Sample Handling Protocol For Hazardous Waste


                                  905R82113
     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
                  U.S. Environmental Protection Agency
                  Region V, Library
                  230 South Dearborn  Street
                  Chicago,  Illinois  60604

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SAMPLE HANDLING PROTOCOL FOR HAZARDOUS WASTE

I. OPERATIONAL PROCEDURES

A. Data Requests

For saaples to be analyzed by the Central Regional Laboratory

(CRL) or by a contract laboratory, all requests should be initiated by

submittal of the ESD'e Fonn-81-01 "Request for Analysis" (see Attach-

ment #1). This form should be submitted, at least two weeks prior to

the survey, to William H. Sanders 111, Director, ESD, for Priority #1

surveys and to Curtis Ross, Director, CRL, for all other requests.
The following is a listing of priority types:
PRIORITY 01 - Highest priority work; immediate response or initiation
of the project by CRL is necessary; or other work already
in progress may be curtailed.

PRIORITY #2 - High priority projects to be scheduled and completed as
soon as possible without disrupting other work already in
progress.

PRIORITY f3 - Projects to be completed around Priority #1 and $2 pro-
jects, but with some definite completion date, usually,
at least two or three months from request date.

PRIORITY 14 - 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 VIAR & Company, Incorporated,

EPA iL-zardo-ah VE.
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on the priority, parameter, and sample type, or other factors. Most
Priority ll 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 KCL 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
#2), 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 Definitions
Generally, samples are divided into three categories: low, medium,
or high hazard.

Low hazard samples are normally b« groundwater, leachate, or sur-
face water. (Concentration ranges from 0 to 10mg/l (10 ppm)) of con-
stituents.

Medium hazard samples are up to 15% (150,000 ppm) of a single
r, - r.-T Cv.--js constituent. They ere, for example , samples of materials
{-'•c'-^ tic' of a drju. 7:,;- "ovrr i.':x;.e for medium ha?.ard eazple?
'- iiV^/l (10 ppffi).
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Hlgh hazard samples are samples of hazardous waste materials, gen-
erally, the contents of drums. (Concentration ranges from 152 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 NE1C 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:
40 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 NCL
(The total number of calendar days is equivalent to 51 calendar days.)
- SAS: No set limitations (see Attachment #1).

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. ORGAK1CS; Water

- 1-one gallon glass bottle (teflon-lined caps) or 2-half gallon
glass bottles; iced to A'C. MAXIMUM HOLDING TIME; 2 days until
extraction.

- 2-40ml glass Volatile Organic Analysis (VOA) vials (duplicates);
iced to 4eC (teflon-lined ceps). MAXIMUM HOLDING TIME: 7 days.

_OF^-','.~:C5: Sr.'Ir pr.c'or Sedisent?

- 1-8 ounce glass wide-mouthed bottle (teller.- iintd c&pk) iced to
1 , ' ' , - - , - • - t V - , r • r - > V ,- t, - • ,-• . V - . 1 1
~ ' ' •' ~ *t_ ^Li^.J I,*'*.- ,*«._..?- _.~^ *_!... fc £_ , _ t ; «
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2. INORGANICS; Water ., /• ft

- 1-one liter high density polyethylene bottle (metals, 3ml 1:1 HN03
preservative).* MAXIMUM HOLDING TIME; 6 months.

- 1-360ml high density polyethylene bottle (Mercury, Sol 1:1 HN03 pre-
servative). MAXIMUM HOLDING TIME; 14 days
high density^plyethylene bottl (Mercury, 2ml\>f
preservative)/ MAX IMUHyHOLDI NIG TIME;
/
- l-500ml high density polyethylene bottle (NH3+TOC, 2ml 1:1, H2SOA
preservative, 4*C). MAXIMUM HOLDING TIME: 28 days

- 1-5 00ml 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 6K 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 t^SO^
preservative). MAXIMUM HOLDING TIME; 28 days.
- 1-one liter high density polyethylene bottle (Phenols, 10ml
H3POA 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 recarsended are consistent with DOT reru^U-

ti::.r, therefore, thf ecrples ctr. be pVpped vie Air Freif%:,
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Field Quality Control

For low hazard water samples, a reagent blank is required for each
type or group of parameters (especially those which require preserva-
tion). In all cases, the bottles oust be the same as the sample bottles
and must be filled with distilled-deionired 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 CRL~\
sample numbers.
Attached is a memo from Robert Leiclav, KLIC (Attachment 03), to
7"r::c,-.£ Yeates, Region V DPO, which ey-el It-11y r ?.'•:---•.& the chain-of-
c-••;,-'; Ft.f E-S u] c b* user ej- e it :;"-:• " - - :?•.:=.'"
cf t e;7.:.r£te c-ftofv retrr.f frr Esr~?~~ rl~J J -~ JJ * t-1
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put more than one survey on the same custody sheet (example: Breiten-
stine, Hershberger 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 may be brought into the CRL; however, samples
nay 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:

1. The SMO Organics Traffic Report
2. The SMO Inorganics Traffic Report
3. The CRL Laboratory Sample Number
A. 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. Stick-On Label removed from the Traffic Report
*8. The Region V ESD Basic Data Form (for samples to CRL only)
*Required of TAT, Regional EPA and FIT personnel.

All samples (organic and Inorganic) are to be shipped via Federal
Express, Purolator, or Emery.

» d~ ~ j \ Charles Elly (or his designated alternative) should be notified
w ' ^
Pri°r 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-
pler to call the SMO or the NCL. This protocol oust 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 Sarpler must provide the following: (FIT is
exempted)

1. Check to cake certain tne stick-on labeils) froc the Organic ar.d.'or
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wlth the Custody Tag(s) and that the Custody Tag(s) coincide with
the CRL Sample Number(s) written on the Traffic Report sheets.

2. 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 Bent 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 PH, CDT).
The Sampler will have to make a copy if he/she desires one; all
other sheets must be enclosed with the samples.
Place the original Chain-of-Custody Form 6heet(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
#2, #3, #6, #8, #9, and #10 completed. Indicate under the "Remarks'
Section the assigned CRL Sample(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

]-f c::rce wide-mouthed, round, clear glass jar with screw-neck
::-..• &;,r teflon-lined cap (KER?. ACSD2 brand or equivalent;
• . f r --: VV" Srie-Mfic - Ciialo,: i;, . t i 69.-?t; ;; fillec
'- :v fc-:;,~r-r lull v.:' '.- £ ... -'.-,, }, l:.c c: ; rr •
PT; VF. MAXItfUM HOLDING TIKE: Not established ye'tT
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INORGANICS*
1-8 ounce wide-mouthed, round, clear plastic or glass jar with
Bcrew-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 distilled-deionized 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 duplicate(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
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Shipping

All medium samples (organics and inorganics) are to be shipped 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 via
Federal Express, Purolator, or Emery.

Samples should be packaged as described in the NEIC 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.

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, Boil, or sedi-
ment" .

'," ;:-.-: £!'] > (cr hit c'e <: 5 >• *•- t <.: t.':: c r:.--_ •. ive ) should be not 1 fie:!
~ • • , .:-:•.: tf tr.'. ££.-_: Vf, EM 7- v!!} cutset the SMO for EPA
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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 KCL. 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

ORGAN1CS 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 No.#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.
1. The SMO High Hazard Iraffic Rtjcrt (r.;: ;
v-M \,t doric &l the CF.I } >
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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 grans
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 Toxicity

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
Obtainable fron W
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2. The NE1C Hazardous Waste Sample Preparation Request
3. The CRL Sample Number
A. 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 hazard form must accompany all samples. This is
A) tf ~
V .> for an NEIC prepared reagent blank. Spike, matrix spike and duplicate
results will be added to the Sample Traffic 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.)

Charles Elly will contact Fred C. Hart Associates approximately
two (2) weeks in advance of each projected on-site sampling survey to
verify whether Rsrt Art: elates will accept the samples. The EPA, FIT
or TAT Sampler izc.s.'*_{-.:• : C ."* e_r_] e F E11 y__b c fore B h i pn e n t to D e r v e r.

Copiee of all the aforer.er.tinnfd items must be forwarded to Charles
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The turnaround time 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
"jtatus 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, CRL's 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 veil 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
h?.z-&rd soils, medium hazard concentration waters, etc.); National
L-'::ttory eac,:les were shipped tc ,'erf'cr KL7C); NEIC Traffic
Number, CRL Numbers, and projected date of return.
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/
G. Data Review - Figure 1
/
/
The NCL 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 prepares a sheet which includes the V1AR, 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 sheet is returned to Charles Elly, the
VIAR, SMO Coordinator. 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 Gilbert Frye, CRL Acting
Organic Section Chief, who assigns a GC/MS person to review the data.
Ms. Yvonne Flynn, CRL Toxic Substances Team Leader, Dr. Sukwha Kim and
Dr. Ray Liu currently serve as GC/MS data experts for the CRL. Inor-
ganic 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
•x
^ Team Leaders are scheduled for other duties.
(A
C Once the data have been reviewed by Organic and/or Inorganic Labor-
o. atory Section reviewers, it is returned to Charles Elly. If quality
^ control (QC) deficiencies or out-of-control audits were noted by the

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audits noted, are returned directly to Charles Elly for final revlev.
The Data Management Coordinator IB responsible for actual data trans-
mlttal to the data user. A xerox copy of the data is aade and attached
with a cover memo (Attachment 14) which notes QC violations, if any,
that affect the data.

QC flags are noted on Attachments #4 and 15 (for organic data only),
Attachment 15 is a draft of the "Regional Review of Uncontrolled Haz-
ardous Waste Site Contract Laboratory Data Package" and may be revised
to suit Regional needs. This review form is to be sent to the SMO when
QC problems requiring total rejection of organic data occur.

The following two Sections and Chapter II explains the criteria
and specific acceptance limits used by the CRL data reviewers.

H. Review of Organic Contractor Data

Until further notice, CRL personnel will use the attached "Instruc-
tional Guide for Reviewing Contractor Laboratory Generated GC/MS Data"
(Attachment 16) to review data. These criteria were based on what the
contract requires, as far as the contents of the data package, and the
limits allowed for each audit are concerned.

Blind audits will occasionally be sent to Contract Laboratories
by the CRL. Acceptance criteria for these samples will be determined
by the CRL QC Coordinator. Results of any blind audits will also be
sent to Dr. Eugene Meier, EMSL-Las Vegas, to aid in the monitoring of
Contract Laboratory performance.

I. Review of Inorganic Contractor Data

The following items are checked, by the CRL Inorganic reviewers,
and deficiencies and/or out-of-cor- trol audits are entered on Attachment
DATA SKIEi:- th:./: f ... ' • ^ ur, \\ ?. t • •'- t:.. i
detection limits should be listed with the instrument noted
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ALL Tasks: Results for each sample to two significant figures
List of detection limits used
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, Kg, Sn, Ag
*lnorganic Quality Assurance forn

TASK 3: a) Low concentration NH3, F, S, CM, pH and TOC results

b) Medium concentration NH^, S, and CN results
Inorganics Quality 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 be reported on the data sheets with the results.

4. INITIAL and CONTINUING CALIBRATION VERIFICATION should be reported
on the Inorganics Quality Assurance forms. Continuing calibration
verification should show no drift larger than +10%. If this drift
did occur, a new initial calibration curve must be included.

5. ICAP INTERFERENCE CHECKS should be run at the beginning, end, and
once every 20 samples. Results are recorded and labeled as "ICAP
Interference Check" on the Inorganics Quality Assurance form,
under Section II.

6. DUPLICATES should be recorded on the Inorganics Quality Assurance
form and not exceed the following limits for concentrations greater
than the detection limit:
1) TASK 1: RPD <20
2) TASK 2: RPD <50
3) TASK 3: RPD <50
7. MATRIX EFFECT SPIKES should be recorded on the Inorganic Quality
Assurance form and not exceed the limits listed in Table 3.
-------
UUt 3
tunux tnxz u OTDU
icr«
Kicktl
n
•0
iii

-------
II. QUALITY CONTROL AND TRANSMITTAL OF DATA

Data that has received QC flags (that render it useless to the
Data Requestor) is brought to the attention of Dr. Alfred Haeberer, EPA
Support Services Branch, and Dr. Eugene Meier, EMSL-Las Vegas. This
invalid data may be remedied by re-analysis or re-sampling and subse-
quent analysis by another laboratory. Continuing problems with parti-
cular 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
NCL data (Sections H & I) regardless of data user QC requirements.
Thomas Yeates, Region V DPO, is in the process of accummulating input
from data users as to the intended objective of the data. Some data
may not require as stringent QC 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 even though limits have been exceeded or de-
ficiencies 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, Region
V will insist that the samples be re-analyzed under the NCL. Unaccept-
able data will not be released to the data user. The data user will
be consulted, if needed, during the decision making process to deter-
mine the degree of QC needed to serve the data objective.

Once the data has bean judged acceptable or preliminary, the CRL
Dite K'rsfenert Coordinator puts the CRL 1st cumbers on all data sheets

-20-
-------
-21-
and makes a copy. Within 24 hours after review, the copy of the data
and Attachment 14 are «ent to the TAT, FIT or EPA data requestor. FIT
and TAT data are transmitted to Cindy Bachunas (Environment & Ecology)
through the mailbox in Thomas Yeates' office.

The entire review and transraittal of data should take no longer
than five (5) work days, after receipt by the CRL. Questions regarding
the status of data should be referred to Charles Elly, SMO Coordinator.
Questions regarding the quality of the data should be referred to Ms.
Marcia Ruehi, CRL Artrteg Qc Coordinator.
-------
• ' #
ATTACHMENT 11
PTV1SIOK gRVlCES

« *» «»•»«-!
the fell***
«rt:
Prlorltjr
U&edUte response or
y BD 1
euit«il«4.
« -
it leist two or three months froa request

Priority 4 - Projects that ~y be Dieted If tUe is .vaiUUe.
Priority « ^ Je^uested due d*te.

Oi.f or
.
,ft.r T.c.ipt of
.s
of "ours, increase tum.round ti« .ceordinjl) .
-------
Sims EKVKOK**™. «DTECT,OK AGENCY
Request For:
TO: project Objective:
Unit Specific Activity
Desired Coition D.t« -- Ufl Authc-rity
Phone
Principal Contact: -- - --
DBte:
Subject: Acknowledgment of Receipt of Work Request
From:
To:
ill do the above work (as specified) frit* .edifications).
T6rget Co.. Datel _BSD Project No. E.t. Cost
Phone
ESD Project Uader: ___ _ . —
Coetsaents:
-------
ATTACHMENT 12
SPECIAL ANALYTICAL SERVICES
-------
MENU OF
CONTACT LABORATORY ANALYTICAL PROGRAM
SPECIAL ANALYTICAL SERVICES PERFORMED"

1. Organic* and Inorganics Analyses - Fast Data Turnaround

„ - Added Capacity
2.

- Analyses for Particular or Specified
3. Compounds

« '- Analyse* at Low Detection Limits

5. Specific Task (Volatile Only, etc.) Analyses

6. Specific PCB Analyses

7. Inorganics "Wet Chemistry" Parameters Analyses

S. Tissue Sample Analyses

9. RCRA Analyses - Identify Characteristics oi Hazardous Waste

10. Fused SUica Capillary Column Analyses

11. Dioxin Analyses (Total and 2.3.7.HCDD)

12. Extracts Analyses

7cnher Special Analytical Services upon request.
-------
«-»—-«-• - —
SPECIAL ANALYTICAL SERVICES
A. Background

In addition to standardized types of analyses provided under the Contract
Laboratory Program, the Sample Analysis Program has established a system to
provide limited custom or Special Analytical Services (SAS) 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 quiCK turnaround analyses, verification analyses,
identification and quantification of non-priority pollutant compounds, general
waste characterizations, RCRA, Dioxin 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.
-------
I. Sampler/Source Initiation Procedures

The Special Analytical Services program is Initiated by the following
procedures.

*• User Request to the Sample Management Office • N
JyvJ^W*- '
To initiate a SAS, an authorized representative contacts the
Sample Management Office by telephone with a description of
sampling and analysis requirements. "Authorized user*1 refers to
an individual previously specified either directly or using proce-
dures established by the Sample Analysis Program Manager.
Information required by SMO to fulfill a SA.S request includes:

o Type of service (task)

o Definition and number oi "units" (includes sample, fraction,
etc.)

o Dates of sample collection, shipment and required data and
receipt.

o Exactly what type of report or data Is required (includes
what information, format, chain-ot-custody, etc.)

o Confirmation of analytical protocols required.

o Sampling personnel/telephone number if known.

.o Site/sample point information.

The Sc-Ttplinf c^yd.^.-'.r tSr-jlc' complete all pre-requesi re-
quirtrt.e-v. t i • •-:-*':1 %'Vich could Include
' • ative egreemtnu, p:c:t"t
-------
~~
T
i
i
i
i
Additionally, a wrinen request document should be forwarded to
SMO after the initial verbal contact.

b. Program Authorization and Protocol Confirmation

As the SAS program b an extension of 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, the Program Manager indicates the reasons lor
denial.

c. Pre-SampUnR Procedures

U 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 after 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.
-------
(3) The SAS sampling coordinator provides all sample and
tracking documents/instructions, etc. to sampling team
leader (communication with SMO if necessary). Sampling
takes place.

(«) Sampling team leader telephones SMO after sampling with
appropriate shipment information which includes:

o Date and time of shipment.
o Any changes in the sample numbers, types, etc. as
specified in the SAS.
o Numbers of gtfntainers, confirmation of sample ID num-
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 laboratory(ies) in accordance with established Program
procedures. SMO wilJ 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 for completeness,
deliverables completion within contractually-specified time per-
'iods, and adherence to all terms of subcontract.

b. The EPA Program Manager and Technical Officer are responsible
tor technical validation of the data results. The EPA QA/QC
Ofl.'Cf is respC'-.jlkk Ir t'"-'- vv',-" '• t'-.r Ercurery of t'*e c-:?'-*y
control data.
-------
c. While all validations (technical and administrative) are being
completed, the relevant data is forwarded to all appropriate
parties (source, EMSL il requested, etc.) SMO will keep a lile
copy for possible future recall.
-------
ATTACHMENT *3
ENVIRONMENTAL PROTECTION AGENCY
OFFICE Or ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
5?. EOX 252?7. DENVER fEDERM
DENVER. COLORADO 10725
Tom Yeates t»n February 10» 19B2
DPO. Region V

Rob Laidlaw
Evidence Audit Unit. NEIC

Chain-of -Custody
As per our earlier discussion, I am enclosing copies of sample tags end
chain-of-custody records filled out as an example of a hazardous waste
site Investigation. Also enclosed are 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 seunple was taken at one location, the records show
a difference of 70 feet. This is a very common type of documenta-
tion problem.

4. All blanks on tags end custody records should be filled out to t-;£
c>'tcrl ri'Silblc, This assorts tv,2t all necessary inforn:tic' "'-'•
, f .
L - w ,
er * s?~; ifcr er: n-:
-------
6. .Airline representatives or Federal Express agents do not need to
' sign the custody record. If a secured container 1s given to them
and a secured container 1s opened by the Ub custodian, then
custody has been maintained.

7. Method of shipment from the field to the laboratory should be
entered 1n the remarks box (see example).

8. Separate custody records must be prepared 1f samples are shipped to
two or more labs (see example, one custody record for a contract
lab and one for the NEIC regulated laboratory).

9. Field crews must retain a copy of all custody records. These
should be matched with laboratory copies once the files are assembled.

10. Recordkeeping should be done at the time of the work. Mistakes
occur If personnel try to reconstruct activities at the end of a
day.

Once the Investigation 1s complete and records are assembled, demon-
stration that custody has been maintained becomes a tracking function.
Each group that has collected samples (EPA or contractor) has the
responsibility to review the Information 1n their possession to determine
that:

1. All samples collected have been Identified and listed on a custody
record.

2. Custody can be traced from the time of collection until shipped.

3. The custody record shows where samples are shipped.

4. Field logbook entries are consistent with other documentation.

5. Analytical results are matched with field records to assure that
lab sample collected had data reported.
•
If this review Identifies custody problems, the Investigator should go
through the available records to see 1f custody can be reconstructed or
explained. Any unresolved problems should be brought to the attention
of the project manager and the case attorney.

Laboratory documentation must also be assembled and reviewed. Custody
records end analytical results should be matched with those from the
field to assure consistency and completeness. Laboratory records should
demonstrate that:

1. Samples were received secured.

2. Contents agreed with the custody record.

3. Custodian signs for receiving on custom re::"c

4. S£-;-Ui w^rc stored in a secure: t-:~.
-------
The situation you mentioned where many different groups participate in
sampling and analyses over a long period of time becomes difficult to
manage. However, 1f each group reviews and verifies integrity of informa-
tion they are responsible for. then consistency and completeness can be
achieved.

The review process and document tracking is time consuming but has often
paid off in satisfying our enforcement needs for producing records and
preparing cases. Records produced for litigation that have not been
reviewed can cause unexpected difficulties, and once the legal process
has begun, we may not have the luxury of time to prepare en effective
case record.

If I can be of further assistance, please feel free to call »e (FTS
234-4706).
Enclosures
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.(12/81).'
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M i i Monni.li i » t
' ' ' UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
-- #

DATE.

r-. Review of Region V Contractor Data; Received for Review on
Curtis Ross, Director
Central Regional Laboratory
1°. Data User:

Ve have reviewed the data for the following Case(s):
Site Kane: SM) Case Mo:
IPA Data Set No: Decision Unit:
CKLNo's:
SMD Traffic No.'B:
Contractor Lab:__ Ferscn-hours required for review;
Following are our findings:
( ) Data are acceptable for use.
( ) BatE ere unacceptable for use.
( } r-;t£ ere prelJrlnary - tMr CEEC h?f beer- forwarded to Dr. Alfred KrcVr;
II-. £upp:r: Services, fcr review - par-crr^, reply.
-------
Regional Review of Uncontrolled Hazardous Waste Site Contract

Laboratory Data Package
TO: O.S. Environmental Protection Agency
Sample Management Office
P.O. Box 818
Alexandria, Virginia 22313
The hard copied (Laboratory Name)
data package received at Region has been reviewed
and the quality assurance and performance data Buimarized. The
data reviewed included:

CASE NO. SAKPIZ
Contract No. requires that specific analytical work be
done and that associated reports be provided by the contractor to
the Regions, EKSL-LV, and SMO. The general criteria used to
determine the performance was based on examination of:

1. Data completeness 5. Duplicate analysis results
2. Spectra matching quality 6. Blank analysis results
3. Surrogate spike results 7. DFTPP and BFB performance
4. Matrix spike results

The results for each of the above groups are detailed within the
body of this memo.
-------
I. DATA CaTLCIENESS

A. Organics analysis data sheets -
B. Base/reutral - sample chronatograms -
C. Acid-sample chromatograms -
D. VDA - sample chromatoryrams -
E. Pesticide - sample chromatograms -
F. Sample spectra - priority pollutants and non-priority
pollutants - ._
G. Blank - ._
H. Duplicate analysis - one duplicate analysis of sample
was reported as required ty contract.
I. Spike data - ._
J. DFTPP criteria forms, spectra and listings - ,
K. BFB criteria forms, spectra and listings - ,
L. Base/neutral - standard reference spectra and chrcciato-
grams - ._
M. Acid-standard reference spectra and chromatograms -
K. \TOA-standard reference spectra and chronatograms -
O. Pesticide-standard chronatogram -
P. Base/neutral sensitivity test -
Q. Acid sensitivity test -
R. Tailing factor data -
-------
II. SPECTRA MATCHING

The spectra were examined and found to be of good matching
quality.

"The spectra were examined and found to be of poor Batching
quality due to:
Gormen ts:
III. SURROGATE SPIKES

The recoveries of surrogate spikes for each parameter group aid
sanple were evaluated. The average results for each parameter
in a number of sanples should.be:

Fraction Surrogate Low Limit High Limit Average
Volatile benzene-d6 70 130
Volatile toluene-d8 70 130
Acid phenol-
-------
JV. MKHIIX SPIKE RESULTS
Matrix Spike Results (MSR) for each parameter group were
evaluated. She parameters that were reported are listed below
along with the MSR guidelines and amount of spike added. A
double asterisk (**) indicates outliers.

... - HMKIX SPIKE RESULTS
Epifce
Added Low Bigh
(ng) Lijnit Lirdt Actual
Fraction Conpound
Volatile Chlorobenzene 60% 150%
Toluene 40% 190%
Benzene 70% 200%
«
Base/neutral 1,2,4-txichlorobenzene 50% 200%
Acenaphtene 35% 200%
2,4-dinitrotoluene 25% 200%
Di-n-butylphthalate 50% 180%
lyrene 50% 150%
N-nitrosodi-n-propylaniine 20% 100%
1,4-dichlorobenzene • 15% 200%

Acid Pentachlorophenol 40% 140%
Rienol 50% 200%
2-chlorophenol 40% 150%
p-chloro-m-cresol 40% 120%
4-nitrophenol 40% 200%

Pesticide Beptachlar 70% 150%
Aldrin 80% 150%
Dieldrin 85% 150%
V. DUPLICATE ANALYSIS RESUUS

The Relative Percent Difference (RPD) for each parameter group
was evaluated.
-------
She duplicate analysis RPD acceptance criteria should be:

Kaxjjrum acceptable
Fraction Percent Difference

Volatile 15%
Base/neutral ' —. . . .50%
' - Acid 40%

Ihe RPD's exceeding the maximum acceptable percent difference were:

Fraction Conpound Actual RPD

Volatile
Base/neutral
Acid
Each duplicate analysis was examined in reference to compounds
detected in each analysis. Those cornpounds which were not cannon
to each analysis for the duplicate sample are listed below.

Fraction Sanple No. Compound Concentration
VI. BLANK ANALYSIS RESULTS •

She blank analysis was reviewed. The contaminants in the blank
are listed below.

Fraction Compound Concentration
-------
VII. DFTPP and BFB PERFOFMANCE RESUUS

The DFTPP performance resets were reviewed and found to be within
the specified criteria.

--"--• The BFB performance results were reviewed and found to be within
the specified criteria.

performance result(B) wasA^ere reviewed and the
.
following abundances were found to fall outside the specified
criteria.

Contractor Required Actual
Conpound Designation n/e Abundance Abundance
She (BFB/tFTPP) performance results which were found
to be outside of the contractually required tuning requirements,
do not have an adverse technical iirpact on the data.

VIII. Chroiretography Checks

Tailing Factors

Acceptance Windows Actual

Benzidine Less than 3
Pentachlorophenol Less than 5
-------
IX. Standards

General shape of the total ion efrrornatogram

AC BA' VCA Pest.
," Peak Shape
Interferences
Background
Area Response
4-Nitrophenol
2,4-Dinitrophenol
Pentachlorophenol
Benzidine
Hexachlorocyclopentadien
Nitrobenzene
Isophorone
Dinitrotoluenes
Reviewere name:
FTS Telephone No.: "
Comercial Telephone No.:]
-------
Instructional Guide
for reviewing
Contractor laboratory Generated
GC-MS Data
-------
-1-
PURP06E

The application of these instructions vill aid in accomplishing
three major objectives:

1. So aid the Regions in determining the quality of -"•
contractor analytical data.

2. "To aid IKSL/LV in the reviewing of contract laboratory
performance.

3. To aid Headquarters in overseeing the overall program
eo that present and future contracts may be codified
to meet the needs of the Regions.

PTOODUCTION

The items listed on the following pages should be checked by
regional personnel during the review of organic contract data.
The criteria established under each item vere derived from the
Hazardous Waste Contract for OC screens and OC/MS Analyses for
Medium Level Samples, the User Guide to the Contract Laboratory
Sample Analyses Program, Methods 608, 624, and 625, and from
routine quality control and data reporting practices at the
Environmental Protection Agency Regions.

The data reviewer is requested to complete the attached data
review form according to the following instructions and submit one
copy to:

U.S. Environmental Protection Agency
Sanple Management Office
P.O. Box 818
MexanSrie, Virginia 22313
-------
Data Review Procedure
Introduction Page - The contractor analytical laboratory name,
case and sanple numbers and the applicable contract number should
JB Data Conpleteness - the checklist should be marked and items
absent should be noted. The reviewer should be aware that
contracts nay differ in requirements and deliverables.

If a required deliverable is emitted it should be
requested from Sanple Management Office (SMO).
•
The data package should include the results of each sample's
analysis, quality assurance information and hardcopy
documentation supporting the quantification of all compounds
identified. This report package should include those items
listed on the Data -Completeness sheet.

XI. Spectra Hatching Quality

The sarnie spectra should be oorpared to "raw" or
manually processed (background subtracted) spectra obtained
from the standards injected into the GC-MS system on same day
that the samples vere analyzed. Generally, the spectra win
be nearly identical if a match is present.

The appropriate statement on the form should be checked,
followed by reviewer comments.
-------
Spot check the mass spectra of the unknowns and check the
reasonableness (The major ions present in the library spectrum
are present in the unknown spectnn and are in the correct
proportions.) of the compounds identified. If it appears that
no data review was done by the contractor then the following
criteria say be used to evaluate the scan data.
~"~ ' "* _. 4- • _» . . . *.._.». _• i. ~~ ^
»
a) All ions present in the library spectrum at a relative
intensity greater than 10% (most abundant ion in the
spectrum equals 100%) Bust be in the baseline
subtracted sample spectrum.

b) The relative Intensities of the ions specified above
most agree within plus or minus 30% between the
library spectrum and the baseline subtracted sample
spectrum.

- c) Ions greater than 10% in the baseline subtracted
sample spectrum but not in the library spectrum trust
be accounted for.

d) Ions greater than 1% found in the baseline subtracted
sanple spectrum which exceed the molecular weight of
the identified conpound spectrum must be accounted
for.

fhe contractor should report the CAS number, conpound name,
and the estirated amount for each identification.
-------
HI. Surrogate Spites

The surrogate spike results for each fraction and for all
samples in a case are summed and averaged. The standard
deviation of these results is calculated and the suniroun and
values are listed.
The auditor should keep in mind that results averaging
less than the ndniroim criteria (or greater than 100%) nay
indicate a chrcmatographic interference or a problem vith the
sample natrix and nay not necessarily be indicative of poor
laboratory performance.
The surrogates percent recoveries should fal? within the
following ranges.

' VOA 70-130

B/N 40-120

Acids 30-100

IV. Matrix Spike Results

Hatrix spike analysis must be performed en one of each 20
samples analyzed or on -one of each Case, whichever is more
frequent or as otherwise specified. • The matrix spike
recoveries result from the addition of known amount of
pollutants to a sample. Analysis of the spike recoveries
yields a measure of extraction/concentration efficiency or
accuracy dependent upon the sample's being a real sample or a
blank.

The results should be recorded on the form along with the
amount of spike added.

The reviewer should verify that the spiked conpounds percent
recoveries fall within the acceptance windows set forth in the
table and record the actual values obtained.
-------
The average percent recoveries for each fraction should fall
within the following ranges:

_ VOft 7CHL30

B/tt 40-120

Acids 30-100

Pests. 70-130

V. Duplicate Analysis Results

The Relative Percent Difference (RPD) for each parameter
group should be evaluated. Duplicate sanple analyses must be
performed on a separate aliquot on one of each 20 field
sanples or on one of each Case or as specified in a contract,
whichever is more frequent.

The RPD's exceeding the maximum acceptable percent
difference should be recorded on the form.

Compounds which are not cctmcn to each analysis should
also be listed on the form.

VI. Blank Analysis Results

Reagent blank analysis must be performed once with every
20 "samples or whenever smples are extracted. A reagent blank
is generated by passing a clean matrix such as organics free
water through the entire analytical scheme.

If a priority pollutant is detected in the blank, the
blank value is utilized in the sample calculation.

Reagent blanks are used in all analyses to verify,
qualitatively, that no false positives will occur and
quantitatively, that concentrations are accurate and do not
reflect contamination.

The reviev«r should list the contaminants on the form.
-------
-e-
Ibr the priority pollutant data, verify that, the reported
values In the blank are less than 1/2 the minimum detection
limit for the compounds.

For the DC/MS Bean data, verify that the compounds found in
the blank are not reported as positive hits in the sample.
-"VII. '-TFTPP AND BFB Performance Results

The calibration procedure using decaQuorotriphenyl-
. pbosphine (DFTFP) and 4-bronofluoroben2ene (BFB) allows an
- - .- operator to evaluate the performance of: the GC column, the
Bangle enrichment device, the ion source, the ion detection
circuits, the analog-bo-digital converter, the data reduction
system and the data output system. The application of this
procedure enhances the overall quality of results emerging
from the systens in use. This procedure is very important to
the validation of data obtained through the use of the GC/HS
system.

A mass spectrometer which meets the criteria of these
tests will, in general, generate mass spectra of organic
compounds which are very similar, if not identical, to
reference spectra for identification of compounds.

Data generated by an improperly tuned BBSS spectrometer
nay require . special review in order to assess the
identification validity of each unknown using a standard
reference spectnsn.

The required 40ng injection of BFB and 50ng injection of
DFTPP is designed as an instrument detection limit test to
verify that a small amount of standard test material can be
chroftatographed by the GC/MS system, give an acceptable
spectrum and at the same time demonstrate a sufficiently low
background signal to allow correct interpretation of that
spectrum if the sample was an unknown.

The data rust be summarized in the data package. A bar graph
spectrum and a mass intensity printout from a background
subtracted spectrum should be provided for DFTFP and BFB.
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-7-
I

DFTPP KEY IONS AND ION ABUNDANCE CRITERIA

. - Ion Abundance Criteria
~S 30-60% of BBSS 198
. 68 less than 2% of mass 69
70 less than 2% of mass 69

127 40-60% of mass 198

197 less than 1% of ness 198
198 base peak, 100% relative
abundance
199 5-9% of mass 198

275 10-30% of mass 198

365 greater than 1% of mass
198

441 present but less than
mass 443
442 greater than 40% of mass
198
443 ~ 17-23% of mass 442
Table n
BFB KEY ION ABUNDANCE CRITERIA

Mass Ion Abundance Criteria

50 15 to 40% of mass 95
75 30 to 60% of mass 95
95 Base Peak, 100% Relative
Abundance
96 5 to 9% of mass 95
173 less than 1% of mass 95
174 greater than 50% of mass
95
175 5 to 9% of mass 95
176 70-90% of mass 95
177 5 to 9% of mass 95
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VIII.
CHECKS;
The toiling factor should be calculated as shown In Figure I.
tailing factor should not exceed 3 for benzidine and 5 for
pentachlorophenol .
TAILING FACTOR* =
/
Exarole calculation: Peak Height « DE » lOOnro
10% Peak Height « BD
Peak Width at 10% Peak Height - AC
• 23rrm

AB » llmra
BC •
12
Therefore: Sailing Factor 11 * 1.1
Figure 1 Tsilir>g factor calculation.
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-9-
JX. STANDftRIS;

The general shape of the total ion chromatograin (peak shape,
interferences, high background, etc.,) for the standard run is
reviewed to check the chrunatography.

The area response intensities of the confounds are checked
with a special enphasis en the hard to chromatograph confounds
}:''". (4-nitrophenol, 2,4 - dinitrophenol, pentachlorophenol,
benzidine hexacWorocyclopentadiene, nitrobenzene, isophorone
and the dinitrotoluenes). -. " ' .- .-

Verify that the contractor has completed Results of Standard
Analysis; and, verify that there was no significant drift
(+^ 20%) from the calibration curve using the calibration
conpounds listed in Table III.

TABI£ III

CALIBRATION OffiCK OOKPCXJNDS

Base/neutral Fraction Acid Fraction

aeenaphthene " ' p~chlorc»-*tv-cresol
l,4-dichloroben2ene ; 2,4-dichlorophenol
hexachlorobutadiene 2-nitrophenol
K-nitrosodiphenylandne phenol
di-n-octylphthalate pentachlorophenol
fluoranthene
ben2o(a)pryene

Volatile Fraction

1,1-dichloroethylene
chloroform
1,2-dichloropropane
toluene
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H4TF DUF
U.S. Environmental Protection Agenqfl
Region V, Library
230 South Dearborn Street
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•-">
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