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DRAFT
SECTION V
SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
25 Method Blank Analysis ,
25.1 Summary - A method blank for water samples is 100 mL of-reagent water
spiked with the SMC and carried through the entire analytical .scheme. A
method blank for soil/solid samples is 6 g of clean quartz sand spiked
with the SMC and carried through the enffire analytical scheme, '^method
blank for oil samples is 1 g of clean*sorn oil spiked with the SMC and
carried through the entire analytics,!- ischeme. Met&pd blanks shall be
carried through the entire analytical^procedure/ ;
NOTE: The Agency will provide the Labor£tg|ry .iriith further instructions
for the analysis of method blanks for wipe samples.
25.2 Frequency
A method blank analysis shJllixbej^ei^omed for each matrix type (water,
soil/solid, or oil) and with leach se'te^ofciSmriipILes., A set of samples is
defined as those samples from^oiae Batch t^psEt""are. Extracted and analyzed
on one instrument during a 24-M«ar analytical sequence.
' ",>.", ,'•",%
25.2.1 The method blank and aptl ^sociated samples shall be
analyzed in the same analfrtical sequence. If samples from a
batch :am analyzed in more than one analytical sequence, the
associated metliod blank must: also be analyzed in the same
analytical sequence. If a method blank extract is used up
because of multljjle analyses, the Laboratory shall
-Substitute an ,ia^.t^a(ie^t.f!blank in place of a method blank in
alt s^sequentivssalia-lpitllajalslisequences. The Laboratory shall
note:4lh|{&;3in the Batch Narrative and shall use the EPA
identiffeatlpii number as described in Exhibit B for this
instrument %|iank.
25 .2^L ~~v'''" An-"iaGp^^able method blank shall be analyzed before running
any samples within an analytical sequence.
When analysing highly contaminated samples using SFE disks
on more tha$ one manifold, the Laboratory should analyze one
method blanJc per extraction manifold. If an unacceptable
method blarik is analyzed and the contamination can be
isolated,Ja»;'a particular manifold, only samples extracted on
-libat maxt|£bld will have to be reextracted. If an
unaccepjfcable method blank is analyzed and only one method
blanfef'fi used, all samples from all manifolds shall be
reextracted at no additional expense to the Agency.
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DRAFT
25.2.4 Criteria for an acceptable method blank is defined in
paragraph 25.4.
25.2.5 If all field samples in a Batch are filtered, the associated
method blank shall also be filtered** If only a partial set
of samples in a Batch are filtered,'t3ben a separate method
blank shall be run through the filter,Extracted, and
analyzed. '= ?,
25.3 Procedure for Method Blank Preparation
25.3.1 Prepare the method blanks^at the frequency listed in
paragraph 25.2. :
25.3.2 Measure out 100 mL of reagent water'•?£or each water method
blank sample aliquot. !- * ;i
25.3.3 Soil/solid method blanks are 6 g ofiselean quartz sand.
f\.
25.3.4 Prepare water and.*soil/solid method blanks as described in
paragraph 14 ar; 15 depending on whether solvent or solid
phase extractions utilized*,^' ",-; ,;J-:
25.3.5 Spike 1.0 g of corn soil witsK 1.0 mL of SMC (0.5 /jg/mL) and
proceed with the pestlfcides>';procedure (paragraphs 16.3 -
16.5). :; ...
<\
25.3.6 Analyze, theypethod blank extracts. Calculate the results
accojr&ilig tcr ;p|ragraph 21. jl
, :-|=' ';),,;
25.4 Technical Acceptance Criteria,
25.4.1 A'ij.;attethod bli&Efl^iS%a3||rlP' analyzed within an acceptable
analytical sequence on a GC system meeting the initial
three-pbiiifeucalibration criteria (paragraph 8) or valid
calibratioiklsefeeck criteria (paragraph 9), and the PVS
;si, ; :«cceptance criteria (paragraph 10).
The SMtfciecovery criteria of 50-150 percent is advisory
only. T^ifjsSMC recovery in the method blank must, however,
be greatefcsjshan or equal to 20 percent and less than or
equal to 2W> percent.
The RTS fdc%the SMC in the method blank must be within ±1.0
:l .percent bebween the blank SMC RT and the mean SMC RT
=! calculated 'from the initial calibration.
"
25.4.4 The'•sisirget compounds or potential interferences in the
method blanks must have a response less than one-half the
D-53-PEST-Q 08/23/94
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DRAFT
response in the corresponding RRT window of the initial
calibration low concentration standards .
25.4.5 A method blank may contain a detectable but acceptable
concentration of a target compound (less than one -half the
response of the initial calibration j&tm , concentration
standard) . ; - " ••<
25.4.6 If all criteria are satisfied, the method blank: analysis is
acceptable and samples may be^analyzed. If the-iae&iod blank
is unacceptable, correctivepasction shall be taken and;, :an
acceptable method blank most be analyzed prior to analyzing
the associated samples . vf • ' '•
25.5 Corrective Action '^V ' .' , , •'-'
25.5.1 If a method blank does not meet the technical acceptance
criteria, the Contractor shall consider the analytical
system to be out of control. It is tile Contractor's
responsibility ^?,,eliminate method interferences caused by
contaminants ii'jSoJfwfepts, i/^eagents , cartridges, disks,
glassware, and other sample jEtoragevand processing hardware
that lead to discrete artifa£$b smM/ot,. elevated baselines in
gas chromatograms . | If contamination is a problem, the
Contractor shall investigate* the source of the
contamination, and appropriate corrective measures shall be
taken and documented before further sample analysis
proceed^ i
-------
DRAFT
perform corrective action which may include a new initial
calibration. DO NOT continue with sample analyses until the
SMC RTS is within ± 1.0 percent.
25.5.6 Any samples processed with a method.blank that is out of
control (i.e., does not meet any >sof K3je, .technical acceptance
criteria) shall be reextracted and/ or reanalyzed at no
additional expense to the Agency.
25.6 Documentation i >
Method blank results are reported on Borms QI-PEST and QVI-PEST.
Reporting requirements are listed in- Ixhibit B. j
26 Instrument Blank Analysis
26.1 Summary
' '^ t
An instrument blank is 1 mL of hexane spiked with5tO;^tL of SMC (5.0
fig/mL) . At least two acceptable instrument blanks sfeall be analyzed
within an analytical sequej^^^fKb^fo^ sample analyses and one
following sample analyses. /]' " ''S-?£>;,J - ,-,, !;
26.2 Frequency -;; ?,• "-'
s
An instrument blank shall be analyze4,?at least twice during the
analytical sequence to ensure that tibe instrument is free from potential
contaminants. The ^ates^nstrument &l«nk analysis shall be performed
after the initial|l±tree-^int calibratlfsn in the initial calibration
analytical seq^B^ce or as 'fee first analysis in a daily calibration
check analytical sequence; f&be second instrument blank analysis shall be
performed immediately befo^w',t|:hewPVS analysis. The Laboratory is
encouraged ta ij»^additigi^-§|ji^p^p^at blanks during the analytical
sequence, especraJ3,^,,when highly contaminated or complex samples are
analyzed. Instrumehi;Jbul«anks must be analyzed after analysis of samples
with high levels of target: compounds or interferents (see paragraph
26.5.6),. •£„,•• ..t ^>;:.
26.3 Procedure for InslTBttisajent Blank preparation
•• , <• .-- •*:*>••!•. ,-. * *•
;s/ '"
^Instrument blank iV4l mL of hexane spiked with 10 uL of SMC (5.0
m
i-; :•£
26.4
Concentract,iei«5,, of tb^ :=SMC and any target compounds in the instrument
blank are cai«pat^4? according to the procedures described in paragraph
21. Note: The tsiilget compound concentrations (detected concentrations
and CRQL values) in the instrument blank shall be reported in the
D-55-PEST-Q 08/23/94
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DRAFT
appropriate concentration units (e.g., report in /tg/L if the associated
samples are water and in ^g/Kg if the associated samples are soil).
26.5 Technical Acceptance Criteria
26.5.1 A minimum of two (2) instrument blariksrshall be analyzed
during an analytical sequence on &- GC system meeting the
initial three-point calibration criteria (paragraph 8) or
valid calibration check criteria (paragraph 9)/-'and the PVS
acceptance criteria (paragrajiit 10). ''"-',
26.5.2 The SMC RT in the instrument blank must be within ±1.0
percent of the mean SMC R1S calculatecMsErom the initial
calibration. : , ^
26.5.3 The SMC recovery criterion 6^y50-3i50 percent is advisory
only. The SMC recovery in the "ttnstxument blank must,
however, be greater than or equal'•%<> 2:0, percent and less
than or equal to 200 percent. , ';-
s^ ,
26.5.4 The target compj£»mits,w 'fjoteqtial interferences in the first
instrument blank (analyzid iameldiately.j after the initial
calibration or before a valii-calibration check) must have a
response less than *ase-half, iSae response in the
corresponding RRT windows &£'"the initial calibration low
level standards. % ""';
26.5.5 Subseqo^t juxstrument blaafess are acceptable with low level
contamination.fiiThese installment blanks may contain target
cong«*und conceiteations up 'tio/rtwice the CRQL (2x CRQL).
26.5.6 Ifotjiowing the i&^.ys,ts,,,of,,ra.,field sample containing high
i _±-»_ _^ .—j-^.i||3»an the field samples run after a high level
iA- •'•:^ssjy\j^ must be'-iftijiiefully evaluated for carryover. The field
/H'•'•""' sampiie immediately proceeding the high level sample shall be
-:k~;J reanalyi^ifed, along with any other samples analyzed after the
#, '5-' high levelltsample which shows evidence of carryover.
,5.7 High level ispunples are defined as being field samples that
,'-|k=, contain ta^gjet compounds at concentration levels that exceed
^'i-ii' ;, twice the li|gh level initial calibration standard
^ ,| ;,;,, concentratltlm and/or interf erents that are detected at
4*l>esyels greater than the mid level initial calibration
response of the nearest target compound.
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DRAFT
26.6 Corrective Action
26.6.1 All groups of samples analyzed shall.be bracketed with two
acceptable instrument blanks. If ellfher instrument blank is
unacceptable, corrective action shall be taken and all
samples not bracketed by two valid 'iastxument blanks shall
be reanalyzed at no additional expense to t£ie Agency. ,
26.6.2 If the response of any target compound in an instrument
blank analyzed after the initial calibration or "before a
valid calibration check statidard is greater than or^tequal to
one-half the response in £he corresponding RRT window of the
initial calibration low ,e0ncentratiou!:ist:andard, corrective
action shall be performed and the system shall be
demonstrated to be clean by 'the analysis of additional
instrument blanks until all'itsEtget Compounds are within QC
limits. i\-
26.6.3 If any target compound in an instrumetifc'lalank analyzed after
field/QC sample analyses is greater than Cwo times the CRQL,
another instrum%nt|bliatac;;shall be analyzed. If on
reanalysis, coniaminationsscili exceeds criterion,
corrective action jslhall be psjblEorme&jifed the system
demonstrated to be iclean. then, all associated field/QC
samples analyzed since the: .last valid instrument blank or
method blank which contain those target compounds or
interferents found in ttofc instrument blank shall be rerun.
26.6.4 If an^'Sinstru&sat blank (otSktr than the first instrument
blank in the analytical sequence) contains target compounds
ojr,-"3Lnterferents:%etween one-Half response and two times the
CRQL, all posijfepre results, (results greater than or equal to
the CRQL) for-ailifeie scoapotmds in samples analyzed after the
last; ••^lld instrument blank shall be flagged with a "B".
26.6.5 Flag all ii^tanaoent blank results "S" if the instrument
SMC does*»psC£t .meet the advisory recovery of 50-150
If the iiSsf$rument blank SMC recovery is less than 20
percent, gif»ater than 200 percent, or if peak interferences
are presen^ sample analyses shall be stopped, corrective
action performed, and another instrument blank shall be
analyzed. ,f!;if the SMC RTS is still outside the criterion
.upon reaniptysis, corrective action which may include a new
> -1jaitiaL;!ejalibration shall be performed. All samples
'&i!a3|rz^9,>J5ince the last valid method or instrument blank
shall.: 1*1 reanalyzed after a valid instrument blank has been
demonstrated.
D-57-PEST-Q 08/23/94
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DRAFT
26.6.7 If the SMC RTS criterion is not met for an instrument blank,
sample analyses shall be stopped and another instrument
blank shall be analyzed. If the SMC RTS criterion is still
out on reanalysis , corrective action -which may include a new
initial calibration shall be perforated. DO NOT continue
with sample analyses until the RTS is *ithin ±1.0 percent.
26.6.8 Any samples not bracketed by valid instumeiit ^blanks or a
valid instrument blank and a method blank shaHqbe
reanalyzed at no additional expense to the Agency,' -r
26 . 7 Documentation ,jf
Instrument blank results are report^ ,pn Forms Qt^PEST and QVI-PEST.
Reporting requirements are listed ins!pihibit Ek,
27 Laboratory Control Samples > ,
27.1 Summary !.
The QTM pesticides LCS mix-|iapii;,ite£lt3^|:l.y .will be supplied to contractors
by the Agency. The LCS mixtiire wili^I'm^iift^Eget compounds at several
known concentrations . The Laboratory shall spSfce Sthe LCS mixture into a
clean matrix that is similar toS'fche samples being analyzed. The spiked
matrix shall be prepared and analyzed,, -iadsing the procedures described for
field samples . Analysis of the ICS atll! assess the performance of the
analytical system prior to analyzingJJfield samples.
'
,
NOTE : The Agency 'rtjS.I'i prosrjjpde the Labd^^tory with further instructions
for the ^a&lysis of t&s for wipe%samples .
27.2 Frequency
An LCS shall be analyzed once per matrix per analytical sequence (24
hours) per instrument;*?* The LCS shall be analyzed after the first
instrument blank in infey^l, calibration analytical sequence or after the
method >l«t^£hi3» -the daily' H^'tifaxation analytical sequence.
' '
_
27 .2i3i An LCS-^feill be analyzed with each:
,^= i?
-. if !
water field samples (LCS prepared from reagent
soil/solid field samples (LCS prepared with
quaf*pz sand); and
SJBt of oily field samples (LCS prepared with corn
D-58-PEST-Q 08/23/94
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DRAFT
27.2.2 The LCS shall be analyzed with all associated samples in the
same analytical sequence. If samples from a batch are
analyzed in more than one analytical -sequence, the
associated LCS shall be analyzed in >the same analytical
sequence. If an LCS extract is used; up because of multiple
analyses, the Laboratory shall use tibe 'original stock mix
diluted into hexane in place of the original LCS sample in
all subsequent analytical sequences. The Laboratory shall
prepare this solution by diluting 100 pL of ^dhfetLCS standard
mixture into 5 mL of hexane ^asd concentrating to 3. mL using
nitrogen blowdown. The LabCQSatory shall note this ^tiy the
Batch Narrative and shall ssltse the EPA identification number
as described in Exhibit B&or this LQS•,solution.
27.3 Procedure
Spike the appropriate matrix with the LCS Sljssaiard mixture and prepare
as follows:
27.3.1 Water LCS ,;, , ;
f>,>*:i"A ,3 „..-'( :,::\--~ .
27.3.1.1 Allow the^S mixti3O-«"Jf^tlfs r to, reach room
temperaturfe'Sbefore opening. '''-The!' -ampules must not be
opened until;;ipr;eparat:S!i»n/analysis is to occur.
Exercise care perform tfeie spiking to -ensure accuracy. Add the SMC
and mix 4&4. ?ar.|y .T-^1;011^^ t*ie extraction and clean-up
"-v ^^>rocess,Miga^b5l»^t^a.;"in paragraph 14 or 15, depending
>-^m- .whether solvent or solid phase extraction is
u£i!J£zed. Proceed with the analysis as described in
paragippfo 19 .
V- '-',% ' *''<-,*.£? f*
'-' ' "*{~; ' ' >';^- ^^
-El?v'3.!l":3 , - ,;'^c«Einal aqu%ot
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DRAFT
27.3.2 Soil LCS
27.3.2.1 Allow the LCS mixture ampules to reach room
temperature before opening. JEhe ampules must not be
opened until preparation/analysis is to occur.
Exercise care in breaking the aa|jules open to avoid
injury. /
27.3.2.2 Spike 6 g of quartz sand with 100 ^L o£Jt&e LCS
standard mixture as described in the instructions
provided with the LCS 'mixtures . Use syringes^tro
perform the sp iking. -Vbo' ensure accuracy. Add the SMC
and mix and carry --^fcrough the esttxaction and clean-up
process as described in paragraph 14. Proceed with
the analysis as described injparagraph 19 .
27 . 3 . 2 . 3 Nominal LCS target compound 'concentrations are as
follows : ; .
alpha - BHC ,,, , 41.7 /ig/Kg
ganmia-BBgb?i &, •,-£••-.•„ 31.7 fig/Kg
Heptachlo% '" * ' x< 4 ? f .7' j|g/XS
gamma -chlor&ane 4 -AO.O '
alpha -chlordaiae ;' 5.0
4, 4' -DDE " c ;• 5.0 Mg/Kg
4,4'-DDD ! 31.7
Endrin aldehyde ' 30.0
sulfate i , 36.7 fig/Kg
-\ 5.0 jig/Kg
{.,*•'" "-f M ,
27.3.3 Oil-'LCS -4,
This section haspHJt been};<^B8iib^$«d£^he LCS conposition and
concentrations for oils are currently being investigated.
27.3.3.1 Allow JtsbfifeLCS mixture ampules to reach room
_..,;;. .;-,; , , temperat^p&siiefore opening. The ampules must not be
v- '.,-'•"-- '-":; 4'. ;;i^p,ened unti^preparation/analysis is to occur.
Ecise care in breaking the ampules open to avoid
27.3.3.2 Spilapl g of corn oil with 1 mL of the LCS standard
as described in the instructions provided with
mixtures. Use syringes to perform the spiking
sure accuracy. Mix and carry through the
action and cleanup process adding 1.0 mL of SMC
|»5 jig/mL) and hexane and further prepare as
ascribed in paragraphs 16.3 to 16.5.
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DRAFT
27 . 3 . 3 . 3 Nominal LCS target compound concentrations are as
follows :
alpha-BHC 2500
gamma - BHC 1900 gg/Kg
Heptachlor 400 ii&f&g
gamma -chlordane 240(0 (Jg/J£g
alpha -chlordane 300 /*g/Kg
4, 4 '-DDE 300 fig/Kg
4,4' -ODD .; 1900 MS/Kg
Endrin aldehyde ? =• 1800 jig/Kg
Endosulfan sulfate »-; 2200 jjg/Kg
Endrin ketone > 300
27.4 Technical Acceptance Criteria ' : , ..:•
27 .U.I All LCS compounds must have recoveries between 30 and 130
percent. Up to two LCS compounds *Bay;, however, exceed the
upper recovery criterion of 130 percent,,
27.4.2 All LCS target,%oapou«^,r!abs,o,lute and relative retention
times must be v^ithin the Windows s established during the
• initial calibration. , ;; ' •' '", ;-,
27.4.3 The RT of the SMC must be, within ±1.0 percent of the mean
RT of the SMC established during the initial calibration.
27.4.4 The SMC; a<<$vi«Gry recovery criterion is 50-150 percent. The
SKC recovery' ^!£, ;the LCS musst, however, be greater than or
equal to 20 petcent and les£, than or equal to 200 percent.
27.5 Corrective Action
27.5.1 If anyjIsCS compound recovery is less than 30 percent or more
than twoQlip^ compounds exceed 130 percent, the LCS shall be
reanalyzed?*c If upon reanalysis, more than two LCS target
s! -';•" compounds are 4rtjifcside the recovery criterion, the LCS and
::,..'!•- alTsMSsSeciated fl^lsi and QC samples shall be reextracted and
/=> reanal^alesd. If one or two LCS compounds are outside the
•• "-.. f - , ;
/, i/ recovery'i^fraterion, proceed with sample analyses, and flag
,;?" all samplelar-esults of compounds that were out in the LCS
"£;' with an "ifrfflag.
•-IT---V ?'-'
27."Sk'2;r ; If the SMGfTecovery is less than 20 percent, greater than
" :, X, 200 percent, or if peak interferences are present in the
sample analyses shall be stopped and the LCS
:ed. If the LCS SMC recovery is still outside the
criterion upon reanalysis, corrective action shall be
performed and the LCS and all associated samples shall be
reextracted and reanalyzed.
D-61-PEST-Q 08/23/94
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DRAFT
27.5.3 If the RT or RRT for any LCS compound is not within the RT
and RRT windows established during the initial calibration,
reanalyze the LCS. If upon reanalysis ,a compound is still
outside the windows, a new initial calibration must be
performed before samples can be analyzed. The instrument
must be recalibrated as described-Iris paragraph 8.
27.5.4 If the SMC RTS criterion is not met for tl»| £CS, sample
analyses shall be stopped and the noneompliant liCS
reanalyzed. If the SMC RTS Jts still outside the^criterion
upon reanalysis, correctiveiaction which may include a new
initial calibration shall ie performed. DO NOT proceed with
sample analyses until thelSMC RTS is s&rithin ± 1.0 percent.
27.5.5 Any samples processed withl/an. LCS tfeftt is out of control
(i.e., does not meet any of^&x&z,tf'sStnical acceptance
criteria) shall be reextracted>an3/or reanalyzed at no
additional expense to the Agency. •• H -
27.6 Documentation
\:'-«.t!-~ '<-}'.... i
Laboratory Control Sample rlsi^ts" ar^'•feSpoBfced «aa ^"orrns QI-PEST, QII-
PEST, and QVI-PEST. Reporting 'requirements are lifted in Exhibit B.
D-62-PEST-Q 08/23/94
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DRAFT
COLUMN RESOLUTION CALCULATION
.a-
% Valley-x/y. 100
8:3O
9:40
B:5O
Time
tCfcOO
Figure 1
D-63-PEST-Q
08/23/94
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DRAFT
Table 1.
List of Pesticides Compounds in Order of Elution*
,
Compound Retention "T?inie (mins)
alpha-BHC 6.28
beta-BHC 6.98
gamma-BHC (Lindane) ," 7.20
delta-BHC :,;! 7.83
Heptachlor X 9.45
Aldrin , ,:' 10.53 .
Heptachlor epoxide 11.93
gamma-Chlordane •••• , 12.58
Endosulfan I , 12:97
alpha-Chlordane 13..08
p,p'-DDE/Dieldrin** 13.82
Endrin 14.48 :
Endosulfan II ., 14.77
p,p'-DDD ',-•:. ;-:-,: j^f ^ ... . 15.18
Endrin aldehyde".:, ' y'~' -., ^15.3B8, -
Endosulfan sulfate - 16.17 •
p,p'-DDT 16.43
Endrin ketone :; - 17.58
Methoxychlor ,-= :,< 18.35
Decachlorobiphenyl (SMC> 23.77
* This elution'^efeder is giveim ,as general guidance and is
based on suggeslfcefd instrumental operating conditions as
given in paragraph. ,7.,
** DIffi,,aJad dieldrin coelute on this column.
"; ! :f
Column: DB^5-,"S6egabore capillary column, 15 m x 0.53 mm I.D.
D-64-PEST-Q 08/23/94
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DRAFT
s -- ,-.,
QUICK TWAROUND MgtfiOM
ANALYTICAL METHOD FOR POLYCHLORl^TED SIIHENYLS (PCBs) AS AROCLORS
D-1-PCB-Q 08/23/94
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DRAFT
TABLE OF CONTENTS
PCBs AS AROCLORS
SECTION Page
I Introduction D-3
II Sample/Extract Storage and Turnaround Times
and Equipment and Standards :, D-4
1 Sample/Extract Storage and Turnaround Times ;";,. .D-4
2 Summary of Method ,i D-4
3 Interferences ,, D- 6
4 Apparatus and Materials »-.,[ D- 6
5 Reagents ,..; ,-., D-12
6 Standards I.,.,. .v'.' D-13
III Instrument Quality Control Procedures and Requirements D-16
7 Instrument Operating Conditions D-16
8 Calibration of the G^-$fjgg^|08i>T-,-Initial Calibration D-16
9 Calibration of the GC%£stem':- GilXbaration Check D-21
10 Calibration of the GC System - PVS^'.V. . D- 24
11 System Performance - GC 'l^solutioal D-28
IV Sample Analysis and Compound Identification and Quantitation D-31
12 Summary ,;,,,, »\ » ,'. D-31
13 Phase Separation.'! 4<-> ^ D-32
14 Solvent Extraction a^d*,,Cleanup. . .\, D-32
15 Solid Phase Extractiora^and Cleanup D-39
16 Samplejfreparation ai|i|?,Extraction - Oil Samples D-45
17 Sample Preparation <|o^|||^^s^t:i^m - Wipe Samples D-46
18 Instrumental; Analysis D-47
19 Dilutions.. ... S.* D-49
20 Identification of SNo^get Compounds D-50
21 Ca3asulatrions ,iii .» D- 52
22 ,|f^micki.Acceptance Cf!|iea:ia D-55
23 ; -Corrective Ac^on D-55
24<; Documentation, y^i D-56
V JS«mple Quality ControlflBrocedures and Requirements D-57
n *&, > '
25"- v'lfe.thod Blank Analysis D-57
26 *l$is*rument Blank^jAnalysis D-60
27 LaKoaasfcory Contfeol Samples D-63
D-2-PCB-Q 08/23/94
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DRAFT
SECTION I
INTRODUCTION
This Quick Turnaround Method (QTM) is designe4'.':for mse in determining
the concentration of polychlorinated biphenyls: (PCBs) as Aroclors in
water, soil/solid, oil, and wipe samples. The method *e$oires an
experienced PCB analyst to determine if an Aroclor pattern jksusts, then
calculate the PCB concentration on the basis of a specific Atxscjsor.
Exhibit C lists the Aroclor mixtures tbjtt will be used as a basis' »f
quantitation for this method along wit!r:±he Contract Required
Quantitation Limits (CRQLs). The method yields iltentification and
quantitation of the Aroclors listed '&&. Exhibit CUftsing single column gas
chromatography/electron capture deteefcorr,(GC/EJU) '•'. Aroclor
concentrations in samples are reported b&«& *2&- received" basis; no
dry weights are calculated. The primary Defective of this QTM is to
provide analytical data in a timely manner for decision- making during
Site Inspections, remediations , and emergency reacriwUfc. activities. The
PCB QTM is to be used when rapid data turnaround is required, when the
data requestor knows of (ol^FtabwS^S^pa^fcts) the presence of PCB
contamination, and when there sis knowle18^^r|f^r4ing potential matrix
interferences at the site. TKe QTM is n^fc -equivalent to, nor a
replacement for, the CLP Organtcs Multi^fedia Multi -Concentration
Analysis. ' :i " '•
The method specifies the use of sulfairic acid and potassium permanganate
to remove interferences,; hThe rigor otts cleanup significantly improves
method performances' for T*SBf. but makes 'like method unsuitable for the
analysis of orgfbjochlorine pesticides. "fSulfuric acid/permanganate
causes significant degradation of heptachlor, heptachlor epoxide,
dieldrin, en&pfai, endrin ai^et^yde,, endosulfan I, endosulfan II, and
endosulfan ' ~
The method is suitable i^for several multicomponent compounds, Aroclors
1016, 1221, 1232, 1242 ;' -.^4^, 1254, and 1260. These compounds produce a
complex.fpa.f±i^ra of overlap^»^tg ,GC peaks; multicomponent compounds are
quantiatalle'd on ^^Jje: -basis of majfer peaks within these patterns.
Sucgiessful use of tlilif; method requires an experienced staff for data
review, because weatfii|fcing or environmental partitioning can alter
jWLJlbicomponent patternsplin samples. This method can also be used for
ffbe analysis of toxaph(J|e if it is added to the initial calibration.
lleipaajse of the difficufjiy in measuring multicomponent pesticides,
tedh&jical chlordane sh^«ld be analyzed by the QTM pesticide method where
the maj^jr,- , Components , ^ technical chlordane (alpha -chlordane, gamma-
are quantitated as separated compounds.
D-3-PCB-Q 08/23/94
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DRAFT
SECTION II
SAMPLE/EXTRACT STORAGE AND TURNAROUND 2IHES
AND
EQUIPMENT AND STANDARDS ,:
1 Sample/Extract Storage and Turnaround Times , ;
1.1 Procedures for Sample Storage , ,
Samples shall be protected from lights^d refrigerated at 4°C (+ 2°C)
from the time of receipt until 60 days after delivery of a complete data
package to the Agency. ;;., :
1.2 Procedure for Sample Extract Storage v- .; /,;;
Sample extracts shall be protected from light ^nd stored at 4°C (± 2°C)
for 21 days after delivery of a complete data package to the Agency.
Samples, sample extracts, an&.,stariiSard£-. shall he stored separately.
1.3 Contract Required Sample Turnaround Times5 ;
,
Samples shall be extracted, analyzed, «ad a summary of the analytical
and QC data shall be reported to tfee>Aa|»propriate EPA Region via
telecommunications network within 4#|fiours (or 72 hours if more than
three fractions are ^analyzed) of Vali|i3a,ted Time of Sample Receipt
(VTSR) . See Exhibits A ''wad^B for specific instructions concerning
sample turnarounds time and'Siata reportiafp requirements .
': •' $**,
Summary of Method >i,
2.1 This analytical aetiiod is a GC/ECD method for the analysis of Aroclors
and toxaphene in wat«r> ^soil/solid, oil, and wipe samples. All target
compounds and the SystestClfQnitor Compound (SMC) shall be extracted from
field and j$G ^samples utill&lijg,, either solvent or solid phase extraction
fiiriiique^>,;':.lf solvent*^jaraction is utilized, field and QC
are seriaIM>sfextracted using two 10 mL portions of hexane (for
•'(.y- "•"•? s
samples) or hexane/acetone (for soil samples). If SPE is
lized, field and Q<3i|sainples are eluted through a disk containing a
matrix (e.g. silfpa) coated with a chemically bonded Cg or C^g
phase (or equi^fiilent) . The target compounds and SMC are then
the extrac^on disk with hexane.
'-•fc -- i
2.2 Sample ani&jrses shail^fae performed using gas chromatographic techniques
and shall be coBducftfeti within a contract-specified analytical sequence
that shall not''esas^ed 24 hours. PCBs are identified and quantitated as
Aroclors on the basis of retention time windows and calibration factors
established during initial calibration. During initial calibration,
D-4-PCB-Q 08/23/94
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DRAFT
relative retention times (RRTs), retention times (RTs), and
identification windows (± 0.005 RRT unit of the RRT or ± 1.0 percent of
the RT) are established for each quantitation peak for each low
concentration Aroclor standard.
2.3 Initial calibration consists of a single low.level, -.standard analysis of
target Aroclors and toxaphene except Arocloxss 1016 ~eej&, 1260 which will
be combined. A three-point calibration will^be perform4d-..with the
1016/1260 mixture to assess instrument linearity. Mean calibration
factors and percent relative standard deviations (%RSD) shall %e t
calculated for the calibration factors,^ all 1016/1260 quantitsalkon
peaks. The %RSD of the calibration faefcors for each quantitation peak
and the SMC must be less than or equal: to 25.0 parc«nt.
2.4 A check of the initial calibration shall be performed no less than every
24 hours, using the mid level concentratm«n offv&roclor 1016/1260 and
SMC. Calibration factors calculated from each .quantitation peak and the
SMC from this calibration check standard must"4fee'within ±35.0 percent
of the mean calibration factors established for each quantitation peak
during initial calibration.. .^.Identification windows sfiall also be
confirmed during the calibs»ti.06a\i^teck»:,,.
2.5 An analytical sequence also includes method blanks and instrument blanks
in which no quantitation peak earn be observed at concentrations greater
than one-half the response in the corresponding RRT window of the
. initial calibration low concentration ^standard. The analytical sequence
shall also include the analysis of "laboratory Control Samples (LCS) and
Performance Verification Standards (ff;SJ . The LCS will be a "go/no-go"
analysis. Thatfis,/ if feheJIL.CS meets performance criteria as stated in
paragraph 27, staple analyses, may procee4. If, however, the LCS does
not meet acceptance criteria,, corrective -action must be taken before
sample analyses, are perforaed,., ,,The ,PVS is two times the concentration
of the low Iev^-4j016/126fl^aagw*5«cfe|,'s and standarJgS,. The SMC is used as a retention time marker to
:e RRTs for tBap^identification of quantitation peaks and to
assess extraction efficiency. When the recovery of the SMC in a field
IS^mple is less than 10,>|iercent, greater than 200 percent, or if peak
'"1irt%xferences are present, absolute retention times are used for
qua^l^tation peak ideafpf ication. The SMC recovery criterion of 50-150
perceftfcj||&-!advisory $lil*y. Reanalyses of samples are not performed if
the SMC rewe^ry is,<^ttside the advisory recovery limts.
''•!.?•/'-, • «'
D-5-PCB-Q 08/23/94
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DRAFT
3.1
3.2
3.3
4.1
Interferences
A variety of chemicals extracted from environmental and waste samples
will produce ECD response and thus complicate the interpretation of
Aroclor patterns. Chemicals such as chlorophenols, organophosphorus
pesticides, aldrin, dieldrin, endosulfan (I aaadTslI-), and endosulfan
sulfate, which are normal PCB interferences aaee removed by the sulfuric
acid/permanganate cleanup in this method. Other organoeblorine
pesticides, particularly, DDT, ODD, and DDE should be removed by the
Florisil cartridge procedure. Chlorina£e",
Phthalate esters are common interfexefets encountered in PCB analyses.
Phthalate interferences may be minimtZiep^by ttoe^.iise of pesticide grade
or ultrapure reagents, thorough cleanup:'geli: ;glaeisware, and avoidance of
plastics materials in lab operations. The Isafeoratory shall use proper
caution to control phthalate contamination. ''•'-••'
, .demonstrated to be frefei'from contamination
method blanks. Cross-
instrument blanks
or other interferents
The analytical system must
under conditions of the a:
contamination problems sha
after samples with high
(see paragraph 26).
Apparatus and Materials ';': : ^
Brand names, suppliers^; and part nunfeeips are for illustrative purposes
only. No endorsement isxljpiied. Equivalent performance may be
achieved using|a|>paratus al^materials'giiier than those specified here;
however, demonstration of e|^tivalent performance meeting the
requirements/of this SOW i^Mhe^r^sjjqnsibility of the Contractor.
^ ' "*'.lgX'<':'>^£'241 '' -"«;>•" '•~'"ify *••* >'
'•-.!•.,i- K 4m9.*~^3i^;in:E•
Gas Chromatograp*h; «)>, The gas chromatography (GC) system shall be
capable of temperatti£eLf«:ogramming and flow control that is stable
throughout an analyticalJj|s^quence. The system shall be suitable for
splitles»s;«f on-,column inj^tion and have all required accessories,
inclutltiig' ifyriBg^s-i,-,analyticSir®olumns, and gases. All GC carrier gas
linelsr-Sshall be consifeutcted from stainless steel or copper tubing. Non-
pall^tetrafluoroethyifei^ (PTFE) thread sealants, or flow controllers with
rt&ber components shalltinot be used.
Gas Chromatograp^ Column - 15 m x 0.53 mm ID bonded phase
!-coated/|Siised silica capillary column (J&W DB:608, or DB-
Restek, ofeiaequivalent) is preferred, but a methyl silicone
.g. S^gtelco SPB-5, J&W DB-5, Restec, or equivalent) may
be substituted. A film thickness of 0.25 to 1.0 ftm is
recommeni
08/23/94
NOTE: The use of a guard column is recommended.
D-6-PCB-Q
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DRAFT
4.1.2 Chromatography Detector - The GC shall be equipped with an
electron capture detector (BCD) .
4.1.3 Gas Chromatography Injector - Cold (ambient) on-column injectors
that allow injection directly into 0.53 mm, ID column may be used
for this method as long as peaks are gauss ian, retention times
stable, and calibration check criteria 'tare
4.2 Data System - The GC shall be linked to a data system capable of
integrating peak areas for any compound detected at or above one-half
the CRQL. It is required that the Laboratory be equipped with a^PC- or
microcomputer-based GC data collection and reduction system for this
purpose. The Laboratory shall posses^ this equipment to provide the
quick turnaround of electronic data,,, -'The Laboratory shall also be
equipped with a microcomputer and contract specified hardware and
software to electronically transfer the QSIM data to the Regions.
4.3 Solid Phase Extraction Processing Station - As SEE is a developing area
in environmental chemistry, the EPA expects that Advances will occur
within the lifetime of the QTM contracts . Therefore:, ; the brand names
listed below are included ^cac',s'I^U%|ara;tipn purposes only. Any
comparable equipment is acc'eptableY^^arcftess, of. . brand.
t \>f- \ "•', " ?- ' ';f'
:i ' '
4.3.1 Extraction disks - Disks sfeall bfc made of Teflon and contain at
least 500 mg of C^g bonded silica (Varian/3M Empore", or
equivalent). Disks shall be :'47 ;mm in diameter. (Note: an
alternative |»basS«B1»ay be used if .this phase can be demonstrated to
meet the QA/QC '"reqmiSsements of tfcds method.)
4.3.2 Vacuum feeptder - The vaeuum holder will be glass and comprised of
five (3) ,J>arts : the •^seuum head, the sample reservoir, a metal
clip to-SlgLd the res§r^rol|r -tsp "*fie head, a large volume receiver
(greater tfcaa ,2,00 mL) for the sample after elution, and a small
volume receives* ;:,,i£its onto ttm^acuum head5.
4,?:|l'3 Vacuum manifold \sflJA 4-6 port vacuum manifold may be used to
d;l-; facilitate simultaneous disk extractions.
of depth fi^fekr (Whatman Multigrade GMF 150, or equivalent) or
materials- -^ach as Celite 545 (diatomaceous earth, Baker #,
or %sqila.valent^Laare encouraged when samples contain particulates.
If dep"t&":£i^,fcepfcs are utilized, each lot shall be tested for
contaminat^lpi /prior to use with this method. The depth filters
may be checked in conjunction with the SPE disks (depth filters
D-7-PCB-Q 08/23/94
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DRAFT
are placed on top of the SPE disks) by following the procedure
outlined in paragraph 4.3.5.
4.3.5 Solid Phase Extraction (SPE) Recovery Cheek
4.3.5.1 Summary "
Before field or QC samples are extracted using the SPE
disks, their efficiency shall be verifi«S., f An
extraction recovery anfl contamination checld shall be
performed in order to Devaluate the recovery df
compounds on the disk,; and to check for contamination.
;;••• -;
4.3.5.2 Frequency : !
''- -C '
A check shall be perfolbaed •&& each individual lot of
disks, and for every 300 tm|ts of a particular lot.
4.3.5.3 Procedure
4.3.5.3.1 "••-' j^eaafe Camples are extracted using a lot
'"?»; :of SPEsd£sfc;r of reage*jt| water spiked with 1 mL of the
{' ~\ high initial calibration 1016/1260
I",;'1 standard (to demonstrate adequate SPE
*• 4^3,5.3.2 The low and high SPE recovery check
: '•'"• standard solutions used to evaluate SPE
, '5'|, disks are prepared by diluting the
;>st; ^original 1016/1260 stock calibration
"5 .-., "'^dilution in methanol. The low and high
;? SPE recovery standard concentrations are
V| equivalent to the low and high calibration
I 1016/1260 standard mix concentrations
^"•'•i respectively. Laboratories shall prepare
,.:,; the SPE recovery check standards in
| f methanol and add one mL of each 1016/1260
,,,, calibration solution to 100 mL of reagent
y •' water. If the Laboratory experiences
solubility problems in preparing the SPE
recovery check standard solution, the
Laboratory shall prepare the SPE recovery
check standards in methanol, add one mL of
D-8-PCB-Q 08/23/94
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DRAFT
each calibration solution to 4 mL
methanol, and add the resulting solution
to 100 mL of reagent; water. The recovery
check samples shall be prepared and
analyzed according;,-to the procedures in
Section IV. '•: " .
4.3.5.3.3 The SPE recovery check standard solutions
shall be analyzed in a valid vinitial
calibration ;or daily calibration
analytical sequence (see paragraph ;3.8.1).
Note: if-the SPE recovery check standards
are the ionly sample^ .analyzed in the
analytical sequences, the method blank
shall bW'&seplacedSwith an instrument blank
and the £6$ sl»2,l;be prepared by diluting
100 fiL of LCS ,^eck mixture into 5 mL of
hexane and concefecating to ImL using
nitrogen blowdown. "'"llbeJEPA identification
for standards as;;klescribed in
.shall be used 'for the low and
" V;high '^PS''%s^Boi!rery
'< '"^
4 'The reco^ry of the c&eek compounds spiked at the
•tf upper limp: of the calibration range must demonstrate
,,,. -: recovery«elE,^3QsJJ,ft;,jpercent to establish that the SPE
••v'• floedia hSis^l^feiisapadtty to retain compounds at the
':?i3t|ji|*e,r end of the calibration range (i.e., no
btfe^t^birough of target compounds is occurring) . The
recoveag^Jcheck at the low concentration level shall be
<:JC;--.,\ ; v evaluate^|jo>!, ;- "" ~"- ':.'J3uc$a levels ''!$&&' does not introduce method
: "interferences. If any compound recovery is less than
SO^^ircent or greater than 110 percent, then that lot
of dffisks shall not be used.
4.3.5.5 Corrective Action
'
If jt&s disks do not exhibit acceptable recovery of any
spiked compound at the low or high concentration
J^rels, the entire lot shall not be used to extract
Isamples, since the system cannot be demonstrated to be
functioning at those levels.
D-9-PCB-Q • 08/23/94
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DRAFT
4.3.5.6 Documentation
All data and related documentation for the SPE
recovery check analysis shall Ise maintained by the
Laboratory during the term o-f ;'the contract and shall
be available to the Agency .Surixig-.on- site laboratory
evaluations or if requested. ;by the XPD or APO.
4.3.6 Extract Cleanup Cartridges - Florisil, 0.5 g solid' $hase glass
extraction cartridges with stainless steel or Teflon frits
(Analytichem Florisil PR, or equivalent) . Bake the glass ilorisil
cartridges at 140°C overnight te-activate (do not exceed 150°C).
4.3.6.1 Florisil Cartridge Check
Each lot number of Florisil -Cartridge must be tested
by the following procedure before the lot is used for
sample cleanup. Add 1.0 mL 6€;the Aroclor 1016/1260
mid point calibration standard >ta»"the top of a
prewashedf^J.;risil cartridge, and eltite it with 9 mL
of hexan«|| sli^yii^st'fcthe final volume to 1.0 mL and
analyze bjr;|SC/ECD .""'•s^8^r':tBctWB^y of each compound must
, be determin^i for evalaatrion-mai reporting purposes.
The lot of Ft»3Eisil cartridges is acceptable if the
Aroclors 1016 ^nd 1 £60 are recovered at 80-110 percent
and if no interfepceiices are detected.
4.3.6.2 J£he "fjfeQrisil cartridge performance check standard
isolutloai|shall be analyzed in a valid initial
calibrat^i or daily calibration analytical sequence
(see pardigfeaph 18.1). Note: if the florisil cartridge
performail^, checkeistandard is the only sample analyzed
::s;ir> the ^aiiyi.ytlica3.! sequence , the method blank shall be
•:.ed in Exhibit B shall be used for this
instilment blank and LCS.
Documentation
; ..All data and related documentation for the florisil
• j/asecovery check analysis shall be maintained by the
Laboratory during the term of the contract and shall
D-10-PCB-Q 08/23/94
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DRAFT
be available to the Agency during on-site laboratory
evaluations or if requested by the TPO or APO.
4.4 Glassware - Sufficient glassware to meet contract requirements shall be
reserved for exclusive use in support of this contract.
4.4.1 Erlenmeyer Flasks - 125 mL.
4.4.2 Beaker - 150 mL. ! ':
4.4.3 Concentrator tubes - 10 mL.r
4.4.4 Kimax concentrator tube (graduated) - 25 mL.
4.4.5 Graduated test tubes - graiaiua,ted from 1 to 10 mL.
4.4.6 Autosampler vials - appropriate for the GC system.
4.4.7 Centrifuge tubes - 40 mL. '
4.4.8 Wide-mouth centr:ii«ge ;$afee&,,(optional).
4.4.9 Powder funnel - 6vcn> <60°). .
4.4.10 Pasteur Pipets. ; >-i
4.4.11 20-mL screw-cap vials (fair sulfuric acid/permanganate
procedurel ;,;> •', ;
4.4.12 Si
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DRAFT
4.5.4 Microsyringe - 10-^L, 50-fiL, and 100-^tL.
4.5.5 Spatula - Stainless steel.
4.5.6 Hot plate stirrer.
4.5.7 Teflon coated magnets.
4.5.8 Glass wool. ., - , ;,
4.5.9 Vortex mixer .
4.5.10 Whatman #42 filter pape*.
4.5.11 Whatman vacuum holder.
4.5.12 Nitrogen blowdown apparatus .
4.5.13 Water bath. ; . ,
5 Reagents ;••', "'" '; "I , -. : , _
> ; .
5.1 Reagent water - Reagent water iss-;,.def ine4, .as water in which Aroclors or
potentially interfering compounds; do ise£ produce a signal greater than
one -half the response in the corresjjosi&ing RRT window of the initial
calibration low concentration standard. Reagent water shall be
generated by one of "tfeeifollowing methods .
,
5.1.1 Reagent ^ter may be ^generated by* pas sing tap water through a
carbon filter bed containing approximately 500 g of activated
carbor*;,{$algon Corp .:; 'ifeLl.tras.orb- 300, or equivalent).
-''"'• -':. • "•£' " ;1, ;,; ' - - -.?
j , .'»••••< ^ i i •>" ?-J\S ZS'-'*' ' f
5.1.2 Reagent watsfer-aaay be generated using a water purification system
(Millipore-O-FltiB with Organex Q cartridges, or equivalent).
5.1.3 Rejageat water may be prepared by boiling for 15 minutes then
^I>sift)"ling'-ci|>iit%minant-fr4fe !-inert gas through the water for one hour
/-jipwhile mainta'iafttllg the water temperature at 90°C. While still hot,
,{£,./ transfer the de^ssed water to a narrow-mouth screw- cap bottle,
;|;J seal with a TefUbtl- lined septum, and cap.
5.2 "^.I^ents - Hexane, mettottiol, acetone, and toluene. Pesticide quality,
or
.
5.3 Sodium hydroxide soMtion (0.5 N) .
•~- '• ^.-'
5.4 Sulfuric acid solistion (0.5 N) .
5.5 Concentrated sulfuric acid.
D-12-PCB-Q 08/23/94
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DRAFT
5.6 Powdered Anhydrous Sodium sulfate.
5 . 7 Hexane/acetone [ (50 : 50) (v/v) ] .
5.8 Potassium permanganate (5 percent aqueous solution).
5.9 5 : 100 methanol/water solution (methanol in water v/V) , ^
5.10 Corn oil. " ••'.'••
6 Standards -' - •'">
6.1 Stock Standard Solutions
& >'
' ', f- ~
Stock solutions may be prepared f rom IpuSle standard materials or
purchased as certified solutions. StandaJSd solutions shall be prepared
by dissolving pure standards in a suitable s^lyent in volumetric flasks.
When compound purity is assayed to be 96 percetst -^r greater, the weight
may be used without correction to calculate the dtoCientration of the
stock standard. Exhibit E, -Section V provides further directions for
preparing and verifying th^Vifftbgjd^p -j&f. .stock standard solutions.
6 . 3
6.2 Secondary Dilution Standards :; r
6.2.1 Using stock standard solutions, ,|f&*epare secondary dilution
standards in hexane. ,(";•"
6.2.2 Secondary diiw^b^a:;standards shaitl be stored at 4«C (± 2°C) with
minimal head^pace anS^ichecked ff^jaently for signs of degradation
or evaporation. Theilikjprocedures'iaije especially important just
prior to preparing calibration standards from them.
NOTE: Standards shall linot*' fee .S^tored in volumetric flasks,
especially ^li^a they are prepared with solvents with low boiling
points. ~?"-\
single low ^^tcentration standard mixture shall be prepared for
' each Aroclor an^g|toxaphene in hexane as specified in paragraph
6.3.2. A separa^, solution must be prepared for each
multicomponent mficiEure with the exception of Aroclors 1016 and
> 1260, which shal| i^e combined. The 1016/1260 mixture and the SMC
f:s|iall also be pri^ared at three concentration levels, the low
concentration, jifS concentration at 5 times the low concentration,
and '-t;b^, high oia^centration at 25-50 times the low level. The low
conceritr^t^n-|si;andard, as specified in paragraph 6.3.2, achieves
the sample ^extract compound concentrations equivalent to the
sample compound CRQLs as listed in Exhibit C. The high
D-13-PCB-Q 08/23/94
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DRAFT
concentration level shall be near the upper end of the linear
range .
6.3.2 Low Concentration Multicomponent Calibration Solutions
Multicomponent Concentration SMC " Concentration
Standard (ng/mL) ' -: (ng/mL)
Aroclor 1016/1260 100/100 Decachlorobiphenyl, , 20.0
Aroclor 1221 200 "Becachlorobiphenyl 20.0
Aroclor 1232 100 DecachloEoMphenyl 20.0
Aroclor 1242 100 - ; /Decachlorobiphenyl 20.0
Aroclor 1248 100 Decacfelorobiphenyl 20.0
Aroclor 1254 100 Decachlorobiphenyl 20.0
Toxaphene 500>;! ,,, ;. - .Decachlorobiphenyl 20.0
' ~" "' '
6.3.3 All standards shall be stored at 4?£ (± 2°C) in Teflon-sealed
glass bottles. Calibrations solutions shall be replaced after 6
months, or sooner, if comparison -with check standards indicates a
problem. b
6.4 Calibration Check Standard/;
The calibratiim^check is a -.daily one-point check of the Aroclor
1016/1260 initial calibration^ ,, .The mid level Aroclor 1016/1260 standard
used in the initial calihj&dfeexEis ";tfc#- calibration check standard. The
calibration check -slfcezulard shall be prepared in a volumetric flask and
diluted to final volisae^ith hexane.
'"*":* , -
6 . 5 System Mcsaitar Compound
' "" ' ' ' ''
(SMC) is decachlorobiphenyl. A stock
so|^it€ion of the SMC ijiacetone shall be prepared as described in
ps|fcagraph 6.1, and a spiking solution at a concentration of 2.0 jig/mL in
shall be prepacefjl from the stock solution. Each field and QC
must be spiked ^|th the SMC before analysis. Water samples (100
be spiked w||tf 10 jiL of the SMC. Soil/solid samples (6 g)
shall "^jlssaked with,40- /iL of the SMC. For oil analysis, prepare
decachlofcfeiflienyl f.trla concentration of 0.2 jtg/mL and add 1.0 mL of
this solutioni^al^ig-of oil sample (see Section IV.) The SMC is
employed to dete%t4Jshifts in retention time of eluting peaks.
Additionally, the SMC will be used to monitor the extraction efficiency.
D-14-PCB-Q 08/23/94
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DRAFT
Note: Reagent grade acetone shall be used to prepare the SMC stock and
working solutions. The Laboratory shall ensure that the acetone used to
prepare the SMC stock and working solutions is free of any
contamination .
6.6 Performance Verification Standard . , \
The Performance Verification Standard (PVS) shall be analyzed at least
once during each analytical sequence to assess system staibll^ty. The
PVS is two times the concentration of tip alow level Aroclor 3:t&l'6/1260
initial calibration standard.
6.7 Laboratory Control Sample
Laboratory Control Samples (LCS) conrteaiifcfcing known amounts of Aroclors
traceable to primary standards will inl!t3^11y?lbe supplied by the Agency.
Following receipt of these initial supplies-, liowever, the Laboratory
shall prepare its own LCS standards. The LCS^s'&ail be spiked into a
clean matrix and prepared using all steps of this^|fieotocol. An
appropriate amount of the LCS .shall be added to reageut water and
analyzed with each Batch o^swafces-- sastpi^s.^ An appropriate amount of the
LCS shall be added to clean "iffaartz skrii" .iapS 'analysed with each Batch of
soil/solid samples. An appropriate amount of!'the,fI&j5erck "sHsKOfitaJJ^d solutions^jsecondary standard solutions, and
•:4 ^working stand^pc^ solutions shall be stored at 4°C (± 2°C) in
3'i?' Teflon-lined s<§|pw-cap amber bottles (also see paragraph 6.3.3).
J&I&.2 All standards shi||l be protected from light.
6.&03..Samples, sample /extracts, and standards shall be stored
D-15-PCB-Q 08/23/94
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DRAFT
SECTION III
INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS
Instrument Operating Conditions
The following are the suggested gas chromatographic analyti&al
conditions. ^ ,'•;
Column: J&W DB-1701, DB-608 or DB-,5 (or equivalent), 15 m x 0.53 mm
ID, 0.25 to 1.0 (an film thickness fused silica capillary
column (FSCC). 5 -
Carrier Gas:
Flow Rate:
Injector Temperature: 205«C
Detector Temperature: 300°C
Initial Temperature: ..,», 140°C
Initial Hold Time: --|s>l; , -5: -1 min
Ramp Rate: '~&. *' •'•
Final Temperature:
Final Hold Time: <;
* Cold (ambient) on-column injectoirs -!fcbat allow injection directly into
0.53 mm ID column may be used for this method as long as peaks are
gaussian, retention-*itimes^are stable,? and calibration criteria are met.
NOTE: The typieal-:run time's&pader these conditions is 25 minutes. It may
be necessary d& 'adjust GC c^pditions on individual instruments to
optimize detection of ArocJ«!rstjpea.ks. It may also be necessary to
adjust detectt)ir-capnditioni|i^|j<^t3^^e instrument sensitivity.
8 Calibration of the GC ."System - Initial-Calibration
8.1 Summary -•• T. :- 3 ,,„
8. l^fJ-'-SPrior to ttie-ips^ilysis of samples and required blanks, each GC
'4f;/ system must be^^Dltially calibrated to ensure that the instrument
J:v* meets the minim^^performance requirements of the method. The
f^;" initial calibrat^n is accomplished by analyzing the low level
'* '-=1^-, Aroclor and toxagllene standards and the low, mid, and high level
*^;$h4li be used to establish the calibration factors used
for Aroclor gaantitati-°11 an<^ to define the retention time windows
for Aroclor identification. Additionally, the low, mid, and high
level 1016/1260 standards will be analyzed to assess instrument
D-16-PCB-Q 08/23/94
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DRAFT
linearity and to determine the mean SMC retention time for
evaluating SMC retention time shifts (RTS) during analyses. All
samples shall be analyzed during the contract specified 24-hour
analytical sequence.
8.1.2 Aroclor identification shall be based on matching patterns of
standards with peaks in samples and by RRT windows for 3-5 ,
quantitation peaks for each Aroclor. These RRT%iSdows will be
established from the low level initial calibration &£jft*dards and
must be used in all field samples .wifaere the SMC recovelcy tis
greater than or equal to 10 percetit and less than or equal -to 200
percent. ?
,'-if /-•
8.1.3 Aroclor identification shall ,b£Abased on gafttern recognition and
the absolute retention time windows established from the low level
initial calibration standards in^iail.fi^fl samples where the SMC
recovery is less than 10 percent, greikt«ix than 200 percent, or if
peak interferences are present. '"•••';
8.1.4 Shifts in the chromatojgraphic peaks shall be evaluated by
comparing the RT of €bfe.,^G;vfta.-all analyses with the mean RT of
the SMC calculated f roll th.e'i$l%$By&B -initial calibration
standards. The retention, time shJUSt'"is''r€f«cred to as RTS or
RT %D (see paragraph 21.4il,). Th£ltT of the SMC for field and QC
sample analyses must be witfein $3t:0 percent of the mean RT
calculated from the 1016/126Q,;itiftial calibration standards.
8.2 Frequency
8.2.1 An initiai-calibratilpishall be performed to determine Aroclor
patterns|l :RRT and RT Endows , calibration factors , and to assess
instrument linear ity-lufiAjnew, initial calibration is required
wheneveT^jlciailibratioiiil^fe-^^^i^Srds or performance verification
standards danzpt satisfy QC criteria. A new initial calibration
is also requiiped'-whenever major instrument maintenance has been
performed such asvcjegojLunm or detector replacement. An initial
calibration must be performed for each GC and for each
' " are used to perform these analyses.
'
An analytical sequence is a contractually-defined sequence of GC
analyses which c^psists of an initial calibration or a valid
calibration chec!^:: field samples, LCSs, method and instrument
blanks, PVSs, an|>-'6ther QC samples run within a 24-hour period
, j,s.ee paragraph l^Syfor the required sequence of samples).
8.2.3 Ana?iyMssof th«-'Initial calibration shall begin with the injection
of the^i^.lffrel 1016/1260 standard followed by the mid level and
low level''lpMf/1260 standards and the single point standards.
D-17-PCB-Q 08/23/94
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DRAFT
8.2.4 The analytical sequence concludes with an acceptable analysis of
an instrument blank and a PVS (see paragraph 10) .
8.2.5 Samples shall be analyzed only after meeting the technical
acceptance criteria for the initial cali&ration or a valid
calibration check standard. ; %,,
8.3 Procedure
8.3.1 The GC system shall be set up per,;tfee requirements of paragraph 7.
8.3.2 Prepare calibration standard soiufrions containing the SMC and
individual Aroclors using the procedure lisced in paragraph 6.3.
. > < • *'"' *
8.3.3 The calibration solutions shall -He,., equilibrated to ambient
temperature before injection (app£O£i3iaJ|gly one hour).
8.3.4 Inject between 1 and 5 /jL of each calibration standard. The same
injection volume shall be used for all calibrations and field/QC
sample analyses. -s>c.
8.4 Calculations "'; *-
8.4.1 The quantitation of Toxap&ene or,Jioclors must be accomplished by
comparing the heights or the areas of three to five major peaks of
the multicomponent compound iJiiatshe sample with the calibration
factors for the same peaks established during the initial
calibration ,,sequ*ia&e. The following table lists the number of
potential .^uantitatilon peaks f oEf-each Aroclor and Toxaphene.
Aroc 1 or/%$xaphene .^- "~ No. of Potential
4, ;,;1J ., .„„.,„,,,„.. Quantitation Peaks
1016/1260 ^ \ ™" "" * ""' 5/5
1221 'OV., 3
|||i-' 1242 '' ^|. 5
1248 p'1 5
4 ;f;' 5
, ;'i '•" 4
8.4.2 The choicfe*!ibS"the peaks used for multicomponent quantitation and
the recognition of those peaks may be complicated by the
D-18-PCB-Q 08/23/94
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DRAFT
environmental alteration of the Aroclors or Toxaphene and by the
presence of coeluting compounds and/or matrix interferences.
8.4.3 Calculate the calibration factor (ratio of the total peak area or
height to the mass injected) for each quai&itaticm peak in the
initial calibration standards and the SMC using equation .D.I (EQ.
D.I): /. ' .
Calibration Factor = Total ^ea °^ak °* Pea* Hei?ht "" ' - EQ. D.I
Mass--injected (ng)
8.4.4 Calculate the %RSD of the calibration faetoors of the low level,
mid level, and high level Aroclof' 3&L6/1J2£0 standard quantitation
peaks and the SMC for the initial caMbisation using the following
equation.
EQ. D.2
V- '*'"; • '\': ,, -,
%, ' ' *, ~
where: SD = standard deviation. .->
Standard deviation is calculated-using the following equation:
EQ. D.3
where: x^' •= individual calibration factor (per peak).
x = meatt >"sp£:'--|three initial calibration factors (per peak)
'"' 'if-' ;.-.<- -:munber of aa|i£bration s tandards.
Equation D.4 is;'^he general formula for the mean of a set of
values.
EQ. D. 4
D-19-PCB-Q 08/23/94
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DRAFT
where: X = mean of values.
X^ = value.
N — number of values. I-
8.4.5 Calculate the RRT for each target compound using the following
equation:
PT ' ' °
RRT = •'"eagpo.K.Bt., EQil'D.'S
8.4.6 Calculate the mean RRT and RT for each quaafcitation peak by using
equation D.4. -I--'
8.5 Technical Acceptance Criteria j ~
8.5.1 The %RSD of the calibration factors for eacti Aroclor 1016/1260
quantitation peak andft&e SMC in the initial calibration must be
less than or equal t
8.5.2 The RT of the SMC in the -standards gnust "be --within ±1.0 percent of
the mean SMC retention tisane calculated from the 1016/1260 initial
calibration standards. V
8.5.3 The peak resolution of Aroclor/,,1016 and 1260 must be evaluated in
the initial eaiilitation before 'proceeding with sample analyses
(see paragraph ' 11 5 . -' ^ '- ,
f- < i ' ,'
8.5.4 The chromatographic peaflc response for all quantitation peaks in
the loj? concentration >5s(t:andard must be greater than 10 percent of
full-scale *Jeflectisrur-jr t -• !
8.6 Corrective Action - :
."' "~\ "'
8.6.1 If ;'the SiRSD for any A3E*ciLor 1016/1260 quantitation peak or SMC in
Sitfee initfaif calibration •!« greater than 25.0 percent, the
*--- ;instrument has;:i«Jt demonstrated adequate linearity to be used for
;':,••' this method. SeJtrective action shall be taken and documented.
If the SMC RT is ^t within ±1.0 percent of the mean SMC
retention time casfcculated from the 1016/1260 initial calibration
'^standards, the Laboratory shall perform corrective action which
may ^include a new initial calibration. DO NOT proceed with sample
analysis ..until 'the RTS is within ±1.0 percent.
8.6.3 If the respbi|ise for any quantitation peak in the low concentration
standard is not greater than 10 percent of full-scale deflection,
the Laboratory shall perform corrective action and make
D-20-PCB-Q 08/23/94
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DRAFT
appropriate adjustments before sample analyses are started, to
ensure that all quantitation peak responses in the low
concentration standard are greater than 10 -percent of full-scale
deflection.
8.6.4 Corrective action may include optimizing'Isyste®. performance by
adjusting gas flows, replacing the GC injector-liner, column, or
the precolumn, or removing 0.5-1 m of the analytical column.
8.6.5 All initial calibration technical,«acceptance criteria s-hall be met
before any samples or required blsaks are analyzed. Any saifrples
or required blanks analyzed when -Sthe initial calibration criteria
have not been met shall require^tieanalysis ^"at no additional cost
to the Agency. = •';;
8.7 Documentation --;•'/ '*!<.>•-.
' -;, "' ' :"' -;-fc- •' -v
9.1 Summary '••• i *~ ' • '-•'••• '-,
A check of the initial calibration sequence shall be performed at the
beginning of every 24-hour analytical, ^sequence that includes field
sample analyses. This check of the;Initial calibration shall be
performed using the'l|t^tXbsvel Arocldr,11016/1260 standard. The percent
difference (%D) JieiCween 'elser^alibratioiarlfactor in the calibration check
standard and tibf^Kaverage calibration factor from the initial calibration
is calculated i?&r each quaiit;l1:ation peak and the SMC, and must meet the
technical acceptance criteii^.^lveA^in paragraph 9.5. The SMC RTS and
Aroclor peak re>s«skution nnlSti^Jigb''»6etf' - 'v ' ;-
^^,|1, Each GC used forgatoalysis shall be checked to verify the initial
1 ^calibration for|»ach twenty-four (24) hour period of operation.
TH^is .^procedure J$: to ensure that the instrument stability has been
maintained. 'j~
''''' ^ •"- ',
•- ,' \ Ay~
9.2.2 An analytical; ^sequence is a contractually-defined sequence of GC
analyses which consists of an initial calibration or a valid
calibration check standard, field samples, LCSs, method and
D-21-PCB-Q 08/23/94
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DRAFT
instrument blanks, PVSs, and other QC samples run within a 24-hour
period (paragraph 18).
9.2.3 The analytical sequence shall be concluded,.with an acceptable
analysis of an instrument blank and a FVS , >
9.3.3 The calibration check solution shall be eqmiJ&ibrated to ambient
temperature before injection (approximately one tiour).
9.3.4 Inject between 1 to fripL of tHe"iEi|leviel .,1016/1260 calibration
standard. The same inj«j(Stion volutes"shall &b used for all
calibrations and field/QGfsample analyses.
"-: _t 1 ;,'
9.4. Calculations
9.4.1 Calculate the•;fcafttferation factaaf ,(rat^° °f t^le total peak area or
height to the mass;injected) for «ach quantitation peak and the
SMC in t&e-'talibratrair.check standard analysis using the following
equation:; '-g ':
< - ''.-Js.,-,-,>«--.,,, .....
'>*''• ;.< •., ;; ;;f<" ' "^ -;'C t ^ . ,v\
";' J-?<. ~5;;^j'^;".g^, ~ ~?'"*n'%z-- Tfr\ T\ c*
calibration m*toz = Total Area of Peak or Peak Height EQ- D-6
? ,--. ,., Mass injected (ng)
D betweiw,.76he calibration factors from the
;,,,'fCalibration *<3Seck standard and the mean calibration factors from
~.' the initial calaabiration using the following equation. (NOTE: For
" the SMC, calcul^lp the %D between the calibration factor
calculated from 4jne calibration check and the mean calibration
r..s factor calculateitjfrom the 1016/1260 standards analyzed during the
' calibraton).
D-22-PCB-Q 08/23/94
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DRAFT
D-7
where: x - mean initial calibration factor for the
appropriate quant i tat ion peak,,
xc = calibration factor from current calibration
check standard .for the appropriate quaiatitation
peak. ' ;'
9.5 Technical Acceptance Criteria , : ,*•
9.5.1 The %D between the calibration factors for> each Aroclor 1016/1260
quantitation peak and SMC in the calibration check standard and
the mean calibration factor for the quantitation peaks or SMC in
the initial calibration must be within ±35,0 percent.
9.5.2 All Aroclor 1016/1260..calibration check standard compound
quantitation peak absolute;and relative retention times must be
within the windows es'tdfelishe'd: 'frim^?tAat''^a^f-calibration standard
during the initial calibration. Report calibration check RT and
RRT data on Form QIB-PCB^;see Exhibit B).
9.5.3 The retention time of the SMC in the calibration check standard
must be within ±1.0 percent of
-------
DRAFT
9.6.3 If the SMC RT is not within ±1.0 percent of the mean SMC RT
calculated from the Aroclor 1016/1260 initial calibration, the
calibration check standard shall be immediately reanalyzed. If
the RTS is still outside criterion upon reanalysis, corrective
action shall be performed, which may inclttfle a new initial
calibration. DO NOT proceed with sample.analyses until the SMC
RTS is within ± 1.0 percent. -K
9.6.4 If the peak resolution criterion is not met, the Laboratory must
perform corrective action and demonstrate adequate resoitrtiion
before samples can be analyzed (see paragraph 11). "<"
9.6.5 All calibration check technical:|acceptance criteria shall be met
before any samples or required Blanks are;,analyzed. Any samples
or required blanks analyzed whe&pt&e calibration check criteria
have not been met shall require reaijalystis at no additional cost
to the Agency. '•' -,;;,
9.7 Documentation
Calibration check standardj,r*i«$;j» jKee.jgeported on Forms QIB-PCB, QV-
PCB, and QVI-PCB. Reportingf^equire"mewfcss;jsr« listed in Exhibit B.
10 Performance Verification StandaM (PVSA '•
~€
10.1 Summary
A performance verification standard ItJPVS) shall be analyzed at the end
of every 24-hour!analytie&|:, sequence. ;i£he analysis of the PVS shall be
started within^M hours aftgtc the inject&on of the first initial
calibration standard or the'lfcnstrument blank analyzed before a valid
calibration, •;,' ,:-. ' \,,":;,,
e"TP$IS jtefst be anISgp&ed at the conclusion of the analytical
The PVSi!^^lysis shall be started within 24 hours after the
of the firlfepinitial calibration standard or the instrument
analyzed beforeXf|fvalid calibration check standard. If a
jligtfccessful PVS analysi^~as not obtained at the conclusion of the
"atpfpiftical sequence, ajji samples analyzed since the last successful PVS,
inililLjIl^calibration, ci^lvalid calibration check standard shall be
reinje'i^S'-.and reana^^ed in a valid analytical sequence at no
additional^^g^ense jjbvfaie Agency. The Laboratory is encouraged to run
additional PVS ^SEaaljSses during an analytical sequence to minimize unpaid
reanalyses. If -^-"^cceptable PVS is analyzed during an analytical
sequence, the Laboratory may continue to collect data under the current
calibration until the conclusion of the current 24-hour sequence. If at
D-24-PCB-Q 08/23/94
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DRAFT
any time an unsuccessful PVS analysis is made, the Laboratory shall stop
sample analysis and immediately reanalyze the PVS. Up to two injections
of the PVS may be used to satisfy the criteria. If on reanalysis the
PVS is still outside QC criteria, the Laboratory shall take corrective
action and recalibrate the GC (run a new initial calibration) prior to
reinitiating sample analyses. Recalibration wl.fl "begin a new analytical
sequence. ' ;
10.3 Procedure
10.3.1
10.3.2
10.3.3
10.3.4
The GC conditions shall be
analyzing samples.
same as those used for
The PVS is two times the ioncentration of the low level
Aroclor 1016/1260 standarxffrased in ttlie initial calibration
(see paragraphs 6.3 and 6.6). :
The PVS solution shall be equilibrated to ambient
temperature prior to injection (approximately one hour).
The same in
samples and sta
be used for all field and QC
PVS.
10.4 Calculations .. ^
'•; ,si „ :
The amount of Aroclor 1016/1260 and-,the SMC in the PVS shall be
calculated using the following equation.
Obseived=
-
w*T m
EQ. D.8
area or peak height of the appropriate PVS
'^',,quantitation peak or SMC.
where:
..,-, '."f&Pji -,~ measbLtsalibration factor established during the
,,;(,;;,'' :" •:-;-,-; , ; initi&i;,yealibration for the appropriate
! -V£-| quantisation peak. (NOTE: For the SMC
X'.-; calculation, use the mean calibration factor
'^calculated from the 1016/1260 initial
iealibration standards).
An ic«B|sa.ge amount (avenge amount observed) of the five quantitation
peaks' l&i^fcoth 1016 &$&' 1260 are then determined using the following
equation.' [V; ^ Y; \,
D-25-PCB-Q
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DRAFT
~X= V -^ EQ. D.9
ft *
where: X = mean concentration.
X^ = individual peak concentration.
N = number of quantitation peaks .
The amount recovered is calculated usis|j the following equation
Amount Recovered = *™*9* ^1* X 100 EQ. D. 10
(ncft
10 . 5 Technical Acceptance Criteria
10 . 5 . 1 All PVS target eoopounds must have a calculated recovery
(mean of the S^^attrilfca^iwa peaks) of 75-125 percent to
report data witftoiat flags.1"-:,- •_- - , , - ,
10.5.2 If recovery of a PVS;; compound is not within 75-125 percent
but still within an expanded recovery window of 50-150
percent, the associated ssaiaple analyses results shall be
flagged "P" (see paragragih 10.6).
10.5.3 All Areclor liQjljS/1260 compound quantitation peak absolute
andvj?elative retention times*»aist be within the windows
established froa^-the low calibration standard during the
initial calibration. Report PVS RT and RRT data on Form
(see ''
10.5.4 The SMC recovery criterion of 50-150 percent is advisory
only. Reana%sis of the PVS is not performed if the SMC
;. , jNeesevery is ou1^i.4e the advisory recovery limts . The SMC
„ -!/;s - ' reco^yy in the P^Srimust, however, be greater than or equal
... * to 20 peanut and less than or equal to 200 percent.
lfV5.5 The SMC RTf~fai the PVS must be within ±1.0 percent of the
"": J" mean SMC Rf-^alculated from the 1016/1260 initial
'• ^<-.°/s calibration-standards.
"''$-i-*i, ,!' ".
10.5.6 i*s i The peak/Resolution for Aroclor 1016 and 1260 must be
: esraluated^in the PVS before proceeding with sample analyses
('see-rgaragraph 11).
D-26-PCB-Q 08/23/94
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DRAFT
10.6 Corrective Action
10.6.1 If recovery of an Aroclor is not within 75-125 percent but
still within an expanded recovery witKiow of 50-150 percent,
flag the Aroclor "P" in all associated field sample results
generated since the last valid PVS,j iaaistial calibration or
valid calibration check standard: •' ,; ,
10.6.2 If either (or both) Aroclor in the PVS is outiMe the
expanded recovery range, thf .WS shall be reanalyze*!
immediately. If, on reana^sls, either (or both) Ar«clor is
still outside the expanded^recovery range, stop sample
analyses, perform corrective action,jron a new initial
calibration, and reanal^e, all samp Jabs run after the last
valid PVS, initial calibration or *Su.id calibration check
standard before proceeding with sample analyses.
10.6.3 If the RT or RRT for any Aroclor lOi^J.260 quantitation peak
is not within the RT and RRT windows ^isissblished from the
low calibration r'Sjtandard during the initial calibration,
reanalyze the iSH$> JB££i%9*ff9 £,?analysis a compound peak is
still outside tnf|v^indowsfs*^|H*w}il^j»al calibration must be
performed before samples can;be analyzed. The instrument
must be recalibratelfl ;-as described in paragraph 8. Reanalyze
all samples run after'.:^he,3Utet valid PVS, initial
calibration, or valid calibration check standard before
proceeding with sample analyses.
10.6.4 If tfcasL^MC RIPS.Criterion ispaot met for a PVS, sample
analyses shalpite. stopped aiidxthe noncompliant PVS
imiiediately reanalyzed. If the SMC RTS is still outside the
«xJ|terion uponjjtaaanal.ysatsj..jcorrective action shall be
peiifojnied, wbiMiiS^JgiiiiciiSle a new initial calibration. DO
NOT d^afcinue with sample analyses until the RTS is within ±
1.0 perce$,t;^,, Reanalyze all samples that were run between
the noncompliant; PVS and the last valid PVS, initial
;I ^-Calibration, or :iml,id calibration check standard before
,J '- "proo^iiing with s^sle analyses.
, .;!« ^ \^{
' •• ^..^
5 The SMC 3e«overy criterion of 50-150 percent is advisory-
only. The||aiC recovery in the PVS must, however, be greater
than or eq^il to 20 percent and less than or equal to 200
percent.
10.6.6':"-V. |i ,,If the F^^SMC recovery is less than 20 percent, greater
20(J^ercent, or if peak interferences are present, stop
perform corrective action, and immediately
reanalyze the noncompliant PVS. If the SMC recovery is
still but on reanalysis, perform corrective action and start
a new analytical sequence. All samples analyzed since the
D-27-PCB-Q 08/23/94
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DRAFT
last valid PVS, initial calibration, or valid calibration
check standard shall be reanalyzed within a valid analytical
sequence. j
10.6.7 If the peak resolution criterion is,:-tiot met, the Laboratory
shall perform corrective action andr-demonstrate adequate
resolution before samples can be^analyze*! (,see paragraph
ID. f ' -.-:
10.6.8 If all PVS criteria cannot bSkmet after having taken
corrective action, reanalyzes'(do not re-extract) the
associated field samples iti another valid analytical
sequence. If on reanalyzes all QC ssaiple criteria are met
and the PVS criteria still cannot bfs aet, then submit all
sample data from both sequences. The Laboratory shall
describe in the Batch narrat^^tdserproblems associated with
the PVS and how the field sample -matrix may have affected
the PVS analyses. If the Laboratory ij|jj?ys technical ^acceptance criteria are not met,
more, *B?equenb|ajaalysis of "flse PVS is recommended, especially
whelUnighly contaminated or?c«mplex samples are analyzed.
10.7 Documentation ' 4 •>;;,'.„-,,,.,, ,„.,,,,
Results of PVS ankjlyses are reported on Forms QIB-PCB, QIII-PCB, and
QVI-PCB. Reporting Requirements are listed in Exhibit B.
11 System EerfonaaTice - GC Reaol-ation
11.1
Ititation of Aroclcep'lB. is primarily accomplished using pattern
iognition and matchiiigftRTs and RRTs of quantitation peaks. Because
Llary columns are i|S£d, peak resolution is not usually a limitation
of %fati»,',omethod. The metticd does require an experienced PCS analyst to
make Ar%ft:®r identifis|iitions and to establish that no significant change
in Arocidr^|>at;terns^liis occurred whenever a calibration check standard
or PVS is ana^jj^eidxi^If a change in pattern is seen, identification and
quantitation is~siiw«rsely affected and the Laboratory shall recalibrate.
D-28-PCB-Q 08/23/94
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DRAFT
11.2 Frequency
11.2.1 Initial calibration - The peak resolution in the PCB pattern
for the low level Aroclor 1016/1260 standard shall be noted
by the analyst before proceeding with sample analyses.
11.2.2 Calibration check standard - The peak resolution for
Aroclors 1016 and 1260 shall be evaluated ' 'f »*.. each
calibration check standard. The analyst shall4establish
that the pattern has not changed before proceeding -irith
sample analyses . : ' -
11.2.3 Performance verification standard - The peak resolution for
Aroclors 1016 and 1260 rshall be evaluated for each PVS that
is analyzed in a. valid analytical .sequence. The analyst
shall establish that the pattern lias not changed before
proceeding with sample analyses. '«
11.3 Technical Acceptance Criteria
11.3.1 Any pair of adj^aet-j^aks.Jfully resolved in the low level
Aroclor 1016/12^.. iniHal-^ali^al&Qn standard must not
exceed 25 percent^valley in £he cMibr&tion check or
performance verification sta&dards.
11.4. Corrective Action . :
11.4.1 If the /AirocSor,, pattern changes and any pair of adjacent
ily^r^olved in thejiiow level Aroclor 1016/1260
calibration standard exceeds the 25 percent valley
crierion in tHe> calibration check, corrective action shall
be .performed. 4% ;;vali,d, calibration check must be
deatei«strated,^^^e.^r)lp|3a|fcial calibration shall be performed
and 'doewented before proceeding with sample analyses.
11.4.2 If the Aroetmrjifpattern changes and any pair of adjacent
jpe^ks fully re^oftsred in the low level Aroclor 1016/1260
4 " ;^nl:t$^xcalibratiGii6.standard exceeds the 25 percent valley
N1 criterlim -in the PVs , the PVS shall be immediately
t; reanalyze!^ If after reanalysis the PVS percent resolution
is still ojafcside criterion, corrective action shall be
performed and a valid calibration check demonstrated or new
initial calibration performed. Reanalyze all samples run
after the.|Last valid PVS, initial calibration, or a valid
' ;== . calibrators check standard before proceeding with sample
-ilaualyses; >-'*
'"''' •'• ; i~
11.4.3 LossV&£ i-column resolution (a higher percent valley) could
indicate injector contamination or column degradation;
therefore, injection port and/or column maintenance may be
D-29-PCB-Q 08/23/94
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DRAFT
required. Maintenance may include replacement of the
injector liner and/or removing 0.5-1 m of the column. If
these measures do not work, column replacement should be
considered. •
11.5 Documentation
Percent resolution results are reported on Forms QII-BCB, QIII-PCB,
and QV-PCB. Reporting requirements are listed in Exhibit |k
D-30-PCB-Q 08/23/94
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DRAFT
SECTION IV
SAMPLE ANALYSIS AROCLOR IDENTIFICATION AND QUANTITATION
12
12.1 This method is designed for use in the rapid analysis of
soil/solid, oil, and wipe samples for PGBs measured as Arocloxsv If,
upon inspection of a sample, the Contractor suspects that the saa^le is
not amenable to this method, contact tfee Regional TPO or the CLASS
contractor for instructions. For Sujierfund emergency removal actions,
contact the Regional TPO or the Hea&fuarters APO 'Jlor instructions. If,
for emergency response actions, the TfO'*»r APOsare not available,
contact the Regional On- Scene Coordinator ^{OSCj: for instructions. The
Laboratory must remember that it shall follow "the requirements in this
SOW without deviation.
12.2 Before samples or required b.ianks can be analyzed, t3te , instrument must
meet initial calibration orC-j^YsOLJIl ©alibration check standard and
column resolution technical" ;^ceptande''ei^t:eTcia^, ,All sample extracts,
required blanks, LCS, PVS, anct calibration staiidards shall be analyzed
under the same instrumental conditions abet shall be allowed to warm to
ambient temperature (approximately, one Kour) before preparation and
analysis. , ; .
12.3 The laboratory shaiil ;:p«tf<>rm sample extraction and cleanup of water
samples utilizing Either 'Solvent (paragraph 14) or solid phase
(paragraph 15) , l^traction %«& cleanup. \"lfoe laboratory must meet all
QA/QC requirements as stated/under this contract using either of these
extraction/ cleanup techniqiSeifL ,,S! Ttie .solvent extraction procedures are
recommended for,: the cleanup land extinction of all samples; however,
Aroclors SPE procedures for waters may be used if equivalency to the
solvent extraction piroeedures can be demonstrated by the Laboratory.
Solvent extraction and tsitesjaup procedures shall be used for non- aqueous
samples, <'•' '"••' •• " • ?? .,
r „:- -,,:< •:, >. v-- ^-
, V '^" -'-'•• ,,f: i;, - K
12.4 BlaBp^samples, such;^ trip blanks and field blanks, supplied by the
Rejgiion and included $£j3n a batch of field samples shall be prepared,
aajtlyzed, and reportediss water samples. Occasionally, a water QC
,$#nle (e.g., field anltitrip blanks) will be included with a batch of
<-ssamples . If the laboratory is not certain whether a water sample
associated with a batcji of soil samples is a QC sample, contact the
or the GEiisS contractor.
NOTE: If water",':1»$Lgaks provided by the Region, such as trip and field
blanks are inclti^&dl.in a batch of soil samples, the Laboratory is not
required to prepare and analyze an associated water method blank or a
water LCS.
D-31-PCB-Q 08/23/94
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DRAFT
12.5 If unusual or high concentration samples are received, see Exhibit D,
Appendix B for general guidance on screening and sample preparation.
13 Phase Separation
Multi-phasic samples shall be phase-separated ''£11120 ;their individual
phases. The phase separation techniques employed will vary according to
the types of samples received. Since it is impossible to know the
number and types of phases that will be present in a sampfleg'-the choice
of phase separation techniques is left tsa the professional ^Sgeaaent of
the analyst. Various techniques can be^femployed to separate tfbey/phases.
These include pipetting off liquid phases (decanting should not be
done), centrifuging to remove suspended solids, and use of spatulas to
remove solids (wooden tongue depressors work wellf). Whenever possible,
phase separation operations should be.::pone with disposable glassware.
The phases should be separated into glasls -cxrajpslners with teflon-lined
screw caps. This allows for storage and handling of the waste in a safe
manner. ',' «
13.1 Samples received containing multiple phases stien !as water, oil,
and soil/solid in the |same sample jar shall be "phase separated"
into individual phase'sft. "•""•i"-!.-"£-r^; '?/ .;;,
13.2 Each individual phase is;-itaken tteBtogh the procedure as a
subsample. Report analytical results for each sample phase.
Note: Each multi-phase sample! slsall be identified using the EPA
sample number convention for multi-phase samples as specified in
Exhibit B. .-: :;; g %
"'*% '•> • r.
'" - '' , ^ '
13.3 Do not aaalyze any pliise that represents less than 10 percent of
the total-:sample volisife..
13.4 In the -fallowing pi^^^B&,i--)f/^fe applicable, references to
"samples" explicitly mean "single phase units."
14 Solvent Extraction
14.1 Samp lelfareparat-ion "and Extraciii,^ - Water Samples
.
A ^d mL aqueous sam^i- is serially extracted using two 10 mL portions
efpiexane. Extractior!|^:\are performed in 125 mL Erlenmeyer flasks with a
stirring bar.s*|Dne gram of NaCl is added to the aqueous sample
after the finsfc hexane extracting solvent is added. Extracts
filtered|;;*fand dried through powdered anhydrous sodium
sulf ate; >«bad concentrated to a 1 mL volume using the nitrogen blowdown
procedure". If^Hom-AroctSrs extractables are removed from the extract with
sulfuric aciTd^?fW!£af»iuni permanganate, and florisil column clean-up
procedures. Fin43L extract volume is 1 mL.
14.1.1 Measure 100 mL of sample into a 125 mL Erlenmeyer flask.
D-32-PCB-Q 08/23/94
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DRAFT
14.1.2 Spike the sample with 10 pL of the SMC (2.0 ug/mL).
14.1.3 Add teflon stirring bar.
14.1.4 Add 10 mL of hexane.
14.1.5 Place the sample on magnetic stirring plate and stir for
three minutes. The stirring rate should be/^tefficient to
mix hexane throughout the sample. '.,
14.1.6 Add 1 gram of NaCl to sample during stirring and stir for an
additional 3 minutes. ":
14.1.7 Remove stir bar and allow ,aqueous and*hexane layers to
separate. ' ,
14.1.8 Transfer the hexane layer by pastemr pipet to a 25 mL
concentrator tube. ~,
14.1.9 Repeat steps 14**l»4 - 14.1.5 and 14.1.7 - 14.1.8. Combine
extracts. Dis-oard^iextract:ed aqueous sample.
14.1.10 Prepare a drying column by pltjgging; ttie bottom of a funnel
with glass wool and" adding approximately 15 grams of
powdered anhydrous sodium salfate. Pour extract through
funnel and collect in a -25 ML graduated concentrator tube.
Rinse the extract contaiiier with minimal volumes of hexane
and poar t3ir«Migh the funraeTL Rinse sodium sulfate twice
with minimal 'volumes of hexane.
; •• - :f,
14.1.11 CoEscentrate extract to approximately 1 mL using the
ftitarogen-blowdo^.,,,EXO,ced!tire in a 30«C water bath. To
minimize analyse?;:3.b;SS;:, occasionally rinse sides of
conceiitxatjor tube with hexane during the blowdown procedure.
Do not tetvesxtract go dry during concentration.
14.1.12,,,.-•;;' >fiSBQ»^ed to extr£te£<.«clean-up step (paragraph 14.3).
^>;, -, "i vy,u\ /<"x. ' ?• =
,/,;;» '" '"''-tv|;/:i_, • tf-
14.2 Sam|it* Preparation :^Eia Extraction - Soil/Solid Samples
gram sample of sofl^is mixed with powdered anhydrous sodium sulfate
, is serially extract!^ with a 20 mL and a 10 mL portion of
acetone (50:50)^sing an ultrasonic probe. Extracts are
combiaB<8^, filtered, ac^idried through powdered anhydrous sodium sulfate,
and coSleisit^rated withiltblvent exchange into hexane to a 1 mL volume
using thev'mS:r.pgen bi^wdown procedure. Non-Aroclors extractables are
removed from''-tfeerTex£fact with sulfuric acid, potassium permanganate, and
florisil column'^tslLean-up procedures. Final extract volume is 1 mL.
D-33-PCB-Q 08/23/94
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DRAFT
14.2.1 Decant and discard any water layer on a soil/solid sample.
Mix samples thoroughly, especially composited samples.
Discard any foreign objects such as sticks, leaves, and
rocks.
14.2.2 Weigh approximately 6 grams of a araf»r«s;sentative sample to
the nearest 0.1 g into a 150 mL beakerT
14.2.3 To the weighed sample add a sufficient amount of; powdered
anhydrous sodium sulfate to prepare a free f lowing mass upon
mixing. Mix well. ,,!' " *' < •-
14.2.4 Spike the sample with lO.ytt'of the SI4C (2.0 ug/mL) , mix
further. "~: ::;
14.2.5 Add 20 mL of hexane/acetone (£0; 5,0)
14.2.6 Sonicate at microtip maximum power? -caecl the sample during
sonication. The sonicator must be set for 50 percent pulse
action. SonicatejEor 3 minutes. The power output may have
to be adjustedffslu-^s^e;, that the sample extract does not
splash excessively'; any ^ig%€icaafc JLoss of sample during
sonication is notlfacceptable4 r XInseB--lCbe sonicator tip after
each sample extraction with% mL of hexane/acetone (50:50).
This rinse liquid shall be-combined with the sample extract.
14.2.7 Remove and collect solvent: layer in a 40 mL centrifuge tube.
14.2.8 Add 10, mil of li^iane/acetone ,(50:5°) and repeat steps 14.2.6
andC'£4.2.7.
14.2.9 Combine extra^ps^and^filter by gravity or vacuum filtration.
-transferring entire sample contents
to fuEibel and rinse with an additional 10 mL hexane/acetone
(50:50)v.,t «;
•v-14~2L9.1 Fo^^cavity filtration, prepare a
":" "•: VS:;, filtr^B^on/drying bed with Whatman #42 filter
!?,1? paper rilled with approximately 15 grams of
t*.v,i powdered anhydrous sodium sulfate in a 6 cm
\v%|powder funnel. Rinse sodium sulfate and
ifpfilterpaper with hexane/acetone (50:50) and
,;;,ijdiscard rinsate. With the filter and sodium
/j!|sulfate wetted, decant combined extracts through
,€5.;;A-'the packed funnel and collect in a 40 mL
;'-, , > centrifuge tube. Rinse the extract container
-~ i-.r,,,|f- with minimal volumes of hexane/acetone (50:50)
;: -' |! and pour through the funnel. Rinse
filter/sodium sulfate with 10 mL of
hexane/acetone (50:50).
D-34-PCB-Q 08/23/94
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DRAFT
14.2.9.2 For vacuum filtration use Whatman #42 filter
paper in a Buchner funnel. Pre-wet the paper
with the hexane/acetone £50:50) solvent and
discard rinsate. Transfer combined extracts
into funnel, apply vacusaa, and collect filtrate.
Rinse filter with an IjO-iiL^of hexane/acetone
(50:50). Pour filtered extacact through a powder
funnel plugged with glass wo6l-,aiad filled with
powdered anhydrous sodium sulfatfeiaiaid, collect in
a 40 mL centrifuge tube. Rinse the 'iext^r-act
container with pinimal volumes of hexane/aeetone
(50:50) and pour through the funnel. Rinse
sodium sulfate;with an additional 10 mL
hexane/acetcpe (50:50).jf
? ' \ : "^''
14.2.10 Concentrate extract to appraxlatatssly 25 mL using the
nitrogen-blowdown procedure in^a. i300C water bath. Transfer
extract concentrate to a 25 mL coticieiitrator tube and
concentrate further to approximately 18 «'S mL. Add 5 mL of
hexane to conceiijxator tube and mix vigor0«sly.
Reconcentrate <6^^pfHDaSiwately 1 mL. To minimize analyte
loss, occasionally rinse"-siSSes sd? centrifuge and
concentrator tubes s>with hexafte durii% ihe blowdown
procedure. Do not'.allow extract to go dry during
concentration. ;'•• ~> ,
14.2.11 Proceed to extract cleaii4ip step (paragraph 14.3).
14.3 Sulfuric Acid Cleatnip -> ~ \-,,
14.3.1 Using a syringe] • . _ , s .
14.3.6 If avSilean phase separation is achieved, proceed to step
14 . 3 .V.
D-35-PCB-Q 08/23/94
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DRAFT
14.3.7 If the hexane layer is colored or the emulsion persists for
several minutes, remove the sulfuric acid layer from the
vial and dispose of it properly. Add another 5 mL of the
clean concentrated sulfuric acid.
NOTE: Do not remove any hexane at: this stage of the
procedure.
14.3.8 Vortex the sample and allow the phases to separate.
14.3.9 Transfer the hexane layer to'a clean 20-mL vial. : ;
-s
14.3.10 Add an additional 1 mL oJr'lhexane to the sulfuric acid layer,
cap and shake. This second extraction is done to ensure
quantitative transfer oifrdphfe. Aroclots and Toxaphene.
'"•- \ * , v'
14.3.11 Remove the second hexane layer and combine with the hexane
from step 14.3.9. :
14.3.12 Add 1 mL of reayge^t water to the combine*! feexane extracts to
remove excess -Spkisiricvaicid .that may still he present.
14.3.13 Vortex and allow ^Hte phases Mo -'separate ''.
* ±. -^?r ' -
14 . 3 . 14 Transfer the hexane iayer ;fco a clean 20 -mL vial .
, f: :
14.3.15 If a water layer is evSidtent in the eluate, remove by the
additi
-------
DRAFT
14.4.2 CAUTION: Make sure that there is no exothermic reaction nor
evolution of gas prior to proceeding.
14.4.3 Cap the vial tightly and vortex for 1 minute. A vortex must
be visible in the vial.
14.4.4 CAUTION: Stop the vortexing immediately if the vial leaks.
AVOID SKIN CONTACT; POTASSIUM PERMANGANATE BURNS.
14.4.5 Allow the phases to separate sf or at least 1 minute. s Examine
the top (hexane) layer, it ;ssTiould not be highly colored nor
should it have a visible eaulsion or cloudiness.
;
14.4.6 If a clean phase separation is achieved proceed to step
14.4.9. ' '"'
14.4.7 If the hexane layer is colored or-t^fcie emulsion persists for
several minutes, remove the permanganate solution from the
vial with a glass pipet and dispose of *4&, properly. Add
another 5 mL oftaeiean aqueous permanganate; -solution.
,''»• '" !";,-*
NOTE: Do not resaove any'ttessaiae ••-afc -*;his, stage of the
procedure. ? .: ! '"'
14.4.8 Vortex the sample and allow the phases to separate.
14.4.9 Transfer the hexane layer to a clean 20 -mL vial.
14.4.10 Add ,311" additional 1 mL of ttexane to the permanganate layer,
ca£>j£he vial securely and s&ake. This second extraction is
dojoe to ensure Jej: '|,; , „. ,, ...
14.4.11 Remove the second hexane layer and combine with the hexane
from step;,';34-.4.9.
14.5 FlorisiJ, r©B«iprldge Proceduife; '.
14. 5s,.! Reduce^^fifefe volume of the combined hexane layers to 1.0 mL
^=t* under a stream of dry nitrogen.
"|&i,5.2 Attach thefH&c Elute vacuum manifold to a water aspirator or
'^fft -•; vacuum pumg;.1with a trap installed between the manifold on
' '--v/J,,- the vacuum*. ^Source. Adjust the vacuum pressure in the
'^ =', ^manifold/tai' between 5 and 10 pounds of vacuum.
"':; .$•• j':;
14.5.3 Pl«c«s;«»e Florisil cartridge into the vacuum manifold for
each-sample extract.
D-37-PCB-Q 08/23/94
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DRAFT
14.5.4 Prior to cleanup of samples, the cartridge must be washed
with hexane. This is accomplished by placing the cartridge
in the vacuum manifold pulling a. vacuum and passing 5 mL of
the hexane solution through the cartridge. While the
cartridges are being washed, adjustSfhe vacuum applied to
each cartridge so that it is appr'
f'.. •• \ ~\
14.5.6 After the volumetric flasks are-, ini place, vacuum to the
manifold is restored and the extract: sfor each field and QC
sample solution is transferred to thef,tap frit of the
appropriate Flq^sil cartridge.
:<•>':•-„
14.5.7 The PCBs in theV^tract etteciepfcrAtres-.sare then eluted through
the column with 95:JffiL of hexaaei-and'cbllsected into the 10 mL
volumetric flasks liB&d in tfefe rack inside of the vacuum
manifold. 's .-*'?*
14.5.8 Transfer the eluate in each volumetric flask to a clean
centri;:R%e'|t3ibe or 10 mLVial. Use two additional 1 mL
hexaaai| rinsesl8«^ the flask:*fao ensure quantitative transfer
ofjtbe cartridgfe seluate. '~K,
14.5.9 Concentrate thf^do^ititp^,,to a 1.0 mL volume using either
nitrijgen blow^»iBa,l^:''S|pU?»tf,"Snyder column. Measure the final
volume iwith a clean syringe or by transferring the extract
to a cleaa?'SEolumetric flask.
' % %
14.5.10 .,« "'If; crystals of%ap£fur are evident or the presence of sulfur
,Th ! Is %S3Bfiected, proved to paragraph 14.6. Sample analyses
r f showiri|^|||ie presence of sulfur are not acceptable and must
.';?- be reanalpsed after sulfur removal.
i5.11 If sulfur IB,not expected to be a problem, transfer the 1.0
;!>, mL of samplpe;.: to a GC vial and label the vial. The extract
'xir:;, ., is ready fjjj£ GC/ECD analysis; proceed to paragraph 18.
\|i; HE, Store thetjextracts at 4°C (± 2°C) in the dark until analyses
'••f «r-e perfoianed.
'<*._,-j^ ^j:t-
14.6 Sulfur Removal '-:-<; ''•"•*
D-38-PCB-Q 08/23/94
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DRAFT
14.6.1 Bright (unoxidized) granular copper is used to remove sulfur
contamination. Add one to three granules of copper to each
hexane extract in a clean vial. Tighten the top on the vial
and shake for 30 seconds. Filter or)centrifuge and then
decant the solution to remove all solid precipitates. If
copper appears bright, go to paragraph 18. If copper
changes color, repeat sulfur removal as necessary.
14.6.2 If only a partial set of the samples in the Battels- require
sulfur cleanup, an additional- reagent blank of hexane spiked
with the appropriate amountf'of the SMC solution and':<£Leaned
with the copper is required.
14.6.3 Proceed to paragraph 18 .tor GC/ECD analysis.
15 Solid Phase Extraction and Cleanup of Water Samples
Solid Phase Extraction using nonpolar Cg (or equivalent) or C^g disks
may be used to extract water samples (Note: an alternative phase may be
used if the new phase can be:; demonstrated to meet the'KJA/QC requirements
of this method.) An additi«ndl.-^li.t«r 4i?H *-s required when water
samples contain particulates?;; Upon'o'peiiiB^ tUT'.package of disks, they
shall be used immediately or 'stared in aJdesiccator, (over Drierite, or
equivalent). For reproducible extraction efficiencies, all directions
given below shall be followed as closely as possible. Note: The
laboratory shall not use SPE for non,~agueous samples.
15.1 Sample Filtration -T : •: '•':-•,., '•
£ ,< -- " - % <-' '">:• s s
-•:%,* ..{,-
All water samples shall be ifiltered. When disk extractions are performed
the filtratiojsrsstep may be iioabined with the extraction by placing a
filter disk ,4el»igned to fi^M^ide..,tfhe.. neck of the sample reservoir and
proceeding wiiili'.iiise water y&ap&gcl&aii&p and extraction as specified in
paragraphs 15.2 '-a,3
15.2 Sample Preparation -
CRQDfc|pte the same as the solvent extracted
'^sample CRQLs-•«£(' 'ftated in Exhibit C.
^-82.1 Pour 100 mfp«f water sample into a clean erlenmeyer flask,
f;:: fleaker beater, separatory funnel, or any other suitable
*"'*»- ?\ •', mixing chan&er.
'*-+i%... -7!
15.2.T' \|r; .Adjust thg^pH of the sample to 5.0 - 7.0 using 0.5 N sodium
'X-:;jbydroxidi|>
-------
DRAFT
15.2.5 Shake sample vigorously to mix thoroughly.
15.2.6 Proceed with sample cleanup and extraction utilizing SPE
disk procedures (paragraphs 15.3 - 15.'5).
15.3 Disk Set-up and Conditioning \
15.3.1 Place the disk onto the frit on'the vacuum-head, place the
reservoir on top of the head and clip together.-
<'','• ''
15.3.2 When filtration is required!*-a filtration disk or :5t>0 mg of
Celite will be placed on taop of the extraction disk.
15.3.3 Turn vacuum pump on and;|f$et pump vacua™ to 10 inches of
mercury. Do not exceed : the manufacturer's recommendation
for manifold vacuum. Flow'-r^es eari be controlled by
opening and closing vacuum manifold valves or pinch clamps.
15.3.4 Wash each disk with four 5 mL aliquotss^of hexane. SLOWLY
open vacuum valxsff to allow the hexane to jpass through the
disk after
15.3.5 Wash each disk wilfh, four 5 mL,4«lIqti«fcs'(of methanol (MeOH).
Let disks drain after each Wash. Do not allow the disks to
drain dry between washes. -, /
' {•"* ' ^
15.3.6 Wash the disks with two/S.':mL aliquots of methanol/water
(5:100), &ll»w the firstiS mL portion to wash through;
however, do'mofirAllow the ':$$fsik to drain dry. Next wash the
last 5 mL portion through, keeping the disk wet. Each disk
must remain moi|s»|- until the entire sample volume is
extracted. DTpfb^CONDITIONING, DO NOT ALLOW DISKS TO DRY.
THIS STEP IS J^^^||^KpoOD RECOVERIES.
15.4 Compound Extraction Basing Disks
15.4.1 ,,,, JSwirl the sample|J.(from paragraph 15.2) for 20 seconds and
decants*^»' sample into the sample reservoir.
'•••&-'• * *
Open manl3|ald valves to allow samples to pass through the
disks at approximately 3-8 mL/min. The flow rate must not
exceed 10 ips/min. If the flow rate slows because of
particulatfe;buildup on the disk or filter, increase the
vacuum to Jatsiintain 3-8 mL/min. flow.
'v&f- ,
JSe'
HOTE: ItSfflust take at least ten minutes for the sample to
pass through the disk.
D-40-PCB-Q 08/23/94
-------
DRAFT
15.4.3 Rinse the sample container with 5-10 mL of methanol/water
(5:100) into the sample reservoir to transfer any remaining
compounds. :
15.4.4 When the entire sample volume has passed through the disks
(approximately 15 minutes), rinse ti& saaple reservoir with
an additional 5-10 mL methanol/w4t:er (5i:J0S) into the disks.
15.4.5 Wash the disks with an additional 5 mL methanbl/srater
(5:100), continue to apply vacuum until the top &£»£iie disk
is dry. Turn off vacuum. *-:, ' ;
15.4.6 Wipe the reservoir dry wit3i clean lab/'lzissues (Kimwipes, or
equivalent) . , > • •
v < ^
15.5 Compound Elution using Disks " :- , ;
15.5.1 Release the vacuum on each filtration,-device, dispose of the
water eluate in the large receiver. fflD.UOT UNCLIP THE
RESERVOIR FROM THE VACUUM HEAD.
-;; ,"-. ,'l'' "•••
15.5.2 Place a clean solvent recelwr^lover;-.the drip tip of the
vacuum head. ~- - -: ',-,'
15.5.3 Add 5 mL hexane to e&iah d±§k~. If additional filtration media
were used, allow the hexaile to stand in the reservoir for 2
minutes prior to applying.-vacuum.
15.5.4 Turnf*7acuum pump on. Adjust,;pump pressure to 5 inches of
mer^mry. '}% '-"•
15.5.5 SLOWLY open the;|»anifp;lds valves to allow hexane to soak into
the /s&rbent b^dfj";'I&SJ'WSSt AUJ3W THE HEXANE TO EUDTE AT THIS
TIME. Close valves and allow disks to soak for 2 minutes.
15.5.6 After 2 mitra^es^, slowly open the manifold valves and collect
; ;,:'S'fNtjtMnat into tfielr^ceiver tube. APPLICATION OF EXCESSIVE
f ! "" VAGOOH MILL RESULTpf ANALYTE LOSS.
.'. f ' 't:'^
15|4S;7 Add a secdppd volume of 5 mL hexane to each disk and elute
, J<- under vacu^an until the disk is dry.
& Proceed wim^cleanup of the hexane extract as described in
; paragraphs§3;5.6 to 15.9.
"'•% '* ^ '.Yt
•-«.:a's. "1;|
15.6 Sulfuric AcM =Cleanxij»:
' ',r' ?'
15.6.1 Usiiig4ia.isyringe or a volumetric pipet, transfer the hexane
solution to a 20-mL vial and carefully add 5 mL of the
concentrated sulfuric acid in a fume hood.
D-41-PCB-Q 08/23/94
-------
DRAFT
15.6.2 CAUTION: Make sure that there is no exothermic reaction nor
evolution of gas before proceeding.
15 . 6 . 3 Cap the vial tightly and vortex for one minute . A vortex
must be visible in the vial.
15. 6. A CAUTION: Stop vortexing immediately if the vial leaks.
AVOID SKIN CONTACT; SULFDRIC ACID BURNS. "-
15.6.5 Allow the phases to separate for at least 1 minute. Examine
the top (hexane) layer; it &pould not be highly colored nor
should it have a visible einsulsion or cloudiness.
.&
15.6.6 If a clean phase separation is achieved, proceed to step
15.9.9. ''M "V- -:'
15.6.7 If the hexane layer is colored or: the emulsion persists for
several minutes, remove the sulfurte'^acid layer from the
vial and dispose of it properly. Add [another 5 mL of the
clean concentrated,, ,sulf uric acid.
"'* ''' "
,
NOTE: Do not refiove any'^sestoe/la-t tbis, stage of the
procedure. :: . -•" -'" -:;;•''
;,
15.6.8 Vortex the sample aim allow *he phases to separate .
' ";'•• • '''3 '
15.6.9 Transfer the hexane layers to a clean 20-mL vial.
15.6.10 Add,«B.'additt«Aal 1 mL of'ljfxane to the sulfuric acid layer,
cap; and shake. :-|::^fhis second'le&traction is done to ensure
quantitative trsjfasfer of the^roclors and Toxaphene.
- ^ "xf
15.6.11 Reac^es the sefee^-^^teslliyer and combine with the hexane
' 15.9.9.
-
15 . 6 . 12 Add 1 mL of l||ift«|gent water to the combined hexane extracts to
; ; , ;r'-'-E«no>ve excess "i;«^M&iric acid that may still be present.
Vortex iand allow the phases to separate.
"its-
Transfer tfcfc hexane layer to a clean 20-mL vial.
If a water,||ayer is evident in the eluate, remove by the
addition dlflsodium sulfate as follows: (Note: water
injected/Jilto the GC may strip the analytical column phase
:^afid may fjause retention time shifts.)
'•3< "' "•"? •,, ,1'$
15:6'j|5/l Add 5 g Na2S04 to the eluate.
D-42-PCB-Q 08/23/94
-------
DRAFT
15 . 6 . 15 . 2 Decant the eluate and quantitatively recover the
Aroclors by adding additional hexane to the
Combine this hexane with the eluate.
15.6.16 Continue with the potassium permanganate (paragraph 15.10)
and florisil (paragraph 15.11) clfsajftaps.iAs described below
if the sample is heavily contaminated. :~ilf ,s,the sample is not
heavily contaminated, the potassium permanganate cleanup may
not be necessary and the laboratory may skip !pai|agraph 15.10
and shall continue with the JEborisil cleanup (paragraph
15.11). ,- '• ;
15.7 Potassium Permanganate Cleanup - ;
15.7.1 Add 5 mL of the 5 percent ^aqueous jkjptassium permanganate
solution to the combined hexstie. fractions from step 15.9.14.
15.7.2 CAUTION: Make sure that there is no exothermic reaction nor
evolution of gas before proceeding. :?'\ ,.
15.7.3 Cap the vial t|ghl^;;ai»5j|ro|:tfx for 1 minute. A vortex must
be visible in thepvial'. ^''1^ X=';-- <; -
,P • |"g ••", .;$' , •>'
15.7.4 CAUTION: Stop the wrtexingJIaramediately if the vial leaks.
AVOID SKIN CONTACT; MTASSUM PERMANGANATE BURNS.
15.7.5 Allow the phases to separate for at least 1 minute. Examine
the top = XheXj&ae) layer, it should not be highly colored nor
should' It have jk visible en&lsion or cloudiness.
" *- •£ •••• ,
•-tf> • •;: '•''•
15.7.6 If a clean phase^separation is achieved proceed to step
,15.10.9. - Jr. . „, , .....
15.7.7 If tM; fejsxane layer is colored or the emulsion persists for
several -misates, remove the permanganate solution from the
vial with a-,jglass pipet and dispose of it properly. Add
, : -.';• another 5 mL otf c&ean aqueous permanganate solution.
NOTE: '%*-;:not remove any hexane at this stage of the
procedure.^-
f^.7.8 Vortex the:,isample and allow the phases to separate.
' •'•*, - :A . I
X.3&. ' -, ••'*•'
15 '.J-^,.,,, Transfer dberhexane layer to a clean 20-mL vial.
15.7.10 '^,'AQd an awitional 1 mL of hexane to the permanganate layer,
cagii;t:h^:;;Vlal securely and shake. This second extraction is
done^i^':ensure quantitative transfer of the Aroclors and
Toxaphene.
D-43-PCB-Q 08/23/94
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DRAFT
15.7.11 Remove the second hexane layer and combine with the hexane
from step 15.10.9.
15.8 Florisil Cartridge Procedure
15.8.1 Reduce the volume of the combined:|jex«Jpe layers to 1.0 mL
under a stream of dry nitrogen. >' :
15.8.2 Attach the Vac Elute vacuum manifold to a water aspirator or
vacuum pump with a trap installed between the manifold on
the vacuum source. Adjust.-tlbe vacuum pressure in the
manifold to between 5 and^O pounds of vacuum.
15.8.3 Place one Florisil cart£$4ge into the vacuum manifold for
each sample extract. >\.i;. :
15.8.4 Prior to cleanup of samples, the cartridge must be washed
with hexane . This is accomplished feynplacing the cartridge
in the vacuum manifold pulling a vacuum and passing 5 mL of
the hexane solution, through the cartridge.. While the
cartridges are S|sl:s%,-^ste4t 4Just the vacuum applied to
each cartridge ~s$?;that Hf':is%4|^J^3K3aa,tely equal. DO NOT
ALLOW THE CARTRIDGES TO GO DRY AFTER THEY HAVE BEEN WASHED.
f i *'
t r , if
15.8.5 After the cartridges >ia tb&pJnanifold are washed the vacuum
is released and a racfe obtaining labeled 10 mL volumetric
flasks is placed inside $&e manifold. Care must be taken to
ensure = that the solvent guide from each cartridge is placed
ins jje SB£ the.iapipropriate ^fslumetric flask as the manifold
topj3i,s replacel|iiEnd that thVsorbent beds do not go dry
they havdifbeen conditioned.
.
15 . 8 . 6 Af^fefer-'-the voldaa^tacfcRi'^La^fess are in place , vacuum to the
restored and the extract for each field and QC
sample scillxEtion is transferred to the top frit of the
appropriateilfl&risil cartridge.
'
15.8.7; ': "The H^R in the eibgi&ct concentrates are then eluted through
£•'„?" the cdl«aia with 9 mL of hexane and collected into the 10 mL
j5 volumetrlfegflasks held in the rack inside of the vacuum
_, 1: manifold. ^
i\ ;•. "t
*l5,|f8*;8 Transfer t&e eluate in each volumetric flask to a clean
'<~ !>",:,: centrifug^ftube or 10 mL vial. Use two additional 1 mL
' V":-:,rE, hexane rinses of the flask to ensure quantitative transfer
-vJ>,o£, the cartridge eluate.
';. 'A* '
15.8.9 Concentrate the solution to a 1.0 mL volume using either
nitrogen blowdown or micro-Snyder column. Measure the final
D-44-PCB-Q 08/23/94
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DRAFT
volume with a clean syringe or by transferring the extract
to a clean volumetric flask.
15.8.10 If crystals of sulfur are evident or./the presence of sulfur
is suspected, proceed to paragraph 15.12. Sample analyses
showing the presence of sulfur are iw>t/;a.cceptable and must
be reanalyzed after sulfur removal.
15.8.11 If sulfur is not expected to be a problem, trscasJer the 1.0
mL of sample to a GC vial an«tMabel the vial. The"' extract
is ready for GC/ECD analyses; proceed to paragraph 18.
Store the extracts at 4«C *|± 2°C) in the dark until analyses
are performed. ,.;
15.9 Sulfur Removal :
>/ 1 *;-:
15.9.1 Bright (unoxidized) granular copper is used to remove sulfur
contamination. Add one to three granules of copper to each
hexane extract in a clean vial. Tightie» the top on the vial
and shake for 3@; s^ecpnds. Filter or centrifuge and then
decant the solt3GC:i«4'V«tjd,peespve, all solid precipitates. If
copper appears b^ght/'lti^olfiaragraph^lS. If copper
changes color, repeat sulfur^fas&moval -as: necessary.
15.9.2 If only a partial set;of tile samples in the Batch require
sulfur cleanup, an additional reagent blank of hexane spiked
with the appropriate amoamt of the SMC solution and cleaned
with the copper is required.
K ' ^M, ,';'; ' i-
15.9.3 Proceed to paragraph 18 f or! 0C/ECD analysis.
16 Sample Preparation and Extaeajcttion. - Oil Samples
NOTE: The Aroclors tsarlet compound CRQL for oil samples is 2000 jtg/k§
for 1221; 5006.?j£g^kj for toxaphene; and 1000 fig/kg for the other
Aroclors. " ;2i,
16.1 Add li,§%"bf 'saofft^j-jto a 10 iSD,g86olumetric flask. (Oily mixtures should
be phase -separated according to the procedures in paragraph 13 of the
,
16.2 1.0 mL of SMC (0.2|pg/mL) to the sample.
'~~'r ?',;: - ^ / ,
A ',,,_ f',t
16.3 Add'tjfiJRane to the volumetric flask until reaching the 10 mL meniscus
mark.'"'-"-\^: . £•
*''**• "'- * •'.''•/*•
16.4 Cap with stoppeafiarast'mix for one minute.
• • ;'; S,
16.5 Pipet exactly 1.0 mL out and proceed with clean-up and final
concentration as specified in paragraphs 14.3 - 14.6.
D-45-PCB-Q 08/23/94
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DRAFT
17 Sample Preparation and Extraction - Wipe Samples
A wipe sample containing PCBs is serially extracted with two portions of
hexane using an ultrasonic probe. Extracts are combined, filtered, and
dried through powdered anhydrous sodium sulfatfis,'and concentrated to a 1
mL volume using the nitrogen blowdown procedure. ,
NOTE: The target compound CRQLs for wipe samples will %e specified by
the Agency. >f,
•*' ~*
17.1 Pour off any free solvent from the sample jar into a clean Erletsaeeyer
flask of appropriate size. =
17.2 Spike the sample with 10 uL of the .SHE, (2.0 ug/mL).
, "*"'> \
17.3 Add enough clean hexane to the sample jax*to ;ce '
17.4 Sonicate at microtip maximum *f«»wer; cool'-ftie 'sastple during sonication.
The sonicator must be set for SIKpercenii pulse action. Sonicate for 3
minutes. The power output may have to^lse adjusted to ensure that the
sample extract does not splash excessively; any significant loss of
sample during sonication is not acceptable. Rinse the sonicator tip
after each sample , -extraction with 1 mL spf hexane.
' ' - -"- ",' 5-
- \' V -v'V "-•"^ ^
17.5 Remove the hexase' layer frcfflC,the sonica~€pon and combine it with the
hexane in the ?i!rlenmeyer fl^jsk. '
17.6 Repeat steps' 1?. 3 v- 17 . 5»,C"?W •Jf-L'-",^- ,r '
17.7 Filter the combined '«4*a**cts by gravity filtration.
-, <
17.7.1 A "^Frepare a fil't^tsiojti/drying bed with Whatman #42 filter
..i/-f*r ""'"~tia'Pie*-<-Silled with^'Aproximately 15 grams of powdered
•™-.Jg^-- * * s«\ Jf & •. ^@,^l; ,r mL hexane /?mn& transfer rinse solvent to powder funnel.
^''H:'^. Rinse powl®: funnel with 10 mL hexane.
17.8 Concentrate «etag*c*^*» approximately 20 mL using the nitrogen blowdown
procedure in a'3&HJ*water bath. Transfer extract concentrate to a clean
25 or 30 mL concentrator tube, and rinse concentrator tube (from
paragraph 17.7.1) with 5 mL hexane. Transfer the rinse solvent to the
D-46-PCB-Q 08/23/94
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DRAFT
25 or 30 mL concentrator tube, and concentrate further to approximately
1 mL. To minimize analyte loss due to volatility, occasionally rinse
sides of centrifuge and concentrator tubes with hexane during the
blowdown procedure .
17.9 Proceed to extract clean-up steps (paragraphs 14,3 - 14.6).
18 Instrumental Analysis
18.1 Set up the GC system per the requirements, in paragraph 7. !- '
ir ' • ;
18.1.1 Solvent-flush manual injection or automated sample injection
is recommended for analysis.
18.1.2 An analytical sequence consists of field sample analyses and
all associated standards, b'laaoks , , and QC analyses performed
within a 24 -hour period on one instrument. There are two
(2) types of analytical sequences* «» initial calibration
analytical sequence and a daily califerat&on check analytical
sequence. All samples shall be analyzed within one of these
analytical
• 18.1.2.1 An iiiicial calibration • -analytical sequence
begins qsfith a t&fjsee-point calibration of Aroclor
1016/1260.;:followed by single-point analyses of
the other :Ax®c3x»rs and toxaphene, an instrument
blank, an 1CS, and a method blank. The initial
r.. -^calibration analytical sequence is as follows:
>; <:'f • 'r ,:, Initial Calibration (analysis of the high
?> ~ 1016/1260 standard proceeded by the mid
I " r. ; ^and^lpw, v1016/1260 standards followed by
; =• ;-,- ,:;:a'-';-l!:^|33^1s^ipoint analyses of the other
s ~ Aroclors and toxaphene) ;
*•
"• : ;* ;(/; Instrument Blank ;
"'*. •' m "' „ ; - ,
"' ; - {; j -^ • Ji1I*aiboratory Control Sample(s);
^ '*$$<-
^;1S • Method Blank(s);
^* Field Sample(s);
Si^
jv5:- Instrument Blank(s) ; and
.-'K
.]:>• ,A ' Performance Verification Standard(s) .
s'- "$.' *"
18.li~2.vl A daily calibration check analytical sequence
begins with an instrument blank, a valid
calibration check standard, a method blank, and
D-47-PCB-Q 08/23/94
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DRAFT
an LCS . The daily calibration analytical
sequence is as follows:
• Instrument Blank; ;,
Calibration Check 'Standard (1016/1260);
Method Blank(s); . ,
• LaboratorydGontrol Sample(s); ;
Field Sample (s) ;
A"' :
Instrument Blank(s);; and
: ; s; - ,
• PerformaneeSerJJIication Standard(s) .
18 . 1 . 3 If all acceptance criteria for thesi? -analyses are met , then
the Laboratory may proceed with sample. analyses .
, •• i.
18.1.4 All analytical :;sie<|u4p«^ '^nclude with an acceptable
>
' ^ -' V '< -
'*'•;>'
-i
instrument blanM^iand a'sfW>ssaitysis. , , The PVS shall be
started within 2&: hours afte^^hen Injection of the first
initial calibration|s,tandarjdllor the first instrument blank
in the daily calibration sequence. NOTE: If a PVS
reanalysis is required ^because of a non-compliant initial
PVS analysis, the PVS reanalysis must be started within 26
hours ,a!f teethe start of-'-Ejte current analytical sequence.
,.r; " :'-| '£
18.1.5 The.'isethod blall:~and all associated samples shall be
asllyzed in th^issame analytical sequence. If samples from a
fetch are anal|^d^J.n,,jtiqr.e,, than one analytical sequence, the
associated m«tMiSifta^«si&t also be analyzed in the same
analytical sequence . If a method blank extract is used up
because : 03| stai^ltiple analyses, the Laboratory shall
substitute' ' #j& instrument blank in place of a method blank in
: -all ^subsequent ,&3Balytical sequences. The Laboratory shall
v-'"- 'hbt«^as4.s in the"1ESj|fech Narrative and shall use the EPA
J'l "' identiMoation number as described in Exhibit B for this
C'ti instrumei&^blank.
.1.6 The LCS shfH be analyzed with all associated samples in the
same analytical sequence. If samples from a batch are
analyzed ik*more than one analytical sequence, the
associatecUSLCS shall be analyzed in the same analytical
s< - i;sequencei;: If an LCS extract is used up because of multiple
aofli;Lys«s; the Laboratory shall dilute the LCS standard
mixta«Ci£ (the original stock mix) and use this solution in
place of the original LCS sample in all subsequent
analytical sequences (see paragraph 27). The Laboratory
D-48-PCB-Q 08/23/94
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DRAFT
shall note this in the Batch Narrative and shall use the EPA
identification number as described in Exhibit B for this LCS
solution.
18.2 Computer reproductions of chromatograms that ascei- attenuated to ensure
that all peaks are on scale over a 100-fold range are acceptable.
However, post analysis attenuation shall be n6 greater than a 100-fold
range. This is to reduce the potential for RTSs of quantitation peaks
due to column overload and to ensure that the detector is" ojpexating
within the calibration range. If any sample quantitation peaJfcs^>exceed
the calibration range (greater than the''high concentration level; of the
1016/1260 initial calibration), they shall be diluted according to
paragraph 19. , i:
18.3 If any saturated non-target compound f^sjsomatogjraphic peaks are evident
or if any chromatographic peaks overlap -mate -titan one RRT and/or RT
target compound quantitation windows, the Laboratory shall use the "E,N"
flags on Form QIA-PCB to indicate this situation.
18.3.1 If saturated chr^aaatographic peaks outside target compound
quantitation RSSSi^a^/fOt-Bf .-windows are evident, flag the
nearest target compound *&ylf* MH^forja QIA-PCB.
18.3.2 If chromatographic |»eaks overlapping more than one target
compound quantitatiowiSRT^aikl/or RT windows are evident,
flag the corresponding 'target compound quantitation peaks
"E,N" on Form QIA-PCB. :>.
18.4 Chromatographic peak response of the quantitation peaks must be
greater than Iphpercent aridVilbess than tdQ percent of full-scale
deflection to;*nsure that iralividual quantitation peaks and
Aroclor patterns will be visible^duri^n^ data review.
> - ' •..•. ^' ''^ •• "f -. * ,' .. '**'"'
'•'••>;<•- ''?. iff""- -„••:!-,. "N „*" 'ia
19 Dilutions "r ; =
19.1 Samples with quantitati%irifj»eaks larger than high level 1016/1260 initial
calibrat356li:~:;$pafes must be"5si^NEp:,ted with the "E" data flag as described
in ExMiMt:f
-------
DRAFT
20
20.1
concentration that exceeds five times the concentration of the low level
initial calibration standard, then the undiluted sample shall be
reextracted and/or reanalyzed at no additional cost to the Agency.
19.2.1
19.2.2
19.2.3
19.2.4
19.2.5
At the request of the Region, sample dilution may be
required prior to the initial extraction and analysis. If
no Aroclors are detected in the diluted sample above five
times the concentration of the low initial calibration
standard, then the undiluted sample shall be-cefeattracted and
reanalyzed as an additional paid sample. , „ „,
Dilutions - Solvent extracted, oil, and wipe samples
19.2.2.1
Dilutions of/.solvent extracted, oil, and wipe
samples shall be .made by using an appropriate
aliquot of the 'iaptBact? diluted in hexane.
After making a dil^rti^n.^ add sufficient SMC
solution to bring up lid -Spc0per concentration (20
ng/mL). : .
Dilutions - SPJJvextr«cted -samples
,-•' • * "'"• '•' ".'" . ,"•,',"•' •. *
19.2.3.1
Dilutions of water samples shall be made by
using a»,;rapprop3:Jiate aliquot of sample diluted
to 100 T&L with-«ethanol/water (5:100) (see
paragraph 1S^2). Continue with sample
extraction and cleanup as described in paragraph
Dilute samples prior to the addition of
Saatple diluti«ys5jihill be analyzed in a valid analytical
sequence which includes the associated method blank and LCS.
j *
If sample r«ea:^.r.actions and reanalyses are required, the
laboratory shi^^lso reextract and reanalyze an associated
method jolank
Identification of Ar'ajjsprs
analyst shall conster the Aroclor pattern in addition to specific
peaks. T^e: choice of the peaks used to identify and
Aroclors may-Sbe complicated by the environmental alteration
of the v$*a,tstern and byf'Sje presence of co-eluting compounds or matrix
interferetobess^ The.diEnre highly chlorinated components of Aroclors are
more stable lia ;|sbe#;|%svironment. Therefore, the analyst should emphasize
the later eluting«.^eaks of a pattern in identifying weathered Aroclors.
D-50-PCB-Q
08/23/94
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DRAFT
20.2 Retention Time Standard - The SMC shall be used as the RT marker for
compound identification. The SMC shall also be used to monitor
extraction efficiency.
20.2.1 The SMC shall be added to all field and QC samples prior to
extraction. , - "
20.2.2 In each analysis, the SMC RT must be within! $ 1.0 percent of
the mean RT of the SMC calculated from the 1014^3,260 initial
calibration standards. ,, '\
20.3 Aroclor identification when SMC recovery is greater than or equal to 10
percent and less than or equal to 200 percent. ; ;
20.3.1 Quantitation peaks shall;%e identifijed on the basis of RRT
in all field samples for whicil the.JSMC recovery is greater
than or equal to 10 percent and' less than or equal to 200
percent. i
20.3.2 Peaks in samplefcbromatograms shall be identified as
quantitation pessfcs:J£;£toef*,£&? is within ± 0.005 RRT units
of the RRT established ftom-aatee-lotir calibration standard
during the initial!' calibration. ; " !
:- 8
20.4 Aroclor identification when SMC *e«overf is less than 10 percent,
greater than 200 percent, or if peak (interferences are present.
20.4.1 Quantitatlsn ;pe,aks shall "fee identified on the basis of
absolve RT la/|all field sapples for which the SMC recovery
is-..less than ioftfercent, greater than 200 percent, or if
peak interferences are present.
-;-," &>i:
20.4.2 Peaks in samplfesiiarda3iog3rams shall be identified as
quantisation peaks if their absolute RT is within ±1.0
percent ^f\ii|jhe RT established from the low calibration
standard difrlt*g,-,the initial calibration.
identified on the basis of absolute RT shall be
flagge&p££h the qualifier "T" (See Exhibit B) .
-'-A'
If the recovery of the SMC is less than 10 percent, greater
than 200 p^cent, or if peak interferences are present for a
sample, acceptable recovery of the SMC must be obtained in
the assocMjfaed method blank and LCS (see paragraphs 25 and
20.5 If multiple p!eakSyar« within the identification windows (target compound
and SMC) , the La&fostory shall use professional judgement to properly
identify the appropriate peak. The Laboratory should consider the
inherent matrix effects of the sample on peak shifting, masking, and
D-51-PCB-Q 08/23/94
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DRAFT
overlaps when making identification determinations. The Laboratory
should take into consideration the mean RT and RRT from the initial
calibration, RT and RRT from the calibration check standard, and the SMC
RT from relatively clean samples analyzed beforehand after the sample in
question as a basis for selecting the most appropriate peak. The
Laboratory shall describe in the Batch Narrative-- the rationale used for
choosing a particular peak (e.g., chose peak Closest: lap the RT of the
peak in calibration check standard) as the target com£oo»d or SMC and
how the field sample matrix may have affected peak identification.
21 Calculations :, ""• ':' ;
21.1 Calculate the RRT of a sample component or a standard using the
following equation:
DOT* — CCrapODfiDt ;< T?O T\ 11
.fuv J ™ ' *•" •• •• " 'ff^ *^^ • *^ • J» J.
***• f.^ ^ .
•^
Where: ,JJ-^-^V:3- V ,-
RRT = relative retention time - - , ' ,' •'; '
RTcomponent = retention time of 4ftie target compound
RTSMC = retention time of the SMC
21.2 Samples will be^xmntitatagd^using the 'Calibration factors determined
from the low co^teentration|&oclors standards from the initial
calibrations. ,1|(NOTE: The l^pc concentration shall be calculated using
the mean SMC,,-calibration f^^o^ calculated from the 1016/1260 initial
calibration standards) . ,:;Jilf,»;S-;;141 , i;y
21; 3 Quantitation of PCBs sjas.jAroclors
21.3.1 , "Tlie concentra'ti^j^pf an Aroclor in a sample is calculated by
,;|-,; '''-av£ra||Hp,g the conjurations of the individual quantitation
;,-/!- peaks/"-pfee response of each peak can be measured by either
,r,|- peak heigpfc. or integrated peak area measurements. Because
,^7' the quantisation peaks are not specified by the method, it
4-;,;A ^s require
-------
DRAFT
peak common to both compounds present in the sample must not
be used to quantitate both compounds.
21.3.3 Water
Concentration (pg/L] = .__ */^v* . >-• EQ- D-12
where : , •••
AX = response for the peak to Jbe measured
CFm = calibration factor of ,fisantitation peak
established from -fjfee,, Low concentration standards
calculated during the Initial calibration.
. .
Vt = volume of total extract (;^L) r(take into account
any ••'dilutions ) . :
.
Vi = volume, of ext±set^ injected
Vs = volume j,«sf, water ^attracted (mL)
'•!-.
21.3.4 Soil/Solid (Wet- weight basis) and Oil
. D.13
,, CFm, "Vj,/"* sesame as given in Equation D.12
:-L-:T voluae;;=
-------
DRAFT
An average concentration of the three to five quantitation
peaks for the Aroclors is then determined using the
following equation:
V* 2i
h «
EQ. D.14
where: -.'
Concavg = mean concentration.
'""*'
Xi = individual pea$| concentration.
N = number of peaks.
21.4 Calculate the SMC amount observed and amount (pef-cetit) recovered using
equations as described in paragraph 10.4.
21.5 RTS shall be monitored usingfthe SMC'^^SilagEaph :2fl.2) . The RTS shall be
measured for all analyses. Y" ' . ,-S
21.5.1 Calculate the retention tiae percent difference (RT %D)
between the RT of the SHCj/in the field and QC samples or
subsequent standards analyzed and the mean SMC RT from the
most reeftst 1016/1260 initial calibration standards using
the £«.llowingi! equation: ~
. D.15
where: '" <\ "
^^£I!M'«-_i retefit^>n time percent difference.
*•" ;^' •
RTS = %; r;v retention time of the SMC in a field and QC
?;-sample or subsequent standard.
RTC = ;,,|JBean retention time of the SMC from the most
-i ?recent initial calibration (mean RT of the
_.-;'-H: 1016/1260 SMCs analyzed during the initial
:•'••. (•'•'' calibration).
D-54-PCB-Q 08/23/94
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DRAFT
22 Technical Acceptance Criteria
22 . 1 Each sample within a Batch shall be analyzed on a -€C system meeting the
initial calibration or valid calibration check standard technical
acceptance criteria (paragraphs 8 and 9). , I
22.2 Each sample within a. Batch shall be analyzed after an acceptable method
and instrument blank, (paragraphs 25 and 26) and after- ass -^acceptable LCS
(paragraph 27) is analyzed. :', „;:
22.3 Each sample within a. Batch shall be run.fwi.thin a valid initial ;
calibration or daily calibration check analytical sequence that
concludes with an acceptable instrument blank (paragraph 26) and an
acceptable PVS (paragraph 10). "\ ,*;
22.4 Each sample within a Batch shall be analyzed and results reported within
the contract required turnaround times . 'i
22.5 Each sample matrix within a Batch shall have an acceptable method blank
analyzed during the same analytical sequence.
22.6 The RTS for the SMC RT must*%«; within- iv^Sspercent;, between any sample
in a Batch and the mean RT of -jiiie SMC cal^iated -ficiom the 1016/1260
standards analyzed during the iialtial calibration. The RTS is not
evaluated if the SMC is not recovered s&r' if peak interferences are
. present.
22.7 The advisory recovexjr.l&it for the S&C is 50-150 percent. Reanalyses
of field samples, aire not made if the SHG .recovery is outside the
recovery lirnts,,^/'. "', ; ,
'''•• j ,,v
22.8 The SMC recoyer^ must be gJpesSLte, r,,ghan, or equal to 10 percent and less
than or equal '>«fe 200 perce&'SHt.-oic^fcfco use RRT for identification
purposes. The idiatitfification window is ± 0.005 unit of the RRT for each
quantitation peak in'it&e low concentration standard analyzed during the
initial calibration, it fhe^ recovery of the SMC is less than 10
percent^, ,!^r^ac«sr.- than 200 ipeajfeent, or if peak interferences are present
(but is ^aldequa1Sfe^;|secovered sin -the method blank), the absolute RT of
the |c«mpounds shaiiv|je used for identification purposes. The
id«Bitification windowV;ts ±1.0 percent of the absolute RT for each
q^fititation peak in tltet, low concentration standard analyzed during the
ttial calibration. ;-'i<\
23 Corrective Action ?"
••A, 'i ' '''
23.1 Flag all'sample results "S" if the SMC is outside the advisory recovery
limits of 50'--ljto gjesrbent.
23.2 Flag all sample results "T" if the absolute RTs are used for
identifications.
D-55-PCB-Q 08/23/94
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DRAFT
23.3 An SMC recovery of less than 20 percent in the method blank or LCS
associated with a sample Batch is an indication that serious problems
may have occurred during the extraction process . ^Corrective action
shall be performed and the unacceptable method MLank and/or LCS and all
samples associated with the unacceptable method blank and/or LCS shall
be reextracted and reanalyzed at no additional %xp"esse to the Agency.
23.4 If the SMC RTS criterion is not met for any 'field sample, «sample
analysis shall be stopped and the noncompliant sample rer^d^s If the RTS
criterion is still out upon reanalysis analyze an instrumenC!4"biank. If
the instrument blank SMC RTS is. outsidefFtihe criterion, perform '
corrective action which may include a _,^sste4,jiniJExhibit B.
'
D-56-PCB-Q 08/23/94
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DRAFT
SECTION V
SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
\
25 Method Blank Analysis , •-••
25.1 Summary - A method blank for water samples is 100 mL o€ reagent water
spiked with the SMC and carried through the entire analytical scheme. A
method blank for soil/solid samples is 6v.j* of clean quartz saaiol spiked
with the SMC and carried through the entire analytical scheme/ 'A- 'method
blank for oil samples is 1 g of clean eorn oil spiked with the SMC and
carried through the entire analytical scheme. Method blanks shall be
carried through the entire analytical .procedure J ;
NOTE: The Agency will provide the LaboraifcsKegr .srith further instructions
for the analysis of method blanks for »%e samples .
25.2 Frequency !
A method blank analysis sbeM-'-ft^-^ea^B^Bked for each matrix type (water,
soil/solid, or oil) and wittii/
-------
DRAFT
25.2.4 Criteria for an acceptable method blank is defined in
section 25.4.
25.2.5 If all field samples in a Batch are filtered, the associated
method blank shall also be filtered. If only a partial set
of samples in a Batch are filtered,:$ken a separate method
blank shall be run through the filter, extracted, and
analyzed. L ',
25.3 Procedure for Method Blank Preparation ,-/-, : :
,!«-,!'" ' $"
25.3.1 Prepare the method blanks^Af the frequency listed in
section 25.2. ^ '" /
25.3.2 Measure out 100 mL of reag«nt wate;r for each water method
blank sample aliquot.
25.3.3 Soil/solid method blanks are 6 g '-of clean quartz sand.
25.3.4 Prepare water and soil/solid method blanks' as described in
section 14 or l3;^i|^e^B|i^g«,on whether solvent or solid phase
extraction is ' *
. ,
25.3.5 Spike 1.0 g of corsk oil withll.O mL of SMC (0.2 /ig/mL) and
proceed with the Aroelors/jftEocedure (sections 16.3 - 16.5).
,, ,, i '•*/;
25.3.6 Analyze the method blaflk^sxtracts . Calculate the results
according t&. ^section 2 IT;. ,
•• '" * f ''1\>S",
25.4 Technical Acceptance Criteria '";=;
>•'-'' & ,
25.4.1 J&.1 method blaj^ks shall be analyzed within an acceptable
aloaiiy^ical sg^^^j^^t^^ system meeting the initial
calibration (section 8) or valid calibration check standard
(section ^^ criteria, and the PVS acceptance criteria
(section
RT in the^thod blank must be within ±1.0 percent
of th^liiean SMC RT ' calculated from the 1016/1260 initial
calibrafci|op,, standards.
The SMC re^^ery criterion of 50-150 percent is advisory
only. The|-J|IC recovery in the method blank must be greater
than or eq^il to 20 percent and less than or equal to 200
percent. i*'%'
* f" ^ -
25.4.4 %sttt^,«ftion peaks or potential interferences in the method
blanfejj, aiust have a response less than one -half the response
in the corresponding RRT window of the initial calibration
low concentration standard.
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DRAFT
25.4.5 A method blank may contain a detectable but acceptable
concentration of a target compound, quantitation peaks, or
interferences (less than one-half the response of the
initial calibration low concentration standard) .
25.4.6 If all criteria are satisfied, the 'teethed blank analysis is
acceptable and samples may be analyzed. :If the method blank
is unacceptable, corrective action shall "be, taken and an
acceptable method blank must be analyzed priorVlto analyzing
the associated samples. , ' ;
X
25.5 Corrective Action '•'
25.5.1 If a method blank does **$£ meet the .technical acceptance
criteria, the Contractor' jsifaiall consistler the analytical
system to be out of controli° jitlt its" the Contractor's
responsibility to eliminate m£tho& interferences caused by
contaminants in solvents, reagents^&artridges, disks,
glassware, and other sample storage iitd processing hardware
that lead to discrete artifacts and/or elevated baselines in
gas chromatogramsl :;.|fe j^oatamination is a problem, the
Contractor shali^|fi,nvest;fga*«Mfp»>, source of the
contamination, anil; appropriate corrective measures shall be
taken and documented before further sample analysis
proceeds. s , ,->>,-
' * *':-
\' t
25.5.2 If a compound is found •;!«; the method blank (less than one-
half the;=i3ispaiise in the -.Corresponding RRT window of the
initial calibration low concentration standard) and is also
detected in an Associated field sample at less than the
CJKgL', the compo^ad shall be reported as a nondetect, i.e.,
with a "U"
25.5.3 If the SMC recovery in the method blank is less than 20
percent, , greater than 200 percent, or if peak interferences
are present., '^"ttxe method blank shall be immediately rerun.
; ?,J.£ -:an reanalyslpithe method blank SMC recovery is still
.j cmtsxidte the recovery- limits, the method blank and all
>' "' associated samples shall be reextracted and reanalyzed at no
: additional -.cost to the Agency.
=25.5.4 Flag all m6pbod blank results "S" if the SMC does not meet
'• ,/ts the adviso^ recovery criterion of 50-150 percent.
25.5.5' v, r,If the R^S,^briterion is not met for a method blank, sample
'•' analysesjMiall be stopped and the noncompliant blank rerun.
llE L*jae$GfcS criterion is still out on reanalysis, perform
corrective action which may include a new initial
calibration. DO NOT continue with sample analyses until the
RTS is within ±1.0 percent.
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DRAFT
25.5.6 Any samples processed with a method blank that is out of
control (i.e., does not meet any of the technical acceptance
criteria) shall be reextracted and/or .reanalyzed at no
additional expense to the Agency.
25.6 Documentation '. ,
Method blank results are reported on Forms QIA-PCB, QIB-f£B, and QVI-
PCB. Reporting requirements are listed in Exhibit B.
26 Instrument Blank Analysis
26.1 Summary
An instrument blank is 1 mL of hexarie jspiked witHi 10 ^L of SMC (2.0
jig/mL). At least two acceptable instrument blanks shall be analyzed
within an analytical sequence, one preceding Sample analyses and one
following sample analyses. "!
™<
26.2 Frequency ,•• , ;<
An instrument blank shall b% Analyzed 'A^iteast , twice during the
analytical sequence to ensure ijtiiat the i^tst:rumeifc ,is free from potential
contaminants. The first instrument bla^fe analysis shall be performed
after the initial three -point caM.brafci.dn in the initial calibration
analytical sequence or as the first; analysis in a daily calibration
check analytical sequence. The seebnil instrument blank analysis shall
be performed immed^^eslyjbefore the BKS analysis. The Laboratory is
encouraged to run-SsdaitrtSjBBStJ instrument:! blanks during the analytical
sequence, especially when ^ghly contaminated or complex samples are
analyzed. Instrument blanks must be analyzed after analysis of samples
with high levels of targe t^i&Dmpounds or interferents (see section
26.5.6). ''•' y .:iM;:^~,tki. ?''-•'
26 . 3 Procedure for Instrutteftt Blank preparation
An instrjpeent fclank is I'mL^.hexane spiked with 10 /iL of SMC (2.0
,•.,
26 . 4 Calxsalations
/f&mcentrations of the ^tC and any quantitation peak in the instrument
4tta$k, are calculated ai^eording to the procedures described in section
21". '-tlto^e: The target ^dmpound concentrations (detected concentrations
and CRXlif^alues) in ti^ instrument blank shall be reported in the
appropri^tseKeoncentss&tiion units (e.g., report in /*g/L if the associated
samples are water and in fig/Kg if the associated samples are soil).
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DRAFT
26.5 Technical Acceptance Criteria
26.5.1 A minimum of two (2) instrument blanks ;shall be analyzed
during an analytical sequence on a GfC system meeting the
initial calibration (section 8) or *i?win^aks, or interferences at
up to twice :,the CRQL (2x CRQL).
- "* "~£ -<<
26.5.6 Following the Sfaalysis of a -field sample containing high
legjl&ls of target compounds or interferents , an instrument
,b!6nk shall beJjiaSfalyzed^and must meet acceptance criteria
analyses. If an autosampler
is utilized, then the field samples run after a high level
sample i*uft:,;;ibe carefully evaluated for carryover. The field
sample imme^KLki^ely following the high level sample shall be
, -pesanalyzed, a5«bg-;.with any other samples analyzed after the
,U.: • ' "M'gttfJLi^wel sample!--isS|ich shows evidence of carryover.
26.;S,7 High levfei'^samples are defined as being field samples that
,V contain taj^et compounds or quantitation peaks at
;|;;!' concentration levels that exceed twice the high level
1016/1260 i^.tial calibration standard concentration and/or
«!-, interferences that are detected at levels greater than the
:.'5, :,%,'„, mid levelJ*!|Q16/1260 initial calibration concentration
"' V;.iresponse,>s»f the nearest target compound or quantitation
26.6 Corrective Action
D-61-PCB-Q 08/23/94
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DRAFT
26.6.1 All groups of samples analyzed shall be bracketed with two
acceptable instrument blanks. If either instrument blank is
unacceptable, corrective action shall "be taken and all
samples not bracketed by two valid instrument blanks shall
be reanalyzed at no additional expense to the Agency.
26.6.2 If the response of any target compound «or «|uantitation peak
in an instrument blank analyzed after the initial
calibration or before a valid calibration cheek standard is
greater than or equal to one;-1ialf the response i« tfae
corresponding RRT window of itshe initial calibration low
concentration standard, corrective action shall be performed
and the system shall be .demonstrated, tso be clean by the
analysis of additional j&strument blraiiiks until all target
compounds and/or quantitatgton peaks'ikre within QC limits.
26.6.3 If any target compound and/or quaatitation peak in an
instrument blank analyzed after fieSJi^QC sample analyses is
greater than two times the CRQL, anotis&r .instrument blank
shall be analyzed* If, on reanalysis, contamination still
exceeds the crJi|e-M*^r -Cjjarxaectiye action shall be performed
and the system aiei»onstrasi!eifeS^,i*e::clean. Then, all
associated field/I^C samples Analyzed since the last valid
instrument blank or method jjjarik which contain those target
compounds, quantitafilon peafes, or interferents found in the
instrument blank at iWels ^greater than twice the CRQL shall
be rerun. ' ;'„;''
26.6.4 If a?l itistrumesiit blank (ot&er than the first instrument
blaaafc in the analytical seqifiepice) contains target compounds,
qaaatitation peilSS, or interferents between one-half
response and tjKM^uaejs J^he. ,CRQL, all positive results
(resa3.£s greattwd^aTOt^'^iual to the CRQL) for those
compotsEBJs in samples analyzed after the last valid
instrumeaty&lank shall be flagged with a "B".
'-. 'f '""
26 .6.5 , „;; lElsig all instrtaaiaaait blank results "S" if the instrument
|;:; -: T>'laiSK;^SpttC does notlipeet the advisory recovery of 50-150
:-~' "* percent^;; _
2&.S'. 6 If the ins^kument blank SMC recovery is less than 20
;;:, percent, gEfkter than 200 percent, or if peak interferences
•'%- "i0••• are preseng^l sample analysis shall be stopped, corrective
; :, < action pei^«rmed, and another instrument blank shall be
*"K*£~' analyzed.;|'§If the SMC is still outside the criterion upon
I', corrective action, which may include a new
l;,,ealibration shall be performed. All samples
since the last valid method or instrument blank
shall be reanalyzed after a valid instrument blank has been
demonstrated.
D-62-PCB-Q 08/23/94
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DRAFT
26.6.7 If the RTS criterion is not met for an instrument blank,
sample analyses shall be stopped and another instrument
blank shall be analyzed. If the RTS smtside recovery limits
on reanalysis , corrective action which may include a new
initial calibration shall be performed. DO NOT continue
with sample analyses until the RTS "is *i thin ±1.0 percent.
26.6.8 Any samples not bracketed by valid ins tumet«:> iblanks or a
valid instrument blank and a method blank and shall be
reanalyzed at no additional expense to the Agency!.'
26 . 7 Documentation
Instrument blank results are reported >on Forms Q1&-PCB, QIB-PCB, and
QVI-PCB. Reporting requirements are -l^Sfted irvllxhibit B.
' ', , * >>"
27 Laboratory Control Samples j ,
27.1 Summary
* -•
NOTE: The Agency: -Mil pr6%S||e the Labo«|tory with further instructions
for the aaaiysis of IpSs for wipe\ssmples .
... ''• \.
27.2 Frequency „' ; - , |§ B,e,, ..... ,,_„
; -~~\ «,JJl.;^mi i'^Jr
An LCS shall be atisHyzed once per matrix per analytical sequence (24
hours) per instrument, ivXhe LCS shall be analyzed after the first
instrument blank in the-ifpsifcLal calibration analytical sequence or after
the method;' Jjlaoik; in the dkilty, Calibration analytical sequence.
'
An LCS'all be analyzed with each:
Set of wa^T field samples (LCS prepared from reagent
water) ; :/,,t
' '-
Set of soij/solid field samples (LCS prepared with quartz
,sand) ;
'• , .
• "Set:: :M:- »lly field samples (LCS prepared with corn oil) .
27.2.2 The LCS shall be analyzed with all associated samples in the
same analytical sequence . If samples from a batch are
D-63-PCB-Q 08/23/94
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DRAFT
analyzed in more than one analytical sequence, the
associated LCS shall be analyzed in the same analytical
sequence. If an LCS extract is used "up because of multiple
analyses, the Laboratory shall use the original stock mix
diluted into hexane in place of th.- /:
*'' , * •
27.3.1.2 Spike 100 mL of aseagfent water with 100 /iL of the LCS
standard mixture Vagi described in the instructions
,f»rovjaeied with the I|CS mixtures. Use syringes to
,;3Jerfbrffl5,,|ifae spiking ,:fee ensure accuracy. Add the SMC
and mix and carry through the extraction and clean-up
process as! described in section 14 or 15, depending on
whether ^^.vent^or solid phase extraction is utilized.
as described in section 18.
27.3.1.3 Nominal aqueous LCS target compound concentrations are
as follows:
Aroclor 1224;:, 25 pg/L
-Amclor 1254 ' 3 Mg/L
HefECachlor epoxide 0.5 /*g/L
••
.3.2 Soil LCS 'n*-
AlloJBr.:the LCS mixture ampules to reach room
tenip/erature before opening. The ampules must not be
o|*eaied until preparation/ analysis is to occur.
Exercise care in breaking the ampules open to avoid
: injury.
D-64-PCB-Q 08/23/94
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DRAFT
27.3.2.2 Spike 6 g of quartz sand with 100 /xL of the LCS
standard mixture as described in the instructions
provided with the LCS mixtures/' Use syringes to
perform the spiking to ensure Accuracy. Add the SMC
and mix and carry through the. .^extraction and clean-up
process as described in section. ,14. Proceed with the
analysis as described in section :18,;
27 . 3 . 2 . 3 Nominal LCS target compound concentrations,, are as
follows: /"',, V •
Aroclor 1221 vi 417
Aroclor 1254 V: 50 pg/ikg
Heptachlor epoxide , 8
27.3.3 Oil LCS '-
,' ;.
This section has not been finalized. ? The LCS composition
and concentrations for oils are currently being
investigated. ,t.; ,
!-! ,'•"" '; • '-•< •;:"-.. U;\, ,-,
27.3.3.1 Allow the pCS mixture ampules to reach room
temperature :feefore openlsig. -"The .ampules must not be
opened until -preparation/ analysis is to occur.
Exercise care in breaking the ampules open to avoid
injury. ' ;- ' •'.:
27.3.3.2 f|>fk^|l;-g of corn oi^ with 1 mL of the LCS standard
-, Itixtuffr^s described?^ the instructions provided with
?£ 'the LCS fejstures. Usfe- syringes to perform the spiking
', ' to ensur6| Accuracy. Mix and carry through the
: s extracti^fc^nd cleanup process adding 1.0 mL of SMC
' ' ; r^v(°-2 /igJiE|l;--«S«i|i»^EBe and further prepare as
;*tescribed in sections 16.3 to 16 . 5 .
27 . 3 . 3 . 3 Nominal: rfljCS target compound concentrations are as
1221 25,000 /ig/kg
>r 1254 3,000
Hep tailor epoxide 500
27.4 *e9|snical Acceptance Cliteria
.^ ,,All LCS offi^iounds must have recoveries between 30 and 130
''
27.4.2 All%08'-"target compound absolute and relative retention
times must be within the windows established from the low
concentration standard during the initial calibration.
D-65-PCB-Q 08/23/94
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DRAFT
27.4.3 The RT of the SMC must be within ±1.0 percent of the mean
SMC RT established from the 1016/1260 initial calibration
standards.
27.4.4 The SMC advisory recovery criterion:is 50-150 percent. The
SMC recovery in the LCS must, however, be greater than or
equal to 20 percent and less thaa or eqaal to 200 percent.
27.5 Corrective Action -,; -.<
27.5.1 If an LCS compound recovery;i:s outside the criterion,
reanalyze the LCS. If upon reanalysis an LCS compound
recovery is still outsider'the criterion, the LCS and all
associated field and QCCamples shall) be reextracted and
reanalyzed. •".''•'
27.5.2 If the SMC is less than 20 percent,.greater than 200 ,
percent, or if peak interferences luce.-present in the LCS,
sample analyses shall be stopped and tiie LCS reanalyzed. If
the LCS SMC recovery is still outside QC '.criteria upon
reanalysis, coireaci3re|;iac|4^n shall be performed and the LCS
and all associated samples sliall be reextracted and
reanalyzed. ,' ,,, '•• ; •
27.5.3 If the RT or RRT fof^any |£S compound is not within the RT
and RRT windows establishes from the low concentration
standard during the initial calibration, reanalyze the LCS.
If uppii aseabalysis a compound is still outside the windows,
a ney l£nitiails^alibration'«ast be performed before samples
can &e analyzed^ The instroaent must be recalibrated as
described in session 8.
27.5.4 I^stfee RTS crit^iojiMs SB»t met for the LCS, sample analyses
shall} tf& ^stopped and the noncompliant LCS reanalyzed . If
the RTSi' "i,s still outside the criterion upon reanalysis,
corrective ^ition which may include a new initial
:< T.calibration shall be performed. DO NOT proceed with sample
,:;i- rs- " 'analyses until tKe||RTS is within ± 1.0 percent.
. ~
27415/5 Any samply^ processed with an LCS that is out of control
;; *$, (i.e., does snot meet any of the technical acceptance
,,*f,l criteria) ijiall be reextracted and/or reanalyzed at no
* -^, , s additional; jekpense to the Agency.
X1'!~! ' ';'
27.6 Docume'misaPCiQn ,-:
-------
EXHIBIT D
APPENBKBS
-------
APPENDIX A - DRY WEIGHT CALCULATIONS
If concentrations of target analytes in soil/solid samples are to be calculated on a dry weight basis the
percent moisture and reported concentrations shall be calculated as follows:
1. Immediately after weighing the sample for extraction, weigh 5-10 g of the soil/solid into a tared
crucible. Determine the percent moisture by drying overnigh^at I05:,- ,100
-------
APPENDIX B - GENERAL GUIDANCE FOR UNUSUAL OR
HIGH CONCENTRATION SAMPLES
Difficulties may be encountered when using the QTM methods for the analysis of unusual matrices (e.g.,
sludges, solvents, paint chips, etc) and samples containing high concentrations of target and non-target
compounds. The following suggestions and general guidance may be useful when such samples are
analyzed using the QTM methods.
1. A screening device such as a PID organic vapor analyzed (OVA) may be ased if samples are
suspected to contain very high levels of volatile organics. Such a screening device would allow the
analyst to approximate sample dilutions to protect instrumentation and to minimize unnecessary
samplereanalyses. ,,; ' ' \>,
2. For highly contaminated samples, the laboratory may consider using smaller injection volumes to
protect the instrumentation. If a smaller injection volume is used, toe instrument sensitivity may
need to be increased so that the contract required ->
4. Some types of soil/solid samples (e.g^i paiatj^ai|») laay need to be agitated prior to headspace
analysis. Agitation through techniques $uch as sdmcit^i will aelp to fractionate and disperse
these types of matrices for more effective extractions and headspace analysis.
-------
APPENDIX C - MODIFIED SOLID PHASE EXTRACTION PROCEDURES
FOR PESTICIDES AND PCBS
The following modified disk extraction procedure for water samples may be used in place of the
corresponding SPE procedures in the QTM SOW for pesticides and PCB& ;-The procedure has been shown
to be effective in the extraction and cleanup of water samples for pesticides and PCBs. However, this
procedure has not been validated by the EPA, therefore, if these procedures are used, the Laboratory must
demonstrate equivalency by meeting all methods QC requirements. : : ;
" <
Because many disk extraction vacuum hardware components are available commerciaBy, the Laboratory
should follow the manufacturers directions for the proper use of these devices. The Laboratory should
also refer to the extraction disk package inserts for additional details on the proper use of the disks and
disk vacuum apparatus.
15.6 Disk Extraction Set-up and Conditioning (Optiatt'lp /
" -f '*'' • •
15.6.1 Place a 47 nun C-18 Empore™ disk onto the base unit of a glass filtration assembly.
Gentry pinch the clamp to assure even pressure around the disk. Use of a manifold for
multiple extractions is acceptable. : ,
NOTE: If the sample contains particulates, use an in-situ prefiltration media such as
Filter Aid 400 or other conaaerdaBy Available membrane-type filter may be advisable.
The prefiltration media shouMfce placed p^M to the wash step. (When using Filter Aid
400, adjust solvent volumes to aBow bed submelston tntwtghout the procedure.)
15.6.2 Wash the extraction apparatus and disk by adding 5 ml of methylene chloride to the
reservoir, rinsing down the sides of the reservoir in the process. Draw a small amount
through the disk with a vacuum; turn off the vacuum and allow the disk to soak for
approximately one miaate. Pull the remaining solvent through the disk and allow the disk
to dry. ,/ • ' ""''v ,-: S|
•' '°V ' * W" £J
f <' .>£ y
15.6.3 Condition the disk by addin|fpproximately 5 mL of methanol to the reservoir, drawing a
small amount through the dM: then letting it soak for approximately one minute. Draw
most of the remaining methaii0l ^apugfe ie disk, leaving 3-5 mm of the methanol on the
surface
NOTE: THE DISK SMQIIfeD NOT BE ALLOWED TO GO DRY FROM THIS POINT
UJO3L 'Pffi.END OF SA!fflJ3E. EXTRACTION. RESIDUAL VACUUM IN THE
eXfRAetl^S^EVICE MttSf&E VENTED TO PREVENT THE DISK FROM
DRYING OUT.t|M|pST VACUUM MANIFOLD DEVICES AUTOMATICALLY
VENT WHEN THW«ACUUM IS TURNED OFF. THE VACUUM LINE MAY
NEED TO BE DISCONNECTED IN ORDER TO VENT THE RESIDUAL VACUUM
IF SUCTION FLASKlfi&RE USED. SHOULD THE DISK ACCIDENTALLY GO
DRY, SIMPLY REPEllr THE METHANOL CONDITIONING STEP.
15.6.4 Add 10 mL of reageat!*vater to the disk. Using the vacuum, pull most of the water
7 3-5 mm of water on the surface of the disk.
' V ,' -¥
15.7 Compound ExtractioHiaaS Elution Using Disks (Option 2)
15.7.1 Add 0.5 mL of methanol to the water sample and mix well.
-------
15.7.2 Add the water sample to the reservoir and filter as quickly as the vacuum will allow.
Drain as much water from the sample bottle as possible.
15.7.3 Remove filter assembly and insert suitable sample tube for eluate collection.
15.7.4 Add 5 mL of methylene chloride to sample bottle. Rinse bottle thoroughly and set aside
momentarily.
15.7.5 Wet the disk with a small amount of acetone - just eaough to wetthe surface
(approximately 0.5 mL) and immediately transfer the methylene chloride from the sample
bottle to the disk with a disposable pipette, rinsing sides of the filtration reservoir in the
process.
15.7.6 Draw half of the solvent through the disk then release the vacuum. Allow the remaining
methylene chloride to soak the disk for approximately 1 minute then draw remainder
through under vacuum.
15.7.7 Repeat the solvent rinse of the sample bottle using 5 ttL of methylene chloride and
transfer to the apparatus, rinsing down the sides of the reservoir. Add 5 mL of methylene
chloride directly on the disk, let soak for approximately 1 minute, and draw through under
vacuum. :
15.7.8 Add 8 g of anhydrous sodiu^.dd£ateK},l|cy^e,,eluate. Pipet the eluate into a
concentrator tube. Rinse the ^collection tubl and sodiian sulfate with two 5 mL portions
of methylene chloride and combine the rinsatesiwfth the sample eluate in the concentrator
tube. NOTE: If large clumps form on addition of the sodium sulfate to the sample
eluate, break up the clumps before adding the rinses.
15.7.9 Pesticides - Concentrate extract to approximately 2 mL under gentle stream of nitrogen
(may be wanned gently - approximately 30 degrees C) Add hexane/acetone (9:1) to bring
volume to 10 ml, then blowliown to 1 ml. '»
PCBs - Coficentrate extract to approximately 2 mL under gentle stream of nitrogen (may
be wanned gently - approximately 30 degrees C.) Add hexane to bring volume to 10 ml,
then blow down to approxsnitefy 4 ;ntl and- adjust to 10 ml final volume with hexane.
NOTE: To minimize analyte loss due to volatility, occasionally rinse sides of centrifuge
and concentrator tubes witli methylene chloride, hexane/acetone, or hexane, as
appropriate, during the blowdown procedure.
;'-J * Y* ^ '
15.7.10 Continue with the florisil cleanup procedure for pesticides analysis or sulfuric acid and
; florisil procedure fot|l?CB analysis as described in the methods.
-------
DRAFT
EXHIBIT E
QUALITY, ASSURANCE/QW&LITY CONTROL
F .^.REQUIREMENTS,
-------
DRAFT
TABLE OF CONTENTS
SECTION
Overview
I Introduction ,,.
II Good Laboratory Practices »,;,. .
Ill Quality Assurance Plan ,', ....
IV Standard Operating Procedures „•,'„
V Analytical Standards Requirements
VI Contract Compliance Screening
'it,' -^ ;.
VII Regional Data Review <*;;'
VIII Performance Evaluation Samples ....
IX Data Package Audits .,..».
X On-Site Laboratory, Evaluations ....
XI Quality Assurance And Datat'^ferend Analysis
XII Data Management
PAGE
E-3
E-4
E-6
E-7
E-12
E-19
E-25
E-27
E-28
E-31
E-33
E-36
E-38
E-2
08/23/94
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DRAFT
OVERVIEW
A comprehensive quality assurance and quality control program is an integral
part of the Environmental Protection Agency's (EPA's) Contract Laboratory
Program (CLP). The quality assurance (QA) component includes management
review and oversight at the planning, implementation;, and completion stages of
the environmental data collection activity to ensure that data provided are of
the quality required. The quality control (QC) system includes- those
activities required during data collection to produce the data <y,.ihe QC system are
corrected. After environmental data are collected:, ;(JA activities focus on
assessing the quality of data obtained to determine ffcs .suitability to support
enforcement or remedial decisions. * :.
This Exhibit describes the overa^s'tppStr^iias^urance/quality control
operations and the processes by witipeh tne tJEBi^eifc*Jthe QA/QC objectives
defined above. This contract requiases a varief^^of'QSI/IJC activities. These
contract requirements are the minimum'^JA/QC activities necessary to satisfy
the analytical requirements associated with :;the determination of the different
method analytes. The requirements are designed to facilitate laboratory
comparison by providing USEPA with data from all Contractors. These
requirements do not release iflie >analytical*45©ntractor from maintaining their
own QC checks on method;and insfcctiment performance.
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SECTION I
INTRODUCTION
Appropriate use of data generated under the wide range of analytical
conditions encountered in environmental analyses requires .reliance on the QC ,
procedures and criteria incorporated into the methods. Thai methods in this
contract have been validated on samples typical of-those received by the
laboratories participating in the CLP. However, the validation, f§£ these
methods does not guarantee that they perform equally well for all-:saiBple
matrices encountered. Inaccuracies can also jifce'sult from causes other-,tfean
unanticipated matrix effects, such as samplMg artifacts, equipment
malfunctions, and operator error. Theref a-^tlfede to cons'fcpscting quality assurance project plans,
quality c^tstrol programs^ *%£ a quality assurance organization. It is,
however,",-aai explanation ofttta&e QA/QC requirements of the program. It also
outlines some minimum standards for QA/QC programs and includes specific items
that .jSf-e required in a QA Pl^O- Delivery of this documentation provides the
Agency*iiSffch, a complete data package which will stand alone, and limits the
need for *GbjStact with the Cajatractor or with an analyst, at a later date, if
the analys is:"fe j-Ques tioned> S;
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To assure that the product delivered by the Contractor meets the requirements
of the contract and allows inter- laboratory data comparison, the Agency has
established the following contract requirements.
• Preparation of and adherence to a written Qualitf- Assurance Plan, the
elements of which are designated in Section I-IIJi ~u
* Preparation of and adherance to QA/QC Standard Operating- procedures
(SOPs) as described in Section IV. ";? =,
i ?* *
, ;-:« > '
• Adherence to the QC and analytical methods specified in the contract.
• Verification of analytical standards ,ahd documentation of the purity of
neat materials and the purity and a«*airacy of so;itttions obtained from
private chemical supply houses. " '•*} -;,, ;j,
''•• , :-2 - , ,;••
• Participation in the analyses of Laboratory, ^valuation Samples,
including adherence to corrective action
Submission of all raw data and pertinent documentation, "for Regional
review.
Participation in on-site laboratory evalyajcibns^ 'including adherence to
corrective action procedures. "'; ; v|:'
Submission of all original documentation generated during sample
analyses for Agency review. -;'
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SECTION II
GOOD LABORATORY PRACTICES .
Good laboratory practices and good automated laboratory practices are
defined as those common sense procedures carried o«,t fey qualified laboratory
personnel to ensure the quality and integrity of die analytical data being
produced. By following the specific analytical and reporting procedures
outlined in this SOW, the Contractor will produce analytical daibaiof known and
documented quality. Data integrity is defined,*as ensuring that data,are
complete, consistent, and without errors, and>|ensuring the prevention, of
information corruption and unauthorized data modification.
.: v"
Good laboratory practices and good aSatomated laboratory practices are
managerial concepts covering the organizat^^^al procefes and the conditions
under which laboratory studies are planned, periorjp*e4, monitored, recorded,
and reported. Good laboratory practices and good;aatomated laboratory
practices include but are not necessarily limited to procedures, programs, or
statements regarding schedules, plans, standard operating procedures,
inspections (procedural, process,/«andsfacility), audits (data, report, and
computer), quality assurance sta§ejii»i:||;^Qbiyes, and staff records. Good
laboratory practices and good autoinated. l5iboisa.to;ry: practices also include but
are not limited to classification !&:•-.work (such-'!as'"R&S'4?S SAS, government vs
private), sample retention procedures^,^equipBSSSt calibration and maintenance,
characterization requirements of samplje^ (st»efti as identification and
stability), method and software validatieaq,'^^approval of supplies and
standards, traceability of standards bacfc'.tsb their origin, sample and data
chain-of-custody, inspec1iitm:fis£>,electronic sand hardcopy data and data
packages, computer and'facilityjjkecurity, stskff training, and monitoring by
the laboratory's quality assurafsleV officer. * ;,
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SECTION III
QUALITY ASSURANCE PLAN
Overview ,,' /
The Contractor shall design and implement a Duality assurance program
with the objective of providing sound analytical chemical measurements .
This program shall specify the quality control procedures , ,»e©rrective
action procedures, and all documentation required during data ;
collection, as well as the quality assessment measures performe4',by
management to ensure acceptable data production. As evidence of such a
program, the Contractor shall prepare ',-& written Quality Assurance Plan
(QAP) which achieves the following. :
• Maintains data integrity, validity, Jand''-tjsability.
• Ensures that analytical measurement systep&s ,,are maintained in an
acceptable state of stability and reproducli>ili.ty .
• Detects problems t&rmjp^^^''.!*8^5313161^ and establishes
corrective action procedures whl«.1S,lSes*|>;t^|e analytical process
reliable. , " '•'••'•
• Documents all aspects of tiie measurement process in order to
provide data which are technically sound and legally defensible.
The QAP shall presetit^in specific t%rms, the policies, organization,
objectives, functional gtai4$lines» and Specific QA and QC activities
designed to acM&ve the dalpt; quality requirements in this contract.
Where applicable, SOPs pertaining to each element shall be included or
referenced a^lgart of the ^^f.^^The ,,,QAP shall be available during the
on -site laborietary evaluat^eStl.^aM^bwtf be submitted within seven days
of written request/|»y the TPO, EMSL-LV, and/or NEIC. Additional
information relevant/ib,- the preparation of a QAP can be found in EPA and
ASTM publications. ' V ,
2 Elemeects'- cff " a:s-QqilttV Assurance JP Ian
\- ' ' ****< "'>-
2 . 1 Onganization and PerSs^onel
, :: VM
/r|;.;l.l QA Policy and Ob^ctives
* Management ^:
Assigboent of QC and QA Responsibilities
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• Reporting Relationships
• QA Document Control Procedures
• QA Program Assessment Procedures "
2.1.3 Personnel =
• Resumes '"- .
• Education and Experience Pertinent to This Contract -^nd as
Specified in Exhibit A '
• Training Programs >
2.2 Facilities and Equipment ':'•• „ ;:
2.2.1 Instrumentation and Backup Alternatives -
2.2.2 Maintenance Activities-and Schedules
''"" *-»." X'V ,;-"'. f ,,
2.3 Document Control '*;., "' *-'"".;ts" /
2.3.1 Laboratory Notebook Policy J
2.3.2 Sample Tracking/Custody Proe<&&ures
2.3.3 Logbook Maitg&esgai$e,-and Archivia^ Procedures
;./7 " '"'^i, 'V-
2.3.4 Case Fil£,!®rganizati%liv Preparatieb, and Review Procedures
2.3.5 Procedures for Prepaf4fe^n-'-A!5P-3roval' Review> Revision, and
Distribidbm of ' '~
2.3.6 Process for ReVisipn of Technical or Documentation Procedures
2.4 Analytical'IKetfeed.ology Si j ,
2.4,/l!-Calibration'Procedures and Frequency
2;*|s=.2 Sample Preparation/Extraction Procedures
'"Si"|4«'Ji Sample Analysis It|?ocedures
2.4.4 ^taaiiards Preparation Procedures
Initiatioti>i>i^ 'Corrective Action
2.4.5 Decisiob.^roc^ses, Procedures and Responsibility for
Act!
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2.5 Data Generation
2.5.1 Data Collection Procedures
2.5.2 Data Reduction Procedures
2.5.3 Data Validation Procedures : -,:
2.5.4 Data Reporting and Authorization Procedures l'!
•
2.6 Quality Control f
2.6.1 Solvent, Reagent, and AdsorbentJgheck Analysis
2.6.2 Reference Material Analysis (
2.6.3 Internal Quality Control Checks
2.6.4 Corrective Action and Determination of QC Iand.£ Procedures
V* ,
2.6.5 Responsibility Designa££$&';- ,; *~
'- / ' 'v %/* '"•- >.
2.7 Quality Assurance ;•••
2.7.1 Data Quality Assessment f :;=
2.7.2 Systems/Internal Audits
2.7.3 PerformanpBii^xtenialll&udits ; ,.;
.: h •$, ''-I
: ; t* ' ( -
2.7.4 CorrectiveAction Procedures
>; ;;-^ , ,
2.7.5 Quality*A|sESurance
2.7.6 Responsibility^l)«|ignation
3 Updating-^aad-ISti&mitting the JQAg
3.1 Initial Submission"'-,
/.: C ,j-
".ng the contract solicitation process, the Contractor is required to
unit their QAP to EMSt-LV and NEIC. Within 60 days after contract
, the Contractor Shall revise the QAP to be in full compliance with
the!4*ejfuirements of thfbs contract. The Contractor shall maintain the
revised-^|HP, on file atffsthe Contractor facility for the term of the
contract/ :4&e>;revise
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DRAFT
3.1.1 Changes resulting from 1) The Contractor's internal review of its
organization, personnel, facility, equipment, policy and
procedures; and 2) The Contractor's implementation of the
requirements of the contract; and :
3.1.2 Changes resulting from the Agency's review io.f - the laboratory
evaluation sample data, bidder supplied documentation, and
recommendations made during the pre-award on-site; laboratory
evaluation. -''. •
3.2 Subsequent Updates and Submissions •" ?
During the term of the contract, the,i@bntractor stiall amend the QAP when
the following circumstances occur:,( :s ;|
• The Agency modifies the contract; '•>« >, - "
• The Agency notifies the Contractor of deficiencies in the QAP;
The Agency notifies the- Contractor of deficiencies resulting from
the Agency's review e£Iftlife r£&a£factor's performance;
• The Contractor identifies deficiencies resdlting from its internal
review of its QAP; '•"' i
'j, ' £*••''
• The Contractor's organization, ^personnel, facility, equipment,
policy, or procedures change; and
• The Contractor identifies deficiencies resulting from the internal
review of_'S±s organi'faition, persofinbl, facility, equipment,
policy, br procedures Jehanges.
The Contractonslmll amerailiJfeeJ^illMl^iiin 30 days of when the
circumstances lis?te*t above result in a discrepancy between what was
previously describee! ,.iiiv>the QAP and what is presently occurring at the
Contractor's facility. : f^ .
ATP"is-i^«^aded, ali'*'-ekinges in the QAP shall be clearly marked
a bar in thtejajargin indicating where the change is found in the
or highligHfclkig the change by underlining the change, bold
tting the change, o&using a different print font). The amended
:tion pages shall hai|i&> the date on which the changes were implemented.
vt&g]Spntractor shall iiieorporate all amendments to the current QAP
docMa^at. The Contractl&r shall archive all amendments to the QAP
document:^«>r future x^lerence by the Agency.
" « 'i^ -^'.
The Contractor is3mpl^ send a copy of the current QAP to the designated
recipients withiiS 'Seven days of a request by the TPO or NEIC.
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3.3 Corrective Action:
If the Contractor fails to adhere to the requirements listed in this
section, the Contractor may expect, but the Agency is not limited to the
following actions: reduction of numbers of samples sent under this
contract, suspension of sample shipment to the'-Contractor, data package
audit, an on-site laboratory evaluation, remedial laboratory evaluation
sample, and/or contract sanctions, such as a Cure Notice,';
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SECTION IV
STANDARD OPERATING PROCEDURES
Overview
In order to obtain reliable results, adherence to prescribed analytical
methodology is imperative. In any operation1- that is peaSfbrmed on a
repetitive basis, assurance of data quality and reproduci-bllity is best
accomplished through the use of SOPs. As,=!defined by the EPAi .an SOP is
a. written document which details an operation, analysis, or action which
is commonly accepted as the method fpri performing certain routine or
repetitive tasks. ; „
%* s" ^ '
SOPs prepared by the Contractor shall! j»y the TPO atip^sr NEIC;
• , ~'. '^Capable of providing for the development of documentation that is
,, '' sufficiently c^^lete to record the performance of all tasks
,;; . required by the
Capable of demonstrating the validity of data reported by the
"^Contractor and ej^lain the cause of missing or inconsistent
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• Capable of describing the corrective measures and feedback
mechanisms utilized when analytical results do not meet protocol
requirements;
• Reviewed regularly and updated as necessary when contract,
facility, or Contractor procedural modifications are made;
• Archived for future reference in useability or evidentiary
situations; - ,,'
• Available at specific work stations as appropriate; and
• Subject to a document control piNocedure which precludes the use of
outdated or inappropriate SOBs,
2 SOP Format:
The format for SOPs may vary depending upon the kind of activity for
which they are prepared. At a minimum, however, t&e following sections
must be included: , ,
• Title Page; 1.•' "'-", ; .,
• Scope and Application;
• Definitions;
• Procedures;
• QC Limits;?' '>
3 SQ? Requirements: .-• J
:;- '-. c.
'me:pontractor shall maintain the following SOPs:
'-V-,v 4K-
3.1 Evidentl^cy,, SOPs: -\/,.
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Evidentiary SOPs for required chain-of-custody and document control are
discussed in Exhibit F, "Specification for Written Standard Operating
Procedures."
3.2 Sample Receipt and Storage:
• Sample receipt and identification logbooks;
• Refrigerator temperature logbooks; E: ,
• Extract storage logbooks; and ,, ,s. - '.''
m Security precautions. , ':' ~
3.3 Sample Preparation: -;"-,-
• Reagent purity check procedures and iSQCtaaentation;
• Extraction procedures; •';=
• Extraction bench she&£s'; \%BQ&;^. •-., ,,
'"'..(?. ' "::- *'•'""!;V " =
• Extraction logbook maintenance. • / " ' '•- '••'-,
3.4 Glassware Cleaning !;; -;'"':
3.5 Calibration (Balances): :
' • '""; ",
• Procedures; V "' fc- •'* •-
•f~: ' V, •'•;
• Frequency-requiremenisi;
• Acceptaheeacriteria£SaSj,-,^EK||^ctiTre actions; and
~ ; ,v J,
• Logbook maintenaac^ authorization.
3.6 Analyticjal>!r«pedures (£or'f&&i$h analytical system):
• ';? -i"Instrument pe^^rmance specifications;
,^4'- 'f|,.
pi:.'s Instrumental operating procedures;
il">' '-"-',!
,*£/-.. . . . "••'!
"* ,~S|Q,, Data acquisition;afystem operation;
• '!KjE»efedures whe^islutomatic quantitation algorithms are overridden;
• QC - req^red ^g^rameters;
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• Analytical run/injection logbooks; and
• Instrumental error and editing flag descriptions and resulting
corrective actions.
3.7 Maintenance Activities (for each analytical system)i
• Preventive maintenance schedule and procedures;
• Corrective maintenance determinants ^and procedures; arid,:
• Maintenance authorization. :- ;'
3.8 Analytical Standards: , ;
• Standard coding/identification arid, :i.syentory system;
• Standards preparation logbook(s);
• Standards preparation^procedures;
• Procedures for equiva%ency/trIc^&Eiiity sanalyses and
documentation; ' =;;: : " '
• Purity logbook (primary standards-iand solvents);
• Storage, replacement, and labeling requirements; and
'• ;•' r ''• '
• QC and corrective" action measures.?.
3.9 Data Reduction ^Procedures: =:,
• Data pro«&sssing sys4©aei,:'o|idRat;f«n;
": j'; •
• Outlier identification methods;
• Idemttficajtion of data-icequiring corrective action; and
• .JjJfrocedures f6^;fpormat and/or forms for each operation.
3.10 O^^imentation Policy/Pj^cedures:
•:-JT f*
m^J, 4>, Laboratory/analyses' notebook policy, including review policy;
' '.5*5 *! '''-'i'
Batch, &.e (CBF) contents;
Complete^ ;Sat
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DRAFT
• Document inventory procedures, including review policy.
3.11 Data Validation/Self Inspection Procedures:
• Data flow and chain-of-command for data .review;
• Procedures for measuring precision and accuracy;
• Evaluation parameters for identifying systematic errors;
• Procedures to assure that hardcopy and electronic deliverable are
complete and compliant with the ilr-equirements in SOW Exhibits B and
H; , ,
• Procedures to assure that hardcopy deliverables are in agreement
with their comparable electronic SfeMveirables;
• Demonstration of internal QA inspection ptsscedure (demonstrated by
supervisory sign-off on personal notebooks, -internal laboratory
evaluation samples, ete,).J
Frequency and type of ijtetiternaT TatiilJBS -;fe^g. «, xandom, quarterly,
spot checks, perceived^t^puble areas}; '•''• *
Demonstration of problem Hfeutifieation-corrective actions and
resumption of analytical processing. Sequence resulting from
internal audit (i.e., QA feedKack); and
• Documentation of 'a&ft$£ reports 'Cisternal and external) , audit
response^ -corrective'^action, etc-;
3.12 Data Management and Handlifi^ ,,„„ -,^-, -,-„,,
• Procedures 'for -.controlling and estimating data entry errors.
• Procedures for revj,e»ing changes to data and deliverables and
ensttrla&g- tcaceabilityJ^fe.updates .
I. " "*,-': ;_ "*i""'
• ,,<;!-Lifecycle manj|gi^ment procedures for testing, modifying, and
;-f '• implementing clffii^es to existing computing systems including
.-!* hardware, softwai^i, and documentation or installing new systems.
- -K 5
: ' &,-, ,^
~»|:;j, j,- Database securitj^ backup and archival procedures including
from system failures .
u ,
System jffiaintenance procedures and response times .
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• Individual(s) responsible for system operation, maintenance, data
integrity and security.
• Specifications for staff training procedures.
4 Delivery Schedule: Updating and Submitting SOPs -;• ;=
4.1 Initial Submission : ; :.
"" ! i, s,.
During the contract solicitation process £ the Contractor is "igeqwired to
submit their SOPs to EMSL/LV and NEIC.jT Within 60 days after contract
award, the Contractor shall revise thesset of SOPs to be in full
compliance with the requirements of this contract* The Contractor shall
maintain the revised set of SOPs on^file at the ^Contractor facility for
the term of the contract. The revised lSSQ.Ps will 'become the official
SOPs under the contract and may be used 'IftJasLgg; 'legal proceedings. The
revised SOPs shall include: ';' •
4.1.1 Changes resulting from A) The Contractor ' s :?i^t.ernal review of its
organization, personnel?, facility, equipment, -policy and
procedures, and B) T&:^x^r3aet:o|:,',s implementation of the
requirements of the extract;
- -s'- .-;; " ' ' • '
'I ••>'' • • '
4.1.2 Changes resulting from the: -Agency ^i review of the laboratory
evaluation sample data, bidder supplied documentation, and
recommendations made during the ?||>re- award on-site laboratory
evaluation. :" :
4.2 Subsequent Updates "and Stibsiissions : ,
- * > ' ^ . v - ,
; . ' ~*i*
During the tesm. of the contract, the Contractor shall amend the SOPs
when the f clipping circums^Ssieices, .occur:
The Agency%edifies the contract;
The Agency notifi!es::$lie Contractor of deficiencies in its SOPs;
?5pp6 "^getey^'^^if ies thtf '<5j?ntractor of deficiencies resulting from
the Agency 's«i^wiew of the Contractor's performance;
' "1;^
y,~n
The Contractor ' sjljprocedures change;
The Contractor identifies deficiencies resulting from its internal
; review of its SOfbjS documentation; or
'" ' ' 5 f •* ' ; '
The y3B$t,ractoip3;dentif ies deficiencies resulting from the internal
";; i,ts procedures .
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The Contractor shall amend the SOPs or write new SOPs within 30 days of
when the circumstances listed above result in a discrepancy between what
was previously described in the SOPs and what is presently occurring at
the Contractor's facility. When the SOPs are ajasnded, all changes shall
be clearly marked (e.g., a bar in the margin indicating where the change
is found in the document, or highlighting the ehauge by underlining the
change, bold printing the change, or using a-diffeBBsrt^print font). The
amended/new SOPs shall have the date on which the changes were
implemented. h
When the SOPs are amended or new SOPs ar« written, the Contractor:shall
document in a letter the reasons for £he changes, and submit the amended
SOPs or new SOPs to the TPO, EMSL-LVs^f^uality assurance/technical SOPs),
and NEIC (evidentiary SOPs). The G|ji$|ractor shajll send the letter and
the amended sections of the SOPs or'ia^r ,SOPs witfein seven days of the
change. An alternate delivery schedule 'ifOT £tar submittal of the letter
and amended/new SOPs may be proposed by the ;J©b&tractor, but it is the
sole decision of the Agency, represented either"by the TPO or APO, to
approve or disapprove the alternate delivery schedule. If an alternate
delivery schedule is proposed.,, the Contractor shall describe in a letter
to the TPO, APO, and the C4o3ftii^:^|g^>^£lcer why he/she is unable to
meet the delivery schedule lifted *i!itf'%lfe;Be«fci,O3tt,, .The TPO/APO will not
grant an extension for greateifkthan 30 dffs for amending/writing new
SOPs. The TPO/APO will not gr^st, an extension for greater than 14 days
for submission of the letter doctoaenting the reasons for the changes and
for submitting amended/new SOPs. St&^i6ontractor shall proceed and not
assume that an extension will be gristed until so notified by the TPO
and/or APO. ,, - .,
The Contractor Miall send 'j^eomplete set? -of current SOPs or individually
requested SOPsf=,%o the reci^p&its he/she designates within seven days of
a request bjri^e TPO, APO ^0J;,,J|E JC ,,^ Documentation of the reasons for
changes to the'^Es shallf^tlSi^i/r^Wipitted along with the SOPs.
4.3 Corrective Action: =:
•' ' ; 5 '.'
If the ,jpo3Etr«HStQr fails tc* ISJiiere to the requirements listed in this
sectieaii; •'ttie^Contxa^tor may fe«|H^ct, but the Agency is not limited to the
folii»n.ng actions : %«i«iuction of numbers of samples sent under this
copeieiract, suspension '^1 sample shipment to the Contractor, data package
pl.t, an on-site laboimtory evaluation, remedial laboratory evaluation
and/or contracd||$anctions , such as a Cure Notice.
*
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SECTION V
ANALYTICAL STANDARDS REQUIREMENTS
Overview
The U.S. Environmental Protection Agency (EPA)'will™tM>;t supply
analytical reference standards either for direct analytical measurements
or for the purpose of traceability. All contract laboratories will be
required to prepare from neat materials -a* purchase from private
chemical supply houses those standards .necessary to successfully
accurately perform the analyses required in this protocol.
Preparation of Chemical Standards fffom the Neat Sigh Purity Bulk
Material '- .•>*• > -1 <
A Contractor may prepare their chemical standards from neat materials.
Commercial sources for neat chemical standards pertaining to compounds
listed on the Target Compound List (Exhibit C) axe -given in Appendix C
of the "Quality Assurance Materials Bank: Analytical;Reference
Standards" Seventh Edition^ 3®xsijigK$/;]L9&&,. Contractors shall obtain the
highest purity possible whetti^urchaiittg^^j£fcj:j:i|emical standards; when
standards are purchased at less than 97%^piri"sfcyv'i'he Contractor shall
document the reason why a higher puritylicould not be obtained.
2.1 Neat chemical standards shall be kept; Tefrigerated when not being used
in the preparation of standard solutions. Proper storage of neat
chemicals is essential|ia order to safeguard them from decomposition.
2.2 The purity of a>eompound cam sometimes %e.misrepresented by a chemical
supply house, ulgince knowleU|j;e of purity :is needed to calculate the
concentration^f solute ia^rsplution, standard, it is the laboratory's
responsibilitys;CO(...have an^jifet^&t.sliqsgtimentation ascertaining that the
purity of each compound is correctly stated. Purity confirmation, when
performed, should use,|tei|her differential scanning calorimetry, gas
chromatography with fllsaa^ SLonization detection, high performance liquid
chromatogr^pf^i :JLnfrared spfjBCtarometry, or other appropriate techniques.
Use ptf,: &^}"o™f"Tie^efe1iindependehieri«ethods is recommended. The correction
fao|%r for impurity|^feen weighing neat materials in the preparation of
solution standards is-:
Equati&f 1 \g,
, weight of impuM compound = ^eigrht of puze compound
,;= •., ;, (percent purity/100)
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where "weight of pure compound" is that required to prepare a specific
volume of a solution standard of a specified concentration.
When compound purity is assayed to be 97 percent5, or greater, the weight
may be used without correction to calculate the/;eoncentration of the
stock standard. If the compound purity is assayed -to De less than 97
percent, the weight shall be corrected when cu'lculatfkig, the
concentration of the stock solution. •/'-•
2.3 Mis -identification of compounds occasionally occurs and it
that a mislabeled compound may be received from a chemical supply house.
It is the laboratory's responsibility :;|E0 have analytical documentation
ascertaining that all compounds used lin the preparation of solution
standards be correctly identified. ^t^pLentificatjipa confirmation, when
performed, shall use gas chromatograplij'J^aass spectrometry analysis on at
least two different analytical columns , *<**:• lotSer appropriate techniques.
2.4 Calculate the weight of material to be weighted; iNit for a specified
volume taking into account the purity of the compound and the desired
concentration. A second person,,, shall verify the accuracy of the
calculations . Check balan4fg^1Bfec^i^a^ac^, with a set of standard
weights. All weighing shoul^be pe^fia"iaifei:-<
Soluti6%s'|of analytic^ reference standards can be purchased by
meet the following criteria:
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DRAFT
3.1 Contractors shall maintain the following documentation to verify the
integrity of the standard solutions they purchase:
3.1.1 Mass spectral identification confirmation of the neat material;
3.1.2 Purity confirmation of the neat material» arid
3.1.3 Chromatographic and quantitative documentation that the solution
standard was checked according to the following section.
3.2 The Contractor shall purchase standards! for which the quality is
demonstrated statistically and analytically. One way this can be
demonstrated is to prepare and analyse three solutions; a high standard,
a low standard, and a standard at tfe^ target concentration (see 3.2.1
and 3.2.2 below). The Contractor shall have documentation that the
analytical results for the high standard and -law standard are consistent
with the difference in theoretical concentrations. This is done by the
Student's t-test in 3.2.4. If this is achieve*!, 'She Contractor shall
then demonstrate that the concentration of the target standard lies
midway between the concentrations of the low and high standards. This
is done by the Student's twfses*,!.$ix 3L.2-.j5... Thus the standard is
certified to be within 10 percent o£ IfKe {$axgga% concentration using the
equations in 3.2.6.
If the procedure above is used, tihe Contractor shall document that the
following have been achieved:
3.2.1 Two solutions-of .Identical concentration shall be prepared
independently from ssefat materials,. An aliquot of the first
solution^sKall be di&fced to the Intended concentration (the
" target ^standard"). p^as aliquot is taken from the second solution
an diluted to a concfBtxation.jten percent greater than the target
standard, j^fbis is .^llktfcttfce^liigh standard". One further
aliquot is '"t^kesn from the second solution and diluted to a
concentration 10:f^ercent less that the target standard. This is
called the " low
k replit^t^jjanalyses ofiseach standard (a total of 18 analyses)
y-shall be per'fl^aed in the following sequence: low standard, target
* standard, high^i^andard, low standard, target standard, high
standard, . .. :sr
1:
\, The mean and varjkpice of the six results for each solution shall
calculated. ,'!'
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DRAFT
MEAN = (yx + y2 + y, + y4 + ys + y6) /e
Equation 3 >
(y? + y22 + y| + yt2 + y| + if - 6*;{«EAW) 2/s
The values Y, , Y2, Y3 ..... represent the results of :ttte six
analyses of each standard. The means of the low, target!,; .and high
standards are designated M.,, Mj, and Mj, respectively. The'?*'
variances of the low, target, ab4':-high standards are designated
Vv V2, and V3, respectively. .additionally, a pooled variance,
V , is calculated. , ,
Equation 4 ':: ' ''',
If the square root offi^Las less than one percent of Mj, then
is to be ti^Jdbte s^fiLue of v in all subsequent
calculations. *" " " ''
3.2.4 The test statistic shall ^ calcxiated:
Equation 5 , -
ZEST STATISTIC = ] (M3/l . 1 ) - .(A^/0 . 9 ) |/ ( V3 )°'S
•" ' .''"":; V
If the tesjt statisticjiexceeds 2.i3;4then the supplier has failed to
demonstrate a 20 percjarit differences between the high and low
standards . In such 4i*«as^*- -fcb£ standards are not acceptable.
i ' ''" - '' " '
3.2.5 The test statistic shall be calculated:
Equation 6 ,;
. s) - (#3/2.2) | / (Vp/4) ° •s
.-ir:
< ••
If the test stata&tic exceeds 2.13, the supplier has failed to
demonstrate that|fSie target standard concentration is midway
between the highiftid low standards. In such a case, the standards
not acceptabfte'.
'
3.2.6 The ~ $>$ -percent Confidence intervals for the mean result of each
standard ^shaiij-'be calculated:
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DRAFT
Equation 7
Interval for Low Standard = M^ ± (2.13) (V^/6)0-5
Equation 8
Interval for Target Standard = A^ ± (3U13 )!;:
Equation 9 :-s ::
Jnterva-Z for High Standard = A£ * (2 . 13) { V6) °'5 :
These intervals shall not overiap. If overlap is observed, then
the supplier has failed to deafcrastrate the Ability to discriminate
the 10 percent difference in concentrations . In such a case , the
standards are not acceptable. '•• : ;• ,, ;;r
In all cases, the Contractor is responsibly ~f or the quality of the
standards employed for analyses under this sboatract.
4 Requesting Standards f rom -tabs Slfefif "Staandards Repository
Solutions of analytical refer«ace materials can =b« ordered from the U.S.
EPA Chemical Standards Repository, depending on availability. The
Contractor can place an order for staialards only after demonstrating
that these standards are not available' from commercial vendors either in
solution or as a neat material. ;~
Documentation oft tAie VerMtpation and gre-paration of Chemical Standards
It is the responsibility ofljeach laboratory to maintain the necessary
documentatiah!;;to show tha£ '^Jig s chemical standards they have used in the
performance of^Cfcl' analyg§S^MBfec«b| 3» the requirements previously
listed. Weighing lo,gbooks , calculations, chromatograms , mass spectra,
etc. , whether produee«catory evaluations. Documentation of
standards "prepasaiipn may be c«guired to be sent to EPA for verification
of jttotitract complimif;^. In those cases where the documentation is
s^|5j»ortive of the aiiajjjrtical results of data packages sent to EPA, such
j3»Sumentation is to be|&ept on file by the laboratories for a period of
year. ^-:f
by the TpKor APO, the Contractor shall submit their most
resent *ptee?rious year.'lUdocumentation (12 months) for the verification
and preparation of iisibemicals standards within 14 days of the receipt of
request to tfeejr^cifjients he/she designates.
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DRAFT
The Agency may generate a report discussing deficiencies in the
Contractor's documentation for the verification and preparation of
chemical standards or may discuss the deficiencies during an on-site
laboratory evaluation. In a detailed letter to t&e TPO, APO, and EMSL-
LV, the Contractor shall address the deficiencies and the subsequent
corrective action implemented by the Contractor-t»-,cprrect the
deficiencies within 14 days of receipt of the-report ;«r the on-site
laboratory evaluation. An alternate delivery schedulejinajr be proposed
by the Contractor, but it is the sole decision of the Ageaaisgr,,,
represented either by the TPO or APO, to,lapprove or disapprove ^he
alternate delivery schedule. If an alternate delivery schedule'is
proposed, the Contractor shall describe! in a letter to the TPO, APO, and
the Contracting Officer why he/she is ,i*mable to meet the delivery
schedule listed in this section. Tt^TPO/APO will not grant an
extension for greater than 14 days reatfllJie Contractor' s response letter
to the standards documentation report. :<33isa Contractor shall proceed and
not assume that an extension will be granted ?until so notified by the
TPO and/or APO. ' ,.
If new SOPs are required to^he written or SOPs are recjuired to be
amended because of the defi-.'* ~
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DRAFT
SECTION VI
CONTRACT COMPLIANCE SCREENING.
Contract Compliance Screening (CCS) is one aspect of ; the Government's
contractual right of inspection of analytical data,, /-CCS -^examines the
Contractor ' s adherence to the contract requirements based I "" '"'" :'^ i •'•<- - -
The Agency may generate a CCS trend; report whibn; summarizes CCS results over a
given period of time. The Agency may; send tbe CCS trend report or discuss the
CCS trend report during an on-site laboratory-evaluation. In a detailed
letter to the TPO and APO, the Contractor shall address the deficiencies and
the subsequent corrective action implemented by the Contractor to correct the
deficiencies within 14 days^slf; receipt of tfee, report or the on-site laboratory
evaluation. An alternate delrasejcy schedule i^say be proposed by the Contractor,
but it is the sole des&ision of tUifi,, Agency , represented either by the TPO or
APO, to approve or, disapprove the Alternate delivery schedule. If an
alternate deliverytschedule is paf^o^ed,, the Contractor shall describe in a
letter to the TPO,sAIp^,,and thei'fclibtKme£3Jgg 'Officer why he/she is unable to
meet the delivery sche1&kl« listed in this section. The TPO/APO will not grant
an extension for greater ttta^a.14 days for the Contractor's response letter to
the CCS trend report. The Comix-actor shall proceed and assume that an
extension willi..t>^|;^j*asited until '-ioptified by the TPO and/or APO.
If new SQfs>are required.;^, be written or SOPs are required to be amended
because «&£ the def iciencies,,f£ind the subsequent corrective action implemented
by the, Contractor , the Contractor shall write/amend and submit the SOPs per
the requirements listed in EMttibit E, Section IV.
' "
If the Ccmtgsac.tor fails to alhere to the requirements listed in this section,
' -V '5-V1- A t .....
the Contracfcesr.pssay expect, ,;feut the Agency is not limited to the following
actions: reduction yof numbers of samples sent under this contract, suspension
of sample shipment *laa; p£h» 'Contractor, data package audit, an on-site
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DRAFT
laboratory evaluation, remedial laboratory evaluation sample, and/or contract
sanctions, such as a. Cure Notice.
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DRAFT
SECTION VII
REGIONAL DATA REVIEW
Contract laboratory data are generated to meet the,-specific needs of the EPA
Regions. In order to verify the useability of data ;for the intended purpose,
each Region reviews data from the perspective of the end-user,:«'*ad based upon
functional aspects of data quality. General guidelines for data'sSfeview have
been developed jointly by the Regions and the,national Program Offiise.., Each
Region uses these guidelines as the basis for 4ata evaluation. Indivfdiial
Regions may augment the basic guideline review process with additional review
based on Region-specific or site-specific £oticerns. Regional reviews, like
the sites under investigation, vary based^jWl the natuj?4 of the problem under
investigation and the Regional response appropriate JC0""the specific
circumstances. '•?''>• ^
Regional data reviews, relating useability of the da£a>vito a specific site, are
part of the collective assessment process. They compieiffieat the screening
performed by the CLASS contractor^ .which is designed to identify contractual
discrepancies, and the review pe3E£oiBfe8>--ft• S&SL-LV which is designed to
determine technical quality and c«nssisteiicy."S i^^e|si,3^diyidual evaluations are
integrated into a collective review; tabiat is necessary'-Coar program and
laboratory administration and managemfemt and way be used to take appropriate
action to correct deficiencies in the;Gontra<5tbr's performance.
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SECTION VIII
PERFORMANCE EVALUATION SAMPLES ,
Overview
Although intra-laboratory QC may demonstrate =€ontxactor and method
performance that can be tracked over time, axi external performance
evaluation program is an essential feature of a QA program. As a means
of measuring Contractor and method performance, Contractors-participate
in inter-laboratory comparison studies cpaducted by the EPA'51; '-litesults
from the analysis of these performance^Valuation samples (PESV<«>111 be
used by the EPA to verify the Contrac,6»rfs continuing ability to produce
acceptable analytical data. The results are also used to assess the
precision and accuracy of the analytical methodspiror specific analytes.
Sample sets may be provided to participating .Contractors as frequently
as on a Batch-by-Batch basis as zero blind (recognizable as a QC sample
of known composition); single blind (recognizable as a QC sample and of
unknown composition); or double blind (not recografcisable as a QC material
and of unknown composition) samples. The laboratory evaluation samples
may be sent to either by t^^^jra^t^ljent or the National Program
Office, and may be used for*v«bgntrac€"-&tS;'c^iv :-,--;,,-
SV; /;•'•" •" -K.''
Contractors are required to analyze the-Camples and return the data
package and all raw data within aihe contract required turnaround time.
At a minimum, the results are evaluated for compound identification,
quantitation, and saffij)i$neontand.natioxit;,. Confidence intervals for the
quantitation of ;£aa*get coagbunds are t*a*S|ed on reported values using
population statistics. ThijS&gency may aifcjust the scores on any given
PES to compensate for any unexpected difficulties with a particular
sample. The Agency will n^^tf^y^b.e^,Contractor of unacceptable
performance. ''" v>\" , -i3;"T-'i <;s'»',-fe- ';s'
2 Contractor Performance ;,t
A Contrac-tiOXl-jS results on ^Itefe-, laboratory evaluation samples will
deteraiije''tKe t^iwaeactor's peTHljsrmance as follows:
2.1 Ac»«ff>table, No Response/ Required (Score greater than or equal to 90
l^rbent): '/f
/yh %-;
fctj^meets most or all|«ff the scoring criteria. No response is
2.2 Acceptabiel./IResponsel-Bxplaining Deficiency (ies) Required (Score greater
than or equal,to 75" percent but less than 90 percent ):
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DRAFT
Deficiencies exist in the Contractor's performance.
Within 14 days of receipt of notification from tHe EPA, the Contractor
shall describe the deficiency(ies) and the actioin(s) taken to correct
the deficiency(ies) in a letter to the APO, TEOj-'and EMSL/LV.
' *;?
An alternate delivery schedule may be proposed by tfce^.Contractor, but it
is the sole decision of the Agency, represented ei their-by, the TPO or
APO, to approve or disapprove the alternate delivery scK«dt&e. If an
alternate delivery schedule is proposed,,-*8;he Contractor shall?;describe
in a letter to the TPO, APO, and the Contracting Officer why hej|&bs is
unable to meet the delivery schedule lasted in this section. The
TPO/APO will not grant an extension ;fjear greater tfean 14 days for the
Contractor's response letter to the ^laboratory ,<^luation sample report.
The Contractor shall proceed and not.a&sume thai an extension will be
granted until so notified by the TPO at&Hfm- ,Af€K
If new SOPs are required to be written or SOPs'Jare required to be
amended because of the deficiencies and the subsequent corrective action
implemented by the Contractor,,, the Contractor shall -write/amend and
submit the SOPs per the requpc^ns^acs listed in Exhibit E, Section IV.
2.3 Unacceptable Performance, Response ExplaJtoing:Ife£t;eiency(ies) Required
(Score less than 75 percent): >j
Deficiencies exist in the Contractorf?s performance to the extent that
the National Program Office has determined that the Contractor has not
demonstrated the capaMlity to meet the contract requirements.
'•$• " ' ": ." ; ,"*
Within 14 days4^f receipt of: notification from EPA, the Contractor shall
describe the deficiency(iesj^ and the actftm(s) taken to correct the
deficiency (ies) in a letter:ito the APO, TPO, and EMSL-LV.
'.;', - •'$ %•'.' is;"'v:-r
An alternate delivery,, schedule may be proposed by the Contractor, but it
is the sole decision,-,df :>the Agency, represented either by the TPO or
APO, to approve or dis^^arjpye the alternate delivery schedule. If an
alterna^ s?etel35|ery scheduler,is,.,proposed, the Contractor shall describe
in a Mfctir-fe»«iJie*a;PO, APO/4i*a the Contracting Officer why he/she is
unable to meet the^ft^Livery schedule listed in this section. The
TEQ-/APO will not graS&ran extension for greater than 14 days for the
.Qbijtrac tor's response '^letter to the laboratory evaluation sample report.
ew SOPs are require^ to be written or SOPs are required to be
ametidejd. because of the|deficiencies and the subsequent corrective action
impleiH|ilfe4 by the Cottfcractor, the Contractor shall write/amend and
submit tHe\1S©Es per^tfee requirements listed in Exhibit E, Section IV.
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The Contractor shall be notified by the TPO, APO, or Contracting Officer
concerning the Contractor's remedy for the Contractor's unacceptable
performance. A Contractor may expect, but the EPA is not limited to,
the following actions: reduction of the number
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DRAFT
SECTION IX
DATA PACKAGE AUDITS
Overview :,
• I - I ' '
Data package audits are performed by the Agency f or jprpgram overview and
specific Regional concerns. Standardized procedures have been
established to assure uniformity of the auditing process., i I>ata packages
are periodically selected from recently -;t?eceived cases. They-ar-e
evaluated for the technical quality of %ardcopy raw data, qualifrjjr
assurance, and the adherence to contractual requirements. This function
provides external monitoring of progacam QC requirements .
" „ - , ;c
Data package audits are used to assess the technical quality of the data
and evaluate overall laboratory perforrfajje«,. 'Ufiey provide the Agency
with an in-depth inspection and evaluation of Ithe Case data package with
regard to achieving QA/QC acceptability. A thorough review of the raw
data is completed including: a check of ins truments, printouts,
quantitation reports, chromatograms , deviations f rom tt&e contractual
requirements, a check for -iteabsiKci|»B;ioj8«,and calculation errors, a review
of the qualifications of th&^laboratoTyi^rseaiJel -involved with the
case, and a review of all current SOPs on/ifile. • ,
Responding to the Data Package Atidit Report:
After completion of the data package "audit , the Agency may send a copy
of the data package %-attdJbt .report to *the Contractor or may discuss the
data package audit. -report, 4aring an oiifsate laboratory evaluation. In a
detailed letter ''lo the TP0|sJAPO, and EHSJJL-LV, the Contractor shall
discuss the corrective actions implemented to resolve the deficiencies
listed in ths;;data package Japdit^ report within 14 days of receipt of the
report. An attenuate delfeidiy ittih£$u&e may be proposed by the
Contractor, but i£ Js the sole decision of the Agency, represented
either by the TPO or.&BD, to approve or disapprove the alternate
delivery schedule. I f: -in (alternate delivery schedule is proposed, the
Contr actor I shall describe"%»'^a letter to the TPO, APO, and the
Contracting "Ofeflgserpwhy he/sBeJis unable to meet the delivery schedule
lis^taila in this secAosa. The TPO/APO will not grant an extension for
gzt^ater than 14 days '^fer the Contractor ' s response letter to the
laboratory evaluations-sample report. The Contractor shall proceed and
/:aot assume that an extiejitsion will be granted until so notified by the
;; -and/or APO. ~:\,
If new jSJDBs are required to be written or SOPs are required to be
amended t>ecat^se of tijte deficiencies and the subsequent corrective action
implemented fcyJiaiej'Gbntractor, the Contractor shall write/amend and
submit the SOPs 'per the requirements listed in Exhibit E, Section IV.
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Corrective Actions
If the Contractor fails to adhere to the requirements listed in this
section, the Contractor may expect, but the Ageaey is not limited to the
following actions: reduction of numbers of samples sent under the
contract, suspension of sample shipment to the Contractor, data package
audit, an on-site laboratory evaluation, re»e4ial lafeeratory evaluation
sample, and/or contract sanctions, such as a'Cure Notitee,.
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DRAFT
SECTION X
ON-SITE LABORATORY EVALUATIONS ;
Overview .
At a frequency dictated by a contract laboratory's1 performance, the APO
or his/her authorized representative will conduct an' tm»nsJ.te laboratory
evaluation. On-site laboratory evaluations are carried"traSs-sto monitor
the Contractor's ability to meet selected terms and conditioiss ;&pecif ied
in the contract. The evaluation process incorporates two separate
categories: Quality Assurance Evaluation and an Evidentiary Audit.
Quality Assurance On-Site Evaluation , ,;" ,:
Quality assurance evaluators inspect the Contractor's facilities to
verify the adequacy and maintenance of instrumentation, the continuity
of personnel meeting training requirements, sajji^the acceptable
performance of analytical and QC procedures. The,:;|Cmtractor should
expect that items to be monitored will include, but ~m>t. be limited to,
the following items: , -'1. ;~ f' ,Si, ,
• Size and appearance of!?£he facility;
• Quantity, age, availability, scbe«tuled maintenance and performance
of instrumentation; •;
• Availability,,, a|fftsf>riateness,|,-Review of tneAj€pntractor's sample analysis/data package
--"-,->' inspection/dat» management procedures.
~^ior to an on-site evaluation, various documents pertaining to
"-^^gprmance of the spe&jbfic Contractor are integrated in a profile
pac1skge,,for discussio^iiluring the evaluation. Items that may be
incluctei,|$re previous>>iarh-site reports, laboratory evaluation sample
scores, R'i^ijopal re-s|^w of data, Regional QA materials, data audit
reports, ana;-^ata,s-alend reports.
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3 Evidentiary Audit
Evidence auditors conduct an on- site laboratory evaluation to determine
if laboratory policies and procedures are in place to satisfy evidence
handling requirements as stated in Exhibit F. \The evidence audit is
comprised of the following three activities . ; ;>
3.1 Procedural Audit: ;f
The procedural audit consists of review jaiid examination of actual SOPs
and accompanying documentation for the iipBllowing laboratory ope^rations :
sample receiving, sample storage, sanfrjfce identification, sample
security, sample tracking (from recent to completion of analysis) and
analytical project file organizatiottJ|4nd assembl^,
3.2 Written SOPs Audit: "'•• •'•, '{
' ^ ,, ,<' '
The written SOPs audit consists of review and examination of the written
SOPs to determine if they are accurate and complete for the following
laboratory operations: sampl«|8-r,^ceiving, sample storage, sample
identification, sample secwi%jj£j*saaif*l*| Bracking (from receipt to
completion of analysis) and:^tolytica'f>*^«J0|Ct 'tfiZLe organization and
assembly. ^"-i-_ ,-"'!' ""'"' -••'
' '• '
3.3 Analytical Project File Evidence. &.udit^
The analytical project file evidenc*:§audit consists of review and
examination of the ^nai^tical proj ectffile documentation. The auditors
review the files ,to: dete'rsti^e:
m
The accuracy of the cl^seument inventory;
The compi*taeness ofi'tt^f^leV]j'"'
The adequacy df&tiUftccuracy of the document numbering system;
Tr-ae^eSblli-ty of samp'le'-Mfc^tivity;
/ rjfltdentif icat£d»i>**f activity recorded on the documents; and
;-- Error correctiong^ethods.
of the On-SJjte Team's Findings
auditors present their findings and
recommendations for ^errective actions necessary to the Contractor
personnel. - : ,_-
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5 Corrective Action Reports For Follow-Through to Quality Assurance and
Evidentiary Audit Reports
5.1 On-Site Laboratory Evaluation
Following an on-site evaluation, quality assutiance and/or evidentiary
audit reports which discuss deficiencies found during £he on-site
evaluation may be sent to the Contractor. In a detailed ietter, the
Contractor shall discuss the corrective actions implementfedtfco resolve
the deficiencies discussed during the onisite evaluation aridb«J,i&cussed
in the reports to the TPO, APO, EMSL-LV;?(response to the qualrtejfe;
assurance report), and NEIC (responseyfeo the evidentiary report) within
14 days of receipt of the finding or ftthin the tiaae agreed upon between
the APO/TPO and the Contractor. Apyaftemate delivery schedule may be
proposed by the Contractor, but it i«,jjtt»e sole,«ecision of the Agency,
represented either by the TPO or APO, tsb,:,<4ppr^e or disapprove the
alternate delivery schedule. If an alternate'-^delivery schedule is
proposed, the Contractor shall describe in a'lefcfcer to the TPO, APO, and
the Contracting Officer why he/she is unable to' ime£-the delivery
schedule listed in this section. The TPO/APO will 'nott-grant an
extension for greater than'^.^^.^ipc^t^e Contractor's response letter
to the laboratory evaluatic^sample'^SjSdlSfc.; "1S»e. Contractor shall
proceed and not assume that ati!-sextensionw£il:%e«£;kanted until so
notified by the TPO and/or APOi _-/:
If new SOPs are required to be wfittejror SOPs are required to be
amended because of the deficiencies aild the subsequent corrective action
implemented by the Costlcactor, the Contractor shall write/amend and
submit the SOPs ,;p«r the'*requirements lifted in Exhibit E, Section IV.
5.2 Corrective Actions -j
f\. • '•• •'--
If the Contfactas^,fails ^.i^bife«l-|t4*yie requirements listed in this
section, the Contractor may expect, but the Agency is not limited to the
following actions: ±»
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DRAFT
SECTION XI
QUALITY ASSURANCE AND DATA TREND ANAJSSIS
Overview
Data submitted by laboratories are subject C© revlewrficpm several
aspects: compliance with contract -required QC, useabHSjjty, and full
data package evaluation. Problems resulting from any of>these reviews
may determine the need for a on-site laboratory evaluation *a%d/pr a
remedial PE sample. In addition, QC paafsiscribed in the methods'^arovides
information that is continually used Jsj&'the Agency to assess sample data
quality, Contractor data quality, ani&rogram da^.; quality via data
trend analysis. Trend analysis is.~l^omplished;%y entering data into a
computerized data base. Statistical-'|p4j*prts ty& evaluate specific
anomalies or disclose trends in many affeks,, including the following, are
generated from this data base: ; ;
• System Monitor Compound Spike Recovery; "-•- .-,,
• Laboratory Control S^«tei,iM^sis?»i:y;
'i ,• --&;/'«! "'• ':. ,
"-• ?- ' " *'& ;&' ';.
••••:- s? ;'• ""
m Method Blanks; -:-«- '•"> •"-•"-
;?.".
• Initial Calibration and Calibration Check Data; and
• Other QC and Method Parameters-/
s N^ *'
Program Benefits •;. •?' /, '\S,
~ ~ ,;,' ," ',,".'•' ;'," ',
Program-wide Statistical results are usei to rank laboratories in order
to observe die,.relative peieSo^Bjancie, of each Contractor in a given
protocol agai-ijiS.fciI.ts pee^9»';^||(^i{g|^%s are also used to identify
trends within la&sratories. The results of many of these trend analyses
are included in ovelrafiL:.evaluation of a Contractor's performance, and
are reviewed to de termini if corrective action or an on-site laboratory
evaluatioH'itsRadicated iri.jteder to meet the QA/QC requirements of the
contra&tfe :' '-'•'"•* ^ll, ,*-, '-J-V .'
-\ '*
'Cri
performairat%.over time is monitored using these trend analysis
to detect cppiartures of Contractor output from required or
levels of qual||jfy control, and to provide an early-warning of
QA/QC probljrais which may not be apparent from the results of
case. fit
i'>' "
As a furtfesr :||enefit)j3fco the Program, the database provides the
information n^ededfcb establish performance-based criteria in updated
analytical proto&olis, where advisory criteria have been previously used.
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DRAFT
The vast empirical data set produced by contract laboratories is
carefully analyzed, with the results augmenting theoretical and
research-based performance criteria. The result -is a continuously
monitored set of quality control and performance ^criteria specifications
depicting what is routinely achievable and expected of environmental
chemistry laboratories in mass production analyses ;of environmental
samples. This, in turn, assists the Agency in meeting dts objectives of
obtaining data of known and documented quality.
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SECTION XII
DATA MANAGEMENT
Overview
Data management procedures are defined as pr«. .'" ",,,/_
The record of changes in the form of corrections and updates to data
originally generated, submitted,9 lland/aa; resubmitted shall be documented
to allow traceability of updates. Be'cotnentation shall include the
following for each change :
• Justification or rationale for t&ie change.
. ;; - " ^;P ---
^
• Initials <-of the persotv.inaking the change or changes . Data changes
shall fee implemented(46^d, reviewed by a person (or group)
>f the ^M^y^^^ting, the deliverable .
Change documenfcatS.on shall be retained according to the schedule
of the original
«e)d electronic v^j|t^a or other deliverables shall be
reinspected as ---a part of the laboratories' internal inspection
process prior fe&^fe submission. The entire deliverable, not just
the changes, sha^t be inspected.
The Laboratory Mfaager shall approve changes to originally
delivei^les.
"
DocomenSation of data changes may be requested by laboratory
auditors ^ •' J,
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DRAFT
Lifecycle management procedures shall be applied to computer software
systems developed by the laboratory to be used to generate and edit
contract deliverables. Such systems shall be thoroughly tested and
documented prior to utilization.
• A software test and acceptance plan inclwliijg test requirements,
test results and acceptance criteria shall be Developed, followed,
and available in written form.
• System changes shall not be made disectly to production, .systems
generating deliverables. Changes^shall be made first to '-a.'""
development system and tested prior to implementation.
V '"
m Each version of the productions system will'Jje given an
identification number, date of siestallatlon, date of last
operation, and archived. " \ \
• System and operations documentation shall.- "be developed and
maintained for each system. Documentation 'Shall include a users
manual and an operations, and maintenance manual.
• This documentation shajll be avaliiaKle' for on-site review and/or
upon written request by^fehe TPO orJHEIC. '
Responsibilities ' ;
Individual(s) responsible for the following functions shall be
identified: _: » -' ; ,-
• System o^ration and'iftaintenance "Including documentation and
trainings/' \ , -
^ - ,_ .-' t^. ,,.,.,.„,,,,
• Data base!~iaitegrity^,ilsc1atfli^-,data entry, data updating, and
quality contxoi,
• Data and system Searsucity, backup, and archiving.
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DRAFT
CHAJN*C^-,CUSTODY, DOCBltENT CONTROL,
OPERATIRg PROCEDURES
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DRAFT
1.0 Sample Chain-of-Custody
A sample is physical evidence collected from a facility or from the
environment. Controlling evidence is an essential .part of the hazardous
waste investigation effort. To accomplish tills, Contractors are
required to develop and implement the following sample identification,
chain-of-custody, sample receiving, and sample tracking procedures.
1.1 Sample Identification - '
To assure traceability of the samples while in possession of the
Contractor, the Contractor shall ha*<6,,a specified method for maintaining
identification of samples throughout^tfee^laboratory.
Each sample and sample preparation container,shall be labeled with the
EPA number or a unique laboratory identifier. If a unique laboratory
identifier is used, it shall be cross-referenced "'to., the EPA number.
1.2 Chain-of-Custody Procedure^i.-ss;'-.^;,'.1;'-,;" ?„ _,
Because of the nature of the^data being .collected, :;the custody of EPA
samples must be traceable from 3jj^e time itihe samples are collected until
they are introduced as evidence'!gaa legpal proceedings. The Contractor
shall have procedures ensuring that EJ?& sample custody is maintained and
documented. A sample is under custody if:
'"' ;8J, i „ ' i
• It is in your possession; or ^
,; 'if",,i 'i-,
• It is in your view afifeer being in your possession; or
• It was in your possession:;saiKi'jioti locked it up; or
• It is in a designated secure area. (Secure areas shall be
accessible only to.|authorized personnel.)
1.3 Sample |fe«lvitig- feeocedures • *}_ '•
The Conttidctor shall designate a sample custodian
responsib&,ifor receiving all samples.
' ,'•-"";
'" "
The Contracstor shall designate a representative to receive
;.; samples icifMie event that the sample custodian is not
"':^ available:.-'
1.3.3 "TStejslcoaiSition of the shipping containers and sample bottles
shaXl".ibe inspected upon receipt by the sample custodian or
his/her representative.
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DRAFT
1.3.4 The condition of the custody seals (intact/not intact) shall
be inspected upon receipt by the sample custodian or his/her
representative.
1.3.5 The sample custodian or his/her repiesentative shall check
for the presence or absence of the ^following documents
accompanying the sample shipment:.; :
• Airbills/airbill stickers; '"•'
• Custody seals; ;!=, ' -
• Quick Turnaround Method CQTM) Traffic Report/Chain-of-
Custody (TR/COC) records,;, s •
• SAS packing lists, if appli,eabj|e* and
• Sample tags. ,,
'* -,
1-3.6 The sample custodian or his/her represeiitafcive shall sign
and date all f^Es^^|e^,g,||TM TR/COC records or packing
lists, and air&tils) "accicHBpii^fia^;-,t%e samples at the time of
sample receipt. ''%« »?- ~ f 'I/
''*•• •• s
';-.-. ."I'1
1.3.7 The Contractor shallfcontact the Regional Program Manager
(RPM) to resolve discrejpasEKcies and problems such as absent
documents, conflictingsirfformation, broken custody seals,
and unsatisfactory samp1# condition (e.g., leaking sample
bottile,). ~rf'jt%e RPM is ncrtfjavailable the Contractor shall
co^feact the Cl&fS contractdfc
1.3.8 Ifae Contractor, Jhall record the resolution of discrepancies
'ai«i . problems ^MS:-j^3fe§h03ii-|Contact Logs .
1.3.9 The follj^bcjg information shall be recorded on Form DC-1 by
the sample'^ssjtodian or his/her representative as samples
-p>are,,,received
of the shipping container;
' ~"j
^il'
Preface or absence and condition of custody seals on
shipfflng and/or sample containers;
< >-.-'•
'2J'
Cust^ay seal numbers, when present;
i^ CoMition of the sample bottles;
' : -f-Pxesence or absence of airbills or airbill stickers;
Airbill or airbill sticker numbers;
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DRAFT
Presence or absence of QTM TR/COC records;
Presence or absence of EPA SAS -packing lists;
Presence or absence of sample tags;
Sample tag identification ••numbers across-referenced to
the EPA sample numbers; .
Verification of agreement or non-agreement ȣ ,
information recorded |:on shipping documents and sample
containers; and -
• Problems or discrepancies. •
1.4 Sample Tracking Procedures * •;;;' , "*
The Contractor shall maintain records documentit^ all phases of sample
handling from receipt to final analysis.
$"'V
2.0 Document Control Procedure^ ' • 14 £jy~ %:,.: -,,;;/> ^,
»<'*. ;* ' 'V'S'K*V' I''; ,>4lT *',/
The goal of the laboratory doiraaanent control program is to assure that
all documents for a specified B^ch wili^be accounted for when the
project is completed. Accountably, dofisaents used by contract
. laboratories shall include, but nctib^flimited to, logbooks, QTM TR/COC
records, sample work sheets, bench %££ets, and other documents relating
to the sample or sample:;:analyses. Tbse^following document control
procedures have been estat>|.;ished to ashore that all laboratory records
are assembled aaw! stored fi|r
-------
DRAFT
for performing the activity at the time an activity is
performed.
2.1.4 Logbook entries shall contain the time of analysis (in
military time) and be dated (montfa/ltay/year) and signed by
the person responsible for performing; "the activity at the
time an activity is performed. ,
2.1.5 Logbook entries shall be in chronological order.;, Entries in
logbooks, with the exceptioji -of instrument run lt>gs -and
extraction logs , shall include only one Batch per page .
2.1.6 Pages in both bound and unbound logbooks shall be
sequentially numbered. --\ •"•
2.1.7 Instrument run logs shall be laBsiBrfeained so as to enable a
reconstruction of the run sequence of individual
instruments. •'; ••.
Because the laboratory must provide copies of the instrument
run logs to EB&., *3th$ tla^mtpry^ may exercise the option of
using only labbnitory or!H^<«asg»l^, identification numbers
in the logs for Staple ID ratfher than government agency or
commercial client tiames to ^reserve the confidentiality of
commercial clients. • ••> ,.'; /
2.1.8 Corrections to supporting documents and raw data shall be
made iy-^b?aw^Bg a single ;l'ine through the error and entering
the.; correct i'^alormation. Corrections and additions to
supporting dociaents and raw; data shall be dated and
initialed. No,|i6aformation shall be obliterated or rendered
, Unreadable . J:»:L. , ,„ ....... ,,
•*:&,. .'•£'&&}:.•&,$*
All notations shall be recorded in blue or black ink.
^ '; ^ *
.;
Unused portions of documents shall be "z'd" out.
2 . 1 . 9\ is -- ' ''" "Tb^ltS^aXiractor sM'll. assign a numerical identifier to each
electrojiis transfer of EPA data.
'-•?
All data 6j|£nsferred using direct electronic transfer
technology:||o the data user shall be printed in hardcopy and
filed in t^ CBF. The Contractor shall record the following
informatLMl?on the hardcopy or on a separate piece of paper
attachedflSo the hardcopy, as well as a sequentially-numbered
^ - /! *,$,;•*
m "-'Ts-flfche laboratory individual responsible for the
electronic transfer;
• The date and time of the electronic data transfer;
F-5 . 08/23/94
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DRAFT
• The individual for whom the data was electronically
transferred;
• The status of the data that was; electronically
transferred (e.g., first subaifctal or second
submittal); and ,; ,'; ,
• The numerical identifier of the eleetSPomc transfer.
2.1.11 If an RPM authorizes the Contactor to transmit;preliminary
form 1 or raw data to the d«ta user via & fax (or fao?)
machine, then the Contractor shall:
,-£•< ,*•
• Assign a numerical ,identifier :£o each fax;
• File the fax originals*fn title CBF;
• Record the information identified in paragraph 2.1.10
on the fax originals; ;:,
Record taB^&B!C^^8aBfe|ej,,of EPA data in a
sequentially-numbered logbook; and
''"'¥• -»•' '• ""' '•'''
Record the aij|torizat3ym information (e.g., Regional
Program Managers name, date, time, and reason for
facsimile transmission).
2.2 Consistency of
The Contractor &hall assigi|t|k Document 'patrol Officer (DCO) responsible
for the organisation and assembly of the CBF.
All copies of laboratory ::*yjiiuments::isfciill be complete and legible.
Original documents wfctl.«3|,. include information relating to more than one
Batch shall be filed in%tsst; CBF of the lowest batch number. The
placed:it|K,|e%e other CBF(s) and the Contractor shall
iyijf^ informatS^if on the copy(ies) in red ink:
• i. .
-Xi "COPY"
7&
IS FILED IN fe
shall S$j$n. and date this addition to the copy(ies).
Before relMs&KEig analytical results, the DCO shall assemble and
cross-check title:in£frmation on samples tags, custody records, laboratory
bench sheets, per^btnal and instrument logs, and other relevant
deliverables to ensure that data pertaining to each particular sample or
Batch is consistent throughout the CBF.
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DRAFT
2 . 3 Document Numbering and Inventory Procedure
In order to provide document accountability of the completed analysis
records, each item in the CBF shall be inventoried and assigned a
serialized number as described in Exhibit B.
All documents relevant to each sample Batch, sinclucybtjg logbook pages ,
bench sheets, chromatograms , re -preparation records, 'reaaalysis records,
records of failed or attempted analysis, custody records", 1 «£c. , shall be
inventoried. -, "•':•• -
The DCO shall be responsible for ensuring that all documents generated
are placed in the CBF for inventory and are delivered to the appropriate
EPA Region or other receiver as designated by EFA:.: The DCO shall place
the sample tags in plastic bags in tlj.e'Vfile .
2.4 Storage of EPA Files :- -
The Contractor shall maintain EPA laboratory documents in a secure
location. »- .
. -•* ,
2.5 Shipment of Hardcopy Data De|iverabTe'^' 4'fJ v , ,.
"i ^ <•''•;- ' , ;
2.5.1 The Contractor shall documejate shipment of hardcopy
deliverables packages; to tihe recipients . These shipments
require custody seals1 it:he containers placed such that
they cannot be opened wil&out damaging or breaking the seal.
The Contractor shall document what was sent, to whom, the
date,,; and fiherfflethod (carrier) used.
of the tiansmittal letter for the CBF shall be sent
to,,NEIC/CEAT a»t: the, .CLASS contractor.
• "•• '- " "' ' '
2.5.2 Authorised Alternative Transfer Methods
If the Regi^a^a. Program Manager authorizes the Contractor to
,; : '-^-latswisfer EPA ;is^||i^C,o the data user by mailing the diskette
, ,}'. '' "ratfeejTs -t;han via aiir«fct electronic transfer technology, then
»;,; - the CbtttsCactor shall follow the procedures described in the
*'-- above patibsferaph 2.5.
.ij ^T?
.&1' '%t.
3.0 ,J1gi?ecifications For Writan Standard Operating Procedures
The Soiitractor shall IpD^e written standard operating procedures (SOPs)
for retMsi|>;t of sampleji|, maintenance of custody, sample identification,
sample stfeage,3 sam|ii tracking, and assembly of completed data.
An SOP is defiri«4|ias a written narrative step -wise description of
laboratory operating procedures including examples of laboratory
documents. The SOPs shall accurately describe the actual procedures
used in the laboratory, and copies of the written SOPs shall be
F-7 08/23/94
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DRAFT
available to the appropriate laboratory personnel. These procedures are
necessary to ensure that analytical data produced under this contract
are acceptable for use in EFA enforcement case preparation and
litigation. The Contractor's SOPs shall provide mechanisms and
documentation to meet each of the following specifications and shall be
used by EPA as the basis for laboratory evideaa
3.2 The Contractor shall have written SOPs :fesr receiving and logging' in of
the samples. The procedures shall ine&ikde but not be limited to
documenting the following i
Presence or absence of QTM TR/IPC; records ^'
: "-; " ,_ if-
Presence or absence of airbills/airbillAStickers;
Presence or absence of SAS packing lists, HE applicable;
Presence or absence of: (.
Condition of the shi^ptng container;
Condition tljp'.•£&& sample bottles;
Verification of aipaesement or non-agreement of information on
Documents^B«4i,sample containers;
iResolution oW^aroblems of discrepancies with the CLASS contractor;
and \'-',~
,
The definition otl^any terms used to describe sample condition upon
receipt (e.g., g0^Ai, fine, ok).
3.3 The C6^fc«|c;tor shall,|^ve written SOPs for maintaining identification of
EPA sanp^^K^ja^roughjMtib the laboratory.
If the Contracdefellassigns unique laboratory identifiers, written SOPs
shall include a description of the method used to assign the unique
laboratory identifier and cross-reference to the EPA sample number.
F-8 08/23/94
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DRAFT
If the Contractor uses prefixes or suffixes in addition to sample
identification numbers, the written SOPs shall include their
definitions.
3.4 The Contractor shall have written SOPs describing all storage areas for
samples in the laboratory. The SOPs shall include ,a list of authorized
personnel who have access or keys to secure storage areas.
3.5 The Contractor shall have written SOPs describing the meliioa by which
the laboratory maintains samples under custody. :;
,-.'. '' "-'
3.6 The Contractor shall have written SOPs*Describing the method by which
the laboratory maintains the securityjbf any areas identified as secure.
3.7 The Contractor shall have written SGf^gfor traciking the work performed
on any particular sample. The tracking SOP skill include:
• A description of the documents used to record sample receipt,
sample storage, sample transfers, sample preparations, and sample
analyses; r, ;
• A description of the^lfecuments'-^yle^,;*^ «ecprd calibration and
QA/QC laboratory work;*; /> I
• Examples of document formats and laboratory documents used in the
sample receipt, sample storage, sample transfer, and sample
analyses; and
• A narrative*step-wCsfe, description*of how documents are used to
track samples. !';|]; ' =:
3.8 The Contractpy of the electronically transferred data.
'*•'*•%,">. - f"
Ensuring:gehad: ;;fche hardcopy is placed in the CBF.
Recording the following information on the hardcopy or on a
separate piece of paper attached to the hardcopy, as well as in a
sequentially numbered logbook:
F-9 08/23/94
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DRAFT
The laboratory individual responsible for the electronic
transfer ;
The date and time of the electronic ^data transfer;
The individual for whom the data !«ras>!; electronically
transferred; ; •' ;;,
The status of the data that was electronically transferred;
and s, -' •:.
The numerical identifier of'-the electronic transfer.
3.9 The Contractor shall have written SCSSfs for the ase of a fax machine to
transmit EPA data or preliminary foTf^-^-or raw'-lfata results to the data
user. The written SOPs shall include the*ffQlio*ring.
• Assigning a numerical identifier to each fax;
• Filing of fax originalss,4n the CBF;
• Recording the information ideni*i^li^l''ixi-^zaigraph 2.1.10 on the
fax originals; ':'V; !V '< •>
• Recording the fax transferikiuf E1E|&. data in a sequentially numbered
logbook as described in paragraph 2.1.11; and
• Recording the,:autl$M:ization information (e.g., Project Officer's
name, date,' ;*trlme,"aj^t reason fordjlfacsimile transmission).
3.10 The Contractor Ssrhall have vafitten SOPs for organization and assembly of
all documents,-:arelating to «&eh Batch. ^Doctoments shall be filed on a
batch-specifre/J^iaesis. Th4i^||t*dMll^s<:i*hall ensure that all documents
including logbook -|Mg§es, sample tracking records, chromatograms,
computer printouts, s^aif .data summaries, correspondence, and any other
written documents having.Vjseference to the Batch are compiled in one
location fiorj'StiJiHiiission €b-:>|8?Ai The written SOPs shall include:
• ,-j; >4 description;--^ the numbering and inventory method;
• f" A description ofps^he method used by the laboratory to verify
.|3 ; '* consistency and igmpleteness of the CBF; and
'• "*:C . 1 •
• '" "'."^Procedures for tl&6 shipment of deliverables packages using custody
4.0 Handling Of t^gMgiteial Information
>I'~*,A
A Contractor conducting work under this contract may receive
EPA-designated confidential information from the Agency. Confidential
information must be handled separately from other documentation
F-10 08/23/94
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DRAFT
developed under this contract. To accomplish this, the following
procedures for the handling of confidential information have been
established.
4.1 All confidential documents shall be under the supervision of a
designated DCO.
4.2 Confidential Information
Any samples or information received with ,a request of confidentiality
shall be handled as "confidential." A Separate locked file shaM be
maintained to store this information and shall be segregated from other
nonconfidential information. Data generated from Confidential samples
shall be treated as confidential, l^on receipt o£ confidential
information, the DCO will log these ;*J®#uments JLnto a Confidential
Inventory Log. The information will theft "i»e available to authorized
personnel but only after it has been signed oat to that person by the
DCO. The documents shall be returned to the locked file at the
conclusion of each working day. Confidential inf«i»ation may not be
reproduced except upon approyal by the EPA APO. The ,B|CO will enter all
copies into the document aeiatxolJL -ssjgrsfsenk described above. In addition,
this information may not be^Stispos'ed^l^cftt upon approval by the EPA
APO. The DCO shall remove aaflDetain thjfe-icovei'-page of any confidential
information disposed of for one^year adS {shall keep a record on the
disposition in the Confidential Inventory Log.
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GLOSSARt &F
AND ACROSUJ 11ST
DRAFT
08/23/94
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DRAFT
TABLE OF CONTENTS
SECTION I: GLOSSARY OF TERMS
SECTION II: ABBREVIATIONS AND ACRONYMS.
PAGE
G-3
S-8
G-2
08/23/94
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DRAFT
SECTION I
GLOSSARY OF TERMS
ALIQUOT - a measured portion of a sample taken for analysis.
ANALYSIS DATE/TIME - the date and military time of ,,£he "itijecfeion of the
sample, standard, or blank into the GC system. -,,
ANALYTICAL SEQUENCE - an analysis sequence consisting of an initial? - ,
calibration or a daily calibration check standard, method blank(s), laboratory
control sample(s) (LCS), field sample(s), iaasttrument blanks, and a performance
verification standard(s). There are two ty|»es of analjtecal sequences: an
initial calibration analytical sequence au&i.a daily calibration check
analytical sequence. An analytical sequence''saaist not exceed 24 hours.
* < \ ', ' ^s,
AQUEOUS NON-MISCIBLE OIL SAMPLE - Oil sample that ii.not miscible with water.
AQUEOUS MISCIBLE OIL SAMPLE - Oil sample that is miscitlLe swith water.
BATCH - a unit within a sample C£^;t^t:U«,r.used to identify a group of
samples for delivery. A Batch is'-.jl^roup o^ii&ld:. Samples (up to 30
fractional analysis) within a Case ^received in>bne SaylS"Data from all samples
in a Batch are due concurrently withfaa the specified turnaround time.
s ^ •: ,
BLANK - for the purpose of this SOW, there iare three required blanks: method,
instrument, and cleanup. All protocols (.1,*., volatile, PAH, phenol,
pesticide, and PCS) require saefihod and installment blanks. A method blank must
be performed with each' ftetchT -f|q&*,each samplS|;ifraction, and for each matrix.
In addition, the pes4Sici.de and P&ijj£protocols ^6quire the analysis of a cleanup
blank if the optional, sulfur cleapop step is employed. Also, an additional
method blank shall;lie analyzed alfttjg.m^h,samples that are filtered.
CALIBRATION CHECK - a dSeek standard analyzed at the start of each daily
analytical sequence to deteigttine if the initial calibration is still valid.
;, 1 C1;
CALIBRATION FA^T<|B..-f -the total*'adjja>,of a peak(s) divided by the mass injected
(in ''"''' ' " "
CASE - apEtnite, usually predetermined number of samples collected over a
given -SipSe period from a paSplcular site. Case numbers are assigned by the
Samplej^anagement Office. A|i^ase consists of one or more Batches.
"!-\||?:-, Zil
CLP Analytical Services Supgi&rt (CLASS) contractor - At times during the
length of tftli.^ntract, tfe^JcLASS contractor acting on behalf of the
Headquarters AP%Jafsd/or R.ejg|6nal TPO, will provide directions to the
Contractors. '«¥ 1*^,4'"
G-3 08/23/94
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DRAFT
CLEANUP BLANK- 1 ml of hexane carried through the pesticide or PCB sulfur
cleanup procedures to determine whether contamination was introduced during
cleanup . :
CONTRACT REQUIRED QUANTISATION LIMIT (CRQL) - target compound quantitation
limits as specified in Exhibit C. ''I
CONTRACTOR - synonymous with Laboratory as used herein. ?;
-; , ,
DAY - unless otherwise specified, day shall me^sa calendar day. -
J>' 'J- ..-
,> •£-.
DATA SYSTEM - for the purpose of this SOW, ^/integrator/computer system that
allows the continuous acquisition and prin^SSCt of timers, intensity data
throughout the chroma to graphic program. , |^/ , |5'
*"*; ***,'.& ** " •
"•" f" -, " ,
DILUTION FACTOR - a dilution factor (i.e., a sjh|gj.e|whole number, such as
"100" for a 1 to 100 dilution of a sample) must fee .^ported for all samples
which are diluted. A sample dilution considers all: factors which affect the
sample CRQL. Some common examples include: extraction or analysis of a
smaller sample aliquot; dilution of.a sample or sample extract; and dilution
of a smaller aliquot of a methanoll «X§i^f:";f or volatile s analysis.
v \'% '"'''' '~^\^^ !?', *3f'ss ',- ' •' > <.
ELECTRON CAPTURE DETECTOR (ECD) - director use^in'lihersanalysis for pesticides
and PCBs in this SOW. .1 ,;?
ELECTROLYTIC CONDUCTIVITY DETECTOR (ELCS:JC%<1|1ALL) - detector used in series
with photo-ionization detector (PID) in tfbel analysis for volatile organics in
this SOW. r-^-^ ^-:"-
~"
i> '£_
EASTERN STANDARD TIME?f?EST) or ElipSERN TIME -^ifee time of the fifth time zone
west of Greenwich thitt includes
EXTERNAL STANDARDS' ^jTaogget com^i^is|^iii^i.^€d at a known concentration prior
to sample analysis to determine calibration factors.
FLAME IONIZATION DETECTOR (FH3_,;r^ detector used in the analysis for PAHs and
phenols in
GOVERNMENT]/ the terms G^^piment and Agency are used synonymously in this SOW
and refefisjrto the US Goverlsi^at or the US Environmental Protection Agency
•tf' 'ik'.
(EPA).^-^
HEATED' 4|P|KPSPACE SAMPLER - device for sampling the headspace gases and for use
in direclf^i^^ption GC volatl^fces analysis.
'
HIGH LEVEL SAMPlJESs'%, field':^amples that contain target compounds at
concentration levels that exceed twice the high calibration standard and/or
interferents that are :!i&|lected at levels greater than the mid level initial
calibration standard concentration response of the nearest target compound.
G-4 08/23/94
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DRAFT
IN-HOUSE - at the Contractor's facility.
INITIAL CALIBRATION - Analysis of three analytical standards at the beginning
of the contract and whenever specific quality control criteria are not met.
Initial calibration defines the linear and dynamic range of response of the
instrument to the target compounds. " . •„
INSTRUMENT BLANK - reagent water (for volatiles) or solvent ;<;for PAH, phenols,
pesticides, and PCBs) analyzed to determine whether carry-over iScom a previous
sample has occurred. ;, -4-,"'>'
LABORATORY - synonymous with Contractor as ve|ed herein.
LABORATORY CONTROL SAMPLE (LCS) - sample prepared andrfOTtified (spiked) with
known quantities of specific compounds anS stibj ecteds-ifco the entire analytical
procedure by the Contractor in order to assess*' tile .accuracy of the method and
to demonstrate that the analytical system is in tsoratsjol and producing
consistent data. ' ;,l- ,
•i • .';/,
MATRIX - the predominant materiaLjof .which the sample to Be' Analyzed is
composed. For the purpose of this 30&,:;;i*%e;; sample matrix is either water,
soil/solid, oil, or wipe. "::* ', ' •'• '':-,;,;j ,:;- •-.-
METHANOL NON-MISCIBLE OIL SAMPLE - Oil sample:j|hat is not miscible with
methanol. Used synonymously with metfoanpl eaitractable oil sample.
METHANOL MISCIBLE OIL SAMPLE - Oil sample' t&at is miscible with methanol.
Used synonymously with met&apol jion-extractable oil sample.
METHOD BLANK - an analytical conical consisting ;!of all reagents and the SMC
carried through the^ame analytic^, procedures =as the field samples. The
method blank is usect to define t^s level of laboratory background
contamination. •-;•%,., , ,--
PHOTO- IONIZATION DEf1^|,,pID) - detector used in series with electrolytic
conductivity detector '-''QEiCD or HALL) in the analysis for volatile organics.
The PID may also be used : for the analysis of phenols in this SOW.
G-5 08/23/94
-------
DRAFT
PROTOCOL - describes the exact procedures to be followed with respect to
sample receipt and handling, analytical methods, data reporting and
deliverables, and document control. Used synonymously with SOW.
QTM TARGET COMPOUND LIST (QTCL) - a list of compounds,.Designated by the SOW
(Exhibit C) for analysis. '=: . ;
Quick Turnaround Method (QTM) TRAFFIC REPORT/CHAIN-OF-CUSTOirry(m/COC) - an
EPA sample identification form filled out by the sampler which acbompanies the
sample(s) during shipment to the laboratory andwhich documents sample.
condition and receipt by the laboratory. T ' !
REAGENT WATER - water in which a target compound or int«rferent does not
produce a signal greater than one-half tht&icesponse intifNEhe corresponding RRT
window of the initial calibration low concecBtifation sjtsandard.
REGIONAL PROGRAM MANAGER - Regional EPA official; -|w*cih as the Regional
Technical Project Officer (TPO) or Regional Site Manage^, Regional Site
Managers may be Site Assessment Managers (NPL listings)-; 'fi»-Scene Coordinators
(emergency response(s)), or RemedJLs%J,.;P.roject Manager (site *remediations).
/.,',|BV4|fo/ ^jif'<,;••/,, , ,,,(
RECOVERY - a determination of the ;4^curacy" o%'-ffl^ '|aBaly,tical procedure made by
comparing measured values of a fortified (spikect) 'sample..against the known
spike values. Recovery is determinedly the Billowing equation:
%Rec = measured ^•yalue x 100%
known
' - 'S1; * ;- -,
REANALYSIS - reanalysis,-
™ "
RESOLUTION 'C&Ltfar termed per^sht valley) - the separation between peaks on a
chromatogram, calbeaiilated by -Dividing the height of the valley between the
peaks by the peak h«iL^l^^ the smaller peak being resolved, multiplied by
100. ~ ".'"-V-
G-6 08/23/94
-------
DRAFT
RETENTION TIME MARKER - standard compound (SMC) used to assess GC system
stability by quantifying shifts in retention time for all analyses.
SAMPLE - a portion of material to be analyzed that is contained in single or
multiple containers and identified by a unique sample number.
SAMPLE NUMBER (EPA Sample Number) - a unique identificatiab, number designated
by EPA for each sample. The EPA sample number appears on the sample QTM
TR/COC form which documents information on that sample. H- J,
SOLID PHASE EXTRACTION (SPE) - a procedure commonly utilizing a cartridge or
disk containing a solid matrix coated with amended organic phase used to
extract and cleanup field and QC water samples.
SOLVENT EXTRACTION - liquid- liquid and liquid-solid ea&raction procedures used
to prepare field and QC samples. . -1
STANDARD ANALYSIS - an analytical determination made sssith known quantities of
target compounds; used to determine calibration factofs^'^eJEine identification
windows , and establish linearity $v@r, the calibration range»
SYSTEM MONITOR COMPOUND (SMC) - aSeampound aiMfed^to^every blank, sample,
laboratory control sample, and standard; used -to. evkluatje analytical
efficiency and stability by evaluatittg recover^ and retention time shift.
These compounds are typically brominafeed, flxisrinated, isotopically labelled,
or compounds not expected to be detected ,ia • environmental media.
TECHNICAL PROJECT OFFICER; (t£H>|= _- Regional ^fficial responsible for monitoring
the technical requireipe»t:s of'1^^;Laboratory*^ contract; the TPO is the first
line of contact when^^te Laboratory requires ^echnical assistance, and along
with the Administrative Project OJficer (APO), is the only person that can
provide instructions,"or clarifications to the Laboratory regarding the SOW.
•• \ ,»?•. :;-%~&^>?''~: ''-.-} •"
TELEFACSIMILE (fax or'%yps) - a system of transmitting and reproducing fixed
graphic material (as printing;} by means of signals transmitted over telephone
lines. ' •; ,;
TIME - when.'.petjdfred^feo.i-.irecord time-jm any deliverable item, time shall be
expressedi&r Military Tim|^ i.e., a 2'"4-hour clock.
•ft
VALIDATJ<$ TIME OF SAMPLE RE^||PT (VTSR) - the date and time on which a sample
is re&gifaed at the Contractolfes facility, as recorded on the shipper's
delive^l^rsceipt and QTM TR/SOfC Record. NOTE: The VTSR date/time is adjusted
for sanipSwitjgeceived during jjpeni-routine working hours (see Exhibit A, Section
III, paragrlpiti^.S, for details).
G-7 08/23/94
-------
DRAFT
SECTION II
ABBREVIATIONS AND ACRONYMS
APO
CADRE
CBF
CCS
CF
CLP
CLASS
CRQL
%D
DCO
DF
ECD
EOT
ELCD
EMSL-LV
EPA
EST
FAX or FACS
FID
FSCC
GC
1C
LCS
NCC
NEIC
NPL
OSC
PAH
PCB
PE
PEST
PHE
PID
PRP -ft
PVS ;!J'
QA ,f.""
OAP ,;0'
QATS :
QC
QTCL
QTM
RAS
%REC
RPM
RSCC
Administrative Project Officer
Computer-Aide Data Review and Evaluatisto
Complete Batch File
Contract Compliance Screening
Calibration Factor
Contract Laboratory Program
CLP Analytical Services Support;
Contract Required Quantitationtllimit
Percent Difference j-, *,*A
Document Control Officer - '*<-t
Dilution Factor
Electron Capture Detector
Electronic Data Transfer
Electrolytic Conductivity Detector
Environmental Monitoring Systems Laboratory - las Vegas
Environmental
Eastern Standard Time'ie ,
Telefacsimile
Flame lonization Detector*'-! -
Fused Silica Capillary Column
Gas Chromatograph \ '
Initial Calibration
Laboratory
National Computer
National JSoforcement
Nationa2*3»riorities
On- Sce3BB'sCoordinator
Polynuclear Aromatic
Polychloriniifeecl,, Biphenyls
Performance Evaliuation
Pesticides "^ '='11:
•estigatioa Center
_ Detecto?- ^'
Potential Responsible Parties
te "^ -*"1-.
Performance Vefep|Lcation Standard
Quality AssuraniSsh-
Quality Assurancef-^lan
Quality Assuranc||fechnical Support
•J^oality Control jjJ!
Turnaroun^^Target Compound List
J Twnaroiajdf5 Method
Routine i-3ftjastlyt|ical Services
Percent Rec&fefaery
Regional Project Manager
Regional Sample Control Center
G-8
08/23/94
-------
DRAFT
%RSD Percent Relative Standard Deviation
RT Retention Time
RT ZD Retention Time Percent Difference
RRT Relative Retention Time ;
RTS Retention Time Shift
SAS Special Analytical Services
SD Standard Deviation
SMC System Monitor Compound v
SPE Solid Phase Extraction
SOP Standard Operating Procedure >;!
SOW Statement Of Work
TCL Target Compound List ,/
TPO Technical Project Officer ,1
TR/COC Traffic Report/Chain-of-Custody?
VOA Volatiles 1. f; -
VTSR Validated Time of Sample Receipt . '\
G-9 08/23/94
-------
EXB3BIT H, ; "
DATA DICTIONARY ANB/fGBMAT FOR DATA
DELIVERABLES IN COMPUTER-READABLE FORMAT
-------
SECTION I
FORMAT A SPECIFICATIONS
1. DATE
Dates are to be YXMMDD format with all characters filled; no
slashes, dashes, or spaces.
Example: March 19, 1989 will be expressed as ^890319".
2. TIME y:
Times are to be expressed in HHMK'rJBormat with all characters
filled, no colon. - !,
Example: 1:30 pm will be expressed as "UfO" .
3. CHARACTER -'- , "
Character data are to be left-justified-udeth all letters
uppercase.
4. NUMERIC =;','! -:', ^ i ,,.
Numeric data are to be%ight-justified wiS&out a positive sign
(+), leading zeros, commas, or exjabirients. Right-justified,
leading zeros not necessary, length includes decimal points and
signs. Negative signing (-}.;, -although unlikely, will decrease the
range of values by one order -«£* magnitude.
Example: Iftimeric'!i6,v3*will accommodate from -9.999 to 99.999.
-•,<: '--t|: '• ,.
5. SPECIAL CASES ", I';
;s«*'
; ^^f1-? .-• ''"-I? -
&•'" J;t.
>•%, Form numbers u*s^|--£hree characters, the first character is a 'Q',
11 the second char^i^er identifies the form type (1= Form QI, 2- Form
,4>;"-e' QII, 3= Form QIlt|| 4= Form QIV, 5= Form QV, 6= Form QVI, and 7=
' ^-.-1(1 , Form QVII) , and ^Ipfc third character denotes the fraction (A= VOA,
''&-•;jr&=, PAH, C= Phenq^, D= Pesticides, E= Aroclors).
'
H-2 05/01/92
-------
Z6/TO/SO
aiu mod
-------
•MI*
FORM QI - VOA
VOLATILES ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142
143-146
147-152
153-156
157
158-167
168-174
175-177
178
179-187
188-193
194-199
200-204
205
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
10
7
3
1
9
6
6
5
1
CONTENTS
Form number
Form suffix
Record type
EPA sample no.
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Matrix
Lab sample ID
Sample wt/vol
Sample wt/vol units
Units > M
D ilutionl Jact^r - •;;.
Instrumen%-]ID
Date received
Time received;
Date analyzed -
Time analyzed
Quantitation type
SMC '•pAS', no.
1 SMC cokeeatration
•SMC % redo^ery
SMC % rec. pout flag
SMC area--'|\ ,, ,
•- SMC RT _;'l^-i:'::>-;>:' ;l
! sac ic RT
RT';'-3SD:;
SMC fti, ;%B, out flag
FORMAT/CONTENTS
"QL4"
"AA* - "ZZ"
"Hi*
^Character
Character
Character
Character
Character :
Character
Character
Character
"SOIL/SOLID", "WATER", or
sfifccified other
Character
Ntamexic 5.1
"G" , ^HL" , other
"UG/L" , '< "1S?/KG" , or other
Numeric 8.0
flhaa^-acter
HHMM
YYMMDD
HHMM
Character (1, 2, or 3)
Character
Numeric 7 .
Numeric 3 .
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
. 3
. 0
H-4
05/01/92
-------
DETAIL RECORD
LENGTH
3
2
2
10 '
13
1
8
8
6
1
6
6
1
6
FORM QI - VGA (Continued)
VOLATILES ANALYSIS DATA SHEET
CONTENTS
Form number
Form suffix
Record type
CAS no.
Concentration
"U" flag (non-detects)
Qualifiers
Reserved for EPA use
RRT
RRT_flag
1C RRT (STDS)
RT ' ;
RT flag
1C Rf (STDS)
FORMAT/CONTENTS
"QIA*
"AA1? - "ZZ"
^
'Numeric 13,, 3
"U" or blank
Character
Character
Numeric 6 . 3
"*" 0r blank
Numeric 6 . 3
6.3
or blank
•fftaaaeric 6 . 3
H-5
05/01/92
-------
FORM QI - PAH
POLYNUCLEAR AROMATIC HYDROCARBONS ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142
143-146
147-152
153-156
157
158-164
165-174
175-181
182-184
185
186-194
195-200
201-206
207-211
212
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
7
10
7
3
1
9
6
6
5
1,,, <;•• ;
CONTENTS
Form number
Form suffix
Record type
EPA sample no .
Lab name
Contract
Lab code
Case no .
Batch no .
Sequence no.
SAS no. - :';
Matrix -',
Lab sample ID
Sample wt/vol
Sample wt/vol units
Units
Dilution^fs&tefT : „ ,
Instrument fo" "''' ' ^
Date received
Time received \
Date analyzed ; ,
Time analyzed
Quantitation type
I&txaction type
'
SMC concfjtration
SMC %
SMC %
.SMC
s»e RT
SHC&G Rf
RT xfr.K' ?; ,
SMC RT10B|»at flag
FORMAT/CONTENTS
"Q1B"
"AA* - "ZZ"
•at* ,
Qaaracter
Character ,
Character
Character ;
Character
Character
Chara«tser
Character
"SGlt/SOLID", "WATER", or
other
Numeric 5.1
"G" , ' "^HL"., or other
"UG/L", "UG/KG", other
Ntimeric 8 . 0
HHMM
YYMMDD
HHMM
Character (1, 2, or 3)
"SOLVENT" or "SPE"
Character
Numeric 7.3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
H-6
05/01/92
-------
FORM QI - PAH (Continued)
POLYNUCLEAR AROMATIC HYDROCARBONS ANALYSIS DATA SHEET
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-30
31
32-39
40-47
48-53
54
55-60
61-66
67
68-73
13
1
8
8
6
1
6
6
1
6
CONTENTS
Form number
Form suffix
Record type
CAS no.
Concentration
"U" flag (non-detects)
Qualifiers
Reserved for EPA use i
RRT I
RRT_flag , {
1C RRT (STDS) , ;
RT '-•
RT flag
1C RT (STDS)
FORMAT/CONTENTS
"Q1B"
"AA» - "ZZ"
Gfearactet, "COMBINEA" for
coeluter '• .;-
Numeric 13. 3 : ::
"U" or blank ••' ',,
Character »-
Character
Numeric 6.3
"*",:«r blank
Numsaric 6 . 3
Nttmeric 6.3
.t*& or blank
Numeric 6.3
H-7
05/01/92
-------
DfeAlt
FORM QI - PHE
PHENOLS ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142 "
143-146
147-152
153-156
157
158-164
165-174
175-181
182-184
185
186-194
195-200
201-206
207-211
212
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
7
10
7
3
1
9
6
6
5
1 '- ~-i
CONTENTS
Form number
Form suffix
Record type
EPA sample no.
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Matrix ' ^
Lab sample ID
Sample wt/vol
Sample wt/vol units
FORMAT/CONTENTS
"QIC*
"Aft.* - "ZZ"
Instrumeritfpp) '
Date received
Time received
Date analyzed
Time analyzed
Quantitation type
type
ation
Character : ;
Character
Character : '••-*'
Character
Character
Character
Character
Character
"S0iL/SOLID", "WATER" , or
sfefecified other
Character
N«met3ic 5.1
"G"', '^Ht«, or other
"UG/L", '"US/KG", or other
Numeric 8.0
Character
(1,
2, or 3)
SPE"
'l SMC conc
SMC 2
SMC
--.-SMC
SMC
flag
HHMM
YYMMDD
HHMM
Character
"SOLVENT" or
Character
Numeric 7.3
Numeric 3.0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
H-8
05/01/92
-------
DfcAft
FORM QI - PHE (Continued)
PHENOLS ANALYSIS DATA SHEET
DETAIL RECORD
13
I
8
8
6
1
6
6
1
6
CONTENTS
Form number
Form suffix
Record type
CAS no.
Concentration
"U" flag (non-detects)
Qualifiers .!?
Reserved for EPA use?-'
RRT J' •
RRT_flag ;
1C RRT (STDS) !
RT '•:.
RT flag
1C Rf (STDS)
FORMAT/CONTENTS
"QlCf
"A&*: - "ZZ"
"COMBINED" and
"COMBINEE1 :,for coeluters
Numeric 13. 3 " •"
"U" or blank ;
Character "
Character
Numeric 6.3
"*" asr blank
Numeric 6.3
liuffleric 6 . 3
*^* or blank
Numeric 6.3
H-9
05/01/92
-------
FORM QI - PEST
PESTICIDES ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137
138-143
144-147
148-153
154-157
158
159-165
166-175
176-182
183-185
186
187-195
196-201
202-207
208-212
213
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
1
6
4
6
4
1
7
10
7
3
1
9
6
6
5
i ;,r.
CONTENTS
Form number
Form suffix
Record type
EPA sample no.
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Matrix
Lab sample ID
Sample wt/vol
Sample wt/vol units
Units
Dilution factor
Instrument .lib.,! .,_;'_ ;
Additional -cleanup
Date received
Time received
Date analyzed
Time analyzed
Quantitation type
BjctcaeStion type
"SMC CA'S,a|o.
SMC conceiStratipn
SMC % recs»irery
SMC y, reje,sbu|; flag,
SMC area^;"5<'-.lv - •• -'•
RT
1C Rf
flag
FORMAL/CONTENTS
"Q1B*
"A&* - "ZZ"
"Hi'*' ,:
Character
"Character5- ;:
Character ;
Character : :'
Character :
Character
Character
Character
"S0IL/SOLID" or "WATER"
Character
5.1
"ML"
:pr "UG/KG"
Numeric 8,'D
Character
". nn or "N"
RT
SMC
HHMM
YYMMDD
HHMM
Character (1, 2, or 3)
"SOLVENT" or "SPE"
Character
Numeric 7 . 3
Numeric 3.0
"*" or blank
Numeric 9 . 0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
H-10
07/30/92
-------
UNI-
QI - PEST (Continued)
PESTICIDES ANALYSIS DATA SHEET
DETAIL RECORD
13
1
8
8
6
1
6
6
1
6
CONTENTS
Form number
Form suffix
Record type
CAS no.
Concentration
"U" flag (non-detects^
Qualifiers -'
Reserved for EPA use ';;
RRT -:•/
RRT flag '•";
1C RRT (STDS) ; >- ,
RT :
RT flag
1C RT (STDS)
FORMAT/CONTENTS
"QIC*
11AA" - "ZZ"
TEL*;,
Character;, " COMBINES'
eoeluters .,->:
Numeric 13.V'-;:j ,,
"U" or blank T
Character
Character
Numeric 6.3
"*"lor blank
NuaJric 6.3
Nuateric 6.3
.«*" or blank
Numeric 6.3
for
H-ll
05/01/92
-------
FORM QI - PCB
AROCLORS ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137
138-143
144-147
148-153
154-157
158
159-165
166-175
176-182
183-185
186
187-195
196-201
202-207
208-212
213
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
1
6
4
6
4
1
7
10
7
3
1
9
6
6
5 r; LJ
-i *'~ '"*"'
DETAIL
COLUM^y
1-3 '"' Ijjh'i ; :
4-5 ""^
6-7
8-17
18-30
31
32-39
40-47
LEK
3
•<%
"l^''
10
13
1
8
8
CONTENTS
Form number
Form suffix
Record type
EPA sample no .
Lab name
Contract
Lab code
Case no.
Batch no .
Sequence no. i
SAS no.
Matrix " -'4
Lab sample ID
Sample wt/vol
Sample wt/vol units
Units ,, ,
Instrxunerift'-iLD
Additional --ipleanup
Date received^,
Time received ;a
Date analyzed
Time analyzed
,/<3taast.||IEation type
'SExtratffeifp type
SMC CAS iffe.
SMC concentration
SMC %
;,SMC
area
RT %D ' S
SMC RT %DXout> flag
uffix
type
C&S, >no.
.^caicentration
:tfc" flag (non-detects)
Qualifiers
Reserved for EPA use
FORMAT/CONTENTS
"Q1E*
"AA";- "ZZ"
'Character ;
Character '• ' ',
Character \
Character
Character
Character
Character
"S0IL/SOLID", "WATER", or
specified other
Character
numeric 5.1
"G",^WML"( or other
"UG/L", "UG/KG", or other
Numeric 8 . 0
-Character
"Y* •&£ '"N"
YYMMDD
HHMM
YYMMDD
HHMM
Character (1, 2, or 3)
"SOLVENT" or "SPE"
Character
Numeric 7 . 3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6 . 3 (minutes )
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q1E"
"AA" - "ZZ"
"Dl"
Character
Numeric 13.3
"U" or blank
Character
Character
H-12
07/30/92
-------
itiit
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18
19-24
25
26-31
32-37
38
39-44
FORM QI - PCB (Continued)
AROCLORS ANALYSIS DATA SHEET
CONTENTS
Form number
Form suffix
Record type
CAS no.
Peak
RRT
RRT flag
1C RRT (STDS)
RT
RT flag
1C RT (STDS)
FORMAT/CONTENTS
"QlEf
"M* - "ZZ"
"B2" ; . ,
Character
Numeric 1.0;
Numeric 6.3 ,\-*
"*" or blank
Numeric 6.3
Numeric 6.3
"*" or blank
Numeric 6.3
H-13
05/01/92
-------
•Ml*
HEADER RECORD
FORM QII - VGA
VOLATILES LABORATORY CONTROL SAMPLE DATA SHEET
FORMAT/CONTENTS
"Q2A*
"AA*' - "ZZ"
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-120
121-124
125-134
135-141
142-144
145
146-154
155-160
161-166
167-171
172
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
6
4
10
7
3
1
9
6
6
5
1
*,
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no . >
Sequence no. ;,
SAS no. <;'
Instrument ID /" ;
EPA sample no. ;J
Lab sample ID
Matrix
Date analyzed
Time analyzed
SMC CAS «»Jl : ,,••';-• n
SMC conce&feation" H;
SMC % recovery
SMC % rec out .flag
SMC area ' ,:
SMC RT ,
SMC 1C RT
,-KaT?t: ,,.
?!SMC*RT-1CI>,?out flag .•
V " f ; '"
st''.f', " "'
DETAIL RECORD ..* . ,'A>
COLUMN
1-3
4-5
6-7
8-17
18-26 /.
27-39 ,r<>
40-42 , "k~
43 , i }f
LENGTH ::|i =
3
2
2
lO;;;;;/;^
?$'
"13
3
1
^-Kt'-. ' '
j r^owTiPwn^f ^ ~~f''f^'' --^ •• -.''"'
K'-T
-------
FORM QII - PAH
POLYNUCLEAR AROMATIC HYDROCARBONS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42;
43 '"
LENGTH
3
2
2 - •:
9
13
3
1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. ;
Instrument ID
EPA sample no. :
Lab sample ID
Matrix
Extraction type
Date analysed
Time anaij|pB$ ':-,4, v: 1
SMC CAS n<£? ""'" ":
SMC concentration
SMC % recovery f
SMC % rec out^lag
SMC area
SMC RT
, sac ;ic |T
ftT %D -;A
SMC RT Xfti.out flag
Form-' &&££i'x.
Record't^e
no.
,,^concentrat ion
Obser| concentration
% reisibvery
% rec|;out flag
FORMAT/CONTENTS
"Q2B*
»AA* - "ZZ"
Character .,
Character "
Character
Character ••
Character
Character
Character
Character
Character
Cilaracter
"SOIL/SOLID", "WATER", or
spJeeaLfied other
"SOLfBIT" or "SPE"
YYMMDD ;
HHMM
Character
Nomekic 7.3
Numeric 3.0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q2B"
"AA" - "ZZ"
"Dl"
Character, "COMBINEA" for
coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
H-15
05/01/92
-------
FORM QII - PEE
PHENOLS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26 f.
27-39 ,y
40-42, •}'••
43 s'«^.-j
LENGTH
3
2
2 ,- ,;
rf°f!" :
V.%
13
3
L.' -^
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no .
Batch no.
Sequence no.
SAS no.
Instrument ID
EPA sample no .
Lab sample ID
Matrix
Extraction type
Date analyzed
Time analyze*!, j« :,
SMC CAS ri©.-, "'"" '"'
SMC concentration
SMC % recovery,
SMC % rec out ;€lag
SMC area
SMC RT
FORMAT/CONTENTS
-KT %D *'.. ...
SMC RT %Bsiout flag
Felpitiumber
Record
?CAS no.
^concentration
u concentration
flag
"AA"; - "ZZ"
"ttL"
Character
"Character
Character v •>
Character f~ •:
Character :.;
Character
Character
Character
Character
Character
*^)IL/SOLID" , "WATER" , or
specified other
"SOttfEST" or "SPE"
YYMMDD
HHMM
7.3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q2C"
"AA" - "ZZ"
"Dl"
Character, "COMBINED" and
"COMBINER" for coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
H-16
05/01/92
-------
MBit
FORM QII - PEST
PESTICIDES LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
18-26
27-39 ,,:
40-42;>:-
43 ~'<
LENGTH
3
2
O ,"
9
13
3
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
EPA sample no.
Lab sample ID
Matrix
Extraction type
Date analyzed
Time ana|5«e^;, • \; ;
SMC CAS noj; ' ; u
SMC concentration
SMC % recovery
SMC % rec out'J£Lag
SMC area ;
SMC RT
FORMATCONTENTS
SMC RT 5£0,,;:out flag
,", % '4,
• -GparrENTs
Fo»i aaumber
Form *a££ix
Record trjspe s
no. "v-'
•> concentrat ion
t> concentration
% recovery
% reO'-out flag
"AA* - "ZZ"
_
Character
Character
Character
Character
Character
Character
Character
Character
Character
i^ OIL/SOLID" , "WATER", or
other
or "SPE"
YXMMDD : r
HHMM
Numeteie 7.3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6 . 3 (minutes )
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q2D"
"AA" - "ZZ"
"Dl"
Character, "COMBINES" for
coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
H-17
05/01/92
-------
Wfft
FORM QII - PCB
AROCLORS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
I
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no .
Sequence no.
SAS no.
Instrument ID
EPA sample no.
Lab sample ID
Matrix
Extraction type
Date analyzed
Time analyzed
SMC CAS 4BCfc,',,;:; J / ,
SMC concesferation
SMC % recovSwey
SMC % rec out flag
SMC area
SMC RT
SMC 1C RT
, „
KT;fU;-out flag
CONTENTJS- ;•.-:' S;^ ,,-•':'" .': <"
number
suffix
RecorSSWtype
CAS not^Yl
concentration
concentration
FORMAT/CONTENTS
out flag
"A&* - "ZZ"
"HI*
Character
Character =,
Character -:: *,
Character >:
Character "• • •
Character
Charauter
Character
Chaa-acter
, CMaracter
.-"^OIL/SOLID" or "WATER"
•^S&BfENT" or "SPE"
YYMWffift .
HHMM "
Character
'-fomeric 7.3
'Ntmeric 3.0
"*" or blank
Numeric 9 . 0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q2E"
"AA" - "ZZ"
"Dl"
Character
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
H-18
05/01/92
-------
FORM QIII - VGA
VOIATILES PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
• 9
6
6
5
1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. ;
Instrument ID ;,
EPA sample no. 0
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC % re&4®&3^?. ~'<' T
SMC % ree:-Npit flag:
SMC area "f
SMC RT __ :
SMC 1C Rf
RT ZD
SMC RT %D out flag
FORMAT/CONTENTS
"ZZ"
"AA*
tJKaractrer
Character :
Character
Character
Character
Character
Character
Chacacter
CbaBteacter
Character
Character
Numeric 7 .'3
Numeric 3.0
blank
9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
LENGTH ,r"?
3
2 "•: ;:
2
10
CONTENTS P -|:
Form number
..Form suffeb£:
• -;|8.«c.ord type
CAS no .
18-26
27-39
40-42
43
44-49
50 f.
9,.
-••&
•'''3
1
6
1
True cora(3«n|:ration
X'%e^s out flag
Res6$yt % valley
ResoljlL % valley out flag "*" or blank
FORMAT/CONTENTS
"Q3A"
"AA" - "ZZ"
"Dl"
Character, "COMBINEC" for
coeluter
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
H-19
05/01/92
-------
IMft
FORM QIII - PAH
FOLYNOCLEAR AROMATIC HYDROCARBONS PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID ;,
EPA sample no.
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC % ree«*(r«%>-7;. •
SMC % rec'laut fla|
SMC area
SMC RT _ •;:,
SMC 1C RT !;
RT %D
SMC RT %D out flag
FORMAT/CONTENTS
"Q3&*
H A &£t" _ « 7 7 *t
Character
Character\_ s ,
Character ;v
Character
Character
Character
Character
Character
Character
Character
ItXMMDD
Charsfeter
Numeric 7.3
Numeric 3.0
•t*Z< or blank
•Nuaesdfc 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
DETAIL RECORD
CONTENTS'.
Form
Form
.Mtecord type
True
coneesifcration
covery
out flag
% valley
Reso^j- % valley out
FORMAT/CONTENTS
"Q3Bn
"AA" - "ZZ"
"Dl"
Character, "COMBINEA" for
coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
"*" or blank
H-20
05/01/92
-------
FORM QIII - PHE
PHENOLS PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43 :.i
44-49 ,;;| ;
50 *ff.
LENGTH
3 ':
2
2
10
9 x .. -s •
,:Ui3H" •'•
sV'3
= " 1
6
1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
EPA sample no.
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC % recsjwwcyj^". f;:
SMC % rec'%«sut flag"1
SMC area
SMC RT __
SMC 1C RT -J
RT %D
SMC RT %D out flag
CONTENTS;;':
Form nuni&fer^ m, ^
Form sy£@&; V'^,;';'' '/'
'^Record type
CAS BO.
True co'iicjeaatxation
.flbser. coiibeiieration
Rese
FORMAT/CONTENTS
"QSC"
"A&* - "ZZ"
•Qhara'ctei: .
Character
Character
Character
Character
Character
Character
Character
Character
.CJB&racter
out flag
% valley
% valley out
Character
Numeric 7/3
Numeric 3 . 0
"*"!;. or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q3C"
"AA" - "ZZ"
"Dl"
Character, "COMBINED" and
"COMBINEE" for coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
"*" or blank
H-21
05/01/92
-------
•Mtt
PESTICIDES
FORM QIII - PEST
PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
44-49
50 ?;, •
~:^l
r s--. . %
LENGTH
3
2
2
10
9
13-*; ^q,
/•'B - • : " '"""
'" ^^\
;•;•' 6
1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID :
EPA sample no .
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC %
SMC %
SMC area
SMC RT __ ' •< ;
SMC 1C RT V
RT %D '
SMC RT %D out flag,
CONTENTS • .
Form numf»e|r .
-JForm sv^fii,
%-eeprd type
'
_
flag"
True '-eseaeentration
Obser. cdlipentration
' '
FORMAT/CONTENTS
"Q3D"
"AA* - "ZZ"
"Hi*-; .
Character
Character
Character
Character
Character
Character
Character
Character
Character
Character
out flag
, % valley
Chariaceer
Numeric 7.'3
Numeric 3.0
*P" ^ors blank
Ntimerib 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q3D"
"AA" - "ZZ"
"Dl"
Character
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
ResSfLv % valley out flag "*" or blank
H-22
05/01/92
-------
FORM QIII - PCB
AROCLORS PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1.
9
6
6
5
1
DETAIL RECORD
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
EPA sample no.
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC %
SMC % rec
SMC area "4:~-.
SMC RT _ '•:•;.,
SMC 1C RT .- =
RT %D
SMC RT %D out flag"
J -f,s f*-t '!* -.. -
•iswt flag -
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
44-49 f ~
50 ;-'£
< .A'i
LENGTH
3 f
2
2
10
9
13- .> -'jt
//3i; ••" •'"'•
n:i
6
1
,'J:: CONTENTS :,i-l
:•""'. Form nunfoir.
'-;;;'f ^ ..Form su£xi^^^ *''\ ^ t '% .
•Sfefeord type
CAS >;»0s.
True: «^«a^entration
% 'j Obser . c?&$i€&&x3,tration
'" :t:-< ^.recovery' --i-g; '
'%;->irec out flag
Reioi. % valley
Resell % valley out
FORMAT/CONTENTS
"Q3R"
"&&?• - "ZZ"
Cjharact:er ,
Character f
Character
Character ;;
Character
Character
Character
Character
Character
.GSaracter
YSMMDD
mass.
Character
Numeric 7,3
Numeric 3 . 0
•f*5 &X blank
Wumeuic 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q3E"
"AA" - "ZZ"
"Dl"
Character
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
"*" or blank
H-23
05/01/92
-------
FOKM QIV - VGA.
VOIATILES INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
DETAIL
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-41
42-49
50-54 ,
55 «£
56-61't?
62
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
RECORD
LENGTH
3
2
2
10
s ;s> ?;
i.$J i;; ' '• •"
•^i£
•',' ?' 8
,.,-,<: ' 5
<-' 1
:- $., 6
;1||X'..i
'''- 1|6>|,'8!,
6 ~ -i>^ * ,
6 X~'V,
6
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. :
Instrument ID ;:;
CAL #1 EPA sample ago,,
CAL #1 lab sample IB
CAL #1 date
CAL #1 time
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab, sample ID
CAL #2
CAL #2
CAL #2 sta&lard cone.
CAL #3 EPA sample no.
CAL #3 lab sample IDj
CAL #3 date . .,'..;
CAL #3 time :v, .'•
CAL-||t3 .standard cone.
CONTENTSj"V
Form numfcei;
Form su^E^st/
leeord type
Low
Resoff % valley
ResqJ;;; % valley out flag
RT
•ritQf Mean
llRT Low
RRT Mid
RRT High
RRT Mean
FORMAT/CONTENTS
"Q4A*
"A&",,- "ZZ"
^Character
Character
Character
Character
Character
Character
Character
Character
Character
Numeric 9.0
Character
Character
YYMMDD
fKaaedcJ-c 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
FORMAT/CONTENTS
"Q4A"
"AA" - "ZZ"
"Dl"
Character
coeluter
Numeric 8.0
Numeric 8 . 0
Numeric 8 . 0
Numeric 8 . 0
Numeric 5 . 1
"*" or blank
Numeric 6 . 2
"*" or blank
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
Numeric 6 . 3
Numeric 6 . 3
"COMBINEC" for
Numeric 6 . 3
Numeric 6 . 3
Numeric 6 . 3
H-24
05/01/92
-------
FORM QIV - PAH
POLYNUCLEAR AROMATIC HYDROCARBONS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12.
12
6
4
9
12
12
6
4
9
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
26-33
34-41
42-49
50-54
55
56-6K ' ,
62 ' "< ;-
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH r'T
3 /" ';•
2 !
2
10
8^ , '
, < , , ;
>• 8
5
1
6
,?:,1
• 16:-
6'V-- ,
6 ' ' * :
6 :-;-
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
CAL #1 EPA sample ,no.
CAL #1 lab sample W ~
CAL #1 date =
CAL #1 time
FORMAT/CONTENTS
"Q4B*
"AA*. - "ZZ"
"SI*
Character
- Character,
Character
Character :
Character
Character
Character
Character
Character
Chracter
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab,, sample ID
CAL #2 date" ';/ -
CAL #2 ti»e "°~ -'- ,< o -,-i-;'
CAL #2 standard cone. ' !'
CAL #3 EPA staple no.-!
CAL #3 lab saigple ID; '
CAL #3 date -\.
CAL #3 time
CAL ;#3 standard c«nc.
CONTENTS ' ;
Form Tn intf%j&y , , , „ , ,
•Form sUiiSs; s ~i~ •-, •, . ~
^RBDord type
CAS -Sao,.
LOW :, ;;
; Hid
-------
FORM QIV - PHE
PHENOLS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-41 -7
42-49 .-••• '*"
50-54 ^V
55 .<••§:••
5 6 - 6 1- 1|^ ''.?, r
/TO '**-* V$
\jt. ••> «-•
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH
3
2
2
10
8-. S",
o *- >• < -^> **>';
*$, - -
: v-8
8
5
1
6
~!A
•sjjji ?
Vlk-
6 "4
6
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no. ;,
SAS no.
Instrument ID •,
CAL #1 EPA sample'$ao,
CAL #1 lab sample"IDS
CAL #1 date
CAL #1 time
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab sample ID
CAL #2
CAL #2
CAL #2 staa&ard cone. /
CAL #3 EPA sample no. r
CAL #3 lab sample ID-/
CAL #3 date -:' '; ;
CAL #3 time , =
CAL #3 standard cone.
CONTENTS .
Form
-: Form
'•"Bsecprd type
Low
'Hid
FORMAT/CONTENTS
"Q4CT?
"AAV- "ZZ"
"HI* ,,
Character
Sharacter ."
Character • .
Character
Character
Character
Character
Character
Character
Character
9.0
Chara^tser
Character
YYMMDD
9 . 0
Character
Character
YYMMDD
HHMM
Numeric 9 . 0
FORMAT/CONTENTS
"Q4C"
"AA" - "ZZ"
"Dl"
Character, "COMBINED" and
"COMBINEE" for coeluters
Numeric 8.0
Numeric 8.0
0
0
% RSl%flag
Reso|L»; % valley
RescjJLy % valley out flag
Mean
RT Low
RRT Mid
RRT High
RRT Mean
Numeric 8.
Numeric 8.
Numeric 5.1
"*" or blank
Numeric 6.2
"*" or blank
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
H-26
05/01/92
-------
FORM QIV - PEST
PESTICIDES INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no. ;
SAS no.
Instrument ID
CAL #1 EPA sample IM>,
CAL #1 lab sample f$
CAL #1 date
CAL #1 time
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab -sample ID
date;!:.
CAL #2
CAL #2
CAL #2 standard cone.
CAL #3 EPA Jlaaple no.
CAL #3 lab sample ID
CAL #3 date n
CAL #3 time ,'.!':
CAL- #3, standard coac.
FORMAT/CONTENTS
"Q4D*
"AA». - "ZZ"
"HI"
Character
Character
Character - • t.
Character
Character
Character
Character
Character
Character
Character
YSfflMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
34-41
42-49 ,r
50-54 .'V
55 ,;..;-"
56-611*-! '«,
62 :
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH.
3
2
2
10
8- : ;.'
8'!, ;!' • .1!
.," ''
• v 4^0
f 8
5
1
6
;CJ-1
'"••;,€ -,;'
6"'';--.fo ' ,
6 "' /•
6
6
6
6
6
•';r CONTENTS I8
Form nuisi3NE$3r - ? ^ • *
-< -, 4fFprm suffiM.'li',::/^-: >; ,-,
' "Rsfeeord type
CAS no.
' " ";\:
°- - LOW """ ,"; *:
, A* • J v ^ v: -..
•*-!„ ,;Hld •!; *>
:*|JB»
% R>|>
"s "
% R£%.fcflag
Resol i % valley
Resci-1 % valley out flag
RT Low
RT'?!Cid
'•.. RflHigh
: -D ,«P Mean
'l %8RT Low
RRT Mid
RRT High
RRT Mean
FORMAT/CONTENTS
"Q4D"
"AA" - "ZZ"
"Dl"
Character, "COMBINES"
for coeluter
Numeric 8.0
Numeric 8.0
Numeric 8.0
Numeric 8 . 0
Numeric 5 . 1
"*" or blank
Numeric 6 . 2
"*" or blank
Numeric 6.3
Numeric 6.3
Numeric 6 . 3
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
H-27
05/01/92
-------
IMP*
FORM QIV - PCB
AROCLORS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-92
93-98
99-104
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
RT Low
RT Mid
RT High
RT Mean
FORMAT/CONTENTS
"AA", - "ZZ"
"HI*
Character
Character
Character
Character
Character
Character
Character
Character
Numeric 6.3
Nuiferic 6.3
Numeric 6.3
6 . 3
HEADER RECORD
COLUMN
1-3
U-5
6-7
8-19
20-31
32-37
38-41
42-50
51-62
63-74
75-80
81-84
85-93
94-105
106-117
118-123
124-127
128-136
137-148
149-160 /
161-166 i
167-17DV
171- It9;r
LENGTH
3
2
2
12
12
6
4
9
12
12
6
4
9
12
12
6
4 ,; •;;..
;?9 ;';' ^::-
'i!2
1 ; "' 12
6
4
9
CONTENTS If,
Form number
Form suffix
Record type
CAL #1 EPA ss
CAL #1 lab sample
CAL #1 date
CAL-$!„ time ; ;
CAL $1. standard conc»
CAL #2"^jjjk sample noi
CAL #2 ifb -sample ID
CAL #2 dlbe
CAL #2 tifite,
CAL #
Cfii, #3 EPA sample no.
CAT, $3 lab sample ID
CAL $
CAL #
#3 staijdakd cone.
lene EPA sample no.
toxaphene lab sample ID
toxa|>hene date
toxapMene time
toxaphene standard cone.
FORMAT/CONTENTS
"Q4E"
*JBt«> "ZZ"
MH2"
Character
Character
YYMMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
H-28
05/01/92
-------
FORM QIV - PCB (Continued)
AROCLORS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
42-50
51-62
63-74
75-80
81-84
85-93
94-105
106-117
118-123
124-127
128-136
137-148
149-160
161-166
167-170
171-179
180-191
192-203
204-209
210-213
214-222
LENGTH
3
2
2
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
DETAIL RECORD '"
COLUMN
1-3
4-5
6-7
8-17
18
19-26
27-34
35-42 ,i.
43-50 I-/'
51-55^ ';
56
57-62
63-68
LENGTH '" ;,
3
2
2
10s !: -?'•;
, ill'1'-''' ' """ :"
> /.-&B"
^ 8
8
8
4-, 5
"|;" JL
•4f5- 1
6-CV , /
CONTENTS
Form number
Form suffix
Record type
1221 EPA sample no.
1221 lab sample ID
1221 date
1221 time
1221 standard cone.
1232 lab sample no.
1232 lab sample ID
1232 date
1232 time :
1232 standard concr.
1242 EPA sample no.
1242 lab sample ID
1242 date
1242 time
1242 standard cone.
1248 EPA.i sample no.
1248 lab Sample'IS
1248 date' ;
1248 time
1248 standardseonc.
1254 EPA sample-no.
1254 lab sample ID".;
1254-.-date •<
,'1254 dtitae ' '••.
1254 stasjpard cone.
number
s' suffix
CAS no. •'..
FORMAT/CONTENTS
"Q4E"
"AA" - "ZZ"
"S3"
Character
•Character -
YYMMDD
HHMM '" .
Numeric 9.0
Character
Character
YYMMBB
HHMH ,
Numeric 9.0
Character
Character
LofelllRT
Numeric 9.
Character
Character
HHMM
Numeric 9.0
Character
Character
YXMMDD
HHMM
Numeric 9.0
FORMAT/CONTENTS
"Q4E"
"AA" - "ZZ"
"Dl"
Character
Numeric 1.0
Numeric 8.0
Numeric 8.0
Numeric 8.0
Numeric 8.0
Numeric 5.1
"*" or blank
Numeric 6.3
Numeric 6.3
H-29
05/01/92
-------
MM*
FORM QV - VGA
VOLATILES CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10
8
8
5
1 -;
$M ;'"
• "~ JL
.'•-,.. ...
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no. '
Sequence no.
SAS no. -';:
Instrument ID , ;,
EPA sample no. ;,— ,
Lab sample ID
Standard concentration
Date analyzed
Time analyzed
SMC CAS no,;<
SMC areaA-J ,• A. '
SMC RT '«;,._""" •*! -~hj'
SMC 1C Rf •' ,i
RT %D " :'.-, ,:j
SMC RT %V out'yElag , i'-
Form
Form sufflas
Record t^e
no ^i|-; ,&j
CF
v..
D out "Sag
% vallky
% valley out flag
FORM&t/CONTENTS
"Q54!"'
"AA*; - "ZZ"
"11*; ,-
Character
Character ,;• .
Character ]•]
Character
Character
Character
Character
Character
Character
.GiSaaracter
9.0
Character «
Numeric 9.0
* .Hosier ic 6.3 (minutes)
"^Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q5A"
"AA" - "ZZ"
"Dl"
Character
Numeric 8.0
Numeric 8.0
Numeric 5.1
"*" or blank
Numeric 6.2
"*" or blank
H-30
05/01/92
-------
FORM QV - PAH
POLYNUCLEAR AROMATIC HYDROCARBONS CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
" 6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10
8
8
5,; • ;.
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no. . :
Sequence no.
SAS no. . :
Instrument ID y
EPA sample no. - 'f.
Lab sample ID ' |;
Standard concentration
Date analyzed
Time analyzed
SMC CAS no..:
SMC area-" -"' '*• •-.? v
SMC RT ^ • ' '' :: &••#
SMC 1C RT f ,{
RT %D
SMC RT %D out
fs" Form number
: Form suffix
Record
^ CAS no*
iUifcba el-
Mid' '• s V,,
% D =; ,. ;£;
5; % D out flasgli-
.. % valley
FORMAT/CONTENTS
"Q5B"
Character ,
Character
Character
Character
Character
Character
Character
Character
Character
Character
Htuneric 9.0
HHMM
Character
Numeric 9.0
6.3 (minutes)
6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q5B"
"AA" - "ZZ"
"Dl"
Character, "COMBINEA" for
coeluter
Numeric 8.0
Numeric 8.0
Numeric 5.1
"*" or blank
Numeric 6.2
. % valley out flag "*" or blank
H-31
05/01/92
-------
FORM QV - PHE
PHENOLS CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10
8
8
c
PL': {-I.'-"*
v '™S>'
' V=" '" 1
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no. ^
Batch no. ;•*•
Sequence no. < ,.,;'
SAS no. .°|
Instrument ID . ;
EPA sample no. 'I ;,,;
Lab sample ID :
Standard concentration
Date analyzed
Time analyzed
SMC CAS no«^
SMC areaj;-';'* f,, v.,r
SMC RT
-------
wait
FORM QV - PEST
PESTICIDES CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
DETAIL
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
RECORD
LENGTH
3
2
2
10
8
8
5
1 , •!, ;; _
,*-j6,,, ''' •:'""
.- all
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no. ;;
Sequence no.
SAS no. :
Instrument ID ,•-.
EPA sample no. , .:,,,
Lab sample ID "'•;
Standard concentration
Date analyzed
Time analyzed
SMC CAS no..,,
SMC area'; 7- ;•',;;, "''
SMC RT r >;' ""':~' f'-'-\
SMC 1C RT ;: f
RT %D ., 1!
SMC RT ZD out;tlag < .':
Form number
Form suffStx
Record
-ntitial CF
FORMAT/CONTENTS
"ZZ"
"A&*
•m*
Character :.
Character
Character
Character
Character
Character
Character
Character
GSkracter
9.0
% D '••;;;
% D out'
Resol. %
% valley out flag
Character
Numeric 9.0
6.3 (minutes)
6.3 (minute s)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q5D"
"AA" - "ZZ"
"Dl"
Character
Numeric 8.0
Numeric 8.0
Numeric 5.1
I1*n or blank
Numeric 6.2
"*" or blank
H-33
05/01/92
-------
ttftlt
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
' 6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18
19-26
27-34
35-39
40
41-46
47
LENGTH
3 ,;
2 ,' -'
' .,K
2 ,"- -
10 ''-'> |
1
8
8
5,.,;W
.^.^^
,;V'V^
§,~?;": 1
FORM QV - PCS
AROCLORS CALIBRATION CHECK SHEET
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no. .;
SAS no. ; ,
Instrument ID ; «= \
EPA sample no. -":-•„
Lab sample ID
Standard concentration
Date analyzed
Time analyzed
SMC CAS nQ.,,
SMC area "|H',;:'>,: , »v
SMC RT 't- " ' ^^t{' '
SMC 1C RT " '
RT ZD
SMC RT %D out-flag
Form
Form suffix
Record
no,
CF
FORMAT/CONTENTS
"Q5E*
"Mwi - "ZZ"
"HI"*,
Gtxaracter
Character S!
Character •;
Character
Character
Character
Character
Character
Character
Character
Ktsaeric 9.0
out
1 . % valley
% valley out flag
HHMM" ,<
Character
Numeric 9.0
: ^eperic 6.3 (minutes)
Nisaefclc 6.3 (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q5E"
"AA" - "ZZ"
"Dl"
Character
Numeric 1.0
Numeric 8.0
Numeric 8.0
Numeric 5.1
"*" or blank
Numeric 6.2
"*" or blank
H-34
05/01/92
-------
FORM QVI - VOA
VOIATILES ANALYTICAL SEQUENCE STMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. ;
Instrument ID V :
Start date
Start time
Stop date
Stop time
Initial calibration
date
FORMAT/CONTENTS
"Q6A*
"AA* - "ZZ"
-si*
> Character.
Character |
Character : ,
Character
Character
Character
Character
Character
YHBBiDD
.YXHMDD
YXMMD1)
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
CONTENTS
Form number
Form suffix
Record type
EPA:sample no.
Lab samp|e ID
Date analyzed
Time analyzed
FORMAT/CONTENTS
"Q6A
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
H-35
05/01/92
-------
FORM QVI - PAH
POLYNUCLEAR AROMATIC HYDROCARBONS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. ;
Instrument ID .,}
Start date ' •:
Start time
Stop date
Stop time
Initial calibration
date , „
CONTENTS !
Form number
Form suffix
Record type
EPA sample no.
Lab sample ID
Date analyzed
Time analyzed
FORMAT/CONTENTS
"Q6B"
"A&* - "ZZ"
^Character
'Character
Character
Character
Character
Character
Character
Character
YXHKDD
YYMMDB
FORMAT/CONTENTS
"Q6B
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
H-36
05/01/92
-------
FORM QVI - PHE
PHENOLS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
CONTENTS
Form number
Form suffix
Record type
Lab name •
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
Start date
Start time
Stop date
Stop time
Initial calibration
date <. .
CONTENTS
Form number
Form suffix
Record type
E£A sample no.
Lab sample ID
Date analfized
Time analyzed
FORMAT/CONTENTS
"Q6C"
"AA" - "ZZ"
•Mil* >
Character
Character
Character '"
Character
Character
Character
Character
Character
1SMMDD
FORMAT/CONTENTS
-Q6C
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
H-37
05/01/92
-------
FORM QVI - PEST
PESTICIDES ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no. ;'
Instrument ID ;
Start date
Start time
Stop date
Stop time
Initial calibration
date
CONTENTS
Form number
Form suffix
FORMAT/CONTENTS
"Q6B"
'- "ZZ"
Character °
Character
Character
Character
Character
Character
Character
YXUHDDD
HHMM
YXMHDP
no.
Lab sample ID
Date anal
Time ar
FORMAT/CONTENTS
"Q6D
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
H-38
05/01/92
-------
FORM QVI - PCB
AROCLORS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID >
Start date "
Start time
Stop date
Stop time
Initial calibration
date , ,,
CONTENTS '•'•„
Form number i
Form suffix
Record type
EPA sample no.
liab sample ID
Date analyzed
Time analyzed
FORMAT/CONTENTS
"Q6B"
"A&"? - "ZZ"
•Wt-
Character
Character
Character
Character
Character
Character
Character
Character
YXM8DD
YYMMDB'
FORMAT/CONTENTS
"Q6E
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
H-39
05/01/92
-------
tttttt
FORM QVII - VOA
VOIATILBS NARRATIVE
HEADER RECORD
COLUMN LENGTH CONTENTS FORMA3VCONTENTS
1-3 3 Form number "Q7A"
4-5 2 Form suffix "A&*
6-7 2 Record type "HI" -
8-32 25 Lab name Character
33-43 11 Contract Character
44.49 6 Lab code Character
50-54 5 Case no. : Character
55-62 8 Batch no. ,;; Character
63-68 6 SAS no. , Character
DETAIL RECORD
CONTENTS ': : .PQBMAT/CONTENTS
Form number ;*Q?Alf
Form suffix "A&* - "ZZ"
Record type "Dl" f
Comment line # Numeric 3.0
Comment „
-------
FORM QVII - PAH
POL7NUCLEAR AROMATIC HYDROCARBONS NARRATIVE
HEADER RECORD
COLUMN LENGTH CONTENTS FORMAT/CONTENTS
3 Form number "Q7JJ*
2 Form suffix
2 Record type
25 Lab name Character
11 Contract Character': •,.,
6 Lab code Character '- ':•
5 Case no. Character
8 Batch no. s Character
6 SAS no. . Character
DETAIL RECORD : !
COLUMN LENGTH CONTENTS ' f FJORftAT/CONTENTS
1-3 3 Form number ;; '^7Bn
4-5 2 Form suffix "M? - "ZZ"
6-7 2 Record type "Dl"
8-10 3 Comment line # Ntuneric 3;~0
11-75 65 Comment-|1 '••'J.i ; Character
H-41 05/01/92
-------
DfcAJt
FORM QVII - FHE
PHENOLS NARRATIVE
HEADER RECORD
COLUMN LENGTH CONTENTS FORMAT/CONTENTS
3 Form number "Q7C*
2 Form suffix "AA,"
2 Record type *?B1" :
25 Lab name Character
11 Contract Character
6 Lab code Character
5 Case no, '.. Character
8 Batch no. ^ Character
6 SAS no. '," Character
DETAIL RECORD , •'.
COLUMN LENGTH CONTENTS ' f F<3BMAT/CONTENTS
1-3 3 Form number fQ^C"
4-5 2 Form suffix *A£" - "ZZ"
6-7 2 Record type "Dl" \\
8-10 3 Comment TJupG # Numeric 3,0
11-75 65 Comment ,;,;j,;;;s!,''',' , Character
H-42 05/01/92
-------
FORM QVII - PEST
PESTICIDES NARRATIVE
HEADER RECORD
COLUMN LENGTH CONTENTS FORMAT/CONTENTS
3 Form number "Q7B*
2 Form suffix "M*
2 Record type nJ£L*
25 Lab name Character
11 Contract Character ;,
6 Lab code Character '-* [•,
5 Case no. . v; Character :;
8 Batch no. : Character
6 SAS no. Character
DETAIL RECORD
CONTENTS ;•< FilgMAT /CONTENTS
Form number :::*Q7D"
Form suffix "A&* - "ZZ"
Record type "D1H> ;
Comment line, # Numeric 3;0
Comment --; - '>• }'• • -'f Character
"
H-43 05/01/92
-------
HEADER RECORD
nut
FOKM QVII - PCB
AROCLORS NARRATIVE
COLUMN
LENGTH
3
2
2
25
11
6
5
8
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
SAS no.
FORMAT/CONTENTS
"Q7I"
"AA;*
Character
Character
Character
Character
Character
Character
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-10
11-75
LENGTH
3
2
2
3
65
CONTENTS
Form number
Form suffix
Record type
Comment line #
Comment s-'_ til? V,i
F0SI1AT/CONTENTS
"SQJE"
"ML* - "ZZ"
"Dl" > .: , _
Numeric :3»0
Character
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL 60604-3590
H-44
05/01/92
-------