United States
Environmental Protection
Agency
Solid Waste
Office of
Solid Waste
Washington, D.C, 20460
EPA/530-SW87011
March 1987
(Revised)
eneric Quality Assurance
Project Plan for Land
Disposal Restrictions
Program ("BOAT")
-------
GENERIC QUALITY ASSURANCE PROJECT PLAN FOR
LAND DISPOSAL RESTRICTIONS PROGRAM ("BOAT")
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Solid Waste
401 M Street, S.W.
Washington, D.C. 20460
James R. Berlow, Chief David Pepson
Treatment Technology Section Project Manager
March 12, 1987
Revised August 6, 1987
-------
Section
1.
TABLE OF CONTENTS
Introduction
2.
EPA's BOAT Data Collection Program
Treatment Facilities
2.1
2.2
2.3
2.4
Data Sources Used to Identify
Initial Plant Selection
Engineering Site Visit
EPA Reports Generated as Part
of the Sampling Program
Generic Quality Assurance Elements of the Site-Specific
Sampling and Analysis Plan (SAP)
3.1 Test Objectives
3.2 Project Organization
3.3 Sample Collection Plan
3.4 Design and Operating Data Collection
3.5 Analytical Quality Assurance/Quality
3.
Control Procedures
4.
Other Quality Assurance Elements of the BOAT Data Collection
Program
4.1
4.2
REFERENCES
Chain of Custody Procedures
Performance and System Audits
Paqe No.
1
3
3
4
5
7
10
10
10
11
13
13
26
26
33
34
-------
LIST OF TABLE
Table 3-1 BOAT Pollutant List 19
LIST OF FIGURES
Figure 3-1 General Project Organization Chart 12
Figure 4-1 Example of Sample Label 28
Figure 4-2 Example Chain of Custody Form 29
Figure 4-3 Example of Tamperproof Seal 30
-------
1.
INTRODUCTION
The Hazardous and Solid Waste Amendments of 1984 (HSWA), enacted on
November 8, 1984, imposed substantial new requirements for the handling
and managing of solid wastes.
One of the requirements specified by the
statute is that EPA establish "levels or methods of treatment" for the
land disposal of hazardous wastes.
Land disposal is broadly defined to
include the placement of a waste in a landfill, surface impoundment,
waste pile, injection well, land treatment facility, salt dome or salt
bed formation, or underground mine or cave.
As explained in the preamble
to the land disposal restrictions rule of November 7, 1986 (51 FR 40572),
the levels of treatment that EPA is specifying for land disposal are
technology based standards which represent best demonstrated available
technology (BOAT).
This document details EPA's program for collecting treatment data and
sets forth the specific quality assurance and quality control parameters
EPA is establishing for its BOAT program.
Section 2 explains all the
elements of EPA's BOAT data collection program.
Section 3 specifies the
quality assurance elements that must be addressed in all site-specific
sampling and analysis plans (SAP).
Section 4 discusses other quality
assurance elements of the BOAT data collection program.
Facilities wishing to submit data for consideration in the
development of BOAT standards should review this document and pay
particular attention to Sections 3 and 4.
While the Agency requests that
1
-------
facilities submit all pertinent data, EPA cautions that, to the extent
possible, these facilities must comply with equivalent quality
assurance/quality control procedures to those used by EPA.
2
-------
2.
EPA'S BOAT DATA COLLECTION PROGRAM
This section of the generic quality assurance plan discusses the
various elements of the Agency's program for collecting data for the
development of treatment standards (BOAT) for wastes subject to land
disposal restrictions.
Section 2.1 describes data sources used to identify candidate plants
for sampling, Sections 2.2 and 2.3 discuss the process by which a
decision is made to sample any individual plant, and finally, Section 2.4
describes the reports that EPA will develop from these sampling and
analysis visits and the data and information to be contained in these
reports.
2.1
Data Sources Used to Identify Treatment Facilities
EPA uses a number of information sources in its initial plant
selection including Stanford Research Institute's (SRI) Directory of
Chemical Producers, EPA's Hazardous Waste Data Management System (HWDMS),
1986 TSDF National Screening Survey, and EPA's Industry Studies Data
Base.
In addition, EPA contacts trade associations to inform them that
the Agency is considering visits to facilities in their industry and to
solicit assistance in identifying facilities for EPA to consider in its
treatment sampling program.
3
-------
2.2
Initial Plant Selection
After EPA has identified waste codes for which inadequate treatment
data exist, the Agency then decides which treatment facilities are
potential sampling candidates for that waste.
Consistent with the regulatory approach described in the preamble to
the November 7, 1986, land disposal restrictions rule, EPA has
established a hierarchy of types of plants to sample for BOAT data
collection.
This hierarchy, described below, is only a general approach
that the Agency prefers to follow.
Final plant selection will be
affected by a number of factors including the types of treatment
technologies at particular facilities, the design and operation of these
technologies, plant layout, whether technologies are full scale or
pilot/bench operations, and statutory time constraints.
A discussion of
these factors is contained in the engineering site visit subsection 2.3
following.
Thus, subject to these constraints, the Agency's priority for
facility sampling is (1) waste generators that also treat the waste,
(2) commercial facilities (other than generators) that treat the waste of
interest, and finally (3) EPA in-house treatment facilities.
Generators are the facilities most likely to treat a waste by itself
or as a significant percentage component of a waste mixture.
Accordingly, such treatment data will best reflect the waste matrix
effects from all the various constituents in a waste, not just those that
4
-------
may pose the most concern from the perspective of health and
environmental effects.
In addition, generators that routinely treat a
waste have the best opportunity to have optimized treatment parameters
for that waste.
Commercial facilities are favored over EPA in-house treatment
facilities because they are probably more familiar with treatment of a
particular waste than EPA and, therefore, would be able to better
optimize treatment parameters.
Also, these facilities demonstrate more
directly the performance of technology under field conditions.
If, in the case of EPA in-house treatment facilities, we cannot
reasonably obtain (i.e., within the Agency's mandated rulemaking time
frame) the actual waste of interest, we will synthesize a waste which we
believe best represents this waste.
The types and amounts of chemical
constituents of these wastes will be described in the site-specific
sampling and analysis plans.
2.3
Engineering Site Visit
Once EPA has identified a plant as a potential sampling candidate,
the Agency then arranges an engineering site visit to evaluate in detail
whether the facility should be sampled.
The engineering site visit
provides the information that EPA uses for its detailed analysis such as:
(a)
Does the waste being treated meet the definition of the waste
code of interest as expressed in the waste code listing (40 CFR
261.31-261.33).
5
-------
(b)
If so, is the waste treated either separately or as a
significant percentage component of a waste mixture.
Is the waste treated on a schedule such that EPA could
reasonably arrange a sampling visit to obtain treatment data on
that waste.
(c)
(d)
Are data available on the design of the system such that EPA can
determine whether the system is well designed, as well as
compare actual operating conditions to design parameters to
assure that results represent operation at optimum levels.
(e)
Are principal operating parameters measured or can they be
obtained during sampling so that EPA can evaluate operating
conditions during the data collection process.
( f)
Are piping arrangements such that EPA can obtain all the samples
it needs to evaluate treatment. Such samples include those
necessary to verify operating conditions such as pH and excess
reactant, as well as characterize untreated and treated
streams. If piping layout is not as needed, what modifications
are required and is the plant willing to modify piping systems.
The site visit also provides an opportunity to obtain a sample prior
to the sampling visit.
Analysis of such a sample can minimize problems
that a laboratory may have in analyzing a particular waste matrix.
This
is especially helpful in analyzing wastes for which no historical data
are available.
The engineering site visit also plays a role in EPA's selection of
the type of facility to sample (i .e., generator, commercial (other than a
generator), or EPA in-house facility).
If the site visit shows that the
preferred plant is not well designed or operated or should not be sampled
for other reasons discussed above, EPA will then investigate another
plant consistent with the hierarchy previously described in Section 2.2.
6
-------
2.4
2.4.1
EPA Reports Generated as Part of the Samplinq Proqram
Sampling and Analysis Plan
If, after the engineering site visit, EPA decides to sample a
particular plant, the Agency will then develop a site-specific Sampling
and Analysis Plan (SAP).
The contents of this plan are discussed in
Section 3.
In brief, the SAP discusses where the Agency plans to sample,
how the samples will be taken, the frequency of sampling, the
constituents to be analyzed and the method of analysis, operational
parameters to be obtained, and specific laboratory quality control checks
on the analytical results.
The Agency will generally produce a draft of the site-specific
sampling and analysis plan within two to three weeks of the engineering
visit.
The draft of the SAP is then sent to the plant for review and
comment; EPA usually provides one week for this review.
With few
exceptions, the draft SAP should be a confirmation of data collection
activities discussed with the plant during the engineering site visit.
EPA encourages plants to recommend any modifications to the SAP that they
believe will improve the quality of the data.
It is important to point out that EPA's sampling of a plant does not
automatically mean that the data will be used in the development of
treatment standards for BOAT.
EPA's final decision on whether or not to
use data from a sampled plant will depend on the actual analysis of the
waste being treated and on the operating conditions at the time of
7
-------
sampling.
Although EPA would not plan to sample a facility that was not
ostensibly well designed and operated, there is no way to ensure that at
the time of sampling the facility will not experience operating problems.
2.4.2
Onsite Engineering Report
Following the sampling visit, EPA will develop a report summarizing
all data and information pertinent to evaluation of the treatment
process; EPA refers to this report as the onsite engineering report.
This report contains the following:
.
Section 1 characterizes the wastes treated including a brief
industry description and the manufacturing process or processes by
which the wastes were generated.
.
Section 2 presents a description of the treatment system
including design parameters, physical equipment, chemical
reagents, and control systems.
.
Section 3 provides an operating log section which presents
operating data during the data collection process as well as
descriptions of any events that could impact the operation of the
system.
.
Section 4 describes all sample collection activities and all
analytical procedures. This section will document the extent to
which the sampling and analysis plan was conducted as designed.
Any changes from the final SAP will be shown in this section as
well as an explanation of why a change was required.
Section 5 presents all analytical data.
.
.
Section 6 presents all laboratory quality control results
including laboratory precision and accuracy results.
.
Section 7 provides plant correspondence. This section would
include letters from the Agency requesting review by the plant of
the SAP and on site engineering report. This section would also
include the comments by the plant on the report as well as the
Agency's response to these comments.
8
-------
After the on site engineering report is completed, the report is
submitted to the plant for review.
This review also provides the plant
with a final opportunity to claim any information contained in the report
as confidential.
EPA generally provides four weeks for this review.
Following the review and incorporation of comments, as appropriate, the
report is available to the public with the exception of any material
claimed as confidential by the plant.
As indicated earlier, completion of the report does not mean that the
data will be used to establish treatment standards.
Certainly the Agency
will consider these data but may, for various reasons including poor
operating conditions at the time of sampling, reject these data as the
basis for BOAT.
9
-------
3.
GENERIC QUALITY ASSURANCE ELEMENTS OF THE
SITE-SPECIFIC SAMPLING AND ANALYSIS PLAN (SAP)
The section identifies generic quality assurance elements of the site
specific sampling and analysis plan.
3.1
Test Obiectives
The site-specific SAP will identify the specific waste code or codes
under study and the specific treatment system being evaluated.
In
addition, this section of the SAP will describe the specific waste being
examined in terms of the industry which generates it and the
manufacturing process by which it is generated.
This section of the SAP
should also present sufficient information on the treatment system so it
is clear what system is being evaluated.
For example, treatment should
be described as fluidized bed incineration, not simply as incineration.
A schematic diagram of the treatment process must be included in the
section of the SAP which specifies the sampling locations.
3.2
Project Orqanization
The EPA Program Manager will have the overall quality assurance (QA)
responsibility for all sampling and analysis data collected for the BOAT
program.
All sampling and analysis plans must be approved by the EPA
Work Assignment Manager (WAM) and the EPA Program QA Officer.
The prime
contractor will be responsible for the subcontractor's implementation of
this generic QAPP and any appropriate site-specific SAP sampling and
10
-------
analysis plan.
Figure 3-1 shows the general organization chart.
An
organization chart will be prepared for each sampling and analysis plan.
3.3
Sample Collection Plan
To determine the quality of data with respect to the characterization
of the waste being treated and the treated residual, the site-specific
sampling and analysis plan must contain the following information:
.
Samplinq point descriptions. Describe the sampling points and
provide the justification for selection of these sampling points.
All sampling points will be identified on the schematic diagram
for the waste treatment system. (Sampling for operation
parameters is discussed in Section 3.4.)
.
Sample collection method. All samples will be collected as grab
samples. Sample collection procedures will be described for each
sample location.
.
Frequency. Frequency of sample collection will vary depending
upon the treatment system. The frequency of sample collection at
each sampling location will be specified in the SAP and will be
selected to best characterize the variability in (1) the waste
stream, (2) the treatment process, and (3) the analytical results.
.
Constituents to be analyzed. For all sampling points, specify
which of the compounds shown in Table 3-1 (BOAT Pollutant List)
will be analyzed. All analyses should be performed using SW-846
(3rd edition). Deviations from this list of compounds should be
justified. (For example, if one sample of the untreated waste is
analyzed, and the data show that particular compounds are not
present, then further analysis of these compounds may not be
required for the other samples from the plant.)
.
Total composition and TCLP extracts. For the treated residuals,
analysis will be completed on both the total composition sample
and the TCLP extracts. For all other samples collected, analysis
will only be completed for total composition.
11
-------
EPA PROGRAM MANAGER
EPA PROGRAM
QA OFFICER
EPA HORK ASSIGNMENT MANAGER
CONTRACTOR PROGRAM MANAGER
CONTRACTOR QA OFFICER
SUBCONTRACTOR
I
ENGINEERING FI ELD SAMPLING LABORATORY
STAFF STAFF COORDINATOR
I
LABORATORY
QC OFFICER
Figure 3-1 General project organization chart.
12
-------
.
Sample containerization and preservation. Procedures for sample
containerization and preservation presented in SW-846 (3rd
edition, Table 2-16) will be followed. Deviations from the SW-846
procedures will be documented and explained. All sampling vessels
and containers will be cleaned prior to the sample collection.
The procedures used will be specified in the site-specific SAP.
3.4
Desiqn and Operatinq Data Collection
To evaluate the treatment design and operation, the SAP must contain
the following:
All design and operating data to be collected, the method of
collecting these data, and the reason for collecting these data;
.
.
The specific frequency for collecting the operating data; and
.
Identified locations for collecting operating data on the
treatment system schematic.
3.5
Analytical Quality Assurance/Quality Control Procedures
This section of the quality assurance plan addresses (1) the
analytical methods to be used, (2) the QC required for determining the
precision and accuracy of the analytical data, (3) the QC for determining
field and laboratory contamination, (4) corrective actions if the QC
objectives are not met, (5) procedures for instrument calibration,
(6) data reduction and reporting, and (7) statistical QC procedures.
3.5.1
Analytical Methods
The following items must be addressed in the site-specific sampling
and analysis plans:
13
-------
A-I
The SW-846 methods (3rd edition) must be cited in the SAP for all
compounds and compositional parameters to be analyzed. If SW-846
(3rd edition) methods are not available for a particular compound or
compositional parameter, the method to be used must be cited in the
SAP.
A-2
If for any reason upon receipt of the samples the methods cited in
the SAP are not appropriate, the EPA WAM will be notified of the new
method to be used.
A-3
The EPA WAM will be notified if sample cleanup methods not cited in
the SAP are required to obtain detection levels of at least 1 ppm in
the matrix for any of the compounds or compositional parameters to
be analyzed. The laboratory is to inform the EPA WAM with regard to
what additional cleanup may be necessary to eliminate interferences
or matrix problems which could prevent achieving this level of
detection for various compounds and the level of effort required for
the additional cleanup procedures. The EPA WAM will determine
whether the laboratory should proceed using these additional
procedures or whether analytical work on the set of samples should
be discontinued.
A-4
Any deviations from the sample
in SW-846 or referenced in the
to handle unusual matrix types
report for the site visit.
preparation and cleanup methods cited
site-specific SAP that were necessary
will be fully documented in the final
3.5.2
Precision and Accuracy QC Requirements
B-1
One laboratory duplicate injection of the spiked sample extract will
be performed for each group of the treated residual samples taken
from the same sampling point. The laboratory duplicate injection
also be completed on the TCLP extract. Analytical results of the
duplicate injection must be within ~20 percent of each other for
values greater than 200 ppb. For values less than or equal to 200
ppb, analytical results for the duplicate injection must be within
~100 percent of each other. If duplicate analyses are not within
these ranges, the samples must be reanalyzed. If these criteria are
not met, the data are not acceptable. Precision will be calculated
using relative percent difference as presented in Section 3.5.7.
B-2
One matrix spike duplicate for each group of treated residual
samples will be performed. The spike constituents will be
determined on a site-specific basis and will be reported in the
SAP. Spiking will be completed at the laboratory prior to
14
-------
extraction or digestion of the sample. The spike concentration must
be within 5 times the measured concentration for the sample. If the
spike concentration is not within 5 times the measured
concentration, the laboratory will respike and reanalyze the
sample. When the compounds of interest will not be present in the
waste because of removal during treatment, samples shall be spiked
at 5 times the target detection limit level for these compounds.
The accuracy will be calculated using equations in Section 3.5.7.
Laboratories must submit the analytical results for the spiked and
unspiked samples so that EPA can adjust the data to reflect recovery
B-3
All laboratories must generate data for developing treatment
standards for the BOAT program using instruments that have
instrument detection limits* equal to the target detection limits
specified in Table 3-1 (BOAT Pollutant List). The laboratory must
provide the EPA WAM and EPA QA Officer with data demonstrating that
the target detection limits can be obtained for the compounds of
intere~t. Oata must have been generated within one calendar year of
the generation of the analytical data submitted to the BOAT program.
B-4
Surrogate recoveries must be performed for each sample as specified
in SW-846. (Note: Because of limited experience with hazardous
waste samples, EPA is not specifying at this time any precision or
accuracy ranges as a condition for accepting the analysis of the
treated residuals. EPA will use these data to establish precision
and accuracy ranges in the future.)
B-5 A reagent blank must be performed for an analytical batch of samples
with a minimum of one blank per twenty samples. The reagent blank
must be carried throughout the entire analytical procedure. In
cases where the concentration of any compound detected in the blank
is 10 percent or greater than the concentration detected in any of
the samples in the batch, the laboratory must at a minimum take the
corrective action steps listed in 3.5.4.
*Instrument detection limit for each compound is the lowest
concentration that when measured by the instrument results in a
reportable value of at least three times the standard deviation
instrument noise level.
from the
15
-------
3.5.3
QC Procedures for Determining Field and Laboratory Contamination
The following QC procedures must be followed to determine whether
field or laboratory contamination was introduced into the samples:
ClOne trip blank which is not opened in the field will be analyzed to
check for sample contamination originating from sample transport,
shipping, or site conditions. The parameters for analysis will be
specified in the SAP.
C-2 Equipment blanks will be taken as needed and specified in the site-
specific SAP. Collection and frequency will be specified in the
SAP. The equipment blank consists of laboratory pure water* or
solvents brought to the field in a sealed container, opened in the
field, and the contents poured over or through the sample collection
device and then collected in the sample container. The parameters
for analysis will be specified in the SAP. If contamination in the
field blank is determined, documentation will be provided that will
explain the effect of the contamination on the samples collected.
C-3 If samples are to be collected for analysis of volatile organic
compounds, a volatile organic blank is collected once a day. This
blank consists of laboratory pure water taken to the field and poured
into a sample container in the area where the treatment system is
located. The volatile organic blank is analyzed for the volatile
compounds specified in the SAP. If volatile organic compounds are
measured in this blank, documentation will be provided which will
explain the effect of the contamination on the samples collected.
3.5.4
Corrective Actions
The following corrective actions must be taken as a first step, if
the QC objectives in Sections B-1 and B-5 are not met:
0-1
Calculations will be reviewed for calculation and transcription
errors;
0-2
The laboratory's QA officer will review the analysis with the
analyst to determine whether procedural errors were made;
*
Laboratory pure water is defined in SW-846 as distilled or deionized
water or Type II reagent water.
16
-------
0-3
0-4
3.5.5
Reagents and equipment will be examined to determine if they were
functioning and used properly;
Instrumentation will be examined for calibration and signal response
Instrument Calibration Procedures
The following procedures will be used for instrument calibration:
E-1
Calibration procedures for all sampling and analytical equipment
required for this project are provided in the SW-846 (3rd edition)
methods.
E-2
Calibration standards are to have purities as reported in U.S. EPA's
Quality Assurance Reference Materials Project: Analytical Reference
Materials Inventories, July 1986 (SP-4440086-37). If compounds are
not listed in this document, the calibration standards are to be
prepared from reagent grade compounds. Reagent grade compounds are
reagents that conform to the current specifications of the Committee
on Analytical Reagents of the American Chemical Society.
3.5.6
Data Reduction and Reporting
Analytical results will be reported in the concentration units
specified in the analytical procedure.
If units are not specified in the
analytical procedure, data from the analysis of samples will be reported
in units of ug/l for all aqueous samples and mg/kg dry weight for all
solid samples.
3.5.7
Statistical QC Procedures
The statistical QC procedures used for this work will include
precision (relative percent difference) and percent recovery.
F-1
Precision will be estimated by calculating the relative percent
difference when two values are being evaluated, using the following
equation:
17
-------
RPD = (D} 02) 100
(D} + 02)/2
where
RPD = Relative Percent Difference
D} = The larger of the two observed values
02 = The smaller of the two observed values
F-2 Accuracy will be estimated according to the following equations:
For Surrogate Spikes:
Percent Recovery = 100 (Measured Value)
Spiked Value
For Matrix Spikes:
Percent Recovery = 100 (Ci Co)
Ct
where
Co
(.
1
Ct
= Concentration of unspiked aliquot
= Concentration of spiked aliquot
= Concentration for spike added
18
-------
Table 3-1 BOAT Pollutant List
Parameter
CAS no.
Target detect 10n 1 imlt
(ug/l )
Vo lat lles
1 Acetonltrlle 75-05-8 100
2 Acroleln 107-02-8 100
3 Acrylonltrile 107-13-1 100
4 Benzene 71-43-2 5
5 Bromcdlchloromethane 75-27-4 5
6 Bromcmethane 74-83-9 10
7 Carbon Tetrachloride 56-23-5 5
B Carbon dlsulflde 75-15-0 5
9 Chlorobenzene 108-90-7 5
10 2-Chloro-l,3-butadlene 126-99-8 100
11 Chlorodlbromomethane 124-48-1 5
12 Chloroethane 75-00-3 10
13 2-Chloroethyl vlnyl ether 110-75-8 10
14 Chloroform 67-66-3 5
15 Chloromethane 74-87-3 10
16 3-Chloropropene 107-05-1 100
17 1,2-01bromc-3-chloropropane 96-12-8 10
18 1,2-01bromoethane 106-93-4 5
19 Oibromcmethane 74-95-3 5
20 TranS-1,4-01chloro-2-butene 110-57-6 100
21 Olchlorodlfluoromethane 75-71-8 10
22 1,1-0Ichloroethane 75-35-3 5
23 1,2-Dlchloroethane 107-06-2 5
24 1.1-Dlchloroethylene 75-35-4 5
25 Trans-1.2-01chloroethene 156-60-5 5
26 1.2-Dichloropropane 78-87-5 5
27 Trans-1,3-01chloropropene 10061-02-6 5
28 cls-l,3-Dichloropropene 10061-01-5 5
29 1,4-0IOxane 123-91-1 200
30 Ethyl cyanide 10712-0 100
31 Ethyl methacrylate 97-63-2 100
32 Iodomethane 74-88-4 50
33 [sobuty 1 a lcoho 1 78-83-1 200
34 Methyl ethyl ketone 78-93-3 10
35 Methyl methacrylate 80-62-6 100
36 Methyl methanesulfonate 66-27-3 20D
37 Methylacrylonltrl1e 126-98-7 100
38 Methylene chloride 75-09-2 5
39 Pyr ld lne 110-86-1 400
19
-------
Table 3-1
(Contlnued)
Parameter CAS no. Target detect lOn 11m i t
(ug/l)
Volatlles (contInued)
40 1,1,1,2-Tetrachloroethane 630-20-6 5
41 1,1,2,2-Tetrachloroethane 79-34-5 5
42 Tetrachloroethene 127-18-4 5
43 Toluene 108-88-3 5
44 Tribromomethane 75-25-2 5
45 1,1,1-Trichloroethane 71- 55-6 5
46 1,1,2-Trlchloroethane 79-00-5 5
47 Trichloroethene 79-01-6 5
48 Trichloromonofluoromethane 75-69-4 5
49 1,2,3-Trlchloropropane 96-18-4 5
50 VInyl chlorlde 75-01-4 10
SemlVolat lles
51 Acenaphthalene 208-96-8 10
52 Acenaphthene 83-32-9 10
53 Acetophenone 96-86-2 10
54 2-Acetylamlnofluorene 53-96-3 1. 000
55 4-Amlnobiphenyl 92-67-1 200
56 Anll ine 62-53-3 20
57 Anthracene 120-12-7 10
58 Aramlte 140-57-8 100
59 Benz(a)anthracene 56-55-3 10
60 Benzenethiol 108-98-6 1,000
61 Benzldine 92-87-5 1,000
62 Benzo(a)pyrene 50-32-8 10
63 Benzo(b)fluoranthene 205-99-2 10
64 Benzo(ghi)perylene 191-24-2 10
65 Benzo(k)fluoranthene 207-08-9 10
66 p-Benzoqulnone 106-51-4 1,000
67 8is(2-chloroethoxy)methane 111-91-1 10
68 B1S(2-chloroethyl)ether 111-44-4 10
69 Bis(2-chloroisopropyl)ether 39638-32-9 10
70 Bls(2-ethylhexyl)phthalate 117-81-7 10
71 4-Bromophenyl phenyl ether 101-55-3 10
72 Butyl benzyl phthalate 85-68-7 10
73 2-sec-Butyl-4,6-dinltrophenol 88-85-7 100
74 p-Chloroanlllne 106-47-8 100
75 Ch lorobenzllate 510-15-6 100
76 p-Chloro-m-cresol 59-50-7 10
77 2-Chloronaphthalene 91-58-7 10
20
-------
Table 3-1
(Cont1nued)
Parameter CAS no. Target detect lon 11m 1 t
(ug/l)
Sem1volat1les (cont1nued)
78 2-Chlorophenol 95-57-8 10
79 3-Chloroprop1on1tr1le 54-27-67 10,000
tJO Chrysene 218-01-9 10
81 ortho-Creso 1 95-48-7 10
82 para-Cresol 106-44-5 10
83 D1benz(a,h)anthracene 53-70-3 10
84 D1benzo(a,e)pyrene 192-65-4 50
85 D1benzo(a,l)pyrene 189-55-9 50
86 m-D1chlorobenzene 541-73-1 10
87 O-D1chlorobenzene 95-50-1 10
88 p-D1chlorobenzene 106-46-7 10
89 3,3'-D1chlorobenz1d1ne 91-94-1 20
90 2,4-D1chlorophenol 120-83-2 10
91 2,6-D1chlorophenol 87-65-0 10
92 D1ethyl phthalate 84-66-2 10
93 3,3'-D1methoxybenz1d1ne 119-90-4 10,000
94 p-D1methylam1noazobenzene 60-11-7 200
95 3,3'-D1methylbenz1d1ne 119-93-7 10,000
96 2,4-D1methylphenol 105-67-9 10
97 D1methyl phthalate 131-11-3 10
98 D1-n-butyl phthalate 84-74-2 10
99 1,4-D1n1trobenzene 100-25-4 100
100 4,6-D1n1tro-o-cresol 534-52-1 50
101 2,4-D1n1trophenol 51-28-5 50
102 2,4-D1n1trotoluene 121-14-2 10
103 2,6-D1n1trotoluene 606-20-2 10
104 D1-n-octyl phthalate 117-84-0 10
105 D1-n-propyln1trosam1ne 621-64-7 10
106 D1phenylam1ne*/
d1phenyln1trosam1nek 122-39-4/86-30-6 10
107 l,2-D1phenylhydraz1ne 122-66-7 10
106 Fluoranthene 206-44-0 10
109 Fluorene 86-73-7 10
110 Hexachlorobenzene 118-74-1 10
111 HexachlorobutadJene 87-68-3 10
112 Hexachlorocyclopentadiene 77-47-4 10
*In GC/MS analys1s, these compounds cannot be d1fferent1ated.
21
-------
Table 3-1
(Contlnued)
Parameter CAS no. Target detect JOn limIt
("g/l)
Semlvolat Iles (cant lnued)
113 Hexachloroethane 67-72-1 10
114 Hexachlorophene 70-30-4 20,000
115 Hexachloropropene 1888-71-7 10
116 Indeno( 1.2.3-cd)pyrene 193-39-5 10
117 [sosafrole 120-58-1 100
118 Methapyr Ilene 91-80-5 200
119 3-Methylcholanthrene 56-49-5 100
120 4.4'-Methylenebls
(2-chloroanlllne) 101-14-4 200
121 Naphthalene 91-20-3 10
122 1.4-Naphthoqulnone 130-15-4 100
123 I-Naphthylamlne 134-32-7 100
124 2-Naphthylamlne 91-59-8 100
125 p-N ltroan lline 100-01-6 50
126 NItrobenzene 98-95-3 10
127 4-N J t ropheno 1 100-02-7 50
128 N-Nltrosodl-n-butylamlne 924-16-3 100
129 N-Nltrosodlethylamlne 55-18-5 100
130 N-Nltrosodlmethylamlne 62-75-9 100
131 N-Nltrosomethylethylamlne 10595-95-6 100
132 N-Nltrosomorphollne 59-89-2 200
133 N-Nltrosoplperldlne 100-75-4 200
134 n-Nltrosopyrrolldlne 930-55-2 200
135 5-Nltro-o-toluldlne 99- 55-8 2JO
136 PentachJorobenzene 608-93-5 10
137 Pentachloroethane 76-01-7 10
138 Pentachloronltrobenzene 82-68-8 100
139 Pentachlorophenol 87-86-5 50
140 Phenacetin 62-44-2 100
141 Phenanthrene 85-01-8 10
142 Pheno 1 108-95-2 10
143 2-Plcollr,e 109-06-8 100
144 Pronamlde 23950-58-5 100
145 P jrene 129-00-0 10
146 ResorcInol 108-46-3 1.000
147 Safrole 94-59-7 100
148 1.2,4.5-Tetrachlorobenzene 95-94-3 10
22
-------
Table 3-1
(Cont lnued)
Pa rarneter CAS no. Target detection limlt
(ug/l )
Semlvo lat lles
149 2,3,4,6-Tetrachlorophenol 58-90-2 100
150 1,2,4-Trlchlorobenzene 120-82-1 10
151 2,4,5-Trlchlorophenol 95-95-4 50
152 2,4,6-Trich1orophenol 88-06-2 10
153 Trls(2,3-dlbromopropyl)
phosphate 126-72-7 10,000
Metals
154 Antimony 7440-36-0 60
155 Arsenlc 7440-38-2 10
156 Ba r lUm 7440-39-3 200
157 Berylllum 7440-41-7 5
158 Cadmlum 7440-43-9 5
159 Chrom 1 um (total) 7440-47-3 10
160 Chrom i um (hexavalent) 10
161 Copper 7440-50-8 25
162 Lead 7439-92-1 5
163 Mercu ry 7439-97-6 0.2
164 N icke 1 7440-02-0 40
165 Se len lUm 7782-49-2 5
166 S llver 7440-22-4 10
167 Tholl ium 7440-28-0 10
168 Vanadium 7440-62-2 50
169 Zinc 7440-66-6 20
Inorqonics
170 Cyanide 57-12-5 10
171 Fluorlde 16964-48-8 500
172 Sulflde 8496-25-8 1000
Orqanoch lor lne Pestlcides
173 A ldrl n 309-00-2 0.05
174 0 1pha -BHC 319-84-6 0.05
175 beta-BHC 319-85-7 0.05
176 delta-BHC 319-86-8 0.05
23
-------
Table 3-1
(Contlnued)
Parameter CAS no. Target detection limlt
(ug/l )
Orqanochlorlne Pestlcldes (contlnued)
177 gamma-BHC 58-89-9 0.05
178 Chlordane 57-74-9 0.5
179 ODD 72-54-8 0.01
180 DDE 72-55-9 0.10
181 DDT 50-29-3 0.10
182 Dleldrin 60-57-1 0.10
183 Endosulfan I 959-98-8 0.05
184 Endosulfan II 33213-6-5 0.10
185 End rl n 72-20-8 0.10
186 Endrln aldehyde 7421-93-4 0.1
187 Heptachlor 76-44-8 0.05
188 Heptachlor epoxlde 1024-57-3 0.05
189 Isodrin 465-73-6 0.1
190 Kepone 43-50-0 0.5
191 Methoxyclor 72-43-5 0.5
192 Toxaphene 8001-35-2 1.0
Phenoxyacetlc ACld Herblcldes
193 2,4-Dlchlorophenoxyacetlc aCld 94-75-7 0.5
194 S llvex 93-72-1 0.5
195 2,4,5-T 93-76-5 0.5
Orqanophosphorous lnsectlcldes
196 D i su lfoton 298-04-0 1.0
197 Famphur 52-85-7 1.0
198 Methyl parathion 298-00-0 1.0
199 ParathlOn 56-38-2 1.0
200 Phorate 298-02-2 1.0
PCBs
201 Aroclor 1016 12674-11-2 0.5
202 Aroclor 1221 11104-28-2 0.5
203 Aroclor 1232 11141-16-5 0.5
204 Aroclor 1242 53469-21-9 0.5
205 Aroclor 1248 12672-29-6 0.5
206 Aroclor 1254 11097 -69-1 1.0
207 Aroclor 1260 11096-82-5 1.0
24
-------
Table 3-1 (Continued)
Parameter CAS no. Target detection limit
(ug/1)
Dioxins and Furans
208 Hexachlorodibenzo-p-dioxins 0.02
209 Hexachlorodibenzofuran 0.02
210 Pentachlorodibenzo-p-dioxins 0.02
211 Pentachlorodibenzofuran 0.02
212 Tetrachlorodibenzo-p-dioxins 0.02
213 Tetrachlorodibenzofuran 0.02
214 2,3,7,8-Tetrachlorodibenzo-p-dioxin 0.02
25
-------
4.
OTHER QUALITY ASSURANCE ELEMENTS OF
THE BOAT DATA COLLECTION PROGRAM
4.1
Chain of Custody Procedures
Chain of custody procedures must be followed during sample collection
and sample analysis to maintain the integrity of the data.
The individual
samples must be maintained under custody and all handling of the sample
must be traceable continuously from the time of collection until all
analytical work is completed.
In the event that chain of custody
procedures are broken, a written explanation providing an analysis of the
risk to the data integrity.
4.1.1
Field Sampling Operations
The field sampler must initiate the chain of custody procedures by
documenting when sampling activities are started.
Once the sample is
obtained, the sampler should keep the sample either in view or in a locked
or sealed storage area, or in a secure area until custody is relinquished
and formal documentation of such transfer is completed.
The initial
documentation should include the following information necessary for sample
identification and custody records:
. Project identifier code;
. Plant;
. Sample location;
. Sample type or matrix;
. Sample date and time;
. Signature of sampler;
. Analysis required;
. Remarks (e. g., preservatives used)
26
-------
Sample custody documentation is maintained until the samples are
delivered to the laboratory or to a common carrier for shipment to the
1 aboratory.
Samples are identified by adhesive backed labels (Figure 4-1)
containing the preceding information.
The labels must be either
waterproof or covered with waterproof tape.
The field custodian is responsible for the proper documentation,
preservation, storage, and shipment of the samples until they are
delivered to the laboratory.
The field custodian fills out a sample
chain of custody record (Figure 4-2); this record sheet is prepared in
duplicate; one copy is sent with the samples; the other is maintained by
the field sample custodian.
A tamperproof seal (Figure 4-3) is attached
to each sample package prior to transmittal to the laboratory to ensure
that the integrity of the samples has been maintained during shipment.
4.1. 2
Sample Receiving
Upon delivery to the laboratory, custody is transferred to the
laboratory sample custodian.
After verifying the number of samples,
their identification, and their integrity, the laboratory custodian signs
the appropriate sample documentation if delivered personally, or
completes the sample shipping/receiving record if delivered by common
carrier.
Any discrepancies are noted on the appropriate form.
Every sample entering the laboratory for analysis is assigned a
unique identity in the laboratory's sample log-in book.
27
-------
18270
18270 Duplicate
Parameter
18270
Parameter
Plant
Task
Sample Location
Matrix
Sampling Comments
Signa tu re
Fioure 4-1
Time/Date
}
}
Affixed to Sample Container
Affixed to Duplicate Sample
(e.g.. VOA Samples)
Entered in Field Notebook as
Permanent Sample Identification
Exa~ple of sample label.
28
-------
CHAIN Of CUSTODY RECORD
N
'-0
I ~_.
PROJECT NO. PROJECT NAME i / PARAMEIlRS
SAMPLERS: fS.......1 W, In'.o) jlfj/////I;
REMARKS
flHD ~ .
SAMf'LE DATE TIME C SAMPLE lOCATION
II:
N~ER u 0
~
-- - -- -~~--
--
- -
-.-
- - -~---------- ~- -- - -- - - - -~- -~ ---- -~-- -~--- --- -~ -
- ----- ---------- n-
- - -
- - - - - - - - _. - - -~---_._-- - --- -~_.
Relin"....hed by: fS.",..,..,.1 De.. I Time R_i.eeI by: fs,g,..,..,.1 Relinquilhed by: fs,g,..,.".1 De.. I Time RKeu,ed by. (SjlJl~lu/.J
I 1
_-
,P.....ed' CPrlnoed' CPrlnoed, IP,IOted)
Relinquilhed by: fs,g,.."".1 De.e I Time R_wed 'Of hb"utOfy by: De.. I Time Re_kl
I IS",..",,.I I
&prlnled. tPunl8d.
p..".....u"". 0........ PI... 0... "'"""-'* SlupmMI .""',.. - ..n_,. Copy.o Coo,dI....or foeld f,'. Iponk!.
Figure
4-2
Example Chain of
Custody Form
-------
Sent by:
Laboratory
Seal Number
5786
Date:
Figure 4-3 Example of Tamperproof Seal.
30
-------
The samples are refrigerated at or below 4 C.
The refrigerators are
either kept in locked limited access area or the refrigerators are locked
4.1. 3
Sample Analyses
The laboratory analyst prepares the laboratory data sheet which
includes the following information:
.
Sample numbers;
Date sample received by the analyst;
Analysis and method number;
Portion required for analysis;
Initials of analyst and dates sample handled;
Initials of chemist checking calculations; and
Detection levels desired.
.
.
.
.
.
.
After obtaining the sample, the analyst verifies the information
on the laboratory data sheet with the information on the sample container
and annotates the records appropriately.
If a question arises, it is
first discussed with the sample custodian.
If this does not resolve the
problem, it is brought to the attention of the person submitting the
sample for analysis.
If the problem cannot be resolved, the EPA WAM
should be notified before the sample is voided.
The analyst keeps the
samples in view or under limited access locked storage.
The analyst
visually inspects the sample to determine that the physical condition is
suitable for analysis.
For any sample whose condition is questionable,
the EPA WAM is to be notified prior to analysis.
The analyst must
maintain proper custodial procedures while analyzing a sample.
Samples
or intermediate solutions must either be in the analyst's physical
31
-------
possession, in view, or in a limited access locked area.
The
laboratories are locked so that only authorized personnel have access.
Analyses should be conducted in accordance with the procedures
specified in the contract statement of work and referenced by number to
the standard method in the laboratory procedures manual.
Any deviation
from these procedures must be annotated.
All data are recorded on the
data sheet.
Associated calibrations must be recorded either directly on
or attached to the data sheet or indirectly by reference to the standard
solution number or instrument number.
4.1.4
Sample Recordkeeping
The sample identification is used on all data sheets, containers,
beakers, etc.
The sample number or name can be used for extra
information, if desired.
Exceptions are instances in which a set of
numbered containers, such as Kjeldahl flasks or ashing crucibles, is
used; here the container number must be matched on the data sheet with
the sample identification.
Associated calibration curves and charts should be signed and dated.
The exact method of analysis must be readily ascertainable.
This is most
easily done by making reference to the standard analytical procedure used
when a method allows for a choice of procedures.
If any portion of the
sample remains after analysis is completed and if storage is required,
the analyst must return it to the laboratory sample storage area.
32
-------
The analyst's calculations are checked as required by an internal
aud it.
The person checking the calculations signs and dates the data
sheet.
The data sheet is returned to the file.
All records must be in
ink.
Errors are corrected by drawing a straight line through the error,
recording the correct entry. initialing, and dating the correction.
Completed records are maintained by the designated laboratory document
control officer.
When all analyses are completed, the report is prepared and
delivered.
A copy of the report, the raw data, and other documents are
provided to the EPA WAM, as well as placed in the files, which are kept
in either locked file cabinets or in a secure limited access area.
4.2
Performance and System Audits
Data generated as part of the analytical quality control program will
be reviewed by the QA Coordinator or a subcontractor's QA officer and the
appropriate site team leader to assure the absence of systematic bias or
trends and that appropriate corrective actions are taken as required.
Quality problems identified and corrective actions taken because of these
reviews will be included in the site report.
Field activities of each contractor will be audited at least once by
a third party representative design~ted by EPA to assure that required
equipment and procedures for sample collection, preservation, shipping,
handling, laboratory, and documentation are used.
33
-------
REFERENCES
1.
U.S. EPA. 1986. U.S. Environmental Protection Agency. Test
Methods for Eva7uating So7id Waste: Physica7/Chemica7 Methods.
SW-846, Washington, D.C.: U.S. Environmental Protection Agency,
Office of Solid Waste and Emergency Response, November 1986.
U.S. EPA. 1986. U.S. Environmental Protection Agency. Qua7ity
Assurance Reference Materia7s Project: Ana7ytica7 Reference
Materia7s Inventories, Washington, D.C.: U.S. Environmental
Protection Agency, July 1986, SP-4440-86-37.
2.
34
------- |