TREATMENT.________________________;_________________I HEREBY DECLARE THAT THE CONTENTS OF THIS CONSIGNMENT ARE FULLY AND ACCURATELY DESCRIBED ABOVE BY PROPERSHIPPING NAME AND ARE CLASSIFIED, PACKED, MARKED, AND LABELED, AND ARE IN ALL RESPECTS IN PROPER CONDITION FORTRANSPORT BY AIR ACCORDING TO THE APPLICABLE INTERNATIONAL AND NATIONAL GOVERNMENT REGULATIONS.^NAME AND TITLE OF SHIPPER
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SR00029I^
FIGURE 3
Attachments
38000292 OBRIENGGERE
ATTACHMENT 1
AR000293
SAMPLE HANDLING PROTOCOLFOR
LOW, MEDIUM AND HIGH CONCENTRATION SAMPLESOF
HAZARDOUS WASTE
E.1 Purpose. This protocol provides guidance on sample volumes,containers, packing, and shipping for low, medium, and high concen-tration environmental samples taken for chemical analysis.
E.2 Applicability. The guidance in this appendix applies to all samplestaken by USAGE for HTW chemical analysis. The requirements areconsistent with those of the Environmental Protection Agency and allstandard chemical methods generally used are included.
E.3 Low Concentration Samples. Low level samples are considered tobe those collected off-site, around the perimeter of a waste site, or inareas where hazards are thought to be significantly reduced by normalenvironmental processes.
A. Waters
1. Organics
a. Bottle and Preservative Requirements
Four 1-liter amber glass bottles, (Teflon-linedcaps), iced to 4° C (may not be held at siteover 24 hours). Remember: Leave someheadspace.
Two 40 ML glass VGA vials (with Teflonsepta), iced to 4°C (may not be held at siteover 24 hours). Fill completely. All airbubbles should be excluded.
The samples above are needed when Method8240 is used to analyze for volatile (orpurgeable) organics, when Methods 8250 or8270 are used to analyze for Acid/Base Neutral(A/B/N) extractable organics, and whenMethod 8080 is used to analyze for pesticidesand PCBs. Two of the 1-L bottles are neededfor 8250/8270 and two for 8080.
Oil and Crease, Total Organic Carbon (TOC)or TRPTTT For each analyte, two 1-liter glassbottle Tteflon-lined cap), H_SOU or Sm 1:1HCI (to pH 2), and 4° C. L H
ARQOG291*
b. Paperwork/ Labels
Chain of Custody Record. See attached exam-ple. It is important to note that only one sitemay be listed per form even if the sites havethe same project number. Top original goeswith the samples; a copy should be saved forthe sampler's files.
Receipt for Samples. See attached example.This form complies with the requirements thatthe owner, operator, or agent-in-charge islegally entitled to: (1) a receipt describingthe samples obtained from the site and; (2) aportion of each sample equal in weight orvolume to the portion retained, if requested.The original form is retained for the ProjectCoordinator and a copy is given to the owner,operator, or agent-in-charge.
Sample Labels. See attached example. Youmust label the sample with a date, time ofcollection, site name, and brief description ona label that will not float/soak off - no mask-ing tape, please. Use only indelible ink on alllabels. Numbered sample labels should beused on a\± samples.
c. Packaging and Shipping
Waterproof metal (or equivalent strengthplastic) ice chests or coolers only.
After filling out the pertinent information onthe sample label and tag, put the sample inthe bottle or vial and screw on the lid. Forbottles other than VOA vials, secure the lidwith strapping tape. (Tape on VOA vials maycause contamination.) Then, secure the stringfrom the numbered approved tag around thelid.
Mark volume level on bottle with grease pencil.
Place about 3 inches of inert cushioning mate-rial such as vermiculite in the bottom of thecooler.
Enclose the bottles in clear plastic bagsthrough which sample tags and labels arevisible, and seal the bag. Place bottles up-right in the cooler in such a way that they donot touch and will not touch during shipment.
000295
Put in additional inert packing material topartially cover sample bottles (more thanhalfway). Place bags of ice around, among,and on top of the sample bottles.
Fill cooler with cushioning material.
Put paperwork (chain of custody record) in awaterproof plastic bag and tape it with mask-ing tape to the inside lid of the cooler.
Tape the drain shut.
Shut lid by taping. Wrap the cooler complete-ly with strapping tape at a minimum of twolocations. Do not cover any labels.
Attach completed shipping label to top of thecooler.
Put "This Side Up" labels on all four sides and"Fragile" labels on at least two sides.
Affix numbered and signed custody seals onfront right and back left of cooler. Coverseals with side, clear tape.
Remember that each cooler cannot exceed the weight limit set by theshipper.
2. Inorganics
a. Bottle and Preservative Requirements
Metals. One 1-liter high density polyethylenebottle (Teflon-lined cap), adjust to pH 2 with1:1 HN03 (usually 3 mL).
Cyanides. One 1-liter high densitypolyethlene bottles (Teflon-lined cap), adjustto pH 12 with NaOH (usually 2 mL of 10NNaOH or 4 pellets), and 4°C.
Sulfide. One 1-liter high density polyethylenebottle (Teflon-lined cap), 4 mL 2.0 N zincacetate and adjust pH 9 with NaOH, and 4°C.
Fluoride. One 1-liter high densitypolyethylene bottle (Teflon-lined cap), nopreservative, and 4°C.
pH. No preservative. Must be measuredimmediately in field. Do not ship.
fiROQ0296
Ammonia, Total Nitrogen, Organic Nitrogen,Nitrate/Nitrite. For each analyte, one 1-literhigh density polyethylene bottle (Teflon-linedcap), adjust to pH 2 with H SO (usually 4mL 1:1 HS0), and 4°C. L 4
b. Paperwork/ Labels
Inorganic Paperwork is the same as describedfor organics (see I.A.1.B. above) and in-cludes the Chain of Custody Record, Receiptfor Samples, and Labels/Sample Tags. Seeprevious examples and explanations.
c. Packaging and Shipment
Follow packaging and shipping requirementslisted for organics (see Section 1.A.1.C.above). "Fragile" labels are optional forcoolers not containing glass bottles. In caseswhere ice is not required (metals), fill coolerwith only packing material. Once again,remember that the cooler must not exceed theshipper's weight limits.
B. Soils/Sediments (Organics and Inorganics)
1. Bottle Requirements
Two 8-ounce glass wide mouth jars at least 3/4 full(Teflon-lined caps), iced to 4°C - one jar fororganics (non-VOA) and one jar for inorganics.For analysis of volatiles in soil, 2-40 mL VOA vials(with Teflon septa or Teflon lined caps), 2-120 mLwide mouth glass vials or 2-8 oz. wide mouth jars(with Teflon lined caps) are used. These shouldbe completely filled and iced to 4°C.
2. Paperwork/ Labels
Follow paperwork requirements listed for watersamples in Section 1.A.1.b. above. See attachedexamples of forms.
3. Packaging and Shipping
Follow packaging and shipping requirements inSection 1.A.1.C. above. Be sure that the shippingcooler does not exceed the shipper's weight limits.
E.4 Medium Concentration Samples. Medium level samples are mostoften those collected on-site, in areas of moderate dilution by normalenvironmental processes.
AROOP297
Water/Liquids (Organics and Inorganics)
Note: Samples are not known to contain highly toxic com-pounds.
1. Bottle and Preservative Requirements
Four 3_2_-ounce wide mouth glass jars (Teflon-linedcaps), no preservatives, and iced to 4°C for A/B/Nextractable organics and PCB/Pest (two jars foreach method). Remember: leave some headspace.
Two 40 mL glass VOA vials (Teflon septa), iced to4°C. Fill completely. No headspace.
Two 18-ounce wide mouth glass jars nearly-full(Teflon-lined caps) one for metals and one forcyanides. (Preserve as for low level 1.2.a.)
2. Paperwork/ Labels
See previous examples. Follow paperwork require-ments in 1.A.1.b. for low concentration samples.
3. Packaging and Shipping
Secure sample jar lids with strapping tape or evi-dence tape. At the same time secure' string fromUSEPA numbered tag around lid.
Mark volume level of bottle with grease pencil.
Position jar in Ziploc bag so that tags may be read.
Place about 1/2 inch of cushioning material in thebottom of metal can.
Place jar in can and fill remaining volume of canwith cushioning material.
Close the can using three clips to secure lid.
Write sample number on can lid. Indicate "ThisSide Up" by drawing an arrow and place "FlammableLiquid N.O.S." label on can. Personnel who shipsamples must be sure to comply with DOT shippingregulations and not knowingly over classify asample prior to shipment. If the person shipping asample knows that the sample is not a "FlammableLiquid" (i.e., a water phase sample or a soil sam-ple), he should not classify it as "Flammable Liq-uid."
Place about 1 inch of packing material in bottom ofcooler.
Place cans in cooler and fill remaining volume ofcooler with packing material. Add ice bags ifrequired.
Put paperwork in plastic bags and tape with mask-ing tape to inside lid of cooler.
Tape drain shut.
After acceptance by shipper, tape cooler completelyaround with strapping tape at two locations.Secure lid by taping. Do not cover any labels.
Place lab address on top of cooler.
Note: Write "Flammable Liquid N.O.S." on side of cooler if thisis not marked on the margin of your DOT label.
For all medium and high concentration shipments,complete shipper's hazardous material certificationform.
Put "This Side Up" labels on all four sides,"Flammable Liquid N.O.S." and "Danger-Peligro" onall sides.
Note: "Danger-Peligro" labels should be used only when netquantity of samples in cooler exceeds 1 quart (32ounces) for liquids or 25 pounds for solids. In otherwords, for our purposes "Danger-Peligro" labels willnever be used for Flammable Solids N.O.S.
Affix numbered custody seals on front right andback left of cooler. Cover seals with wide, cleartape.
B. Soils/Sediments/Solids (Organics and Inorganics)
1. Bottles and Preservatives
For analysis of volatiles, 2-40 mL VOA vials (withTeflon septa or Teflon lined caps), 2-12-mL VOAvials, or 2-8 oz wide mouth jars 9with Teflon linedcaps) are used. These should be completely filledand iced to 4°C.
Two 8-ounce wide mouth glass jars, 3/4 full(Teflon-lined caps), no preservatives, one jar fororganics (non-VOA) and one jar for inorganics(metals and cyanide) or
Four 4-ounce wide mouth glass jars each 3/4 full(Teflon-lined caps), no preservative; two jars fororganics (non VOA) and two jars for inorganics.
ARGOG299
2. Paperwork/ Labels
See previous examples. Follow paperwork require-ments listed in Section 1.A.1.b. for low concen-tration samples.
3. Packaging and Shipping
Follow packaging and shipping requirements listedin Section 11.A.3 for medium concentration wa-ter/liquids above substituting "Flammable LiquidN.O.S." with "Flammable Solid N.O.S."
E.5 High Concentration Samples (Hazardous; Determined Not to beD.O.T. - Defined Poison A). High concentration samples include thosefrom drums, surface impoundments, direct discharges, and chemicalspills, where there is little or no evidence of environmental dilution.High concentration (or high hazard) samples are suspected to containgreater than 15% concentration of any individual chemical substitute.
A. Liquids (Organics and Inorganics)
1. Bottle and Preservative Requirements
One 8-ounce wide mouth glass jar filled 1/2 to 3/4full (Teflon-lined cap). No preservative.
2. Paperwork/ Labels
a. See previous examples. Follow paperwork require-ments listed in Section I.A.I.b. above.
b. Shipper may require special forms to be completedbefore shipment of high hazard concentration sam-ples.
3. Packaging and Shipping
Follow packaging and shipping requirements listedin Section 11.A.3. above for medium concentrationwater/liquids.
B. Soils/Sediments/Solids (Organics and Inorganics)
1. Bottle and Preservative Requirements
One 8-ounce wide mouth glass jar filled 1/2 to 3/4full (Teflon-lined cap). No preservative.
2. Paperwork/ Labels
See attached examples. Follow paperwork require-ments in Section I.A.I.b. above.
AROQQ300
3. Packaging and Shipping
Follow packaging and shipping requirements listedin Section 11.A.3. for medium concentration wa-ter/liquids, substituting "Flammable Liquid N.O.S."with "Flammable Solid N.O.S." .;
TABLE 1
ppm = mg/L or ug/mL or mg/kg
ppb = ug/L or ug/kg or ng/g
*fl00030
SAMPLE CONTAINERS, PRESERVATIVES, AND HOLDING TIMES
Low Concentration Samples
Maximum HoldingTimes:
1 1 3 4Matrix Parameter Container Preservation Extraction Analysis
Water volatiles 2 x 40 mL2 Ice to 4°C — 14 d
Water B/N/A 2 x 1 L5'8 Ice to 4°C 7 d 40 d
Water PCBs/ 2x1 L5'8 Ice to 4°C 7 d 40 dPesticides Amber G
Water Metals6 1 x 1 L P HN03 to PH 2 ~ 6 m°6
Water TRPH 2 x 1 L G Ice to 4°C -- 28 d
Water Commoj? 1 x 1 L7 G Ice to 4°C — 28 d7anions
Water Explosives 2 x 1 L G Ice to 4°C -- 7 d
Water Cyanide 1 x 1 L P NaOH to pH 12 — 28 dIce to 4°C
Soils/ B/N/A, PCBs 1 x 8 oz G Ice to 4°C 7 d 40 dSediments Pesticides
Soils/ Metals/ 1 x 8 oz G Ice to 4°C — 6 mo6Sediments Cyanide (Cyanide & TRPH) (TRPH:
28 d)
SROQ0302
SAMPLE CONTAINERS, PRESERVATIVES, AND HOLDING TIMES
Medium Concentration Samples1 2 3Matrix Parameter Container Preservation
Water/Liquid Volatiles 2 x 40 mL G, Ice to 4°C 8Septa Vial
Water/Liquid B/N/A5 2 x 32 oz wide Ice to 4°C 8mouth jars, G
Water/Liquids PCBs5 2 x 32 oz wide Ice to 4°C 8Pesticides mouth jars, G
Water/Liquid Metals 1 16 oz wide HN03 to PH 2mouth jar, G
Water/Liquid Cyanide 1 x 16 oz wide Ice to 4°Cmouth jar, G
Soils Volatiles 2 x 4 ml G2 x 120 mL G,or 2-9 oz G
Soils B/N/A, PCBs 1 x 8 oz widePesticides mouth jar, G
Soils Metals, Cyanide 1 x 8 oz wide Ice to 4°CTRPH mouth jar, G (Cyanide & TRPH)
High Concentration Samples
Matrix Parameter Container Preservation
Liquid All organic 1 x 8 oz wide —and organic mouth jar, Ganalyses
B/N/A = Base/Neutral/Acid extractables; TRPH = Total RecoverablePetroleum Hydrocarbons
All containers must have Teflon-lined seals (Teflon-lined septa for VOAvials). G = Glass; P = High density
Samples preservation will be done in the field immediately upon samplecollection.
When only one holding time is given, it implies total holding' time fromsampling until analysis.
Three bottles are required on at least 5-10% (but at least one) sampleso that laboratory can perform all method QC checks for SW-846 meth-od. '. ' •
/5R000303
Total Recoverable Metals for water samples. Holding time for Hg is- 28days in glass and 13 days in plastic containers; for CR (VI) is 24hours.
C1~, Br~, N03~, NO ~ PO 3', SO 2~ 1 L for each method;orthophosphate_ requijes filtration. Holding time for extraction is 48
~ ~hours for N02, N03, and PO^ ) .
Samples with residential chlorine present will be dechlorinated withsodium thiosulfate as specified in SW-846 (third edition).
Holding times for medium concentration samples are the same as thosespecified for low concentration samples.
ATTACHMENT 2
AR000305
US ARMY CORPS OF ENGINEERS
REQUIREMENTS FOR CHEMICAL QA/QC
1. Normally, for every 10 samples or for every sample set (whichever
results in a higher number of QA/QC samples) sent to the lab for
analysis, one field blank and one split or duplicate sample shall
also be sent for internal QC purposes. The same frequency is
required for external QA. A field blank may be any one of the
following, depending on the type of sample collected:
a. A trip blank is organic-free deionized water accompanying the
sample containers sent into the field from the lab. This trip
blank is to be used when samples are collected for volatile
organic analysis and is to be included in all shipments con-
taining samples which are to be analyzed for volatile organic
compounds.
b. A rinsate blank is the collected rinse water from the final
rinses of the sampling equipment. These final rinses are to
be accomplished with organic-free deionized water. This
blank is to be used in conjunction with semi-volatile analysis
as well as for volatile organic analysis. For general inorganic
analysis, a rinsate blank, preserved in the same manner as
the inorganic samples, is to be used. In some instances, an
ultra-pure organic solvent may be more appropriate as the
final rinse.
AR000306
c. Soil blanks may be used in instances where there is reason-
able assurance that it is free of the analytes of concern. Soil
blanks are generally not recommended.
2. The additional definitions below are to be understood during
preparation of any QA/QC plan.
a. A split is a subsample of the original sample. The amount of
subsample taken will be determined by the number of splits to
be taken, usually such that all subsamples and the original
sample will contain an equal amount of material, except for
where the sample contains volatiles, when a compositing step
shall be described for soils. The sample should be homoge-
neous before splitting. Soil QA samples should be splits.
b. A duplicate is a separate sample collected at the same location
as the original sample. QA/QC samples to be analyzed for
volatiles must be duplicates.
c. A background soil sample is a sample of soil taken at an
uncontaminated location near the site. This sample is
required unless the contamination is so pervasive that there
is no reasonable chance of obtaining appropriate "background"
samples.
d. A set if a group of samples which have nearly identical
matrices, identical preservation requirements, and identical
2 .AR000307
collection methods, and have been collected under identical
conditions (such as the same day, same sampling crew, same
weather conditions, etc.). Any significant change in any of
the above parameters shall define a new set. When it is not
obvious as to whether or not a particular change is "signifi-
cant", the QA lab should be consulted.
e. A matrix may be considered as the composition of the material
containing the analyte, the interactions of which cause the
analytical result to show the concentration to be other than
the actual concentration. Examples of different matrices are
soil, sediment, sludge, surface water, leachate water, ground
water, drinking water, seawater, and air. In defining a
matrix, consideration must be given to the intended use of
the data, the analytical method to be used and the associated
detection limits and likely interferences. The QA laboratory
should be consulted in defining a matrix and deciding if
groups of samples can be combined to form a set.
3. The following may serve as an example of the 10% frequency of
blanks, duplicates, and splits. Eight samples are collected on the
same day in the field consisting of the same matrix and are to be
submitted for analysis for semi-volatiles. One of these samples is
split, giving a total of nine samples. A field blank (rinsate blank)
is added to this collection giving a new total of 10 samples which
will be sent to the contract lab (Wilson). In addition, another
field blank and another split (not necessarily a split of the sample
3 AROOQ308
that was split previously) will be sent to the external QA lab
Missouri River Division (MRD). The end result is 12 samples
.which satisfy Corps QA/QC requirements.
4. The following may serve as an example of one duplicate or split
and one blank collected per set. If the eight samples identified
above were collected on different days, those samples would con-
stitute two ore more sets, the number being equal to the number
of days used to collect them. If period, there would be two
blanks and two splits for each day (one blank and split for ex-
ternal QA and one blank and split for internal QC) giving a total
of 12 QA/QC samples as opposed to four such samples used in the
paragraph above.
A field set may not necessarily be the same as a lab batch.
If all eight samples are collected on the same day consisting of the
same matrix and using the same analytical procedure, the require-
ments are met for one field set. However, if these samples are
not analyzed without an overnight break for other significant dis-
continuity), these samples constitute more than one batch. For
the lab, this means the field blank should be reanalyzed in addi-
tion to following other standard QC practices. Unless a resampling
effort is indicated, however, no further QA/QC samples are
required from the field.
AR000309