vvEPA
United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
DIRECTIVE NUMBER: 9240,0-05'.
TITLE: Decentralization of Superfund Bottle
Re^pository Functions
APPROVAL DATE: SEP I 1939
EFFECTIVE DATE:
ORIGINATING OFFICE:
0 FINAL
Office of Solid Waste
D DRAFT
STATUS:
[ ] A- Pending OMB approval
{ j B- Pending AA-OSWER approval
[ ] C- For review &/or comment
[ ] D- .In development or circulating
headquarters
REFERENCE (other documents):
OSWER OSWER OSWER
/£ DIRECTIVE DIRECTIVE Di
-------
ea environmental ??-3tec:ion Agency
Wisnington. DC 20*60
OSWER Directive Initiation Request
»
OSWER 9240,0-05*
2. Originator Information
Name of Contact Person
Mike Carter
I Man Coo*
1 OS-240
I Office
I OERR/HSED/AOB
iTweonore Coce
! 382-7909
Decentralization of Superfund Bottle Re^pository Functions
4. Summary of Directive (mcuce onet statement ol purpose)
The purpose of this memo is to provide guidance for decentralization of the
acquisition of Superfund sampling bottles from OERR to the Regions and their
support contractors.
a. *«yv»oras Superfurd, CEPCTA, SARA
i«. Ooes This Oirec'jve Suotrscat Previous Oirective(S)?
b. Ooes It Supplement Previous Directived)?
No.
No
Whit flirectiv* (numeer. title)
Yes Wh«t tfr«ct>»e (numeer. We)
A - Signed by AA/DAA
B - Signed by Office Director
C - For Review & Comment
I - In OevetoQtnent
8.
Document
to
be
distributed
to
States
by Headquarters? lx 1 Y«
No
Thl« fl«cu«*t Mxu OSWgfl Directive* Syitem Format SUncUfeU.
9. Signature of Ltta Office Oirectn/es Coordinator
Betti VanEpps, OERR Publications Coordinator
10. Name and Title ol Approving Official
Henry L. Longest II, Dir., OERR
Date
I Date
EPA Form 1315-17 (Rev. 5-«7) Previous editions are oosoiete.
OSWER OSWER OSWER O
VE DIRECTIVE DIRECTIVE DIRECTIVE
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON. D.C. 20460
SEP I 193^
OFFICE OF
SOLID WASTE AND EMERGENCY RESPONSE
MEMORANDUM QBaER Directive #9240.0-05
SUBJECT: Decentralization of Superfund Bottle Repository Functions
FROM: j^ Henry L. Longest II, Dir< _
W Office of Emergency and Remedial^Response
TO: Addressees
Purpose: The purpose of this memorandum is to provide guidance for
decentralizing the acquisition of Superfund sampling bottles from
OERR to the Regions and their support contractors. This memorandum
reiterates and expands on information previously provided to the
Environmental Services Division Directors and their staffs
responsible for bottle acquisition.
Background; Superfund sampling bottles have been available to the
regions through national bottle contracts. This service was
originally provided through contracts because of a lack of
commercial availability of suitable bottles. Today, sample
containers are commercially available. Presently, each current
bottle contractor (I-Chem and Eagle Picher) markets sample bottles
prepared according to OERR specifications. These sources are
immediately available to the regions. Both organizations have also
arranged to distribute sample containers through chemical supply
companies with nationwide distribution systems. In addition, other
private companies have also expressed their intention to enter this
market. Superfund's support contractors such as REM, FIT, TAT and
ARCS are already responsible for the direct acquisition of other
supplies related to sampling and analysis and in some cases have
previously purchased bottles directly.
Objective: Decentralizing the acquisition of sample containers to
the regions will assign responsibility for program operations
consistent with EPA, OSWER and OERR policy on delegation of
operational functions to the regions ano guidance and oversight
functions to Headquarters. Further decentralization from the
regions to each of the individual support contractors will
implement OSWER policy of full contractor responsibility for the
functions necessary for successful accomplishment of the contract
mission. This contractor delegation will free up regional and
Headquarters federal resources from day-to-day operational tasks
and allow them to be used on broad quality assurance guidance and
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oversight. Regions/contractors will have increased flexibility to
respond to local variability regarding demand, supply, vendor
availability, proximity and price while maintaining the benefits of
consistent national guidance regarding specifications and quality.
Implementation: We are phasing out and discontinuing the national
bottle program which has provided Superfund sampling bottles to the
regions on a centralized basis. Based upon the regions' projected
usage rates, we estimate that the capacity remaining in the
existing contracts is sufficient to last through September, 1989.
Authorized requestors should continue to order bottles at a rate to
cover current sampling needs and not to build inventories above
those necessary for this purpose. The contract project officer
will monitor bottle demand and sample analysis projections for
consistency in the phase down. If bottle orders deviate
significantly from projections, individual delivery orders may be
monitored and approved by the project, officer, and if excessive
inventories appear to have been built, they may be reallocated. No
new national bottle contracts will be procured by OERR upon
exhaustion of the capacity in the existing contracts. For FY 90,
the current Headquarters funding level of $1.0 million annually for
these contracts will be allocated to the regions through the normal
regional SCAP planning and budget allocation process.
The responsibility for acquiring containers is delegated to
the regions and their support contractors effective with the
exhaustion of existing contract capacity, expected not later than
September 30, 1989. The regions and their contractors should
establish their own programs for obtaining needed sample bottles
prior to this date. The specific approach to be used for acquiring
sample bottles is up to the region. However, it is not my
expectation that one national bottle contract program is to be
replaced with ten regionally operated bottle contract programs, as
this would limit meeting the above stated objectives of freeing up
federal resources from day-to-day operations and of full contractor
responsibility. Nor would having one or more support contractors
in the region responsible for providing containers to all other
contractors support the full contractor responsibility policy
objective unless the individual contractors chose to subcontract
with another contractor - in fact, in this case some contractors
would be dependent upon a competitor for their performance.
Instead, I strongly encourage you to consider an approach which
fully delegates the responsibility for acquisition, storage and
assuring specifications are met to the individual responsible
support contractors as is already the case in their acquisition of
reagents and other supplies for sampling and analysis. Federal
oversight should be integrated into the region's existing quality
assurance oversight program for sampling and analysis activities.
- 2 -
-------
OERR's Analytical Operations Branch (AOB) is committed to
working with you in the transfer of responsibilities AOB has
prepared a summary of FY 88 and FY 89 bottle utilization by reciion
which is attached for your use in planning. This information
previously has been provided to the Regional Sample Control Centers
(RSCCs) and Contract Laboratory Program (CLP) Deputy Project
Officers (DPOs) in the Environmental Services Divisions. AOB has
evaluated the existing bottle preparation specifications, revised
those requirements as needed, and developed new specifications
which may be needed to accommodate lower detection limit
requirements. As a result of these efforts, a draft package of
standardized specifications was distributed on May 9, 1989, to
regional CLP DPOs for review and comment. The attached final
specification package (OSWER Directive 9240.0-05), which contains
only minor changes from the draft, can be used as a guide to
procure bottle services from a wider range of vendors.
I am requesting that you indicate what approach the region has
selected for acquiring sample bottles and what the status of its
implementation is by September 18. This response and any questions
you may have may be directed to Mike Carter of the Analytical
Operations Branch on FTS 382-7909.
Attachments
Addressees:
Director, Waste Management Division
Regions I, IV, V, VII, VIII
Director, Emergency and Remedial Response Division
Region II
Director, Hazardous Waste Management Division
Regions III, VI
Director, Toxic and Waste Management Division
Region IX
Director, Hazardous Waste Division
Region X
Director, Environmental Services Division
Regions I-X
cc: CLP Deputy Project Officers
Regional Sample Control Centers
Superfund Branch Chiefs
Frank Rzasa, CMD
Bill Topping, PCMD
Lloyd Guerci, OWPE
Susan Bromm, OWPE
Russ Wyer, HSCD
Tim Fields, ERD
Penny Hansen, SAB
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Program
Total
BOTTLE UTILIZATION
REGION I FY88
Bottles Per Program
19,364
Total
S Per Program
FIT
REM
REM II
REM III
TAT
TES IV
ESD
MASSDEQE
USFWS
588
1,008
2,208
9,528
660
272
2,820
1,980
300
1,910.04
4,033.68
5,686.56
25,236.24
1,482.84
677.96
8,452.32
5,250.60
1,272.72
54,002.96
Program
REGION I FY89
Bottles Per Program
6,842
Total
S Per Program
FIT
REM
REM II
REM III
TAT
TES IV
ESD
MASSDEQE
USFWS
ARCS
**' . .
3,354
0
0
936
1,332
96
372
0
0
752
8,352.18
0.00
0.00
3,224.04
3695.64
303.84
908.64
• o.oo
0.00
2,162.00
18,646.34
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Program
Total
BOTTLE UTILIZATION
REGION II FY88
Bottles Per Program
52,544
Total
S Per Program
ESD
FIT
REM
REM II
REM III
TAT
6,864
8,196
27,870
5,898
1,380
2,336
14,079.60
24,420.00
65,949.06
13,679.34
3,669.60
7,763.96
129,561.56
REGION II FY89
Program
Total
Bottles Per Program
26,100
Total
S Per Program
ESD
FIT
REM
REM II
REM III
TAT
636
12,174
9,870
2,880
0
540
1,542.00
29,732.46
31,563.42
9,737.16
0.00
1,993.20
74,570.24
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Program
Total
BOTTLE UTILIZATION
REGION III FY88
Bottles Per Program
55,714
Total
S Per Program
REG
CRL
FIT
REM II
REM III
TAT
8,940 :.
7,802
14,118
2,204 :
16,302 "
6,348
25,822.44
20,883.38
39,743.82
7,417.04
41,489.82
13,537.20
148,893.70
Program
Total
REGION III FY89
Bottles Per Program
39,868
Total
S Per Program
REG
CRL
FIT
REM II
REM III
TAT
2,640
15,100
7,158
3,060
9,138
2,772
6,553.56
36,187.36
19,066.26
9,066.24
28,808.46
4,349.52
104,031.40
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BOTTLE UTILIZATION
REGION IV FY88
Program
REG
ESD
FIT
REM
TAT
TES III
REM V ARCS
Total
Bottles Per Program
S Per Program
Program
REG
ESD
FIT
REM
TAT
TES III
REM V ARCS
Total
2,188
4,784
5,432
5,072
2,948
352
0
20,776 Total
REGION IV FY89
Bottles Per Program J
0
3,776
6,024
7,556
4,828
1,084
2,520
25,788 Total
6,016.24
11,721.92
15,250.16
17,513.36
10,030.88
1,382.44
0.00
61,915.00
Per Program
0.00
10,537.28
16,580.64
20,075.24
16,173.76
3,023.20
8,172.36
71,562.48
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BOTTLE UTILIZATION
REGION V FY88
Program
REG
FIT
TAT
REM
Bottles Per Program
2,616
3,792
3,068
9,812
Total
19,288
Total
S Per Program
5,514.72
8,762.40
8,335.76
22,696.28
45,309.16
REGION V FY89
Program
REG
FIT
TAT
REM
Bottles Per Program
42,266
4,968
432
3,900
Total
51,566
Total
S Per Program
108,907.76
10,646.88
1,406.64
9,399.60
130,360.88
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Program
Total
BOTTLE UTILIZATION
REGION VI FY88
Bottles Per Program
20,676
Total
S Per Program
REG
FIT
TES
TAT
REM
492
19,266
918
0
0
1,372.56
50,521.32
2,706.72
0.00
0.00
54,600.60
Program
Total
REGION VI FY89
Bottles Per Program
15,140
Total
S Per Program
REG
FIT
TES
TAT
REM
8,024
3,216
192
228
3,480
21,140.00
8,023.56
467.52
748.44
8,527.32
38,906.85
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Program
REG
FIT
TAT
ESD
REM
TES
BOTTLE UTILIZATION
REGION VII FY88
Bottles Per Program
22,868
8,712
0
0
0
0
Total
31,580
Total
S Per Program
56,932.40
24,386.88
0.00
0.00
0.00
0.00
81,319.28
REGION VII FY89
Program
REG
FIT
TAT
ESD
REM
TES
Bottles Per Program
,7,794
168
0
0
0
0
Total
7,962
Total
S Per Program
16,594.32
406.56
0.00
0.00
0.00
0.00
17,000.88
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Program
Total
BOTTLE UTILIZATION
REGION VIII FY88
Bottles Per Program
26,050
Total
S Per Program
REG
FIT
TES
REM
TAT
8,016
4,936
2,550
10,254
294
18,626.28
12,480.52
7,331.88
24,222.60
940.68
63,601.96
REGION VIII FY89
Program
Total
Bottles Per Program
14,460
Total
S Per Program
REG
FIT
TES
REM
TAT
9,672
4,788
48
0
0
24,207.72
11,701.68
87.36
0.00
0.00
35,996.76
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Program
REG
FIT
TAT
REM
Total
BOTTLE UTILIZATION
REGION IX FY88
Bottles Per Program
2,616
3,792
3,068
9.812
19,288
Total
S Per
5,514.72
8,762.40
8,335.76
22,696.28
45,309.16
REGION IX FY89
Program
REG
FIT
TAT
REM
Total
Bottles Per Program
8,652
600
0
460
9,712
Total
S Per Prnpram
20,688.36
1,603.20
0.00
1.247.56
23,539.12
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BOTTLE UTILIZATION
REGION X FY88
Program
Total
Bottles Per Program
13,880
Total
S Per Program
REG
FIT
TAT
REM
5,282
5,976
2,622
0
13,509.20
15,398.88
8,189.28
0.00
37,097.36
REGION X FY89
Program
REG
FIT
TAT
REM
Total
Bottles Per Program
7,412
0
0
0
7,412 Total
S Per Program
20,540.36
0.00
0.00
0.00
20,540.36
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OSWER DIRECTIVE #9240.0-05
SPECIFICATIONS
AND
GUIDANCE
FOR OBTAINING
CONTAMINANT-FREE SAMPLE CONTAINERS
JULY, 1989
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TABLE OF CONTENTS
SECTION TITLE PAGE
I. INTRODUCTION 1
II. SAMPLE CONTAINER
AND COMPONENT MATERIAL SPECIFICATIONS 3
III. SAMPLE CONTAINER PREPARATION
AND CLEANING PROCEDURES 13
IV. SAMPLE CONTAINER QUALITY ASSURANCE
AND QUALITY CONTROL REQUIREMENTS 15
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SECTION I
INTRODUCTION
The Environmental Protection Agency's (EPA) Office of Emergency and
Remedial Response (OERR) has undertaken the task of decentralizing Superfund's
Sample Container Repository program. Under that program, sampling containers
were prepared on a centralized basis in accordance with defined cleaning
procedures and strict quality control analysis requirements to meet the
contaminant-free specifications required for Contract Laboratory Program (CLP)
analyses.
In conjunction with the decentralization of Superfund's bottle program,
OERR has prepared "Specifications and Guidance for Obtaining Contaminant-Free
Sample Containers" to assist the Regions in obtaining sample containers from
either national or local vendors. This document provides standardized
specifications and guidance on appropriate cleaning procedures for preparing
contaminant-free sample containers that meet CLP requirements. Although the •
specifications and guidance procedures contained in this document are based on
CLP requirements, they also are suitable for use in other analytical programs.
Specific needs of EPA Regions will dictate which cleaning procedures are used
by the designated bottle preparer.
Specifications and guidance for preparing contaminant-free sample
containers are provided in the sections summarized below 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 which are as effective and efficient as the guidance provided in
Section III may be used, sample containers must meet the maximum contaminant
level specifications identified in Section II.
SECTION II
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. Most Superfund sampling and analysis
activities require all component materials (caps, liners, septa, packaging
materials, etc.) provided by the bottle preparer to meet or exceed the
criteria limits of the current CLP bottle specifications listed within this
Section.
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SECTION III
The purpose of this Section is to provide guidance on cleaning
procedures for preparing contaminant-free sample containers that meet the
specifications contained in Section II. The procedures provided in this
section meet all current CLP inorganic and organic Statement of Work (SOW)
requirements.
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.
SECTION IV
The two aspects of quality assurance (e.g., 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 this Section 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
constituents, cost, and availability.
Container types A through L (Figure 1, pages 5-6) 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 may also 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 C^iantitation Limits (CRQL) which represent the minimum detectable
quantities needed to support the hazardous substance identification and
monitoring requirements necessary for remedial and other actions at hazardous
waste sites.
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 container 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
CRDL/CRQL contributed by the container, resulted in the establishment of
• contamination limits by container type.
/ For inorganic sample containers, the CRDLs listed in Table 1, page 7,
/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.
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The CRQL specifications for organic sample containers are listed in
Table 2, pages 8-12. 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
C. GROSS CONTAMINATION
Gross contamination is defined as greater than two hundred times the
acceptable concentration values in Tables 1 and 2, 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 1
SAMPLE CONTAINER
SPECIFICATIONS
Container
Type Specifications
V Container: 80 oz. amber glass, ring handle
bottle/jug, 38 mm neck finish.
Closure: black phenolic, baked polyethylene
cap, 38-430 size; .015 mm teflon liner.
Total Weight: 2.45 Ibs.
3 Container': 40 mL glass vial, 24 mm neck
finish.
Closure: black phenolic, open-top, screw cap,
15 cm opening, 24-400 size.
Septum: 22 mm disc of .005 inch teflon
bonded to .120 inch silicon for total thickness
of .125 inch.
Total Weight: .72 oz
j Container: 1 liter high-density polyethylene,
cylinder-round bottle, 28 mm neck finish.
Closure: white polyethylene, white 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: white polypropylene cap, 48-400 size;
.015 mm teflon liner.
Total Weight: 4.41 oz.
E Container: 16 oz tall, wide mouth, straight-
sided, ;..flint glass jar, 63 mm neck finish.
Closure: black phenolic, baked polyethylene
cap, 63-400 size; 0.15 mm teflon liner.
Total Weight: 9.95 oz.
F Container: 8 oz. short, wide mouth, straight-
sided, flint glass jar, 70 mm neck finish.
Closure: black phenolic, baked polyethylene
/ cap, 58-400 size; .030 mm teflon liner.
Total Weight: 7.55 oz.
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FIGURE 1
SAMPLE CONTAINER
SPECIFICATIONS
(Continued)
Container
Type Specifications
Container: 4 oz. tall, wide mouth, straight-
sided, flint glass jar, 48 mm neck finish.
Closure: black phenolic, baked polyethylene
cap, 48-400 size; .015 mm teflon liner.
Total Weight: 4.70 oz.
Container: 1 liter amber, Boston round, glass
bottle, 33 mm pour-out neck finish.
Closure: black phenolic, baked polyethylene
cap, 33-430 size; .015 mm teflon liner.
Total Weight: 1.11 Ib.
Container: 32 oz. tall, wide mouth, straight-
sided, flint glass jar, 89 mm neck finish.
Closure: black phenolic, baked polyethylene
cap, 38-400 size; .015 mm teflon liner.
Total Weight: 1.06 Ib.
Container: 4 liter amber glass, ring handle
bottle/jug, 38 mm neck finish.
Closure: black phenolic, baked polyethylene
cap, 38-430 size; .015 mm teflon liner.
Total Weight: 2.88 Ib.
Container: 500 mL high-density polyethylene,
cylinder-round bottle, 28 mm neck finish.
Closure: white polypropylene cap, white
ribbed, 28-410 size; F217 polyethylene liner.
Total Weight: 1.20 oz.
-------
7
TABLE 1
INORGANIC ANALYTE
SPECIFICATIONS
Analyte
Contract Required
Detection Limit
(ug/L)
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
100
5
0.5
20
0.5
1
100
10
10
10
100
2
100
10
0.2
20
100
2
10
100
10
10
20
10
200
100
-------
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.
Volatlles
Acetone
Benzene
Bromochlorome thane
Bromodichlorome thane
Bromoform
Bromome thane
2-Butanone
Carbon Disulfide
Carbon Tetrachloride
Chlorobenzene
Chloroe thane
Chloroform
Chlorome thane
1 , 2 -Dibromo - 3 - chloropropane
1 , 2 -Dibromoethane
Dibromochlorome thane
1 , 2 -Dichlorobenzene
1 , 3 -Dichlorobenzene
1,4 -Dichlorobenzene
1 , 1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethene
cis-1, 2-Dichloroethene
trans -i, 2-Dichloroethene
1 , 2 -Dichloropropane
cis-1 , 3-Dichloropropene
trans- 1, 3-Dichloropropene
Ethylbenzene
2-Hexanone
Methylene Chloride
Quantitation Limits
Water
CAS Number (ue/L)
67-64-1
71-43-2
74-97-5
75-27-4
75-25-2
74-83-9
78-93-3
75-15-0
56-23-5
108-90-7
75-00-3
67-66-3
74-87-3
96-12-8
106-93-4
124-48-1
95-50-1
541-73-1
106-46-7
75-34-3
107-06-2
75-35-4
156-59-4
156-60-5
78-87-5
10061-01-5
10061-02-6
100-41-4
591-78-6
75-09-2
5
1
1
1
1
1
5
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
1
5
2
-------
TABLE 2
ORGANIC COMPOUND
SPECIFICATIONS
(Continued)
31.
32.
33.
34.
35.
36.
37.
38.
39.
40.
41.
42.
Volattles
CAS Number
4-Methyl-2-pentanone 108-10-1
Styrene 100-42-5
1,1,2,2-Tetrachloroethane 79-34-5
Tetrachloroethene 127-18-4
Toluene
1,1,1-Trichloroethane
1 , 1 , 2-Trichloroethane
Trichloroethene
Vinyl Acetate
Vinyl Chloride
o/p-Xylenes
m-Xylene
108-88-3
71-55-6
79-00-5
79-01-6
108-05-4
75-01-4
95-47-6/106-42-3
108-38-3
Quantitation Limits
Water
(ug/L)
5
1
1
1
1
1
1
1
1
1
1
1
-------
10
TABLE 2
ORGANIC COMPOUND
SPECIFICATIONS
(Continued)
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
Acenaphthene
Acenaphthylene
Anthracene
Benz [ a ] anthrac ene
Benzo [ a ] pyrene
Benzo [b ] f luoranthene
Benzo [ k ] fluoranthene
Benzo [ g , h , i ] perylene
Benzole acid
Benzyl alcohol
4-Bromophenyl-phenylether
Butylbenzylphthalate
Di-n-butylphthalate
4-Chloroaniline
4-Chloro-3-methylphenol
bis - ( 2 -Chloroethoxy)me thane
bis-(2-Chlorethyl)ether
2 , 2-oxybis - (1-Chloropropane)
2-Chloronaphthalene
2-Chlorophenol
4-Chlorophenyl-phenylether
Chyrsene
Dibenrf a, h] anthracene
Dibenzbfuran
1,4-Dichlorobenzene
3,3' -Dichlorobenzidine
2 , 4-Dichlorophenol
Diethylphthalate
2,4-Dimethylphenol
Dime thy Iphthalate
Ouantitation Limits
Water
CAS Number Cue/L}
83-32-9
208-96-8
120-12-7
56-55-3
50-32-8
205-99-2
207-08-9
191-24-2
65-85-0
100-51-6
101-55-3
85-68-7
84-74-2
106-47-8
59-50-7
111-91-1
111-44-4
108-60-1
91-58-7
95-57-8
7005-72-3
218-01-9
53-70-3
132-64-9
106-46-7
91-94-1
120-83-2
84-66-2
105-67-9
131-11-3
5
5
5
5
5
5
5
5
20
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
-------
11
TABLE 2
ORGANIC COMPOUND
SPECIFICATIONS
(Continued)
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.
J60.
61.
62.
63.
\
Semivolatiles
4 , 6 -Dinitro - 2 -methylphenol
2,4-Dinitrophenol
2 , 4-Dinitrotoluene
2 , 6 - D ini tr o to luene
bis - ( 2 - Ethylhexyl) phthalate
Fluor an thene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachlorocyclopentadiene
Hexachloroe thane
Indeno (1,2,3- cd) pyrene
Isophorone
2-Methylnaphthalene
2 -Methylphenol
4 -Methylphenol
Naphthalene
2-Nitroaniline
3-Nitroaniline
4-Nitroaniline
Nitrobenzene
2-Nitrophenol
4-Nitrophenol
N-Nitrosodiphenylamine
N-Nitrqso-di-n-dipropylamine
Di-n-octylphthalate
Pentachlorophenol
Phenanthrene
Phenol
Pyrene
1 , 2 , 4-Trichlorobenzene
2,4, 5 -Trichlorophenol
2 ,4 , 6-Trichlorophenol
Quantitation Limits
Water
CAS Number (ue/L>
534-52-1
51-28-5
121-14-2
606-20-2
117-81-7
206-44-0
86-73-7
118-74-1
87-68-3
77-47-4
67-72-1
193-39-5
78-59-1
91-57-6
95-48-7
106-44-5
91-20-3
88-74-4
99-09-2
100-01-6
98-95-3
88-75-5
100-02-7
86-30-6
621-64-7
117-84-0
87-86-5
85-01-8
108-95-2
129-00-0
120-82-1
95-95-4
88-06-2
20
20
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
20
20
20
5
5
20
5
5
5
20
5
5
5
5
20
5
-------
TABLE 2
ORGANIC
SPECIFICATIONS
(Contirr^d)
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.
Pesticides/PCBs
Aldrin
Alpha -BHC
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
Beta-BHC
alpha- Chlordane
gamma -Chlordane
Delta-BHC
Dieldrin
4, 4' -ODD
4, 4' -DDE
4,4'-DDT
Endosulfan sulfate
Endosulfan I
Endosulfan II
Endrin
Endrin ketone
Ganona-BHC (Lindane)
Heptachlor
Heptachlor epoxide
Methoxychlor
Toxaphene
CAS Numhpr
209-00-2
219-84-6
12574-11-2
11104-28-2
11141-16-5
524,69-21-9
12572-29-6
11097-69-1
11095-82-5
219-85-7
5103-71-9
5103-74-2
219-86-8
60-57-1
72-54-8
72-55-9
50-29-3
1031-07-8
559-98-8
32213-65-9
72-20-8
52494-70-5
58-89-9
76-44-8
1024-57-3
72-43-5
£001-35-2
r..«~ri cation limits
Water
.025
.025
.25
.25
.25
.25
.25
.5
.5
.025
.025
.025
.025
.05
.05
.05
.05
.05
.025
.05
.05
.05
.025
.025
.025
.25
.5
-------
13
SECTION III
SAMPLE CONTAINER PREPARATION AND CLEANING PROCEDURE
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 identical to those specified for the Superfund Sample Container
Repository program.
A. Cleaning Procedure
1. Cleaning Procedure for Container Types: A, E, F, G, H, J, K
Sample Type: Extractable Organics (Types A, E, F, G, H, J and K); and
Metals (Types E, F, G, and J) 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 tap water to remove detergent.
c. Rinse with 1:1 nitric acid (reagent grade HN03, 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 hexane or pesticide grade
methylene chloride using 20 mL for 1/2 gallon container; 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 Lot number, and pack in case.
/
/ 1. Label exterior of each case with Lot number.
/
m. Score in contaminant-free area.
-------
14
2. Cleaning Procedure for Container Types: B, D
Sample Type: Purgeable (Volatile) Organics.
a. Wash glass vials, teflon-backed septa, teflon liners, and caps in
hot water using laboratory grade nonphosphate detergent.
b. Rinse three times with tap water.
c. Rinse three times with ASTM Type I organic-free water.
d. Oven dry vials, caps, septa, and liners at 105°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 Lot number, and pack in case.
i. Label exterior of each case with Lot number.
j. Store in contaminant-free area.
3. Cleaning Procedure for Container Types: C, L
Sample Type: Metals, Cyanide, and Sulfide.
a. Wash polyethylene bottles and caps in hot tap water using
laboratory-grade nonphosphate detergent.
b. Rinse three times with tap water.
c. Rinse with 1:1 nitric acid (reagent grade HN03, diluted with ASTM
Type I deionized water).
d. Rinse three times with ASTM Type I deionized water.
e. Invert and air dry in contaminant-free environment.
f. Cap bottles.
g. Label each container with Lot number, and pack in case.
/
/ h. Label exterior of each case with Lot number.
i. Store in contaminant-free area.
-------
15
SECTION IV
SAMPLE CONTAINER QUALITY ASSURANCE AND QUALITY CONTROL PROCEDURE
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.
Major QA/QC activities should include the inspection of all incoming
materials, QC analysis of cleaned Lots of containers, and monitoring of the
containers' 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 (i.e., preparation/QC logs,
analytical data, data tapes, storage log) should also be stored in a central
location within the facility.
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 in which cases should
be identified by material type, purchase order number, and delivery date
should be maintained. The date of incoming inspection and acceptance or
rejection of the material should be recorded on this log.
2. Quality Control Inspection of Cleaned Lots of Containers:
Following container cleaning and labeling, two containers should be
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 QC container per Lot 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 extractable and volatile organics,
pesticides, metals, and cyanide should be utilized.
For each representative Analysis QC Container(s), the appropriate QC
/' number should be assigned to the related Lot of containers. For
/ example, the QC number could be a six-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
-------
16
sequentially in numerical order starting with "0001" for the first Lot
to undergo QC analyses, 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.
A laboratory standard and a blank should be run with each QC analysis.
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. The date the container is placed in the storage
area should be recorded in the storage QC container log.
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) periodically. Analysis of the
Storage QC Container should be performed if contamination of the
particular container Lot comes into question at any time following
shipment. Upon removal, containers should be logged out of the storage
area. .-"-
The designated storage area should be monitored continuously for
volatile contaminants. 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 the monthly report.
-------
17
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:
• Extractable organics and pesticides;
• Volatile organics;
• Metals; and
• Cyanide.
QC analyses should be performed according to the container type and
related sample type and utilize the specific method(s) described below.
1. Determination of Extractable 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.
- Add 50 mL of pesticide-grade hexane 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 1 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 13) directly to a KD
."•' apparatus, and proceed as above.
b. Extractable Organics Sample Analysis:
Instrument calibration should be performed as described in the
current CLP organics SOW with the following exceptions:
y
/ (1) Semivolatile internal standards should be added at 20
ng/uL instead of 40 ng/uL.
-------
18
(2) 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.
(3) The low concentration (20) standard should be used for the
continuing calibration standard for semivolatile analyses.
(4) The percent difference window should be widened to ± 30%.
Inject 3 uL of solvent into a gas chromatograph/mass spectro-
meter (GC/MS).
GC/MS operating conditions are listed in Figure 3.
- Any peaks found in the container solvent that are not found in
the solvent blank or with peak heights or areas not within
+ 50% of the blank peak height or area should be cause for
rejection. \
Identify and quantitate any contaminant(s) that cause
rejection of a container Lot.
- A standard mixture of the 10 semivolatile organic compounds
listed in Table 2 with concentrations in the 20-50 ppb range
should be analyzed to ensure that the required sensitivities
are achieved.
A blank should be run with each analysis.
c. Pesticides Sample Analysis:
Instrument calibration should be performed as described in the
current CLP Organics SOW.
Inject 1 uL of solvent into a gas chromatograph (GC) equipped
with an electron capture detector (ECD).
,-- GC/ECD operating conditions are listed in Figure 4.
Any peaks found in the container solvent that are not found in
the solvent blank or with peak heights or areas not within
+ 50% of the blank peak height or area should be cause for
rejection.
- A standard mixture of the 5 pesticide organic compounds listed
in Table 2 with concentrations in the 0.10 to 1 ppb range
should be analyzed to ensure that the required sensitivities
are achieved.
A blank should be run with each analysis.
-------
19
2. Determination of Volatile Organics:
Container Types: B and D
a. Sample Preparation:
Fill the container with ASTM Type I organic-free water.
Instrument calibration should be performed as described in the
current CLP Organics SOW with the following exceptions:
(1) Volatile internal standards should be added at 25 ng/mL
instead of 50 ng/mL.
(2) 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.
\
(3) The low concentration (20) standard should be used for the
continuing calibration standard for volatile analyses.
(4) The percent difference window should be widened to + 30%.
b. Sample Analysis:
- Analyze for volatile organics by EPA Method 624 using GC/MS
with the operating conditions specified in Figure 5.
Any peaks not found in the blank or with peak heights or areas
not within + 50% of the blank peak height or area should be
cause for rejection.
Identify and quantitate any contaminant(s) that cause
rejection of a container Lot.
- A standard mixture of the 5 volatile organic compounds
listed in Table 2 with concentrations in the 20-50 ppb range -
should be analyzed to ensure that the required sensitivities
are achieved.
A blank should be run with each analysis.
3. Determination of Metals:
Container Types: C, E, F, G, J, and L
/
' a. Sample Preparation:
- Add 50 mL of ASTM Type I deionized water to the container, and
acidify with 0.5 mL reagent-grade HN03. Cap and shake well.
-------
20
- Treat the sample as a dissolved metals sample. Analyze the
undigested water using the most current CLP Inorganic SOW.
The detection limits should not exceed the detection limits
shown in Table 1.
b. Sample Analysis:
Instruments used for the analysis of the samples should meet
the contract required detection limits in Table 1.
The rinse solution should be analyzed before use on the
bottles that are designated for analysis to ensure that a
contaminated solution is not used for rinsing the bottles.
Calibration verification standards should be analyzed at the
beginning, end, and every ten samples within an analysis run
(a continuous analytical sequence consisting of prepared
samples and all associated quality assurance measurements).
The verification standards should be three to five times the
values in Table 1. The percent recovery factor for the v
verification standards should be between 90 to 110 % or ± 10%
of the actual value of the verification standard.
Calibration blanks should be analyzed at the beginning, end,
and every ten samples within an analysis run. A calibration
blank is a solution made up exactly like the sample
preparation solution. The calibration blank should be below
the values 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.
Concentrations at or above the detection limit for each
parameter (listed in Table 1) should be cause for rejection of
the Lot of containers. Note: Sodium detection limit for
container types E, F, G, and J is 5000 ug/L.
4. Determination of Cyanide:
Container Types: C and L
a. Sample Preparation:
- Cyanide should be determined by EPA Method 335.1, 335.2, or
335.3 by placing 250 mL of ASTM Type I deionized water in the
container. Add 1.25 mL of 6N NaOH. Cap the container, and
shake vigorously for two minutes.
-------
21
b. Sample Analysis:
- Analyze an aliquot by the EPA method selected. The detection
limit should be 10 ppb or lower.
- A blank should be run by analyzing 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.
The detection of contaminants of 10 ppb cyanide should be
cause for rejection of the Lot of containers. (Note:
Contamination could be due to the container, the cap, or the
NaOH).
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.
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:
a. Allocate the appropriate number of sample containers (Figure 1) to
a designed container Lot.
b. Recommended Lot size for each container should be based on the
recommended number of items per case.
3. A permanent eight-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.
/
a. The first digit represents the container type in Section II
(Figure 1).
-------
22
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 digit represents the daily Lot number.
e. The final digit represents the identification of the person who
prepared the Lot.
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.
Figure 2
95th day of
the year
Container
Type A
\
\
\
\
\
A 9 095 01 _
\
\
\
Repository Code
Belongs to the 1st Lot
washed that day.
Year 1989
Lot Number Sequence
-------
23
Figure 3
GC/MS Operating Conditions for Extractable Organics QC Analysis
OPERATOR:
JOB NUMBER:
SOLVENT: Hexane
DATE:
SAMPLE
IDENTIFICATION: Container Lot number
ANALYTICAL
METHOD: 605. 44 FR 69464.
Extractable Oreanics Fraction
COLUMN
Type Glass
Length 6'
Diameter 2 mm ID
Liquid Phase (% wt)
3% SP 2250
Support Supelcoport
Mesh 100/120
CARRIER GAS Helium
Rotameter 60
Inlet Pressure, psig 1.5
Flow Rate, mL/min 30
SCAVENGER GAS
SPLIT
FID GLASS
Hydrogen, mL/min
Air, mL/min
CHART SPEED, cm/min
DETECTOR Mass Spectrometer
Range 50-350 a.m.u.
Attenuation
TEMPERATURE, °C
Detector
Injection Port 225
Column
Initial 70°/3 min
Program 10°/min
Final 270°C
INSTRUMENT
-------
OPERATOR:
JOB NUMBER:
24
Figure 4
GC/ECD Operating Conditions for Pesticides QC Analysis
DATE:
SOLVENT: Hexane
SAMPLE
IDENTIFICATION: Container Lot number
ANALYTICAL
METHOD: 608. 44 FR 69464.
Pesticide Fraction
COLUMN
Type Glass
Length 6'
Diameter 4 mm ID
Liquid Phase (% wt)
1.5% SP2250/I.95% SP2401
Support Supelcoport
Mesh 100/120
CARRIER GAS Nitrogen
Rotameter
Inlet Pressure, psig
Flow Rate, mL/min 30
SCAVENGER GAS
SPLIT
FID GLASS
Hydrogen, mL/min
Air, mL/min
CHART SPEED, cm/min 1 cm/min
DETECTOR Electron Capture
Range IP'12
Attenuation 16
TEMPERATURE, °C
Detector 350
Injection Port 250
Column
Initial 200 isothermal
Program
Final '
INSTRUMENT
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OPERATOR:
JOB NUMBER:
25
Figure 5
GC/MS Operating Conditions for Volatiles QC Analysis
DATE:
SOLVENT: Hexane
SAMPLE
IDENTIFICATION: Container Lot number
ANALYTICAL
METHOD: 625. 44 FR 69464.
Volatile Organics Fraction
COLUMN
Type Stainless Steel
Length 8'
Diameter 2 ""i ID
Liquid Phase (% wt) .•
1% SP 1000
Support Chromosorb W
Mesh 60/80
CARRIER GAS Helium
Rotameter 60
Inlet Pressure, psig 15
Flow Rate, mL/min 30
SCAVENGER GAS
SPLIT
FID- GLASS
Hydrogen, mL/min
Air, mL/min
CHART SPEED, cm/min
DETECTOR Mass Spectrometer
Range 40-300 a.m.u.
Attenuation
TEMPERATURE, °C
Detector
Injection Port 150
Column
Initial 70°/3 min
Program 10°/min
Final 220°C
INSTRUMENT
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