905-R-83-115
SAMPLE HANDLING PROTOCOL FOR HAZARDOUS WASTE
REM/FIT CONTRACT
U.S. ENVIRONMENTAL PROTECTION AfiENCY
REGION V
ENVIRONMENTAL SERVICES DIVISION
536 SOUTH CLARK STREET
CHICAGO, ILLINOIS 60605
MAY 3, 19R3
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION V
GATE MAY Og 1983 905R83115
JBJECT Sample Handling Protocol for Hazardous Waste, REty/rii contract
FROM: William H. Sanders III, Director
Environmental Services Division
T0: Richard BarteU, Chief and Michael Harris and Joseph Petrilli, FIT
Remedial Response Branch CH2W1LL, Incorporated Ecology & Environmen
Attached is a copy of the Region V Environmental Services Division
"Sampling Handling Protocol for Hazardous Waste REM/FIT Contract".
When it is known that samples will be shipped to a National Contract
Laboratory for analysis, this protocol must be followed in total by
all authorized samplers.
While this protocol is applicable for the analysis of water, oils
and solid wastes, the same procedure must be used for air analysis
requests. These requests will be processed under special analytical
services (see page 2 of protocol).
For additional information, please contact Charles E.lly, Sample Analyses
Coordinator, at the Central Regional Laboratory at 353-R370.
William H. Sanders III
Attachment(s)
cc: Sanders
Yeates
Dikinas
Ross
Adams
Constantelos
Vanderlaan
Diefenbach
Getty, FIT
EPA FORM 132M .SEV3-76)
-------
REM/FIT PROTOCOL
The following procedures shall apply with regard to data review and
sample handli ng.
I. CASE SET-UP AND LOGISTICS OF SAMPLE HANOIING
A. Cl^MHILL will set-up its own cases to secure National Contract
Laboratories (NCL's) by telephoning the EPA, Sanpling Management Office
(SMO) in Alexandria, Virginia (702-557-24%, Ms. Eileen O'Connor). For
high hazard samples which require inorganic analysis, D^MHILL will have
to first contact Ms. O'Connor, followed by a written request from the
EPA Regional Counsel or the ESft Director (copy to SMO X Regional Lab)
to Or. Theodore Meiggs, Assistant Laboratory Director, EPA, National
Enforcement Investigations Center (NEIC)(303-234-4661).
R. CH-jMHILL will provide Mr. Charles Elly, EPA, Region V, Environ-
mental Services Division, Central Regional Laboratory (CRL) with copies
of the case number, NCL and yellow copy of the chain-of-custody form
for each study. This should occur not more than two (2) days after
samples have been shipped to the NCL. If sampling will occur frequently,
than reports should be submitted to Mr. Elly on a weekly basis.
C. Charles Elly or other CRL personnel will prepare all Special
Analytical Services requests (SAS's), secure NCL's and case numbers for
the SAS's and send the information to CH?MHILL and to Paul Friedman
of the SMO. Dr. Friedman will review all SAS data. Following are
examples of when SAS's will he required.
1. Priority Pollutant Organic and Metals Analysis of Oils
are requested.
2. EP Toxicity, Flashpoint and other RCRCA Solid Waste
parameters are requested.
3. Dioxins are requested by the Region VII or High Resolution
Method.
4. Parameters other than the 114 Priority Pollutant Organics
or the Task 1 and 2 Metals or Task 3 Inorganics are requested.
5. Lower detection limits than those in the regular IFB's
are requested. Other quality control which is more extensive than the
IFB calls for.
6. Quicker turnaround times than the normal 30 to 40 days are
requested.
7. Other requests not covered above.
-------
D. Packaging and Shipping
CH2MHILL shall use as a guide the Region V "Sampling Handling
Protocol for Hazardous Waste", May 27, 1982 and the "Users Guide to
the EPA Contract. Laboratory Program", August 1Q82 (Attached).
II. DATA REVIEW
One copy of the data initially will he sent by the National Contract
Laboratory to the SMO (Paul Friedran) and one copy will be sent to the
CRL.
A. Dr. Paul Friedman will review all of the data.
B. Ms. Marcia Kuehl, CRL Duality Control Coordinator wil 1 establish
formal procedures for insuring that Or. Friedman is reviewing data
correctly. (This protocol will be formally tracked, since this is a
pilot study).
C. Paul Friedman will forward his findings to the CRL. The CRL
Coordinator will forward Dr. Friednan's findings (following verification)
and all of the raw data to CHgHMILL.
III. TRAINING
Charles Elly and Kathy Getty or Cindy Bachunas of FIT will provide
a one-day training session concerning implpmentation of the National
Contract Laboratory Program.
IV. RESOLUTION OF PROBLEMS
All problems involving samples should be referred by SMO to CHpMHRL,
and all problems regarding data should he referred to Or. Paul Friedman.
All correspondence on these issues should be copied to Charles Elly and/or
Marcia Kuehl.
Attachments
-------
REGIONV
UMITED STATES ENVIRONMENTAL PROTECTION AGEHCY
0 3 1982
SUBJECT: Revised Sample Handling Protocol for Hazardous Waste
William H. Sanders III, Director
Environmental Services Division
TO! Gerald Regan, CDO
A.R. Winklhofer. EDO
Joseph Petrilli, FIT
Scott McCone, TAT
Attached is a newly revised copy of the Region V Environmental Services
Division "Sample Handling Protocol for Hazardous Waste". When it is known
that samples will be shipped to a National Contract Laboratory for analysis,
this protocol must be followed in toto by all authorized samplers.
While this protocol is applicable for the analysis of water, oils and solid
wastes, the same procedure must be used for air analysis requests. These
requests will be processed under special analytical services (see Attach-
ment #2 of protocol).
For additional information, please contact Charles Elly, Sample Analyses Co
ordinator, at the Central Regional Laboratory at 353-8370.
Attachment (s)
cc: Sanders
Yeates
Wagner
Ross
Adams
Constantelos
Bartelt
Vanderlaan
Diefenbach
Klepitsch
Kee
Schaffer
'•Sutfin
Bryson
K»A ro*M
mev.
-------
SAMPLE HANDLING PROTOCOL
FOR HAZARDOUS WASTE
U.S. ENVIRONMENTAL PROTECTION AGENCY
REGION V
ENVIRONMENTAL SERVICES DIVISION
536 South Clark Street
Chicago, Illinois 60605
May 27, 1982
-------
SAMPLE HANDLING PROTOCOL FOR HAZARDOUS WASTE
*• OPERATIONAL PROCEDURES
A. Data Requests
For samples to be analyzed by the Central Regional Laboratory
(CRL) or by a contract laboratory, all requests should be initiated by
submittal of the ESD's Form-81-01 "Request for Analysis" (see Attach-
ment 11). This form should be submitted, at least two weeks prior to
the survey, to William H. Sanders 111, Director, ESD, for Priority tl
surveys and to Curtis Ross, Director, CRL, for all other requests.
The following Is a listing of priority types:
PRIORITY II - Highest priority work; immediate response or Initiation
of the project by CRL is necessary; or other work already
in progress may be curtailed*
PRIORITY 12 - High priority projects to be scheduled and completed as
soon as possible without disrupting other work already in
progress.
PRIORITY. 13 - Projects to be completed around Priority fl and #2 pro-
jects, but with some definite completion date, usually,
at least two or three months from request date*
PRIORITY IA - Projects that may be completed if time is available. No
requested due date.
Samples will be analyzed either at the CRL or by a National Con-
tract Laboratory (NCL) administered by the V1AR & Company, Incorporated,
EPA Hazardous Waste Investigations, Sample Management Office (SMO),
hereafter referred to as "SMO". The decision of whether the samples
will be analyzed at the CRL or by a contractor laboratory will depend
-------
-2-
on the priority, parameter, and sample type, or other factors. Most
Priority II samples will be analyzed at the CRL. (The Division Direct-
or and the CRL Director make the determination*)
With regard to samples sent to a National Contract Laboratory,
Charles Elly is the EPA Region V SMO Coordinator. Elly will determine
Whether samples will be sent to a NCL or to the CRL to be analyzed.
All prospective Samplers (FIT excluded - FIT and TAT have designated
SMO Coordinators) must contact Elly. Elly also arranges for all analy-
ses to be done under Special Analytical Services (SAS - see Attachment
f2), as well as distribute SMO Traffic forms. Curtis Ross determines
the disposition of "Toxics" or other types of samples.
Charles Elly resolves questions as to whether to analyze samples
which were not collected according to the SMO protocol, inclusive of
FIT collected samples.
When completing the ESD Sample Request form, as much information
as possible should be provided about the site. This will help to
assure the safety of laboratory personnel handling the samples and will
assist in the proper selection of analytical methods.
Contractor Pefinitions
Generally, samples are divided Into three categories: low, medium,
or high hazard.
Low hazard samples are normally be groundwater, leachate, or sur-
face water. (Concentration ranges from 0 to 10mg/l (10 ppm)) of con-
stituents.
Medium hazard samples are up to 152 (150,000 ppm) of a single
hazardous constituent. They are, for example, samples of materials
lying along side of a drum. The lower range for medium hazard samples
is 10mg/l (10 ppm)*
-------
-3-
High hazard samples are samples of hazardous waste materials, gen-
erally* the contents of drums. (Concentration ranges from 15Z to 100Z.)
These samples are usually sent to the National Enforcement Investiga-
tions Center, Regulated Substances Laboratory in Denver, Colorado, for
dilution and extraction, and then sent to a NCL, the NEIC or the CRL
for analysis. Following are the turnaround times which NCL's are
required to provide:
- Low Hazard Samples: waters; organic and inorganic analyses:
AO calendar days.
- Low and Medium Soil and Sediments: Organic and Inorganic analy-
ses : 30 calendar days.
. Medium waters: 30 calendar days.
- High Concentration Samples: 21 calendar days at the NEIC and
30 calendar days at a MCL
(The total number of calendar days is equivalent to 51 calendar days.)
- SAS: No set limitations (see Attachment fl).
B. LOW HAZARD SAMPLES (Water, Soil, Sediment)
Bottles, Preservation, Holding Times, Forms,
Quality Control, Custody and Shipping Procedures
Each low hazard sample collection by either FIT, TAT, or EPA
personnel shall consist of the following:
1. ORGANICS: Water
• 1-one gallon glass bottle (teflon-lined caps) or 2-half gallon
glass bottles; iced to 4*C. MAXIMUM HOLDING TIME: 2 days until
extraction*
. - 2-40ml glass Volatile Organic Analysis (VOA) vials (duplicates);
iced to 4*C (teflon-lined caps). MAXIMUM HOLDING TIME; 7 days.
Soils and/or Sediments
- 1-8 ounce glass wide-mouthed bottle (teflon-lined caps) iced to
4*C (filled no more than three-fourths full with sample)*
-------
-4-
2. INORGANICS; Water
- 1-one liter high density polyethylene bottle (metals, 3ml 1:1 HN03
preservative).* MAXIMUM HOLDING TIME; 6 nonths.
- l-360ml high density polyethylene bottle (Mercury, 3ml 1:1 HN03 pre-
servative). MAXIMUM HOLDING TIME; 14 days
- l-360ml high density polyethylene bottle (Mercury, 2ml of HNC>3-»*.2Cr207
preservative). MAXIMUM HOLDING TIME; 28 days.
- l-500ml high density polyethylene bottle (NHj+TOC, 2ml 1:1, ^SO^
preservative, 4*C). MAXIMUM HOLDING TIME; 28 days
- l-500ml high density polyethylene bottle (pH+F~, General Chen., no
preservative, 4*C). MAXIMUM HOLDING TIME; 48 hours.
- 1-one liter high density polyethylene bottle (CN~, 5ml 6N NaOH
preservative, 4'C). MAXIMUM HOLDING TIME: 14 days.
- 1-one liter high density polyethylene bottle (S~, 8ml, Zinc acetate
preservative, 4*C). MAXIMUM HOLDING TIME: 7 days.
- 1-one quart glass wide-mouthed bottle (Oil/Grease, 10ml 1:1 ^SO^
preservative). MAXIMUM HOLDING TIME; 28 days.
- 1-one liter high density polyethylene bottle (Phenols, 10ml CuS04-
preservative, iced to 4*C). MAXIMUM HOLDING TIME; 48 hours.
INORGANICS; Soils and/or Sediments
- 1-8 ounce plastic wide-mouthed bottle (iced to 4°C). (Filled no more
than three-fourths full with sample).
*NOTE: The pH of the sample should be checked in the laboratory, upon
receipt of sample. If the pH is over 2, more HN03 should be
added to bring it to 2 or below.
All low hazard samples should be preserved before arrival at the
CRL (or a NCL), according to procedures listed above, Which are consis-
tent with those on pages VI-4 thru VI-6 of the Draft NEIC Manual (en-
titled "Enforcement Considerations-for Evaluations of Uncontrolled
Hazardous Waste Disposal by Contractor's" Manual, National Enforcement
•• Investigations Center (NEIC), Denver, Colorado; April, 1980. The
.amounts of preservatives recommended are consistent with DOT regula-
tions, therefore, the samples can be shipped via Air Freight.
-------
-5-
Field Quality Control
For low hazard water camples, a reagent blank IB required for each
type or group of parameters (especially those Which require preserva-
tion)* In all cases, the bottles must be the same as the sample bottles
and must be filled with distilled-delonited or carbon-free water and
the preservative, if any. This "field" blank should be taken to the
site where the real samples are collected and handled under the same
conditions as the samples.
For low hazard water and soil/sediment samples, a "field" dupli-
cate is required for every ten samples collected.
The requirements for a field blank(s) and duplicate(s) is an EPA
national quality assurance mandate and is fully implemented in Region
V. The purpose is to detect laboratory and/or field contamination and
variation.
As a minimum, there should always be at least one field reagent
blank and duplicate per survey. Ideally, one blank and duplicate per
ten samples should be collected where practical. If only one or two
samples are collected and are critical, the Sampler should use judgment
regarding collection of the blank and duplicate.
Chain of Custody Procedures
EPA Region V and FIT/TAT personnel must use the Region V "Chain-
of-Custody Record" (from the EPA's Office of Enforcement) and Custody
Tags. All samples to be tracked by CRL personnel must contain CKL
sample numbers.
Attached is a memo from Robert Laidlaw, NE1C (Attachment 13), to
.•Thomas Yeates, Region V DPO, which excellently highlights the chain-of-
custody and should be used as a reference. Please note the requirement
of a separate custody record for samples shipped to different labora-
tories and a separate custody sheet for each sampling site. Do not
-------
-6-
put more than one survey on the same custody sheet (example: Breiten-
•tine, Bershberger and Lake County Landfill surveys were all put on
the same custody sheet). Each site of a facility should be listed
separately.
Low hazard samples »ay be brought into the CRL; however, samples
•ay also be shipped from the field, providing the following protocol is
strictly adhered to - all samples which will be sent to a NCL should be
accompanied by:
The SMO Organics Traffic Report
The SMO Inorganics Traffic Report
rlmiauuy Cample Number •
Jt. The Region V BSD Chain-of-Custody Form(s)
>. The Region V BSD Custody Tag(s)
>. The Region V BSD Custody Seal
F. Stick-On Label removed from the Traffic Report
__J The-*egluu V BSD Bablc DaLa Fuim (for samples \
*Required of TAT, Regional EPA and FIT personnel.
All samples (organic and inorganic) are to be shipped via Federal
Express, Purolator, or Emery.
W Charles Elly (or his designated alternative) should be notified
prior to shipment of the samples. Elly will contact the Sample Manage-
__
ment Office (SMO) for EPA and/or TAT, obtain a case number, and the NCL
to which the samples will be sent. Under no circumstances is the Sam-
pier to call the SMO or the NCL. This protocol must be adhered to by
EPA and TAT personnel. FIT personnel make its own shipping arrange-
ments with the SMO.
Packaging and Shipping
' Before shipment, the Sampler must provide the following: (FIT is
<. -exempted)
1. Check to make certain the stick-on label(s) from the Organic and/or
Inorganic Traffic Report form(s) is sticking to the bottle(s), along
-------
-7-
vith the Custody Tag(s) and that the Custody Tag(s) coincide with
the CRL Sample Number(s) written on the Traffic Report sheets.
Complete all of the information on the Organic and/or Inorganic
Traffic Report(s). The top (SMO copy) and pink (Regional copy) of
the Organic and/or Inorganic Traffic Report(s) should be sent to
Charles Elly no later than two (2) work days after sampling.
NOTE: The Air-Freight Bill Number and Carrier Company has to be called
in to Charles Elly the same day of shipment (before 4;00 PM, CDT).
The Sampler will have to make a copy if he/she desires one; all
other sheets must be enclosed with the samples.
3. Place the original Chain-of-Custody Form sheet(s) in a plastic,
water-proof envelope and enclose it with the samples. Send the
yellow copy of the Custody Sheet to Charles Elly. The Field Samp-
ler keeps the pink copy. Also, send Charles Elly a partially com-
pleted CRL Priority sheet (ESD and TAT personnel only) with Items
12, 13, 16, 18, 19, and 110 completed. Indicate under the "Remarks"
Section the assigned CRL Sampie(s) Number and where the samples
were sent.
The same protocol is to be followed for samples brought (self-
delivered) to the CRL for shipment. The partially completed Priority
sheet should be given to Charles Elly to fill in the appropriate CRL
Data Set Number(s), Sample Number(s), Case Number(s), and the location
of where the samples will be shipped.
C. MEDIUM CONCENTRATION SAMPLES (Water, Soil. Sediment)
Bottles, Preservation, Holding Times,
Forms, Custody and Shipping Procedures
The following requirements apply for:
ORGANICS
I
1-8 ouncewide-mouthed , round, clear glass Jar with screw-neck
finish and teflon-lined cap (KERR AC802 brand or equivalent;
available from VWR Scientific - Catalog No. #1694-063); filled
one-half to three-fourths full with the sample. No ice or preserv
ative. MAXIMUM HOLDING TIME; Not established yet.
-------
-8-
INORGANICS* -> 5 O
S
1-8 ounce wide-mouthed, round, clear plastic or glass jar with
•crew-neck finish and teflon-lined cap; filled one-half to three-
fourths with the sample. No Ice or preservative* MAXIMUM HOLDING
TIME: Not established yet.
*A separate sample must be collected for organic and inorganic, since
the samples will be sent to two different laboratories.
Field Quality Control
For medium hazard water or liquid samples, a reagent blank is re-
commended for each type or group of parameters, for example, one blank
for organics, one blank for sulfides, etc. The bottle should be the
same type as the sample bottles and must be filled one-half to three-
fourths full with diatilled-deionlzed or carbon-free water. This
"field" blank should be taken to the site where the real samples are
collected and handled under the same conditions as the samples.
For medium water and soil/sediment samples, a "field" duplicate is
required for every ten samples collected.
The requirement for a field blank(s) and dupllcate(s) is an EPA
quality assurance mandate and is fully implemented in Region V. The
purpose is to detect laboratory and/or field contamination and varia-
tion.
As a minimum, there should always be at least one field reagent
blank and duplicate per survey. Ideally, one blank and duplicate per
ten samples should be collected where practical. If only one or two
samples are collected, the Sampler should use judgment regarding collec-
tion of the blank and duplicate.
Chain-of-Custody Procedures
•• t , • - "
The same procedures as outlined for low hazard samples (see page
"5" of this protocol) should be used.
-------
-9-
Shipplng
All medium samples ( organic s and Inorganics) are to be chipped via
Federal Express, Purolator, or Emery Air Freight*
Guidelines for shipment of medium concentration hazardous waste
samples are contained in the Draft NE1C Manual, 1980. Sampling should
be carried out so as to collect only one phase per sample, if possible.
Medium hazard concentration samples^ must^ be , shipped in cans v^a
Express,
Samples should be packaged as described in the NE1C Manual, and
shipped according to DOT regulations. Each sample is packaged in an
outer metal can with clips, tape or other positive seal. Each can
is marked with the destination name and address; indicate "Flammable
Liquid, N.O.S." (if not liquid, "Flammable Solid", N.O.S.) and "Cargo
Aircraft Only" on the outside.
I
Inside the can, the sample is sealed inside a plastic bag. Vermi-
culite is used to cushion the sample inside the can. Traffic or labor-
atory numbers should be written on the inside sample tag and outside of
the cans. Hazardous labels should also be placed on the inside and out-
side of cans.
If Federal Express is the carrier, the form "Federal Express Ship-
ping Certificate for Hazardous Materials" (FEC-S-0147) must accompany
the shipment. Other carriers have an equivalent form.
The same SMO Traffic forms are required, as for low hazard samples.
However, on the Organic and Inorganic Traffic Reports it must be noted
that the samples are "medium hazard concentration water, soil, or sedi-
ment"*
Charles Elly (or his designated alternative) should be notified
prior to shipment of the samples. Elly will contact the SMO for EPA
-------
*
-10-
and/or FIT, obtain a case number, and the NCL to which the samples
will be sent. Under no circumstances is the Sampler to call the SMO
or the NCL. This protocol must be followed for EPA and TAT personnel.
FIT personnel makes Its own arrangements for shipment with the SMO.
D. HIGH HAZARD SAMPLES (Organic/Inorganic Liquid or
Other Phases Collectable From Drums or Around Drums)
All high hazard samples should be collected according to the Draft
NEIC Manual.
Bottles, Preservation, Holding Times,
Forms, Custody and Shipping Procedures
ORGAKICS AND INORGANICS (All fractions; liquids and solids)
1-8 ounce wide-mouthed, round, clear glass jar with screw-neck
finish and teflon-lined cap (KERR AC802 brand or equivalent; avail-
able from VWR Scientific - Catalog Ko.#1694-063); filled one-half
to three-fourths full with the sample. No ice or preservative.
MAXIMUM HOLDING TIME; Not established yet.
Table I contains an itemization of the sample sizes which are re-
quired to analyze each fraction.
Field Quality Control
A blank Is not required. Duplicate sample (s) should be collected,
wherever possible.
Chain of Custody Procedures
The same procedures as outlined for low and medium hazard samples
(see page "5" of this protocol) should be used.
REQUIRED FORMS t
1. The SMO High Hazard Traffic Report (not required If analyses
will be done at the CRL).
-------
TABLE 1
SAMPLE CONTAINER AND QUANTITY REQUIREMENTS
Requests
Recommended
Quantity
Required
Shipping
Container'
ROUTINE REQUESTS;
Total Metals, Strong, 60 grams
and Weak Acid Anions
Total Mercury 3 grams
Base/Neutral, Acid, 6 grams
and TCDD
Pesticides/PCB 6 grams
Volatile Organics 6 grams
8 ounce or smaller jar
with Teflon-lined cap
8 ounce or smaller jar
with Teflon-lined cap
8 ounce or smaller jar
with Teflon-lined cap
8 ounce or smaller jar
with Teflon-lined cap
8 ounce or smaller jar
with Teflon-lined cap
SPECIAL REQUESTS;
EP Toxiclty
Corrosivity
Ignitability
300 grams 1 quart glass jar with
Teflon-lined cap
1 liter 1/2 gallon glass jar
with Teflon-lined cap
1 liter 1/2 gallon glass jar
I
* Obtainable from VWR Scientific; Catalog No. 116194-063.
-------
S
-12-
2. The NEIC Hazardous Waste Sample Preparation Request
3. The CRL Sample Number
4. The Region V ESD Chain-of-Custody Form(s)
5. The Region V ESD Custody Tag(s)
6* The Region V ESD Custody Seal
7. The Region V ESD Basic Data Form (for samples analyzed at the
CRL only)
Packaging and Shipping
The requirements are the same as outlined for medium hazard samples.
(Please read carefully and follow guidelines as outlined on pages 9, 10,
and 11.)
Shipment of high hazard samples directly from the field is encour-
aged. The samples are mailed to the EPA, NElC-Regulated Substances
Laboratory, c/o Dr. Steven Kunen, Fred C. Hart Associates, (an EPA
Contractor), Denver Federal Center, Building 53, Box 25227, Denver,
Colorado, 80225.
One extra high hazaTxSf^unr'must accompany all samples. This is
for an NEIC preparejt-re'agent blatok. Spike, matrix spike and duplicate
results will^e added to the Sample Trafi^c form.
The Air-Freight Bill Number and shipping company? must be phoned in
to Charles Elly the same day, or early the next morning (as soon as
possible). (FIT exempted.)
4 Charles Elly will contact Fred C. Hart Associates approximately
i? two (2) weeks in advance of each projected on-slte sampling survey to
V ''
verify whether Hart Associates will accept the samples. The EPA, FIT
of' TAT Sampler must contact Charles Elly before shipment to Denver.
Copies of all the aforementioned items must be forwarded to Charles
Elly immediately after shipment (24 hours or less). (FIT exempted.)
-------
-13-
Tbe turnaround tine quoted by EPA, NEIC and Hart Associates Is
twenty-one (21) days for routine samples. (NOTE: This Is only for
extraction.) Further organic and inorganic analyses will be done at
the CRL or a NCL, which will require additional turnaround time (prob-
ably -30 more days).
For samples which go directly from the NEIC (or Hart Associates)
to a NCL, the Sampler forwards the SMO High Hazard form mentioned above.
The NCL will forward the final sample analyses results to the Region V
CRL.
E. Tracking of Samples
Tracking of EPA and TAT forwarded samples is done by Charles Elly.
This is accomplished through the use of the attached Table (2) entitled
"Status of Region V Hazardous Waste Samples". This Table is kept in a
logbook and includes information beginning from the time of collection
of the samples through the date of final analysis. The CRL Data Manage-
ment Coordinator tracks data at the CRL after a copy of the Traffic
Form(s) and Custody Sheet is given to William Sargent, CRL16 Shipping
and Receiving Clerk, who logs in the sample numbers and assigns a data
set number (for EPA and TAT samples).
F. FIT Tracking of Samples
The FIT Contractor tracks its own samples. This was delegated
from ESD to FIT to lessen the paperwork and burden on Region V EPA
personnel, as well as to speed up data turnaround.
As a minimum, FIT transmits weekly (each and every Tuesday), to
Charles Elly, the following:
Sample collection date; sample shipment date; sample type (low
hazard soils, medium hazard concentration waters, etc.); National
Laboratory samples were shipped to (and/or NEIC); NEIC Traffic
numbers (Inclusive of the total number of samples); SMO Case
Number, CRL Numbers, and projected date of return.
-------
±tir^tLL4 .-L-i
r-l ••
u
'>;!!!!!'!!
» : • • I » I I i I I
J I I i I l «_• \. ' I
• I
^"isS"
J C M O -O
•• 3 > c
« o o • a
W -H • ON O
Q • UJ \O —« W
«C O •** •"" *
S » •• c
4J W •• 0) W"
.. H PC w 3
<-s <: to H
_ O *-vM -O
a -H u > •
C «H CO
.c a c o o «s
w so re w -H
U 6C *J •*
• O (1 4J 01 4J
C o c «-» «
M •>—' 0) B. ^
.»s^ co B i_i
0) «g O CO 05
Z 0) •
C »-03 03 60
O . cn w >» C
«H ^ •-• O t-l «rt
w « te >
y ...» Ui C i-l
ft) /-» 03 4J « O •
r-t U l-i X 01-
r-4 *H W W C « O
o c * o as «
O 0) E 4) -H •* W
60 3 4J U 60 01
. W. C «6 O C 3
.» O O « -H O"
v-/ o u a a>
.« M . AJ O.B5
a) O W in K ft
6 M SS ~i W .E O
•rl (d CO JJ
4J Z . •* •
fsl W 00'^ • ^»
o . *^ QJ <_i V M
r-l 00 .0 C 3
t,. £ .« m O
.• u 3 <— e ^
« /^ 4) C O « C
(A U £ -H 60-H
.-.^ § o c a*-"
C 3 -H « C
n -js «« M «
6C «w ki £ T3
CT> n T!
.. Vj 4J B O W
• O 1> Wi C W •«-'
O C W H -H *J *J
. >H >-» eg -H
o >^ n <-s o e
4J O BS 0>
p4 $ S "c »S •• w
«-i eg > >< h
.« > J 6D JD 4J
0> K ki •
4J . O O I~- T3 «
-^ r» c -* ft) *J
05 . M > as
• • «•< x^ •» >rl "O
Q) /-N-* ^^0)
• O Bi O O Q)
.*< T< 0) '
I- H C W
t
c M
to 3 o> > « 'i.p
Ift 6TJ3 6C W^
I- E • Wi W *
. o a <» o « -<
•-I <^/ B ••* ^^ *O «M
to
i
*
*
-------
-15-
G. DATA SUBMITTAL AND RESPONSIBILITIES (FIGURE 1)
The NCLP data are sent directly to the CRL. A date of receipt is stamped
on the data and-it is given to the Data Coordinator. The Data Coordinator
logs the data onto the Internal Tracking Sheet (Form 3) which includes the
SMO Case and Traffic numbers. CRL Number(s), Decision Unit, Site Name and
CRL Data Set Number; date information is assigned; listing of outstanding
data not received; and the date the data is sent to the user. The Data
Coordinator-also completes and attaches a form entitled "Review of Region V
Contractor Data" (see Attachment *4). Elly passes the organic data on to
Kendall Young, CRL Organic Section Chief, who assigns a organic reviewer
to the data. Inorganic data is passed from Charles Elly to either
Dr. John Morris, CRL Metals Team Leader or Ms. Andrea Jirka, CRL Minerals/
Nutrients Team Leader for review. Charles Elly may also review inorganic
data, if the Team Leaders are scheduled for other duties.
Once the data have been reviewed by Organic and/or Inorganic Laboratory
Section reviewers, it is returned to Charles Elly. If quality control
(OC) deficiencies or out-of-control audits were noted by the reviewer(s),
the data is passed to Ms. Marcia Kuehl, CRL Acting Quality Control Coordinator.
Ms. Kuehl tallies these OC deficiencies and makes a recommendation as to
whether the data should be released to the data user. Recurring OC violations
and deficiencies with laboratories are documented and Dr. Eugene Meier,
EMSL-Las Vegas, is notified through Dr. Alfred Haeberer. If the data are
considered unacceptable for use, Elly is notified and the data are returned
to him to arrange either additional sampling or re-analysis.
Data that has passed through review hy the Organic and/or Inorganic Laboratory
Section reviewers with no OC deficiencies or out-of-control audits noted,
are directly returned to Charles Elly for final review. The Data Management
Coordinator is responsible for actual data transmittal to the data user.
A xerox copy of the data is made and attached with a cover memo (Attachment #4)
which notes OC violations, if any, that affect the data.
QC flags are noted on Attachments #4 and #5 (for organic data only).
Attachment #5 is a draft of the "Regional Review of Uncontrolled Hazardous
Waste Site Contract Laboratory Data Package" and has been revised to suit
Regional needs. This review form is to he sent to the SMO when OC problems
requiring total rejection or organic data occur and is routinely sent to
the data user.
The following two Sections explain the criteria and specific acceptance
limits used hy the CRL data reviewers.
H. REVIEW OF INORGANIC CLP DATA
The following items are checked, hy the Inorganic reviewers, and deficiencies
and/or out-of-control audits are entered on Attachment 44. Form #6 must be
completed for all SAS case data and sent to SMO only.
-------
oF
-16-
*€Y»ti>J
f Smo \
*'. i >
I I
-------
- 17-
1. DATA SHEETS should be legihle, in sequential units anrl the minimum
detection limits should be listed with the instrument noted.
ACTION: Call SMO
2. FINAL DATA PACKAGE should contain:
ALL Tasks: Results for each sample to two significant figures
List of detection limits used, supporting raw data
TASK 1: ICAP or validated alternate results for Al, Cr, Ba, Be,
Cd, Co, Cu, Fe, Pb, Ni, Mn, Zn, B, V, Ca, Mg, Na
*Inorganic Quality Assurance form
TASK 2.: Flame/furnace AA results for As, Sb, Se, Tl, Hg, Sn, Ag
Mnorganic Quality Assurance form
TASK 3: a) Low concentration NH3, F, S, CN, pH and TOC results
b) Medium concentration NH3, S, and CN results
Inorganic Duality Assurance form
*Inorganic Quality Assurance forms contain initial calibration veri-
fication, continuing calibration verification, duplicate and spike
results.
3. METHOD BLANKS should contain less than one-half the minimum detection
limit and should he reported on the data sheets with the results.
ACTION: Flag affected samples as contaminated
4. INITIAL and CONTINUING CALIBRATION VERIFICATION should be reported on
the Inorganics Quality Assurance forms. Continuing calibration
verification should show no drift larger than that listed on form 1.
If this drift did occur, a new initial calibration curve must be included.
ACTION: Flag affected samples as having unreliable quantitation
5. ICAP INTERFERENCE CHECKS should be run at the beginning, end, and
once every 20 samples. Results should be recorded and labeled as
"ICAP Interference Check" on the Inorganics Quality Assurance form,
under Section II.
ACTION; Flag affected sample data as possible biased
6. LAB DUPLICATES should be recorded on the Inorganics Quality Assurance
fprm and not exceed the following limits for concentrations greater
tWn the detection limit:
' * ' ' 1) TASK 1: RPD <20
2) TASK 2: RPD <50
3) TASK 3: RPD <50
-------
-fe-
7. MATRIX EFFECT SPIKES should be recorded on the Inorganic Quality
Assurance fprm and not exceed the limits listed in form 1.
ACTION; Flag the affected sample element(s) data as biased
8. FIELD PC
Field prepared duplicates should not vary by more than + 20%. Field
blanks should be examined for contamination levels > I/? the detection
limit.
CORRECTIVE ACTION: Flag all sanples in case as being of >20% precision
and/or containing bottle/sampler introduced contamination (if field
blank contents vary from lab method blank contents, call field team
to check on possible sources of contamination or imprecision).
. REVIEW OF ORGANIC CLP DATA
At a minimun, data reviewers must review the following eight items in
judging organic data. Additional review items are listed to be pursued
only when time and suspect data quality dictates it. Forms *4 and #5
must be completed for all routine and SAS CLP cases. Form #6 is for
SAS data and is sent, to SMO only. Form #2 gives the current criteria.
A) MINIMUM REVIEW ITEMS: (Not in order of importance)
1. BFP/DFTPP Specs must meet those in contract.
ACTION: Flag affected samples data- if the out-of-control mass
not meeting specs, was used to ID or quantify a pollutant, it is
invalid.
2« BLANKS must be clean (< method detection limit) and sample
concentration must he >10 X blank to he considered valid.
ACTION: Flag affected sample data appearing at <10 X blank
contamination level as due to lab and/or field contamination.
3. POSITIVE PRIORITY POLLUTANT hits must be verified by visually
checking MS, sample and retention time match up against standard.
ACTION: Cross-out incorrect pollutant and flag as not detected.
4. TENTATIVE IP's must be visually checked against spectra supplied -
"elegant" compounds should be verified to see if they could survive
the GC/MS conditions or if they are artifacts of the operator's
imagination.
ACTION: Cross-out unreasonable compound match and note as unknown
-------
n
-19-
5. HOLDING TIMES should be checked, this is only to be done if sample
is a natural water or sediment. Drum samples are excluded as the
time is not crucial.
ACTION: Negative hits should be noted as possibly being biased low
for samples with holding times exceeded, positive hits need to be
qualified as not meetiny holding times.
6. DUPLICATE PRECISION for both field and lab should be within the
criteria.
ACTION: Flag only the affected samples/duplicate compound data
as imprecise, give actual RPD. If a compound is not detected at
all in one sample or duplicate, flag that compound as questionable
if the concentration level is <10 X detection. If the concentration
level is >10 X detection, flag the precision of that compound as
erratic. Note any non-homogeneity of sample in qualifying statement.
7. SURROGATE SPIKE RECOVERIES should fall within the criteria. If any
lab notation is made of lab accidents or reruns, flag data accordingly,
ACTION: Flags depend on the number and severity of deviations from
the limits. Note that only fractions per sample are flagged unless
a generalization over the whole case can be made. Guideline levels
are given below.
I
-------
FRACTION
rVQA;
d5 Toluene
dg Benzene
-EO-
TOTAL NUMBER f ACCEPTABLE
2
1
0
ACin/B/N: 4
d5-phenol(A)
2-fluorophenol(A)
d^-nitrobenzeneCB/N)
2-fluorobiphenyl(B/N)
TCDO:
17773,4-TCDD
4
3
1
0
1
0
SAMPLE FRACTION
QUALIFIER
acceptable
related conpound data invalid
unacceptable and/or biased
matrix problem.
acceptable
acceptable with qualification:
note compound class with out-
of-control recovery
if both A or B/N, that class
of compounds invalid biased
if one A and one B/N-data qualified
as suspect
one class data invalid, other
suspect
both compound classes unacceptable
or biased, matrix problem?
dioxin data valid
dioxin data invalid, matrix
problem?
*'
-------
-21-
8. MATRIX SPIKE RECOVERIES should fall within the advisory limits criteria.
If any lab notation is made of lab accidents or reruns, flag data
accordingly. The flags only apply to the sample chosen as the spike.
ACTION: Flags depend on the number and severity of deviations from
r the limits. Guideline levels are given below:
FRACTION
VOA:
Chlorobenzene
Toluene
Benzene
I COMPOUNDS * ACCEPTABLE SAMPLE QUALIFIER
acceptable
actual level of the
specific compound outside
limit may be biased
(compound flaj)
flag compound(s)
unacceptable biased
matrix problem?
B/N: 7
T72~,4-tri Chlorobenzene
acenaphthene
2,4-dinitrotoluene
di-n-butylphthalate
pyrene
N-ni troso-di-n-propylami ne
1,4-diChlorobenzene
ACID:
pentachlorphenol
phenol
2-chlorophenol
p-chloro-m-cresol
4-nitrophenol
PESTICIDES;
heptachlor
aldrin
deildrin
1
0
7 acceptable
6 acceptable, flag compound(s)
5 acceptable, flag compound(s)
4 B/N data biased and/or
erratic, flag compounds
3 B/N data biased and/or
erratic, flag compounds
2 matrix problem? unacceptable
biased
1 matrix problem? unacceptable
0 biased
5 acceptable
4 acceptable, flag compound
3 acceptable, flag compounds
2 B/N or acid data biased and/
erratic, flag compounds
1 unacceptable, biased matrix
problem?
0 unacceptable biased, matrix
problem?
3 acceptable
2 acceptable, flag compound
1 unacceptable biased matrix
problem?
0 unacceptable biased matrix
prohl em?
Note'that all of a case's positive sample results for matrix spike compounds
may nee0. to, be qualified if the sample chosen as the spike 1s representative
of the entire case.
-------
-22-
B) AnniTIONAL REVIEW ITEMS:
1. New or additional surrogate and matrix spike compound recoveries.
r •
2. Initial and continuing calibration.
3. Tailing factor, benzidine and pentachlorophenol response.
4. Internal standards response stability.
5. Choose one positive hit sample/case and walk through all calculations
for A/B/N, pesticides, VOA's.
6. Chromatogram quality (GC/MS & GC/EC)
7. Blind OA audit results if applicable.
I. DATA USAGE RECOMMENDATIONS
Data that has received QC flags (that render it useless to the Oata Requestor)
is brought to the attention of Or. Alfred Haeberer, EPA Support Services
Branch and Dr. Eugene Meier, EMSL-Las Vegas. This invalid data may be remedied
by reanalysis or resampling and subsequent analysis by another laboratory.
Continuing problems with particular laboratories or analyses is also brought
to the attention of these two support people.
Presently, the CRL reviewers use the same protocol to review all CLP data
(Sections II ft III) regardless of data user OC requirements. Thomas Yeates,
Region V OPO, is in the process of accumulating input from data users as to
the intended objective of the data. Some data does not require as stringent
OC as others. Data from sites indicated as less critical, or data intended
as only a screening process will continue to be reviewed under the same
protocol. Violations of limits and deficiencies will still be indicated
on Attachment *4, but data may still be judged acceptable ev«»n though limits
have been exceeded or deficiencies found. The data user will have full
knowledge of the quality of the data and may request follow-up analyses.
Once the decision has been made to invalidate sample data, no matter what
objective it was to serve, Region V will insist that the samples be reanalyzed
under the CLP. Unacceptable data will not be released to the data user.
The data user will be consulted during the decision making process to determine
the degree of OC needed to best serve the data objective.
Once the data has been judged acceptable or preliminary, the CRL Data
Management Coordinator puts the CRL lab numbers on all data sheets and makes
a .copy. Within 24 hours after review, the copy of the data and Attachment *4
are -sent to the TAT, FIT or EPA data requestor. FIT and TAT data are
transmitted to Cindy Bachunas (Environment * Ecology) through the mailbox
in Thomas Yeates1 office. REM/FIT data will be initially reviewed by
Paul Friedman, SMO and verified by Marcia Kuehl before release.
-------
- 23-
The entire reivew and transmittal of data should take no longer than five (5)
work days, after receipt by the CRL. Questions regarding the status of data
should he referred to Charles Elly, SMO Coordinator. Questions regarding the
quality of the data should be referred to MS. Marcia Kuehl, CRL QC Coordinator.
V'
-------
TAILT i. ewrrwi. WHITS iw WOUGAJCIC ANALYSES
Atomic Abtorptloa
SpcctroMtry
tiac
Arttnie
Aattaooy
tureury
Stltnli
Tin
Othtr
Cy«nld»
Sulfite
•5
•0
71
•0
•5
U
75
•0
•0
•5
11*
115
120
122
115
115
112
125
120
120
115
2.
STUB SAffU UCOVWT U*"S
-------
*•.
LOOT* x» MM una.
uunt um o» tncu UMUJOB
I. «. * trtHi»i>.««l
• n**t Itmiti »n In
It » >«^lt «t>eul| w
feu 1* •vmlltkl*. tu*t*it Iteitt fill
i VD4* * US
1/1 S KB
AtU 1 401
-M-1JJ
-Tt-lII
-4V1J1
-M-1U
-M-1M
-17-US
-4V111
-1VX1J
•13-11?
->*-U4
•2J-4J
-JV107
•U-1M
•U-tl
•4V113
-43-10*
-34-111
i»t« that tk» Umlti »rt •• l»4tr rvceld »ff. Sn«ttt|*tl*»
»ft«r tb> ••itlfit »h»v*d tlttt r«oorot«r u it tUv* tk* limit*. n»t llmitf. ttarmfwrt.
fa
-------
t-i
m
a g
in C
^ w
ft
z ~
B) Z
ft |
CT
ft
D
•
C
I o
cr n
ft tu
1 Wl
ft
-0
tu
CU
3
ft
r+
ft
•%
VI
2
r
70
o
v>
£ J?B
v>
-------
4
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION V
DATE: r
SUBJECT: Review of Region V-CLP Data
Received for Review on
FROM: Curtis Ross, Director
Central Regional Laboratory
TO: Data User:
We have reviewed the data for the following case(s).
SITE NAME: SMO CASE NO.
No. of
EPA Data Set No. Samples DU/Activity No.
CRL No.'s
SMO Traffic No.'s
Contract Lab; Hours required for review:
Following are our findings.
( ,-).Data are acceptable for use.
( ) Data are acceptable for use with qualifications noted above.
( " j) -Da
-------
REGIONAL REVIEW OF UNCONTUOUn) HAZARDOUS WASTE SITE CONTRACT
LABORATORY DATA PACKAGE
TO« U.S. environmental Protection Agency CASE NO.
S**ple Management Office (SMO)
F.D. Bo* BIB
r Aleiandris, Virginia 22313
•
The hardpopied (laboratory news) data package received st
Region _nM D**n reviewed and the quality aaaurance and performance data sum*
The data reviewed included!
SMO Sample Cone.a SMO Sample Conc.i. SMO Sample Conc.i
No. Matrix No. Matrix No. Matrix
Contract No. ._ r»qulr«« that tpeciric •n«lyllc»l work b« 6on« »r«l thtt w«oel«t*d
toportt b* provided by tr* contractor to the Rt^ions, EMSl-LY, »nd SHQ. T>» gtrwtkl crlttrl*
used to detacnine th« performance were based on an examination eft
• Data completeneaa • Duplicate analytia reaults
• Spectra welching quality • Blank analyaia reeulta
• Surrogate apike results • DTTPP and BTB performance results
• Matrix spiks results
The deta revleu forms for each of the above review itens are contained within the body of this
Cotmentss
15
-------
DELIVERABLE
CASE *_
CONTRACTOR
CONTRACT I
SECTION TITLE
KARRATIVt
Contains: Case I, Contract I, turn* 17 of any QC, sample, shipoent and
analytical problem*, documentation of any Internal decision tree process
used.
II
ry SUHKART
*A. Surrogate t recovery sMsaaary fora.
f*B. Reagent blank suasary form.
pC. Matrix splice duplicate/recovery fora
. Instruaent tune & perforaance suaaary form
III
SAHPLt DATA PACKET
A. Saaple Data in increasing SMO I ordert
1) RSL results.
2) CC/KS tentative ID sheet, sven if noue found*
3) Rav data (VOX. AjB/H. P«»t, Diozia)
i. Cnrooatogrca(s)
11. Data Systea printout
ill. HSL spectra with standard (dual display)
Iv. CC/KS library search spectra
T. Quantltatlon/calculatlon of tentative ID eopcentration
IV
A. Cross-reference table (lab's internal)*
B. VOA standards chronato&raas and data systea printout*
C. A/B/N standards chroaatograas and data systea printouts.
D. Pesticide standards chroaato&r&a* and data systea printouts.
C. Dtoxin standards chroaatograas and data systea printouts.
*F. Intenud standard verification data sKest.
*C. FSCC Initial calibration data.
*H. Calibration check.
I. Current list of lab detection Halts.
Designates new fons.
(_)33 - OS8
-------
•prpiEST TV" " •"••--—---
in progress may DC cu**...
Priority 2 - High priority projects to Ve scheduled and completed
as soon as possible without disrupting other wort, in
progress.
Priority 5 • Projects to Ve completed around Priority I and 2 pro-
jects, but with some definite completion date, usually
at least two or three BontKs Croa xequest date.
-- -•— i. ,vai - -
-———•
-------
§O.,«CT,
For:
-to. Project Ob3"*ive:
Decision Unit
Desired Completion Date
Principal Contact:
Specific Activity
Prom:
Target COB. Date:
ESD Project Uader:
.*'.*
tSD project Wo.
Phone
*»*. re*
I f
r' '
-------
ATTACHMENT 12
PECIAL ANALYTICAL SERVICES
-------
.
I
1
,. cyanic,
,.
PCB
MENU OF
M
Fast Data Turnaround
-**'
_ Added Capacity
Compounds
,.
Sample Analyses
, s
,. RCRA Analyses
M. Fused SUicaCapmar, Column Ana.y.«
12.
Analyses
-------
I
SPECIAL ANALYTICAL SERVICES
A. Background
In addition to standardized types ot analyses provided under the Contract
Laboratory Program, the Sample Analysis Program has established a system to
provide limited custom or Special Analytical Services 1SAS) which are beyond the
scope of the current laboratory contracts and/or available protocols but which are
consistent with Program objectives. Upon a sampler's request and Program
authorization, the Sample Management Office will arrange for analytical services
Including but not limited to quicKtumaround analyses, verification analyses,
Identification and quantification of non-priority pollutant compounds, general
waste characterizations, RCRA, Dioxln and other specific analyses. The Sample
Management Office, In Its continuing performance of sample scheduling, data
integration functions, and data base preparations, procures these Special Analytical
Services by subcontracting with laboratories currently in the Contract Laboratory
Program to perform the required task.
B. SAS Initiation
Depending on the complexity of the Special Analytical Service request,
special services can be Initiated in fairly short periods of time; however, because
the SAS program requires SMO to procure laboratories on a competitive basis, at
least a weeks lead-time is recommended. In general, the institution of Special
Analytical Services, because of protocol diversity and specific laboratory procure-
ment procedures, demands greater advance planning and more lead-time than
• •
required for the standard laboratory analyses programs.
m-i
-------
I
I
1
pr
ocedures.
^ * authorlzetrrepresentau oi
,< rcauired data
reeel?t'
-------
I
I Additionally, ft written request document should be forwarded to
SMO after the initial verbal contact.
I
1
1
b. Program Authorization and Protocol Confirmation
As the SAS program b an extension ol the Contract Laboratory
Program, the EPA Program Manager must review and approve
qualified SAS requests. If a SAS request b authorized which
requires a non-program methodology, the Quality Control/Quality
Assurance Officer (EMSL/LV) confirms the validity of the
requested analytic protocol, amending It as necessary. If the
request is denied, tht Program Manager indicates the reasons for
denial.
C. Pre-Samplina Procedures
li accepted, the Sample Management Office telephones the SAS
requestor to coordinate the sampling, sample shipment and analy-
sis requirements.
(1) SMO and the sampling coordinator agree to sample label
numbers and any site or specific coding Information to place
on tracking documents and sample bottles. SMO provides
the name and address of the analytical laboratory alter a
subcontract Is awarded.
(2) SMO forwards tracking documents to the SAS user, or
arranges to have them supplied by the EPA Regional con-
tact.
-------
I
I
1
I
1
I
1
(3) The SAS sampling coordinator provides all cample and
tracking documents/instructions, etc. to sampling team
leader (communication with SMO if necessary). Sampling
takes place.
(4) Sampling team leader telephones SMO after sampling with
appropriate shipment information which includes:
I o Date and time of shipment.
o Any changes in the sample numbers, types, etc. as
| specified in the SAS.
o Numbers of containers, confirmation of sample ID num-
I bers, special instructions.
o Air carrier and airbill number.
2. Sample Tracking
SMO will track the sample/sample fraction from the sampling site
through the labor atory(ies) in accordance with established Program
procedures. SMO will provide and monitor all sample tracking forms
and related documentation.
3. Data Receipt
a. The laboratory will forward all data and other relevant document
copies to SMO. SMO validates the data tor completeness,
deliverables completion within contractually-specified time per-
'tods, and adherence to all terms of subcontract.
b. The EPA Program Manager and Technical Officer are responsible
lor technical validation of the data results. The EPA QA/QC
Officer is responsible for the validity and accuracy of the quality
control data.
m»*
-------
c.
while
conned. «. r«.e«n« *. k .or-W - -
p,,.-* bourc*. EMSL B reined, etc.) SMO w
copy 1« possible future reall.
-------
ATTACHMENT f3
. • . ENVIRONMENTAL PROTECTION AGENCY
OWCE O? ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
KNVU. COIORAOO ao«s
Tom Yeates *n February 10,19B2
10 . . &PD. Region V
..o* . Rob Laldlaw
Evidence Audit Unit, MEIC
Chain-of-Custody
As per our earlier discussion, 1 am enclosing copies of sample tags and
chaIn-of-custody records filled out as an example of a hazardous waste
site investigation. Also enclosed ere EPA sample control and chain-of-
custody procedures (October 1980).
•
Some specific concerns regarding documentation of custody are:
1. All members of the sampling team for a particular investigation
should be listed on the sample tags and custody records. This
provides a consistent record of individuals participating.
2. All information recorded on a sample tag should be identical to the
custody record (station No., station description, date, time,
project name* etc). This also provides consistency of documentation.
3. Station location descriptions need to be designated and all personnel
refer to them in the same manner. Elimination of estimating by
different investigators is desirable. For example,
one person records on a tag. station Ol...leachate 10 yds from SE
corner of storage shed,
another person records on a custody record, station 01... leachate
^ . 100 feet from SE corner of storage shed.
•
Even though the sample was taken at one location, the records show
a difference of 70 feet. This is a very conroon type of documenta-
tion problem.
*"
»^ 4. VA11 blanks on tags and custody records should be filled out to the
' extent possible. This assures that all necessary information is
recorded.
.» S. The first name in the "Relinquished by" box on the custody records
must be one of the names listed as a sampler on line 2 (see example).
If not, there is a potential break in custody in the documentation.
-------
2.
3.
4.
5.
Federal Express »9° JRetTto them
.
, —
""' «•«"
1 jfli samples «»— —
"^ . .__, _ t*. tta of colUdion untU shipped.
. «*
receded secured.
were stored in a secured area.
S. Bench records show names of analysts.
-------
ese resort. ^ w (ns
„ , «., be of further .ssUUnce. »1e«e fee! free to
234-4706).
Enclosures
-------
-ir
-------
ctdafe fa* 51
ri
-------
-------
Projeel Cod*
COO
Sution No
Tune
Otvgn«tc.
z
i
0
co
o
o
i
i
Sui-on locai'Oit
S
tf /o'
Z6
O
to
Starters (Signature*)
0
r>
.BOO Anions
So.'idj USSIlTOSMSS
ANALYSES
*
t
I
-------
-------
*'.! /
-------
r'OtltttO*
'..»' -•'
• I
-------
-------
DELIVERY ORDER
Under Provisions of
EPA Contract No. 6S-01-656S
Order No.
Date of Order
FROM:
(Requestor
name, address
& telephone)
TO:
Emergency Order:
(date & time order called in)
(signature)
Repository Project Manager - Analytical Services Center
Ecology & Environment, Inc. - P.O. Box D - Buffalo, NY 14225
Telephone: 716/631/0360
Please ship the following items for arrival by:
Order is designated for shipment to a temporary field location (e.g., hotel, local carrier
office). Please ship order to arrive no earlier than:
(date)
CONTRACTOR
USE ONLY
Ite
N.
1
2
3
4
5
6
sm N
o. Description
1/2 gallon amber glass bottle
40-mL borosilicate glass vial
1-L high-density polyethylene bottle
500-mL polyethylene bottle
16-oz wide-mouth glass jar
8-oz wide-mouth glass jar
Ship To:
(Designee
street address)
Attention:
lo. of Items No. of Cases No. of Cases
Per Case Ordered Shipped
12
100
76
161
4&
96
CONTRACTOR USE ONLY
The above materials have been shipped as requested.
Date Shipped: Mode of Shipment:
' - ' * ' A/B, UPS BOL No:
Signature:
Type of Order: Routine
Emergency
Partial Complete_
DISTRIBUTION: White - Repository Copy, Yellow - Repository Copy for Return to SMO,
v. Pink - SMO Copy, Gold - Requestor File Copy
-------
\
)
CURRENT CLP SMO IFB ANALYSIS LABORATORIES
: -"
Organics - Multimedia
California Analytical Laboratories, Inc. (916) 381-5105
5895 Power Inn Road
Sacramento, CA 9582*
Attn: Bonnie McNeil 'ALTERNATE: .Julia Frey - ^
(916) 381-5105
Organics - High Hazard
California Analytical Laboratories, Inc. (916) 381-5105
5895 Power Inn Road
Sacramento, CA 9582*
Attn: Bonnie McNeil ALTERNATE: Julia Frey •
West Coast Technical Service " (714)523-9200
17605 Fabrica Way, Suite D
Cerritos, CA 90701
Attn: Linda Krokenberger PRIMARY: Jack Northington
Inorganics • Multimedia
United States Testing Company, Inc. * (201) 792-2400 -ext 253
1*15 Park Avenue
Hoboken, N3 07030 (Hudson)
Attn: AlTordini ALTERNATE: Richard Posner (ext 320)
Rocky Mountain Analytical Laboratories, Inc. (303)421-6611
5530 Marshall Street
Arvada, CO 80002
0. ;r - Attn: TonyMaiorana PRIMARY: Mark Carter
Ghem tech Cons-jlting Group, Ltd. ' (212)255-2100
36b West .11. th Street .
'•' NeW'ToVlq-NY 1001* ' - -. • ;
;; */f> -•< * ^ - -
,, -.-„ , ^AUn: ^5r. Alan Schof iman ALTERNATE: Frank Brezynski
r~.vj* "^"•'•^y v -•
' ff^r^ff- • ' - -,' -
,'. ^^ri'/Mefe'- ; (703)750-3000 •
,'1se>2i K
,. '.v:iAhh:.3$netBeckman • PRIMARY: Richard Ronan
* C.1" -i^1'" I. '.•'•'
-------
Inorganics - Multimedia (cont'd)
University of Washington
College of Fisheries
108 Fisheries, WH-10
Seattle, WA 98195 -
Attn: Dr. A. Nevissi
California Analytical Laboratories, Inc.
5895 Power Inn Road
Sacramento, CA 9582*
Attn: Bonnie McNeil
3TC Environmental Consultants, Inc.
7979 Old Georgetown Rd.
Bethesda, MD 2001*
Attn: Deb White
(206) 543-4259
ALTERNATE: John Sung
(916) 381-5105
ALTERNATE: Julia Frey
(301) 656-5850
ALTERNATE: Jeanne Hankins
West Coast Technical Service
17605 Fabrica Way, Suite D
Cerritos.CA 90701
Attn: Linda Krokenberger
Energy Resources Company, Inc.
185 Alewife Brook Pkwy.
Cambridge, MA 02138
Attn: Dallas Wait
Mead Compu/Chem
P.O. Box 12652
3308 Chapel Hill/Nelson Hwy.
Research Triangle Park, NC 27709
Attn: Angie Frye
Laucks Testing Laboratories, Inc.
9*0 South Harney
King County
Seattle, WA 98108
Attn: Mike Nelson
California Analytical Laboratories, Inc.
5895 Power Inn Road
Sacramento, CA 9582*
Attn: Bonnie McNeil
Organics - GC Screen
(714) 523-9200
PRIMARY: Jack Northington
(617) 661-3111
PRIMARY: Tyrone Smith
(919) 549-8263 ext 224
PRIMARY: Becky Siebert/ALTERNATE:
(206) 767-5060
ALTERNATE: Barbara McNatt
(916) 381-5105
ALTERNATE: Julia Frey
Paul Mi'
-------
\
Organics - GC Screen (cont'd)
)
U.S. Testing Company, Inc.
1*15 Park Avenue
Hoboken, N3 07030 (Hudson)
Attn: AlTordini •
Hazleton-Raltech
3301 Kinsman Blvd/P.O. Box 7545
Madison, Wl 5370*
Attn: David Hills
EAL Corporation
2030 Wright Avenue
Richmond, CA 9*80*
Attn: George Caesar, 3r.
High Hazard Containment
Fred C. Hart Associates (312) 234-2683
Regulated Laboratory
Denver Federal Center
Building 53 (Green Trailer)
Denver, CO 80225
Attn: Steve Kunen
(201) 792-2400 ext 253
ALTERNATE: Richard Posner (ext 320)
(608) 241-4471
ALTERNATE: Chris Alstetter/Emilio Sturino
'frti":
Revised 1/3/83
/TV /' J
* * t'
-------
SECTION TITLE
KAU QC PATA FADTT
A. PFTP?
•1) CC/MS performance standard fom.
2) Bar graph apectrua.
3) H;Z ll«ting.
i.
*1) CC/MS performance ataodard fora.
2) B*r graph •p*ctrua.
3) H/Z littinj.
C« Chroaatogtaphy Cbtck Data
1) B«uidia«
2) ?civtachlorophcnol ZICT'a/calculattona.
3) CC/EC eoluan ch*c\u
BlanV Pata(ln order VOA. A./B/W. Fettlcide. Ptorta)
1) Chrcaatograaa.
2) D*t* «y»t«k printout.
E. Katrlx Spike Pata(in ordar VOX.
1) Chzoaatograaa.
2) Data ajatca printout.
t ?e»ticld«)
7. Matrix SptVe Duplicate Pata(ln order VCAt A/B/W, ?e»tlcidO
1) Chroaatogram*.
2) Data aystea printout. _
VI
SATIP1X PR£PA]UkTIOH PACKET
/ A* S&apl* control aheat (lab's inttroal).
1. Screan data (in order VOA, A/J/H, peaticldO
1) CC/FID chrcaatograaa.
2) CC acreen data aheeta.
*Deaigoataa new fora.
-------
TENTATIVELY IDENTIFIED COMPOUNDS-UK£fcASDA}A&UEr
r
Sample Fraction • Compound Scan flT PurUy Concentration
-------
Exhibit B
Page 22 of 42
CSJ
00
trt
4-»
"i
FORM III
-------
Exhibit B
Page 23 of 42
FORM III (continued)
-------
Exhibit B
Page 25 of
FORM V
-------
Exhibit B
m
<
1
* *
S«
i
O \+J *•
< -J
gg;
O — i
ec _i
I 3 ^J
ie «j
oc
•W «K
•E Gi
o uj
Cat
'•.d
o >
a: ty
"s"'
— < O V uj O V
|O O _i • fc • _j • F. •
"o, — — •- po •- •- a e»
ce uj . H- — ^ « • >— L*
u* oe vj < *i «j — •— < v *J —
1— «_!*• *« X — 1 — «»
U. •—
i"»ae 2i of 42
1
i
1 \
\
\
\
\
\
\
* •
o «•»
UJ • C
00 |
5 *™ £ ^
(_ •) *J -
!/l ^ J
UJ — C
a. u, —
FORM IV
-------
IVHL *NU rfcKtUKflANtt SUfttlAKY
CASE NO. CONTRACTOR CONTRACT HO.
LOW LEVEL MED. LEVEL HIGH LEVEL *"
WATER """ SOIL/SED. OTHER(Specify)
DFTPP and BFB Performance Results;
The DFTPP performance results were reviewed and found to be within
the specified criteria.
The BFB performance results were reviewed and found to be within
the specified criteria.
DFTPP BFB
Mass Ion Abundance Criteria Mass Ion Abundance Criteria
51 30-60 percent of mass 198 50 15-40 percent of mass 95
68 less than 2 percent of mass 69 75 30-60 percent of mass 95
70 less than 2 percent of -ass 69 95 base peak, 100 percent
127 40-60 percent of mass 198 96 5-9 percent of mass 95
197 less than 1 percent of BBSS 198 173 less than 2 percent of mass 174
198 base peak, 100 percent 174 greater than 50 percent of mass 95
199 5-9 percent of mass 198 175 5-9 percent of mass 95
275 10-30 percent of mass 198 176 greater than 95 percent, but
365 greater than 1 percent of mass 198 less than 101 percent of 174
441 present but less mass than 443 177 5-9 percent of mass 176
442 greater than 40 percent of mass 198
443 17-23 percent of mass 442
Deviations; Required Observed
Date/Time Instrument^ File f Compound m/z Abundance Abundance
FSCC AUDIT SUMMARY;
50 ng benzidine detectable for all runs?
Pentachlorophenol response factor >.05 relative to D-10 anthracene for
•11 runs?
',*'.* '
Comments:
-------
VIXX. DttOHATQCRVKY OCOCS
r Type ef Colu»n; Fecked Column ______ Fused Silice Cepillsry Column
-"- Fecked Column Chrometogrephy
Telling Tectore accept ence Windoxs Hctusl
Benzidine .Lee* then 3
Leu than J
FSCC Chroff«to9r>phy Check
S0>ng benzidine detectable? Yes _____ No
Fentechlorophenol responss rector? Yes No
lte«srket
24
-------
IX. STUOMDS
.*- r
-^;. Central ah«p« of thr total ion
'..*".•'
Volttlltt f»»ticid«»
Intcrf*
Background
4-nitroph«nol
cMorophvnol
Btnzidin*
He*»chlorocyclop»nt«di*n>
Itophoron*
Dinitrotoluvrw*
• .HS Ttltphonc Ito.i
Coan*relal Tclaphorw No.t
-------
on the Introduction Fe,e.)
No
Ol-n-octylpHth«l«U
Fluor anthem
Him
D.t. of: C«Hbr«tion
Acid fraction:
2,«-dichlorophenol
2-nitrophenol
Phenol
Pentachlorophenol
Nsan
D.t* of: C«li»r«ttan
Verification
Analyti*
Volitllt Traction:
1,1-dichlotoethylen»
Chloroform
1,2-dichloropropam
Toluene
Cthylbenzene
Keen
Date of: Calibration
Verification
Analyala
to b« In calibration during analyaiat Yea
No
26
-------
SPECIAL ANALYTICAL SERVICES
REVIEW DOCUMENT
A. Client
B. Laboratory(s)
C. SAS Number
Task
CodeU)
D. Specific Request: Organic*
Inorganics
Other
Protocol
Code(s)
E. Analytical Methodologies: Organics
Inorganics
Other
F. Methods Source
G. Reviewer Name
H. Reviewer Function or Title
The purpose of this inquiry is to gain information and recommendations from the SAS Pro-
gram Principals directly, in order to improve the methodology(ies), QA/QC requirements, or
reporting formats for future similar Special Analytical Services. Therefore, please respond
in a timely fashion to all questions and requests.
V
. t '
-------
SPECIAL ANALYTICAL SERVICES
CLIENT REVIEW INQUIRY
Please return this inquiry document to SMO after review of the data package for this
Special Analytical Service.
A. General Methodologies
«•
1. Did the referenced methodology(ies) or protocol provide technically useful information
lor this specific SAS request? If not, please explain.
2. Describe any changes in methodology or other technical improvements that you
recommend in order to more adequately perform this specific SAS task.
*'
-------
r B. QC Requirements
i. Were the QC procedures adequate for determining the quality of the data for this
specific SAS request? If not, describe any problems encountered with the QC
•information.
2. Describe any changes in the QC requirements that you recommend in order to more
adequately perform this specific SAS task.
-------
r C. Data Sheets and Report Format
1. Were the reporting deliverable* clear and understandable? If not, please explain.
2. What changes in report or deliverable format do you recommend?
D. Other Comments
Enter here any comments or recommendations for items not covered above.
------- |