A540/R-93/051
United States Office of Publication 9240.0-05A
Environmental Protection Solid Waste and EPA540/R-93/051
Agency Emergency Response PB93-983316
Washington, DC 20460 December 1992
Superfund
&EPA Specifications and
Guidance for
Contaminant-Free
Sample Containers
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TABLE OF CONTENTS
SECTION TITLE PAGE
I. INTRODUCTION 1
II. SAMPLE CONTAINER AND
COMPONENT MATERIAL SPECIFICATIONS 4
III. SAMPLE CONTAINER PREPARATION
AND CLEANING PROCEDURES 14
IV. SAMPLE CONTAINER QUALITY ASSURANCE
AND QUALITY CONTROL REQUIREMENTS 17
ill
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SECTION I
INTRODUCTION
In August 1989, the Environmental Protection Agency's (EPA) Office of Emergency and Remedial
Response (OERR) decentralized Superfund's Sample Container Repository program (OSWER Directive
#9240.0-05). In conjunction with the decentralization of Superfund's bottle program, OERR issued
specifications and guidance for preparing contaminant-free sample containers to assist the Regions in
obtaining appropriate sample containers from commercially available suppliers.
The December 1992 version of "Specifications and Guidance for Contaminant-Free Sample
Containers" revises the specifications and provides a single source of standardized specifications and
guidance on appropriate cleaning procedures for preparing contaminant-free sample containers that meet
all Contract Laboratory Program (CLP) detection/quantitation limits, including those for low
concentration analyses.1 Although the specifications and guidance procedures contained in this document
are based on CLP low concentration requirements, they also are suitable for use in other analytical
programs.
Specifications and guidance for preparing contaminant-free sample containers are provided in the
sections that follow and are intended to describe one approach for obtaining cleaned, contaminant-free
sample containers for use by groups performing sample collection activities under Superfund and other
hazardous waste programs. Although other cleaning procedures may be used, sample containers must
meet the criteria specified in Section II. In certain instances, the user of the sample containers may
require exact adherence to the cleaning procedures and/or quality control analysis described in this
document. In other instances, the user may require additional or different cleaning procedures and/or
quality control analysis of the sample containers. The specific needs of the bottle user will determine the
requirements for the cleaning and quality control analysis of the sample containers as long as the
minimum criteria are met. It is the responsibility of the bottle user to define the sample container
preparation, cleaning, and quality control requirements.
The document has been extensively reviewed and revised since the August 1989 iteration, and
important enhancements have been incorporated, including:
Removing references to the color of the closures;
Allowing the use of polypropylene closures as an alternative to phenolic closures;
Referencing CLP Low Concentration Organics and Inorganics Statements of Work for the
analysis of calibration verification solutions and blanks;
Including cleaning and quality control procedures for fluoride and nitrate/nitrite;
Removing the hexane rinse from the cleaning procedure for container types A, E, F, G, H, J,
and K (semivolatile organics, pesticides, metals, cyanide, and fluoride in soils and water);
1 Because this document does not address the procurement of contaminant-free sample containers, the
title was changed from "Specifications and Guidance for Obtaining Contaminant-Free Sample Containers"
to "Specifications and Guidance for Contaminant-Free Sample Containers."
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Adding the recommendation that the bottle vendor establish and submit a Quality Assurance
Plan (QAP);
Changing the QA/QC documentation requirements so that copies of the raw data from the
analyses of the QC containers are available upon request and not automatically sent to the
bottle purchaser;
Changing the permanent lot number assignment to a nine-digit number from an eight-digit
number, where the extra digit represents the analysis parameter;
Adding Chemical Abstract Services (CAS) registry number for the inorganic analytes in
Table 1; and
Recommending an annual demonstration of the bottle vendor's ability to meet detection
limits and establish reproducibility of the cleaning techniques.
OERR and the EPA Regions decided to use the most stringent CLP requirements available to set
the specifications for obtaining contaminant-free sample containers. As a result, the CLP Inorganics and
Organics Low Concentration Statement of Work (SOW) requirements were selected as the basis for these
specifications. Major factors in this decision included the desire to have a set of bottle cleaning
specifications that met or exceeded all analytical requirements and the related need to avoid potential
misuse of cleaned bottles (e.g., using a container cleaned by a multi-concentration procedure for a low
concentration sample). OERR will reevaluate this decision if the low concentration requirements are
deemed to be too stringent.
Most environmental sampling and analytical applications offer numerous opportunities for sample
contamination. For this reason, contamination is a common source of error in environmental
measurements. The sample container itself represents one such source of sample contamination. Hence,
it is vital that sample containers used within the Superfund program meet strict specifications established
to minimize contamination which could affect subsequent analytical determinations. Superfund sampling
and analysis activities require all component materials (caps, liners, septa, packaging materials, etc.)
provided by the bottle preparer to meet the criteria limits of the bottle specifications listed within Section
II.
Section HI provides guidance on cleaning procedures for preparing contaminant-free sample
containers that meet the specifications contained in Section II. The procedures provided in this section
are intended to provide sample containers that meet all current CLP Low Concentration Inorganics and
Organics detection/quantitation levels.
In selecting cleaning procedures for sample containers, it is important to consider all of the
parameters of interest. Although a given cleaning procedure may be effective for one parameter or type of
analysis, it may be ineffective for another. When multiple determinations are performed on a single
sample or on a subsample from a single container, a cleaning procedure may actually be a source of
contamination for some analytes while minimizing contamination in others. It should be the responsibility
of the bottle supplier to verify that the cleaning procedures actually used satisfy the quality control
requirements set forth in Section IV.
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Two aspects of quality assurance (i.e., quality control and quality assessment) must be applied to
sample containers as well as to the analytical measurements. Quality control includes the application of
good laboratory practices and standard operating procedures especially designed for the cleaning of sample
containers. The cleaning operation should be based on protocols especially designed for specific
contaminant problems. Strict adherence to these cleaning protocols is imperative. Quality assessment of
the cleaning process depends largely on monitoring for adherence to the respective protocols. Because of
their critical role in the quality assessment of the cleaning operation, protocols must be carefully designed
and followed. Guidance is provided in Section IV on design and implementation of quality assurance and
quality control protocols.
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SECTION II
SAMPLE CONTAINER AND COMPONENT MATERIAL SPECIFICATIONS
This Section identifies sample containers commonly used in the Superfund program and provides
specifications for contaminant-free sample containers for each bottle type.
A. CONTAINER MATERIAL
A variety of factors affect the choice of containers and cap material. These include resistance to
breakage, size, weight, interferences with analytes of interest, cost, and availability.
Container types A through L (Figure 1, pages 6-7) are designated as the type of sample containers
that have been used successfully in the past. Kimax or Pyrex brand borosilicate glass is inert to most
materials and is recommended where glass containers are used (i.e., pesticides and other organics).
Conventional polyethylene is recommended when plastic is acceptable because of its lower cost and lower
adsorption of metal ions. The specific sampling situation will determine the use of plastic or glass.
While the sample containers shown in Figure 1 are utilized primarily for Superfund sampling
activities, they also may be used for sampling activities under other programs, such as the Resource
Conservation and Recovery Act (RCRA).
B. MAXIMUM CONTAMINANT LEVEL SPECIFICATIONS FOR SAMPLE CONTAINERS
The CLP, through a series of technical caucuses, has established inorganic Contract Required
Detection Limits (CRDL) and organic Contract Required Quantitation Limits (CRQL) which represent
the minimum quantities needed to support the hazardous substance identification and monitoring
requirements necessary for remedial and other actions at hazardous waste sites.
For inorganic sample containers, the CRDLs listed in Table 1, page 8, are the specifications for
maximum trace metal contamination. Concentration at or above these limits on any parameter should
preclude these containers from use in collecting inorganic samples.
The CRQL specifications for organic sample containers are listed in Table 2, pages 9-13. When
the CRQL in Table 2 is multiplied by the appropriate factor listed below, the resulting value then
represents the maximum concentration allowed for particular sample containers based on organic CLP
sample sizes for routine analyses.
Container type Multiple of CRQL
A 1.0
B 0.5
D 10.0
E 8.0
F 4.0
G 2.0
H 0.5
J 0.5
K 2.0
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The philosophy used for determining the maximum permissible amount of contamination in a
sample container was to consider the number of aliquots of sample that are available in the containet and
assume that the contamination present would be uniformly distributed in all of the aliquots. This
assumption, and the assumption that there should be no more than one-half the CRQL contributed by the
container, resulted in the establishment of contamination limits by container type. For example, the
volume of container type D is sufficient to allow 20 volatile determinations. Therefore, if 10 times the
CRQL of contaminant is present in the cleaned bottle, each aliquot tested will contain one-half of the
CRQL of contaminant due to the contribution from the bottle.
C. GROSS CONTAMINATION
Gross contamination is defined as greater than two hundred times the acceptable concentration
values in Tables 1 or 2 (multiplied by the appropriate factor), unless the cleaning procedure is successful
in reducing the amount of contamination to within specifications. If this is not achieved, the grossly
contaminated materials should be discarded and replaced to prevent cross contamination with other
batches of containers. The bottle preparer should inspect all materials to ensure conformance with the
required specifications.
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FIGURE I
SAMPLE CONTAINER
SPECIFICATIONS
Container
Type Specifications
A Container: 80-oz amber glass, ring handle
bottle/jug, 38-mjn neck finish.
Closure: polypropylene or phenolic cap,
38-430 size; 0.015-in Teflon liner.
Total Weight: 2.45 Ibs.
B Container: 40-mL glass vial, 24-mm neck finish.
Closure: polypropylene or phenolic, open-top,
screw cap, 15-cm opening, 24-400 size.
Septum: 24-mm disc of 0.005-in Teflon
bonded to 0.120-in silicon for total thickness
of0.125-in.
Total Weight: 0.72 oz.
C Container: 1-L high-density polyethylene,
cylinder-round bottle, 28-mm neck finish.
Closure: polyethylene cap, ribbed, 28-410 size;
F217 polyethylene liner.
Total Weight: 1.89 oz.
D Container: 120-mL wide mouth, glass vial,
48-mm neck finish.
Closure: polypropylene cap, 48-400 size;
0.015-in Teflon liner.
Total Weight: 4.41 oz.
E Container: 16-oz tall, wide mouth,
straight-sided, flint glass jar,
63-mm neck finish.
Closure: polypropylene or phenolic cap,
63-400 size; 0.015-in Teflon liner.
Total Weight: 9.95 oz.
F Container: 8-oz short, wide mouth,
straight-sided, flint glass jar,
70-mm neck finish.
Closure: polypropylene or phenolic cap,
70-400 size; 0.015-in Teflon liner.
Total Weight: 7.55 oz.
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FIGURE 1
SAMPLE CONTAINER
SPECIFICATIONS
(Continued)
Container
Type Specifications
G Container: 4-oz tall, wide mouth,
straight-sided, flint glass jar,
48-mm neck finish.
Closure: polypropylene or phenolic cap,
48-400 size; 0.015-in Teflon liner.
Total Weight: 4.70 oz.
H Container: 1-L amber, Boston round, glass
bottle, 33-mm pour-out neck finish.
Closure: polypropylene or phenolic cap,
33-430 size; 0.015-in Teflon liner.
Total Weight: 1.11 Ibs.
J Container: 32-oz tall, wide mouth,
straight-sided, flint glass jar,
89-mm neck finish.
Closure: polypropylene or phenolic cap,
89-400 size; 0.015-in Teflon liner.
Total Weight: 1.06 Ibs.
K Container: 4-L amber glass, ring handle
bottle/jug, 38-mm neck finish.
Closure: polypropylene or phenolic cap,
38-430 size; 0.015-in Teflon liner.
Total Weight: 2.88 Ibs.
L Container: 500-mL high-density polyethylene,
cylinder-round bottle, 28-mm neck finish.
Closure: polypropylene cap, ribbed, 28-410 size;
F217 polyethylene liner.
Total Weight: 1.20 oz.
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TABLE 1
INORGANIC ANALYTE
SPECIFICATIONS
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
Fluoride
Nitrate/Nitrite
CAS Number
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-70-2
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92-1
7439-95-4
7439-96-5
7439-97-6
7440-02-0
7440-09-7
7782-49-2
7440-22-4
7440-23-5
7440-28-0
7440-62-2
7440-66-6
57-12-5
16984-48-8
1-005
CRDL1 (/ig/L)
100
5
2
20
1
1
500
10
10
10
500
2
500
10
0.2
20
750
3
10
500
10
10
20
10
200
100
CRDLs are based on the CLP Inorganics Low Concentration SOW
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TABLE 2
ORGANIC COMPOUND
SPECIFICATIONS
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
Volatiles
Chloromethane
Bromomethane
Vinyl Chloride
Chloroethane
Methylene Chloride
Acetone
Carbon Disulfide
1,1-Dichloroethene
1,1-Dichloroethane
cis- 1 ,2-Dichloroethene
trans-l,2-Dichloroethene
Chloroform
1,2-Dichloroethane
2-Butanone
Bromochloromethane
1,1,1 -Trichloroethane
Carbon Tetrachloride
Bromodichloromethane
1 ,2-Dichloropropane
cis- 1 ,3-Dichloropropene
Trichloroethene
Dibromochloromethane
1 , 1 ,2-Trichloroethane
Benzene
trans-l,3-Dichloropropene
Bromoform
4-Methyl-2-pentanone
2-Hexanone
Tetrachloroethene
1 , 1 ,2,2-Tetrachloroethane
CAS Number
74-87-3
74-83-9
75-01-4
75-00-3
75-09-2
67-64-1
75-15-0
75-35-4
75-34-3
156-59-4
156-60-5
67-66-3
107-06-2
78-93-3
74-97-5
71-55-6
56-23-5
75-27-4
78-87-5
10061-01-5
79-01-6
124-48-1
79-00-5
71-43-2
10061-02-6
75-25-2
108-10-1
591-78-6
127-18-4
79-34-5
CRQL1 (Mg/L)
1
1
1
1
2
5
1
1
1
1
1
1
1
5
1
1
1
1
1
1
I
1
1
1
1
1
5
5
1
1
1 CRQLs are based on the CLP Organics Low Concentration SOW
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
31.
32.
33.
34.
35.
36.
37.
38.
39.
40.
Volatiles
1,2-Dibromoethane
Toluene
Chlorobenzene
Ethylbenzene
Styrene
Xylenes (total)
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1 ,2-Dichlorobenzene
1 ,2-Dibromo-3-chloropropane
CAS Number
106-93-4
108-88-3
108-90-7
100-41-4
100-42-5
1330-20-7
541-73-1
106-46-7
95-50-1
96-12-8
CRQL1 (Mg/L)
1
1
1
1
1
1
1
1
1
1
1 CRQLs are based on the CLP Organics Low Concentration SOW
10
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
Semivolatiles
Phenol
bis-(2-Chlorethyl)ether
2-Chlorophenol
2-Methylphenol
2,2'-oxybis-(l-Chloropropane)
4-Methylphenol
N-Nitroso-di-n-dipropylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
bis-(2-Chloroethoxy)methane
2,4-Dichlorophenol
1 ,2,4-Trichlorobenzene
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Methylnaphthalene
Hexachlorocyclopentadiene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronaphthalene
2-Nitroaniline
Dimethylphthalate
Acenaphthylene
2,6-Dinitrotoluene
3-Nitroaniline
Acenaphthene
CAS Number
108-95-2
111-44-4
95-57-8
95-48-7
108-60-1
106-44-5
621-64-7
67-72-1
98-95-3
78-59-1
88-75-5
105-67-9
111-91-1
120-83-2
120-82-1
91-20-3
106-47-8
87-68-3
59-50-7
91-57-6
77-47-4
88-06-2
95-95-4
91-58-7
88-74-4
131-11-3
208-96-8
606-20-2
99-09-2
83-32-9
CRQL1 (Mg/L)
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
20
5
20
5
5
5
20
5
1 CRQLs are based on the CLP Organics Low Concentration SOW
11
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
31.
32.
33.
34.
35.
36.
37.
38.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48
49.
50.
51.
52.
53.
54.
55.
56.
57.
58.
59.
60.
Semivolatiles
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
4-Chlorophenyl-phenylether
Fluorene
4-Nitroaniline
4,6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3'-Dichlorobenzidine
Benz[a]anthracene
Chyrsene
bis-(2-Ethylhexyl)phthalate
Di-n-octylphthalate
Benzo[b]fluoranthene
Benzo[kjfluoranthene
\
Benzo[a]pyrene
Indeno(l,2,3-cd)pyrene
Dibenz[a,h]anthracene
Benzo[g,h,i]perylene
CAS Number
51-28-5
100-02-7
132-64-9
121-14-2
84-66-2
7005-72-3
86-73-7
100-01-6
534-52-1
86-30-6
101-55-3
118-74-1
87-86-5
85-01-8
120-12-7
84-74-2
206-44-0
129-00-0
85-68-7
91-94-1
56-55-3
218-01-9
117-81-7
117-84-0
205-99-2
207-08-9
50-32-8
193-39-5
53-70-3
191-24-2
CRQL1 (Mg/L)
20
20
5
5
5
5
5
20
20
5
5
5
20
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
1 CRQLs are based on the CLP Organics Low Concentration SOW
12
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
Pesticides/PCBs
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4,4'-DDE
Endrin
Endosulfan II
4,4'-DDD
Endosulfan sulfate
4,4'-DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
alpha-Chlordane
gamma-Chlordane
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
CAS Number
319-84-6
319-85-7
319-86-8
58-89-9
76-44-8
309-00-2
1024-57-3
959-98-8
60-57-1
72-55-9
72-20-8
33213-65-9
72-54-8
1031-07-8
50-29-3
72-43-5
53494-70-5
7421-36-3
5103-71-9
5103-74-2
8001-35-2
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
CRQL1 (Mg/L)
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.10
0.02
0.02
0.01
0.01
1.0
0.20
0.20
0.40
0.20
0.20
0.20
0.20
1 CRQLs are based on the CLP Organics Low Concentration SOW
13
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SECTION III
SAMPLE CONTAINER PREPARATION AND CLEANING PROCEDURES
This Section is provided as guidance for the preparation of sample containers that meet the
contaminant-free specifications contained in Section II. There are various procedures for cleaning sample
containers depending upon the analyses to be performed on the sample. The following cleaning
procedures are modeled after those specified for the Superfund Sample Container Repository program.
Other suitable cleaning procedures exist and may be used as long as the sample containers meet the
criteria established in Section II. In some instances, the specific needs of the bottle user may dictate exact
adherence to the sample container preparation and cleaning procedures that follow; while in other
instances, modifications may be required. It is the responsibility of the bottle user to define the sample
container preparation, cleaning, and quality control requirements.
A. Cleaning Procedure for Container Types: A, E, F, G, H, J, and K
1. Sample Type: Semivolatile Organics, Pesticides, Metals, Cyanide, and Fluoride in Soils and Water.
a. Wash glass bottles, Teflon liners, and caps with hot tap water using laboratory grade
nonphosphate detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse with 1:1 nitric acid (reagent grade HNO3, diluted with ASTM Type I deionized water).
d. Rinse three times with ASTM Type I organic free water.
e. Oven dry bottles, liners, and caps at 105-125°C for one hour.
f. Allow bottles, liners, and caps to cool to room temperature in an enclosed contaminant-free
environment.
g. Rinse bottles with pesticide grade methylene chloride (or other suitable solvents specified by
the bottle user) using 20 mL for 1/2-gallon containers; 10 mL for 32-oz and 16-oz containers;
and 5 mL for 8-oz and 4-oz containers.
h. Oven dry bottles, liners, and caps at 105-125°C for one hour.
i. Allow bottles, liners, and caps to cool to room temperature in an enclosed contaminant-free
environment.
j. Place liners in lids and cap containers.
k. Label each container with the lot number and pack in a case.
1. Label exterior of each case with the lot number.
m. Store in a contaminant-free area.
14
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2. Sample Type: Nitrate/Nitrite in Soils and Water.
a. Substitute reagent grade sulfuric acid (H2SO4) for nitric acid in step A.I.e.
b. Follow all other steps in the cleaning procedure described in part A. I above.
B. Cleaning Procedure for Container Types: B, D
1. Sample Type: Purgeable (Volatile) Organics in Soils and Water.
a. Wash glass vials, Teflon-backed septa. Teflon liners, and caps in hot water using laboratory
grade nonphosphate detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse three times with ASTM Type I organic-free water.
d. Oven dry vials, caps, septa, and liners at 105-125°C for one hour.
e. Allow vials, caps, septa, and liners to cool to room temperature in an enclosed contaminant-
free environment.
f. Seal 40-mL vials with septa (Teflon side down) and cap.
g. Place liners in lids and cap 120-mL vials.
h. Label each vial with the lot number and pack in a case.
i. Label exterior of each case with the lot number.
j. Store in a contaminant-free area.
C. Cleaning Procedure for Container Types: C, L
1. Sample Type: Metals, Cyanide, and Fluoride in Soils and Water.
a. Wash polyethylene bottles and caps in hot tap water using laboratory-grade nonphosphate
detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse with 1:1 nitric acid (reagent grade HNO3, diluted with ASTM Type I deionized water).
d. Rinse three times with ASTM Type I deionized water.
e. Invert and air dry in a contaminant-free environment.
f. Cap bottles.
g. Label each container with the lot number and pack in a case.
15
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h. Label exterior of each case with the lot number.
i. Store in a contaminant-free area.
2. Sample Type: Nitrate/Nitrite in Soils and Water.
a. Substitute reagent grade sulfuric acid (H2SO4) for nitric acid in step C.l.c.
b. Follow all other steps in the cleaning procedure described in part C.1 above.
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SECTION IV
SAMPLE CONTAINER QUALITY ASSURANCE AND QUALITY CONTROL REQUIREMENTS
A. Quality Assurance
The objectives of this Section are to: (1) present procedures for evaluating quality assurance (QA)
information to ensure that specifications identified in Section II have been met; and (2) discuss techniques
for the quality control (QC) analysis of sample containers to be used in conjunction with the cleaning
procedures contained in Section III.
The bottle vendor should establish a Quality Assurance Plan (QAP) with the objective of
providing sound analytical chemical measurements, production procedures, and tracking systems. The
QAP should incorporate procedures for the inspection of incoming raw materials; preparation, cleaning,
and labeling of container lots; quality control analyses of cleaned container lots; document control,
including all documentation required for analysis, packing, shipping, and tracking of container lots; any
necessary corrective actions; and any quality assessment measures implemented by management to ensure
acceptable performance. The QAP should be available and provided to the bottle purchaser upon request.
Major QA/QC activities should include the inspection of all incoming materials, QC analysis of
cleaned lots of containers, and monitoring of the container storage area. Complete documentation of all
QC inspection results (acknowledging acceptance or rejection) should be kept as part of the permanent
bottle preparation files. QA/QC records (e.g., preparation/QC logs, analytical data, data tapes, storage log)
also should be stored in a central location within the facility.
Documentation indicating that the container lot has passed all QA/QC requirements should be
provided by the bottle vendor to the bottle purchaser with each container lot. Documentation should
include a signed and dated cover statement affirming that all QA/QC criteria were met. Copies of raw
data from applicable analyses of the QC containers, laboratory standards, check samples, and blanks should
be available and provided upon request. Original documentation should be retained for at least 10 years.
Minimum documentation that should be available, if applicable, for each lot of containers includes:
A statement that "Sample container lot meets or exceeds all QA/QC criteria
established in 'Specifications and Guidance for Contaminant-Free Sample Containers;'"
Reconstructed Ion Chromatographs (RICs) from volatile and semivolatile organics
determinations, including calibration verification standards, check samples, and blanks;
GC chromatographs from pesticides determinations, including calibration verification
standards, check samples, and blanks;
» ICP, hydride-ICP, or ICP-MS instrument readouts from metals determinations, including
calibration verification standards, check samples, and blanks;
AA raw data sheets and instrument readouts from metals determinations, including
calibration verification standards, check samples, and blanks; and
Cyanide, fluoride, and nitrate/nitrite raw data sheets and instrument readouts from these
determinations, including calibration verification standards, check samples, and blanks.
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Prior to the first shipment of containers, and at least annually thereafter, the bottle vendor should
demonstrate its ability to meet the CRDLs and CRQLs, and establish the reproducibility of the cleaning
techniques for each bottle type. The ability to meet the CRDLs and CRQLs is accomplished through the
determination of instrument detection limits (IDLs). The bottle vendor should use the procedures in the
current CLP Low Concentration Inorganics and Organics SOWs to determine IDLs. IDLs should be
below the CRDLs or CRQLs. To establish the reproducibility for each bottle type, the bottle vendor
should randomly pick seven containers from a cleaned lot and analyze as described in the Quality Control
Analysis part of this Section. Parameter concentrations should be at or below the CRDL or CRQL for
each bottle type. Documentation from these analyses should be available and provided upon request.
1. Incoming Materials Inspection:
A representative item from each case of containers should be checked for conformance with
specifications provided in Section II. Any deviation should be considered unacceptable. A log of
incoming shipments should be maintained to identify material type, purchase order number, and delivery
date. The date of incoming inspection and acceptance or rejection of the material should also be recorded
on this log.
2. Quality Control Inspection of Cleaned Lots of Containers:
Following container cleaning and labeling, containers should be randomly selected from each
container lot to be used for QC purposes. The two categories of QC containers should be as follows:
a. Analysis QC Containers:
One percent of the total number of containers in each lot should be designated as the analysis QC
container(s). For lots of less than 100 containers, one container should be designated as the
analysis QC container. The sample container preparer should analyze the analysis QC
container(s) to check for contamination prior to releasing the associated container lot for
shipment. The QC analyses procedures specified in the Quality Control Analysis part of this
Section for determining the presence of semivolatile and volatile organics, pesticides, metals,
cyanide, fluoride, and nitrate/nitrite should be utilized.
For each analysis QC container(s), an appropriate QC number should be assigned that cross-
references the QC container to the related lot of containers. For example, the QC number could
be a seven-digit number sequentially assigned to each lot that has undergone QC analysis. Under
this numbering scheme, the first alphabetical character would be the container type letter from
Figure 1, the next four digits would be assigned sequentially in numerical order starting with
"0001" for the first lot to undergo QC analyses, the sixth character would indicate the number of
QC container for the lot, (e.g., "1" for the first QC container in the lot, "2" for the second, etc.)
and the last character would be either a "C" to indicate clearance or an "R" to indicate rejection.
If the representative analysis QC container(s) passes QC inspection, the related lot of containers
should be released, and the appropriate QC number should be entered in the preparation/QC log
to indicate clearance of the lot for shipment.
If the analysis QC container(s) are found to be contaminated per the specified QC analysis
procedures, the appropriate QC rejection number should be assigned and entered in the
preparation/QC log. Any container labels should be removed and the entire lot returned for
reprocessing under a new lot number. Excessive QC rejection for a particular container type
should be noted for future reference.
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A laboratory standard, check sample, and a blank should be run with each QC analysis. A
calibration verification standard should be analyzed once every 12 hours. All QC analysis results
should be kept in chronological order by QC report number in a central QC file. The QC
numbers assigned should be documented in the preparation/QC log, indicating acceptance or
rejection and date of analysis.
A container lot should not be released for shipment prior to QC analysis and clearance. Once the
containers have passed QC inspection, the containers should be stored in a contaminant-free area
until packaging and shipment.
b. Storage QC Containers:
One QC container per lot should be designated as the storage QC container. The storage QC
container should be separated from the lot after cleaning and labeling and should be stored in a
designated contaminant-free area for one year. The date the container is placed in the storage
area should be recorded in the storage QC container log.
If contamination of the particular container lot comes into question at any time following
shipment, the storage QC container should be removed from the storage area and analyzed using
the QC analysis procedures for that container type (see Quality Control Analysis, this Section).
Upon removal, containers should be logged out of the storage area.
The designated storage area should be monitored continuously for volatile contaminants in the
following manner. A precleaned, 40-mL vial that has passed a QC inspection should be filled with
ASTM Type I organic-free water and be placed in the storage area. This vial should be changed at
one-week intervals. The removed vial should be subjected to analysis for volatile organics as
described in the Quality Control Analysis part of this Section. Any peaks indicate contamination.
Identify contaminants, if present, and include the results in a report to all clients who purchased
bottles from the affected lot(s).
B. Quality Control Analysis
The types of QC analyses correlate with the types of containers being analyzed and their future
use in sample collection. The QC analyses are intended for the determination of:
Semivolatile organics and pesticides;
Volatile organics;
Metals;
Cyanide;
Fluoride; and
Nitrate/Nitrite.
QC analyses should be performed according to the container type and related sample type and
utilize the specific method(s) described below.
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1. Determination of Semivolatile Organics and Pesticides:
Container Types: A, E, F, G, H, J, and K
a. Sample Preparation:
Add 60 mL of pesticide-grade methylene chloride to the container and shake for two
minutes.
Transfer the solvent to a Kuderna-Danish (KD) apparatus equipped with a three-ball
Snyder column. Concentrate to less than 10 mL on a steam bath. Split the solvent into
two 5 mL fractions for semivolatile and pesticide determinations.
Add 50 mL of pesticide-grade hexane (for pesticide determinations only) to the KD
apparatus by slowly pouring down through the Snyder column. Concentrate to less than
10 mL to effect solvent replacement of hexane for methylene chloride.
Concentrate the solvent to I mL using a micro-Snyder column.
Prepare a solvent blank by adding 60 mL of the rinse solvent used in step "g" of the
cleaning procedure for container types A, E, F, G, H, J, and K (Section III page 14)
directly to a KD apparatus, and proceed as above.
b. Semivolatile Organics Sample Analysis:
Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW with the following exceptions:
(1) If problems are encountered meeting the %RSD criteria on the initial calibration
for semivolatiles, the high concentration point should be deleted and a four-point
calibration used.
(2) The low concentration standard should be used for the continuing calibration
standard for semivolatile analyses.
(3) The percent difference window should be widened to ± 30 percent for all
compounds.
Inject 1 (iL of solvent into a gas chromatograph/mass spectrometer (GC/MS).
Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Organics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Organics
SOW.
If compounds other than those listed in Table 2 are found in the container blank that
are not in the solvent blank at a peak height or peak area greater than 20 percent of the
nearest internal standard, the containers should be rejected (See Section II, Table 2 for
compound specifications).
Identify and quantitate any contaminant(s) that cause rejection of a container lot.
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A standard mixture of the nine semivolatile organic compounds listed in Table 3 (nage
26) with concentrations in the 5-20 ppb range should be analyzed to ensure that
sensitivities are achieved that will meet contract required quantitation limits. This
standard should be prepared from a different source from the calibration standards.
c. Pesticides Sample Analysis:
Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW.
Inject 1 IJ.L of solvent into a gas chromatograph (GC) equipped with an electron capture
detector (ECD).
Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Organics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Organics
SOW.
If compound peaks other than those listed in Table 2 are at a peak height or peak area
greater than 5 percent of the peak height or peak area of tetra chloro-m-xylene, the
containers should be rejected (See Section II, Table 2).
Identify and quantitate any contaminant(s) that cause rejection of a container lot.
A standard mixture of the seven pesticide compounds listed in Table 3 (page 26) with
concentrations in the 0.01 to 1 ppb range should be analyzed to ensure that sensitivities
are achieved that will meet contract required quantitation limits. This standard should
be prepared from a different source from the calibration standards.
2. Determination of Volatile Organics:
Container Types: B and D
a. Sample Preparation:
Fill the container with ASTM Type I organic-free water.
Cap the container and let stand for 48 hours.
b. Sample Analysis:
Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW with the following exceptions:
(1) If problems are encountered meeting the %RSD criteria on the initial calibration
for volatiles, the high concentration point should be deleted and a four-point
calibration used.
(2) The low concentration standard should be used for the continuing calibration
standard for volatile analyses.
(3) The percent difference window should be widened to ± 30 percent.
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Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Organics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Organics
SOW. The blank should consist of an aliquot of the ASTM Type I water used in the
sample preparation.
If compounds other than those listed in Table 2 are found in the container blank that
are not in the solvent blank at a peak height or peak area greater than 20 percent of the
nearest internal standard, the containers should be rejected (See Section II, Table 2 for
compound specifications).
Identify and quantitate any contaminant(s) that cause rejection of a container lot.
A standard mixture of the five volatile organic compounds listed in Table 3 (page 26)
with concentrations in the 1-5 ppb range should be analyzed to ensure that sensitivities
are achieved that will meet contract required quantitation limits. This standard should
be prepared from a different source from the calibration standards.
3. Determination of Metals:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
Add 100 mL of ASTM Type I deionized water to the container, and acidify with 1.0 mL
of reagent-grade HNO3. Cap and shake for three to five minutes.
Cap the container and let stand for 48 hours.
Treat the sample as a dissolved metals sample. Analyze the undigested water using the
most recent CLP Low Concentration Inorganics SOW.
b. Sample Analysis:
Instruments used for the analysis of the samples should meet the contract required
detection limits in Table 1.
The ASTM Type I deionized water should be analyzed before use on the bottles that are
designated for analysis to ensure that contaminated water is not used for rinsing the
bottles.
Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
Blanks should be analyzed as described in the most recent CLP Low Concentration
Inorganics SOW. A calibration blank is a solution made up exactly like the sample
preparation solution. The calibration blank should be less than the values contained in
Table 1.
A set of standards in the expected working range should be analyzed with each analytical
run. The acid matrix of the standards, blank, and quality control samples should match
that of the samples.
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Concentrations at or above the detection limit for each parameter (listed in Table I)
should be cause for rejection of the lot of containers. NOTE: The sodium detection
limit for container types A, E, F, G, H, J, and K is 5000 ^g/L unless the containers will
be used for low concentration analyses, then the detection limit is 500 ng/L.
4. Determination of Cyanide:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
Place 250 mL of ASTM Type I deionized water in the container. Add 1.25 mL of 6N
NaOH (for container types F and G use 100 mL of ASTM Type I deionized water and
0.5 mL of 6N NaOH). Cap the container and shake vigorously for two minutes.
b. Sample Analysis:
Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
SOW.
The detection limit should be 10 /ig/L or lower.
Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
A set of standards in the expected working range, a check sample, and blank should be
prepared exactly as the sample was prepared.
The detection of 10 /jg/L cyanide (or greater) should be cause for rejection of the lot of
containers. NOTE: Contamination could be due to the container, the cap, or the
NaOH.
5. Determination of Fluoride:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
Place 250 mL of ASTM Type I deionized water in the container (for container types F
and G use 100 mL of ASTM Type I deionized water). Cap the container and shake
vigorously for two minutes.
b. Sample Analysis:
Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
SOW.
The detection limit should be 200 ^g/L or lower.
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Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
A set of standards in the expected working range, a check sample, and blank should be
prepared exactly as the sample was prepared.
The detection of 200 pg/L (or greater) of fluoride should be cause for rejection of the lot
of containers. NOTE: Contamination could be due to the container or the cap.
6. Determination of Nitrate/Nitrite:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
Place 250 mL of ASTM Type I deionized water in the container (for container types F
and G use 100 mL of ASTM Type I deionizec. water). Cap the container and shake
vigorously for two minutes.
b. Sample Analysis:
Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
SOW.
The detection limit should be 100 /zg/L or lower.
Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
Blanks should be run as described in the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
A set of standards in the expected working range, a quality control sample, and blank
should be prepared exactly as the sample was prepared.
The detection of 100 ^g/L (or greater) of nitrate/nitrite should be cause for rejection of
the lot of containers. NOTE: Contamination could be due to the container or the cap.
C. Preparation and Labeling
Sampling for environmental specimens requires that sample containers be transported to field sites
prior to sample collection. As a result, considerable time may elapse between the receipt of sample
containers and collection of the samples. Because of the large number of samples taken at any one site,
accounting for all sample containers can become extremely difficult. The following guidance on the
identification and tracking of sample containers is based on procedures that have been used successfully in
the CLP bottle program.
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1. Each shipment should be inspected to verify that the requested number of cleaned and prepared
sample containers have been supplied and meet the requirements specified in Section II (Tables 1
and 2). If any shipment fails to meet the required specifications, it should be discarded and
replaced with a supply of sample containers that meet the required criteria.
2. The sample containers should be removed and prepared in accordance with the methods
designated below.
3. A permanent nine-digit lot number should be assigned to each lot of sample containers for
identification and tracking purposes throughout the life of the containers. Figure 2 provides an
example of a lot number sequence.
FIGURE 2
LOT NUMBER SEQUENCE
95th day
of i
the year
Analysis Parameter
_Repository
Code
2 095 01
Container |
Type A
Year 1992
_Belongs to the 1st Lot
washed that day
a. The first digit represents the container type in Section II (Figure 1).
b. The second digit represents the last digit of the calendar year.
c. The next three digits represents the day of the year on which the sample containers were
washed.
d. The sixth and seventh digits represent the daily lot number.
e. The eighth digit represents the analysis parameter where:
A = Semivolatile organics, pesticides, metals, cyanide, and fluoride;
B = Metals, cyanide, and fluoride;
V = Volatile organics;
S = Semivolatile organics and/or pesticides;
M = Metals;
C = Cyanide;
F = Fluoride; and
N = Nitrate/nitrite.
f. The final digit represents the identification of the person who prepared the lot.
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4. The lot number for each container should be entered, along with the date of washing, type of
container, and number of containers per lot, into the preparation/QC log book.
5. Lot numbers printed with solvent resistant ink on a nonremovable label should remain with the
corresponding containers throughout the cleaning procedure.
6. After sample container cleaning and drying, the label should be affixed to the containers in a
permanent manner.
7. At least one face should be clearly marked, excluding the top and bottom faces, of each case of
sample containers with the assigned lot numbers.
TABLE 3
STANDARD MIXTURES OF ORGANIC COMPOUNDS TO VERIFY SENSITIVITY
Volatiles
Semivolatiles
Pesticides
Methylene Chloride
Acetone
2-Butanone
Trichloroethene
Toluene
Nitrobenzene
4-Chloroaniline
2,6-Dinitrotoluene
Diethylphthalate
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol
Di-n-butylphthalate
bis(2-Ethylhexyl)phthalate
Gamma-BHC
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
Aroclor 1260
26
*U.S. G.P.O.:1993-341-835:81056
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