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ANALYSIS (Iype ot Report)
REPORT NO.:
MSL-6249 ESC-UA6-86-I31
J08/PR0JECT NO.: 760.28-6264
OATE: DECEMBER 4. 1986
TITLE:
ANALYSIS OF TWO AUGUSTA PLANT MATER SAMPLES FOR PCS FORMULATIONS
AUTHORS: ABSTRACT:
8.M. HUGHES, 0. McKENZIE, and 8. SIMPSON
Two water samples from the Augusta Plant were analyzed for PCS forumlatlons. One sample designated NPDES was sent In quadruplicate for quality control purposes. These water samples were analyzed to confirm that no Pt3s are present In NPDES samples from the Augusta Plant. Previous results from ETC Indicated large amounts of PCBs were present In these samples. ETC reviewed their data and found It to be In error. The present study cpnflrms that no Aroclor formulations are present In these water samples with a level of detection of 1 part-per-bllllon. For further Information concerning previous analyses, see report number MSL-59S5.
TECHNICAL APPROVAL
Paul Sherman Environmental Sciences Center Senior Research Group Leader
APPROVED BY
Environmental Sciences Center Quality Assurance Specialist
APPROVAL OATE :
/~7t /
MOMS 024461
COMPANY CONFIDENTIAL
This document is the property of Monsanto Company end the recipient is responsible for its safekeeping end disposition. N contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorized persons or sent outside the Company without proper authorization
COPY NUMBER
T HIB U rIO N
ABSTRACT ONLY
1. B.M. Hughes - U4E 2. 0. McKenzie - U4F 3. B. Simpson - U4F 4. F. Hiller - 31 (Augusta Plant) 5. A. M. Ford - U4 6-8. Reports Library - R2C 9. Chesterfield Information Center - AA3A
P. L. Sherman - uiF
HONS 024462
COMPANY COMHDFNTIAI
This reoort has been assigned to you When it is no longer needed, you are resoonsibie for returning it to:
ii
if you transfer it to anyone else, please let your librarian know, so the record! can be changed
Time Scamp <861203.1620> ANALYSIS REPORT
DATE: November 17, 1986
LOG NUMBER: U-86-U-06-01
PROJECT NO: 760.28-6264
TO: Fred Hiller, Augusta Plane
FROM:
Envlronmaneal Sciences Cancer Monsanto Company 800 N. Lindbergh Blvd. SC. Louis, Mo. 63167
Phone No: (314) 694-1464
Title: Analysis of Tvo Augusta Plant Voter Samples for PCB Formulations.
ABSTRACT
Two water samples from the Augusta Plant were analyzed for PCB forumiatlons One sample designated NPDES was sent in quadruplicate for quality control purposes. These water samples were analyzed to confirm that no PCBs are present in NPDES samples from che Augusta Plant. Previous results from ETC indicated large amounts of PCBs were present In these samples. ETC reviewed their data and found it to be in error. The present study confirms Chat no Aroclor formulations are present in these water samples with a level of detection of 1 part-par-billion. For further information concerning pre vious analyses, see report number M$L*5953.
INTRODUCTION
In Che first quarter of 1985, ETC reported that PCBs wars prasant In waste vecer samples from the Augusts Plane. ETC was asked to review their data and found it to ba in error. Plant parsonal racantly sane tvo vasts water samples to confirm that undetected PCBs raporcad in MSL-5955 also applied to their NPDES discharge sample. Samples were extracted using Standard Extraction Method VSEXOS and analyzed via Standard Analysis Mathod ECAN02. All samples vara spiked wleh pentachlorobenzene and 2.4,6-trichlorobiphanyl as surrogate spiking compounds. Surrogate recoveries ranged from 62 to 90%. In addi:mr tvo of eh# samples wars spiked with Aroclor 1248 st levels corresponding .o l and 10 ppb. Recoveries ware respectively 141 and 121%. The samples --eve found to contain no deeecceble Aroclor formulseions with a level of detection of 1 ppb.
SUMMARY
Table 1 summarizes the results of these analyses. Note that no PCB
formulations wars datsetsd in chase samples with a limit of detection of
1 ppb. Quality control measures, such es spiking che samples with surrogate
compounds and with two coneancracions of Aroclor 1248, indicate chat che re
ported results are correct.
(continues
HONS 0244*3
Page 2, A26430 (conc'd)
QC RESULTS
Table 1 summarizes the recoveries of Aroclor 1248 spiked Inco cvo staples a: 1.0 and 10.0 ug/L. Results show that PCB formulations could have been de tected in chaaa lavals If chay had baan prasanc. In addition. recoveries for surrogate compounds indicata chac chasa data ara corracc.
DETAILS Standard Sampling Method Mo(s): Samples suppliad by Mr. Frad Hlllar of the
Augusta Plant. Standard Extraction Method Ho(s): WSEXOS (Saa USFSOS for method flow sheet : Standard Analysis Method No(a): ECAN02 (Saa ECFS02 for method flow sheet). Sample Identification^): Veil *1, NPDES Permit *1, NPDES Permit *2, NPDES
Permit #3, and NPDES Permit *4. Final Report File No(s): A26430:HH Table File No(s); B26430:MH Also included in this report ara:
(1) Brief descriptions of Standard Extraction and Analysis Methods used (2) Extraction details for samples associated with this project. (3) Raw data documentation, Included a preliminary report sent on 10/2/86 (4) Analytical raquaat Information recorded at sample login. (5) Brief daacripciona of terminology used in Quality Aesurenca/Quallcy
Control, Analyta Extraction, and Instrumental Analyels. ANALYST(S); B. Maaon Hughaa, David McKenzie, end Brenda Stepson ANALYST APPROVAL: ^ -'Turn-ByJ
HONS 024464
Table 1. Suaaary of Aroclor 1248 Spiking Concentration* and Racover.es along with Surrogate Recoveries for Augusta water samples.
NOTE: No Aroclor forauletlons were detected In eny of these saoples except those saaples which were spiked with Aroclor 1248 for quality control purposes.
ESC Project No: 780.28 8264
Date: Noveober 17, 1986
Saaple I. D.
(!) Surrogate Recovery
Aroclor 1248
CL5benzene
2.4.6-CL3biphenyl
Aoount Added Recover',
(ug/g)
U)
3 NPDES PERMIT + LS(a)
76
84
1.0 Ul
4 NPDES PERMIT * HSU)
79
90
10.0
121
WELL el
72 80
*1 NPDES PERMIT
67 80
2 NPDES PERMIT-DUP 64 75
DEIONIZED HATER TRIP BLANK
66
72
B & J HATER-METHOD BLANK
62
67
Footnotes: e.
LS - low level native spike. HS - high level native spike. Aroclor 1248 was used as the native spiking agent.
TABLE FILE NO: 826430:MH
HONS 024465
Th. following p.g.. dw.crib. St.nd.rd S.npling, Extr.ctlon. .nd/or An.l7.ls N.chod. ussd for chi. projsct.
HONS 024466
ESC Standard Extraction Mathod (SEM) TITLC: tflda scan axtraetlon aathod
for vatar.
MATRIX:
vaear
ESC Standard Extraction Method No: WSEX05
TYPICAL SAMPLE SIZE
(Litars)
TYPICAL EXTRACT VOLUME (d
TYPICAL ANALYTES: Aroclora. PCBa, priority pollutant*
0.01 - 4
1 - 40
ESC Standard Analvsls Mathod Nos: ECANxx and MSANxx
INTERFERENCES: Various; Saa individual intarfaraneaa for Individual analytas.
TYPICAL SURROGATES
TYPICAL RECOVERIES ()
phanol-dS CL-phanol-d4 CL2-banzana*d4
naphthalan#-d8 pyrana-dlO chry*ana-d!2 pantachlorobanrana 2.4,6-trlchloro-
blphanyl
20-80 20-80 50-120 50-120 50-120 50-120 50-120
50-120
APPARATUS AMS MATERIALS: Burdick and Jackaon aathylana chloride
Separatory funnala Sodlua aulfata for extract drying Sodlua hydroxide and sulfuric acid for pH adjuacaenca Nitrogen for extract voluae reduction Vacer bach and K*D apparatus for extract voluae reduction
LIMITATIONS: Sufficient saaple aaount to provide CC-MS LOD.
SAFETY PRECAUTIONS: See Safe Laboratory Practleaa.
DATES OF METHOD CREATION AND UPDATES: 5/16/84, 10/5/84. 12/7/84
HONS 024467
FLOW SHEET WSFSOS FOE ESC EXTRACTION METHOD VSEX05
sample id: ................................................................................. mrc extract ............. ................................................................................. LOG NO: ..........................
EXTRACTION DATE and TIME: ........................................................./....................................
RECORD NATIVE pH...................... WAS pH ADJSTED YES/NO IF YES TO WHAT pH
PLACE SAMPLE INTO AN APPROPRIATELY SIZED SEPERATORY FUNNEL (1/2 HEAD SPACE SUGGESTED FOR ADEQUATE MIXING)
[] . .
SAMPLE VOLUME ...................................... SURROGATE SPIKE
IF pH ADJUSTED
( ) ADJUST WITH,SOI NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN ( ]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 mL SOLVENT. .
100 aL SAMPLE 13 aL SOLVENT) .
SHAKE SAMPLE ONE TIME
[]
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKES BETWEEN VENTING
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED 10
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED FOR EACH EXTRACTION
I I)
I
\l / V
2)
3)
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[]
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT.
till ..
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
, ( ] EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
(] .
REDUCE EXTRACT VOLUME TO 1 aL BY K-D TECHNIQUE AND OR NITROGEN SOLVENT VOLUME REDUCTION
[] . . .
t 1 TRANSFER EXTRACT INTO VIAL FOR ANALYSIS
EXTRACT NO: ...................................... DATE/TIME COMPLETED............................. /....................
ANALYST:
ESC JOB NO:
HONS 024468
CSC Standard Analysis Method (SAM) TITLE: Aroelor Formulations In Solvents
ESC Standard Analysis Mathod Mo ECAM02
ANALYTICAL INSTRUMENT AND MODE OF OPERATION: HP-5880 Capillary CC/EC inter faced eo an HP-3357-LAS Laboratory Data Syseaa
TYPICAL ANALYTE
TYPICAL INSTRUMENT LEVEL OF DETECTION (LOD)
(ug/ml)
Aroelor formulations 1232. 1242, 1248. 1254. 1260. and 1262
0.1
TYPICAL PRECISION @ 10X LOD
<%>
30
TYPICAL ACCURACY 10X LOD
(%)
30
INTERFERENCES AND LIMITATIONS: Any alaetron capturing spaelaa In tha reten tion else region of trlchloroblphenyl through octachloroblphenyl Isosera are potential Interferences. Exact retention tlaes of aose likely PCg Isomers can be obtained from the analysis of Aroelor 1248. Aroelor 1254 or Aroelor 1260 foraulatlons.
CHROMATOGRAPHIC COLUMN: 30-aeter fused silica J&tf DB-5 (0.25 uM) with vide bore (0.32am).
COLUMN TEMPERATURE PROGRAM: 130<l)/4/300
INJECTION TYPE: SpUcless
CALIBRATION AND STANDARDIZATION: Use Internal standard quantitation teehnlquo and calibrate instrument response factors froa authentic Aroelor formulation standards. Use a alnlaun of 10 PCB Isoaers for the determination of forau-
iaelon identity and quantity.
CALCULATIONS:
Formulation concentration (Isoaer RRF)(lsoaer area/lntemal standard area)
vhere: RRF is the relative response factor for the appropriate PCB isomer in a given formulation. Formulation concentra tion le obtained from the average of at least 10 such cal culations.
SAFETY PRECAUTIONS: Saa PCB handling protocols In laboratory safety manual
DATE OF METHOD CREATION: 10/25/83, 2/3/84 Time Stamp <861203.1620>
HONS 024469
FLOW SHEET ECFS02 FOE ESC ANALYSIS METHOD ECAN02
EXTRACT ID:
ESC EXTRACT *
LOG NO:
EC LOGBOOK PAGE NUMBER: .......................................................................................................................
EXTRACT COLOR AND DESCRIPTION .........................................................................................................
PLACE ISO uL EXTRACT
OR AROCLOR STANDARD.
AND ISO uL INTERNAL
[)
STANDARD SOLUTION CONTAINING .
0.0A ug/nL CL6-BENZENE IN .
BENZENE IN A 1.6 aL
.
AUTOSAMPLER VIAL.
.
PLACE VIAL IN AUTOSAMPLER TRAY OF HP-5880.
RECORD ELECTRON CAPTURE AND GAS CHROMATOGRAPHIC OPERATING PARAMETERS AND 33S7-LAS FILE INFORMATION IN INSTRUMENT LOGBOOK.
(] .
[]
CALCULATE RRFs FOR 10 30 PCB CONGENERS
IN THE APPROPRIATE AROCLOR FORMULATION.
USING THE AROCLOR CONCENTRATION AS THE
........................[ !
ANALYTE CONCENTRATION
. FOR EACH PCB CONCENER.
( ] CALCULATE CONCENTRATION OF AROCLOR FORMULATION BY AVERAGING THE VALUES DETERMINED FROM THE 10 30 PCB CONGENERS
Whir*:
(conganar araa In Aroclor standard) RRF Ralaclva Rasponaa Factor - .....................................................................................................
(CL6-bansana araa)(Aroclor concantratlon)
(conganar araa)
Aroclor Concantratlon (CL6-banzana araa) (RRF)
THESE EQUATIONS ASSUME THAT THE SAME AMOUNT Or INTERNAL STANDARD IS ADDED TO EXTRACTS AND STANDARDS.
Tha abova calculations ara parfomad for 10 - 30 PCB conganars and tha valuas avaragad to ylald an avaraga Aroclor formulation concantratlon.
MS FILE NUMBER: .................................. DATE/TIME COMPLETED ................................. / ANALYST: ......................................................... Esc J0B N0: ..................................................
HONS 024470
Tho following pogos show ixtraction docails for suplss tssoclstsd vlch this projoec.
HONS 024471
FLOW SHEET WSFSOS
FOE ESC EXTRACTION METHOD VSEXOS
WELL ml
US-1337
SAMPLE ID:
....................................................................... MRC EXTRACT .................
U-86 -11-06-01
NOVEMBER 10, 1986
LOC NO: .................................
EXTRACTION DATE nd TIME: 5
---/..........................................................
RECORD NATIVE pH .................
WAS pH ADJSTED NO IF YES TO WHAT pH
PLACE SAMPLE INTO AN
1 LITER (X] SAMPLE VOLUME .............................
APPROPRIATELY SIZED SEPERATORY FUNNEL
.
SURROGATE SPIKE
(1/2 HEAD SPACE SUGCESTED FOR ADEQUATE MIXING)
.
-DEM 121483-02 (lug/al AND 2ug/ml>-
( ] ................................................................................
IF pH ADJUSTED
( ) ADJUST WITH,50% NmOH OR H SO 24
ADD METHYLENE CHLORIDE IN [X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 mL SOLVENT, .
100 mL SAMPLE IS mL SOLVENT) .
SHAKE SAMPLE ONE TIME
[X]
AND VENT THROOCH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKES BETWEEN VENTING
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED SO
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 L
1 i \i / V
n30 aL
2)30 L
3)-
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-YELLOW COLOR NOTED. EMULSION FORMED UPON SHAKING....................
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
(X] [X] ..
IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT.
(] .
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 mL METHYLENE CHLORIDE)
(XI . . .
. . .................................................. . . [ ] EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 mL
[X] .
REDUCE EXTRACT VOLUME TO 1 mL BY K-D TECHNIQUE AND OR NITROGEN SOLVENT VOLUME
REDUCTION
WS-1837
EXTRACT NO: ............................... SIMPSON
ANALYST: ......................................
[X] .
[X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
- DATE/TIME COMPLETED.......................... /.................. 760.28-6264
- ESC JOB NO: ...............................................................
HONS 02447E
FLOV SHEET WSFS05
FOR ESC EXTRACTION METHOD WSEX05
#1 NPDES PERMIT
US-1838
SAMPLE 10:
....................................................................... HRC EXTRACT ....................
U-86-11-06-01 ....................................................................... LOG NO: ..................................
NOVEMBER 10, 1986
EXTRACTION DATE Mid TIME: ........................................................./ 5
RECORD NATIVE pH .................
WAS pH ADJSTED NO IF YES TO WHAT pH
1 LITER
PLACE SAMPLE INTO AN
(X) SAMPLE VOLUME .............................
APPROPRIATELY SIZED
SEFERATORY FUNNEL (1/2 HEAD SPACE SUGGESTED
.
SURROGATE SPIKE
FOR ADEQUATE MIXING)
. -DEM 121483-02 (lug/ill AND 2u(/al>-
[]
IF pH ADJUSTED
( ) ADJUST WITH, 50% NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN [X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 aL SOLVENT. .
100 aL SAMPLE IS aL SOLVENT) .
SHAKE SAMPLE ONE TIME
[X]
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKES BETWEEN VENTING
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED 80
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 aL
i i
M/ V
D2)3)
30 L 30 aL
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-YELLOW COLOR NOTED. EMULSION' -FORMED UPON SHAKING......................
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
(X) [X] ..
IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT.
[] .
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[X] . . .
. [ ] EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
[X] .
REDUCE EXTRACT VOLUME TO
1 aL BY K-D TECHNIQUE AND OR NITROGEN SOLVENT VOLUME REDUCTION
WS-1838 EXTRACT NO: ...............................
SIMPSON ANALYST:
[X] .
[X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
- DATE/TIME COMPLETED.......................... /.................. 760.28-6264
- ESC JOB NO: ............................................................... HONS 024473
FLOW SHUT VS7S05
FOR ESC EXTRACTION METHOD WSEXOS
#2 NPDES PERMIT
WS-1839
SAMPLE ID: ................................................................................. MRC EXTRACT *...................
DUPLICATE
U-86-11-06-01
................................................................................. LOG NO: ................................. NOVEMBER 10. 1986
EXTRACTION DATE and TIME: ........................................................./
5
RECORD NATIVE pH .................
WAS pH ADJSTED NO IF YES TO WHAT pH
PUCE SAMPLE INTO AN
1 LITER [X) SAMPLE VOLUME ..............................
APPROPRIATELY SIZED
SEPERATORY FUNNEL (1/2 HEAD SPACE SUGGESTED FOR ADEQUATE NIXING)
. .
SURROGATE SPIKE -DEM 121483-02 (lug/al AND 2ug/al)
[]
IF pH ADJUSTED
( ) ADJUST WITH.SO* NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN [X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 aL SOLVENT. .
100 aL SAMPLE 15 aL SOLVENT) .
SHAKE SAMPLE ONE TIME
[X]
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKES BETWEEN VENTING
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED SO
.
RECORD AMOUNT METHYLENE CHLORIDE ADDEO
FOR EACH EXTRACTION
60 aL
I 1)........................... I 30 aL
\l /
2)........................
V 30 aL
3)..........................
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
YELLOW COLOR NOTED. EMULSION -FORMED UPON SHAKING....................
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
[X] (X] ..
IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT.
(] .
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[X) . . .
. . .................................................. . . [ ) EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
[X] .
REDUCE EXTRACT VOLUME TO 1 aL BY K-D TECHNIQUE AND OR NITROGEN SOLVENT VOLUME REDUCTION
WS-1839 EXTRACT NO: ...............................
SIMPSON ANALYST: ......................................
[X] .
[XI TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
- DATE/TIME COMPLETED.......................... /.................. 760.28-6264
- ESC JOB NO: ................................................................
MONS 024474
FLOW SHUT VSFSOS
FOR ISC EXTRACTION METHOD WSU05
3 NPDES PERMIT
US-1840
SAMPLE ID: ................................................................................ MRC EXTRACT ....................
LOU SPIKE
U-86-11-06-01
................................................................................ LOG NO: ...................................
NOVEMBER 10. 1986 EXTRACTION DATE nd TIME: ...........................................
5
/
RECORD NATIVE pH.................
UAS pH ADJSTED NO IF YES TO UHAT pH
PLACE SAMPLE INTO AN APPROPRIATELY SIZED
1 LITER (X) SAMPLE VOLUME ...............................
SEPERATORY FUNNEL
.
SURROGATE SPIKE
(1/2 HEAD SPACE SUCGESTED FOR ADEQUATE MIXING)
. (1
-DEM 121683-02 (lug/ml and 2ug/al)-DEM 010385-02 (lOug/al)........................
IF pH ADJUSTED
( > ADJUST WITH,50* NaOH OR H SO 26
ADD METHYLENE CHLORIDE IN [X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 aL SOLVENT. .
100 aL SAMPLE 15 aL SOLVENT) .
SHAKE SAMPLE ONE TIME
[X]
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKIS BETWEEN VENTING
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED 80
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 aL
1 i \i / V
D30 aL
2)30 aL
3)-
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-YELLOW COLOR NOTID. EMULSION FORMED UPON SHAKING....................
REPEAT EXTRACTION PROCEDURE TOO NONE TIMES
[X] [X] ..
IF ACID OR BASE HASHED RECORD TYPE AND AMOUNT.
(] .
ACID/BASE HASH COMENTS
DRY EXTRACT WITH 6 INCH SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[XI . . .
. . .
.M
.................................................. EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
[X] .
REDUCE EXTRACT VOLUME TO
1 aL BY K-D TECHNIQUE AND
OR NITROGEN SOLVENT VOLUME
REDUCTION
WS-1840
EXTRACT NO: ............................... SIMPSON
ANALYST:
[X]
[X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
- DATE/TIME COMPLETED.......................... /--............. 760.28-6266
- ESC JOB NO: ...............................................................
HONS 024475
FLOW SHEET WSFSOS
FOE ESC EXTRACTION METHOD VSEX05
4 NPDES PERMIT
ws-mi
SAMPLE ID:
MRC EXTRACT ......................
HIGH SPIKE
U-86-U-06-01
LOC NO: ...................................
NOVEMBER 10, 1986
EXTRACTION DATE and TIME:
3
RECORD NATIVE pH................... WAS pH ADJSTED NO IF YES TO UHAT pH
1 LITER
PLACE SAMPLE INTO AH
[X] SAMPLE VOLUME ...............................
APPROPRIATELY SIZED
SEFERATORY FUNNEL
SURROGATE SPIKE
(1/2 HEAD SPACE SUGGESTED
FOR ADEQUATE MIXING)
-DEM 12U83-02 (lug/al AND 2ug/al) -
! ] -DEM 010385-02 (lOOug/al)......................
IF pH ADJUSTED
( ) ADJUST WITH,50* NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN [XI THE APPROPRIATE AMOUNT (1 L SAMPLE 30 aL SOLVENT, 100 aL SAMPLE IS aL SOLVENT)
SHAKE SAMPLE ONE TIME
[X]
AMD VERT THROUGH STOPCOCK
REPEAT DOUBLING THE NUMBER
OF SHAKES BETWEEN VENTING
SAMPLES UNTIL THE NUMBER OF
SHAKES EXCEED SO
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 aL
D30 aL
\l /
V
2>30 aL
3>-
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-YELLOW COLOR NOTED. EMULSIONFORMED UPON SHAKING......................
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
IF ACID OR BASE HASHED RECORD TYPE AND AMOUNT.
[X] [X]
U
'
ACID/BASE WASH COMENTS
DRY EXTRACT WITH A INCH SODIUM SULFATE COLUMN
(COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[X]
! EXTRACT DRYINC NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
[X] .
REDUCE EXTRACT VOLUME TO
[X!
1 aL BY K-D TECHNIQUE AND
OR NITROGEN SOLVENT VOLUME
REDUCTION
WS-1841
[X) TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
EXTRACT NO: ...................................... DATE/TIME COMPLETED.......................... /........................
SIMPSON
760.28-6264
ANALYST: ............................................. ESC JOB NO: .....................................
HONS 024476
FLOS SHEET WSFS03
FOE ESC EXTXACTIOlf METHOD VSEX03
DEIONIZED WATER
WS-1842
sample id: ................................................................................. mrc extract *...................
TRIP BLANK
U-86-11-06-01
................................................................................ LOC NO: .................................
NOVEMBER 10, 1986
EXTRACTION DATE And TIME: 5
................................/..................................
RECORD NATIVE pH...................... WAS pH ADJSTED NO IF YES TO WHAT pH..............
1 LITER
PLACE SAMPLE INTO AN
[X] SAMPLE VOLUME ...........................................
APPROPRIATELY SIZED
.
SEPERATORY FUNNEL
.
SURROGATE SPIKE
(1/2 HEAD SPACE SUCCESTED
FOR ADEQUATE MIXIKC)
-DEM 121483-02 (lug/al AND 2ug/al)-
IF pH ADJUSTED
( ) ADJUST WITH,30* NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN (X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 mL SOLVENT. .
100 aL SAMPLE 13 aL SOLVENT) .
SHAKE SAMPLE ONE TIME
(X)
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBLING THE NUMBER .
OF SHAKES BETWEEN VENTINC
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED 80
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 aL
1 i \i / V
l)2)3)--
30 aL 30 aL
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-CLEAR COLOR NOTED. YELLOW PLASTIC FROM CAP-TAPE IN SAMPLE......................
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
[X] [X] ..
IT ACID OR BASE WASHED RECORD TYPE AMD AMOUNT.
[] .
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH SODIUM SULFATE COLUMN
(COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[X] .
. .
. .
. . []
-................................................ EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
[X] .
REDUCE EXTRACT VOLUME TO
1 aL BY K-D TECHNIQUE AND
OR NITROGEN SOLVENT VOLUME
REDUCTION
US-1842
EXTRACT NO: ............................... SIMPSON
ANALYST: ......................................
[X] .
[X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS 11/17/86
- DATE/TIME COMPLETED.......................... /................. 760.28-6264
- ESC JOB NO: ...............................................................
HONS 024477
FLOW SHUT WSFSOS
FOH ESC EXTEACTION METHOD VSEX05
B & J WATER
US-184}
SAMPLE ID: ................................................................................ METHOD BLANK
MRC EXTRACT #.................
LOG NO:
NOVEMBER 10. 1986 EXTRACTION OATE and TIME: ...........................................
5
RECORD NATIVE pH .................
WAS pH ADJSTED NO IF YES TO WHAT pH
1 LITER
PLACE SAMPLE INTO AN
[X] SAMPLE VOLUME.............................
APPROPRIATELY SIZED SEPERATORY FUNNEL (1/2 HEAD SPACE SUGGESTED
.
SURROGATE SPIKE
FOR ADEQUATE MIXING)
. -DEM 121483-02 (lug/al AND 2ug/ml)-
[ 1 ................................................................................
IF pH ADJUSTED
( ) ADJUST WITH.50% NaOH OR H SO 24
ADD METHYLENE CHLORIDE IN [X]
THE APPROPRIATE AMOUNT
.
(1 L SAMPLE 30 aL SOLVENT. .
100 aL SAMPLE IS aL SOLVENT) .
SHAKE SAMPLE ONE TIME
[X)
AND VENT THROUGH STOPCOCK
.
REPEAT DOUBUNC THE NUMBER .
OF SHAKES BETWEEN VENTINC
.
SAMPLES UNTIL THE NUMBER OF .
SHAKES EXCEED 80
.
RECORD AMOUNT METHYLENE CHLORIDE ADDED
FOR EACH EXTRACTION
60 aL
I 1).......................... I 30 aL
\l /
2)........................
V 30 aL
3)..........................
OBSERVATIONS
ALLOW PHASES TO SEPARATE
[X]
-LICHT YELLOW COLOR NOTED.
REPEAT EXTRACTION PROCEDURE TWO MORE TIMES
IF ACID OR BASE WASHED RECORD TYPE AND AMOUNT.
[XJ [X] ..
(] .
ACID/BASE WASH COMENTS
DRY EXTRACT WITH 4 INCH
SODIUM SULFATE COLUMN (COLUMN PRERINSED WITH 30 aL METHYLENE CHLORIDE)
[X]
. . .
.
. .................................................. . . ( 1 EXTRACT DRYING NOT REQUIRED
RINSE SODIUM SULFATE COLUMN WITH 2 X 30 aL
{XI . ..
REDUCE EXTRACT VOLUME TO
(X] .
1 aL BY K-D TECHNIQUE AND
.
OR NITROGEN SOLVENT VOLUME .
REDUCTION
[X] TRANSFER EXTRACT INTO VIAL FOR ANALYSIS
WS-1843
11/17/86
EXTRACT NO: ...................................... DATE/TIME COMPLETED.........................../.................
SIMPSON
760.28-6264
ANALYST: ............................................. ESC JOB NO: ................................................................
HONS
024478
Tho following p*g* show calculation* or row doc* docuaantation of roportad raaulta.
024*^9 HONS
HONS 024480
AMPLITUDE/1000 (Enlargad x 29.0)
m.L
87.94L
jff I
8i.aaL
18.14.
118.78L
A.
B.a_____ i_____ 1------- ---1. . j--------- 1-------- --------- 1-------- --------- 1-------- --------- 1-------- --------- 1_____ .
is.as ia.87 ia.7s aa.aa 2a.sa 24.37 8a.as aa.u RT In ainutaa
SAMPLE: P1B36 Nath: PC8SSM
INJECTED AT 20: OS: 17 ON MOV 11. 1966
Raw: 6R119
Proc: BP119
I
M.aa
HONS 02*481
Ths following pagas show ehaln-of-custody Information for this projaet. HONS 0a4482
Tin* Scaup - <861022.1307> ESC Ch*ln-of-CuAtody Fora
Monsanto Coapany/Envlronaental Sclancaa Center
600 N. Lindbergh Bird.
MO.St. Louis.
63X67
(314) 694-1464
ESC Project Nunber: ESC Project Naae:
PCft AaJAct'Vj^ - ylcGoiT/w
ESC Projtcc
10Saaple
Dcrlptlon
fttaark*
SAMP^M " > /jfioei crruMeir
OAI tiled. temAe&.rc
cot
SaaaM *<?ACV WAlAff
owe uml C*4S / rt
UC>Q|IflL
SaaAPi.* AS >JP0*i ffui*xr
0UC U TgMm fanpn,rte
AJeMeias
%JUPi. * <4 A/Pm gFFUjeur
<ve unM_
Bunhurt
n/UcrAKoCxtSL.
dfrauttett
0*i CiTVL.
DU)afM7E1iLMlTcao^
i4MulT M'S
tUcc UJATMiC
<5ajC LtTVL ________ ___________________
A%.<A<*XTh -_1 __
Relinquished by
Transport Carrlar
Received by
(Signature) Data/Tina (l.e. Air Bill No., ace.) (Signature) Daca/Tlaa
S\3ot
a *2 2 */azSlSlTim^
J.'tSfm. //"d'fd y AtLfU^yi
/
BCHA1N:MH:22
MOWS 024483
Tho following pagas doacrlbo Analytical Raquait Information ganaratad for thli projact.
HONS 024484
XlM Scaup - <861204.0840>
MONSANTO COMPANY/ENVXRONXENTAL SCIENCES CENTER
ANALYSIS REQUEST
DATE: NOVEMBER 6, 1986
LOG NO: U-86-11-06-01
REQUESTER: AUGUSTA
PROJECT NO: 760.28-6264
LOGIN NOTEBOOK PAGE: 46
REPORT RESULTS TO: FILES/MEES, SHERMAN, hughes, McKenzie, SIMPSON ANALYSIS REQUESTS SENT TO: FILES, NEES. SHERMAN, HUGHES, HcKENZIE
SAMPLE PICKUP BY: SIMPSON
SAMPLE LOCATION: U414
SAMPLE DESCRIPTION FOR 2 SAMPLES
SAMPLE IDENTIFICATION
NUMBER OF BOTTLES
ESC NUKBER(S)
NPDES EFFLUENT SAMPLE *i
1X1 LITER
PCB-1838
NPDES EFFLUENT SAMPLE *2 NPDES EFFLUENT SAMPLE *3
I X I LITER 1X1 LITER
PCS-1839 PCB-1840
NPDES EFFLUENT SAMPLE *4
1X1 LITER
PCS-1841
DEIONIZED WATER
1X1 LITER
PCB-1642
WELL WATER
1X1 LITER
PCB-1837
BURDICK AND JACKSON HPLC WATER
FOB-1843
NOTE- NPDES SAMPLES *1, *2, *3. AND *4 ARE ALL THE SAME SAMPLE AND WERE SENT FOR QUALITY CONTROL PURPOSES.
RECORDED BY : SIMPSON
REQUIRED ANALYSES: PCS
EXTRACTION LOGBOOK NOTEBOOK PAGE: 158619
ANALYTICAL TECHNIQUES: TECHNIQUE (EN)
DATE COMPLETED
ESC STANDARD ANALYSIS METHOD
INSTRUMENT LOGBOOK PAGE
x GC/EC (30)
11-14-86
ECAN02
157283
FINAL REPORT NOTEBOOK PACE: 3440418 OTHER NOTEBOOK PACES: 3,434,438
HONS 024485
QUALITATIVE: X
SEMIQUANTITATIVE:
QUANTITATIVE: X
REQUIRED QA/QC: SEE GOOD LABORATORY PRACTICES MANUAL
COMPLETION DATE REQUESTED:
COMMENTS:
SAMPLE DISPOSITION: HOLD FOR 60 DAYS
SAFETY PRECAUTIONS: SEE SAFE LABORATORY PRACTICES MANUAL
ANALYSIS REQUEST FILE NAME: AA264:LI
HONS 024486
The following soctlono deacrlba laportant tatalnology uaad In Quality Aaauranca/Quallty Control. Analyta Extraction and Inatruaantal Analyala. ESC and ESC/UAG Good Laboratory Practical Manuala can ba obtained by con tacting 1111 Maaa (DAE) HETS JAA-1499.
HONS 024487
Quality Assurence/Quallty Control Terminology
This t*cclon describes commonly used terminology and phrases which ara uaad in conjunction with Quality Assurance/Quality Control (QA/QC). This infor mation may ba helpful In understanding soma datails of QA/QC procaduraa which hava baan Incorporated in ehe prasanc raporc. Tha following two sac* tlons also give useful Information concerning terminology used in analyta extraction and Instrumental analysis of samples and sample extracts.
Quality Assuranca/Quallty Control - Terminology used to describe activities which ara designed to produce analytical results of known quality. In an effort to minimise costs of environmental analyses, specific QA/QC elements have been incorporated into ESC/UAC extraction and analysis steps which should not unduely burden analytical studies with large development and method validation costs. This approach has been taken so that sets of samples can be analysed for various analytes without extensively validating methods over wide concen tration ranges and without using methods which are designed for only one matrix.
One price which one pays for this approach is that analytical pre cision and accuracy are sacrificed, somewhat. However, in many cases, when clearly defined regulatory limits have been set, confirming that ehe analyte is present at levels well below or well above tha limit dees not need the type of accuracy that is required when the regulated analyte concentration is in the vicinity of the regulatory limit. In these latter cases, more extensive QA/QC proceedures are required chan are included in the present study.
Precision - Terminology used to evaluate the reproducibility of a certain determination. Parameters which affect analysis precision range from sample acquisition, to sample storage, to sample extraction, and finally to sample extract analysis, normally, the major factor which affects the precision of the analysis is the sample extraction stop. This step normally results in sample analysis precision on the order of or 30%.
The precision of a result can be determined in a number of ways.
Replieata analyses of ehe seme sample, followed by the calculation
of a pareant relative standard davlatlon for ehae determination Is
Che most popular maehod of assasslng precision. However, this cal
culation should not be made when there are lees chan ehrea replieaee
points from which to calculate tha paresne relaeive standard devia
tion. In addition, replicaea extractions and instrumental enalysee
must ba performed. Therefore obtaining percent relative standard
davlatlon data can ba vary expansive and is not normally obtained un
its* large studies are being conducted. A second aothod of essossing
precision Is with the use of duplicate snelyses. The present report
Includes results of at least one sample which was analysed In dupli
cate . NOTE! I It Is tha responsibility of tha analysis requestor to
rvisw these data and draw his own conclusions concerning tha preci
sion of tha determination, and, wore Importantly. If the precision jf
eh* determination meets his needs.
-
(continued)
HONS 024488
Pag* 2, Quality Aasurance/Quality Control Terminology
Accuracy - Terminology used to daearmlna tha correctness" of cha data. Tha accuracy of oat steps In tha analysis of saaples Is typically on tha ordar of 10%. However, whan analyte concentrations in cha sample extracts approach cha laval of dacactlon of a datarmlnacion, accuracy as wall as praclslon can approach 100% or greater. Tha accuracy of a determination of an analyte which is present at concentrations which are auch greater than tha Instruaencal level of detection Is aost strongly affected by tha hoaogenlety of cha saapla aacrlx and cha praclslon of cha extraction step, which results In typical accuracies in environmental analyses to be on the ordar of 30%. Normally, tha accuracy of standard solutions which are used to callbrata analytical Instrumentation is wall below this amount, and therefore la normally not an Important factor in producing inaccurate data. From time to time, analyte responses of standard solutions from different sources will be compared to standard solutions used for instrument calibration. This information Is normally included in the section entitled "QA/QC Results'1.
The accuracy of a result can be estimated In a number of ways. The
current study usee surrogate standard recovery and native analyte
recovery Information to aid in assessing the accuracy of a result.
This recovery information, normally reported as percent recovery,
gives you information concerning the percent of surrogate standards
and native analytes which were recovered after adding to your sMple
matrix and performing the various extractions, clean-ups. end instru
mental analyses associated with the determination. The use of sur
rogates also assumes that the spiked surrogates are bound In the
matrix in the same way as the analytes of Interest. Surrogate stan
dards are added to every sample while native analytes are added
to only 10% of each set of samples. Therefore surrogate standard
recovery data could be used to correct the reported results of an
analyte concentration. If the user of the data feel such corrections
are warranted. HOTltt Ho data ronorted in this scurfy
correction for uwati
d recovery. It ta eha raanonalhlllcv
of tha Parson remiaatina the analvi to annlv appropriate recovery
enfMeelflM. If ha/aha feels that much corrections an wrvawrad
lias - Terminology used to describe how the eccurecy of a determination may be affected. A low bias means that values below the correct value are normally measured. A high bias means that values above the correct value are normally measured. The instrumental analysis step of extract analysis normally does not contribute slgnlflcanely to analysis bias. Host bias In environmental analysis is intro duced in Che sample extraction step. A low bias is Introduced
when the sample is not completely extracted and the extract does not contain 100% of the analyte. A high bias is introduced when the final volume of the extract is less chan the correct volume.
Surrogate Standards (SS), which are discussed in the next section, can be used to determine the amount of bias which is incorporated in Che reported result. SQTEiJ No data reported in ehls report Includes anv correction for this bias. le is the responsibility at tha person reaumaelna the analyses to apply anoronriata bias corrections. If ha/iha faals that such corracclons are warranted.
(continued)
HONS 024489
Page 3, Quality Assurance/Qualiey Control Terminology
UtiI of Decoction (LOD) - Terminology used to indicate whet analyte concentretlon will product a signal-to-noise ratio of 10. For tha present report, this valua Is not axpariaantally determined. Normally, a Limit of Quantitation la usad to datarvina tha ehraahold concantra don abova which an analyca can ba dattctad.
Limit of Quanticatlon (LOQ) - Terminology usad to indicate tha lovaat analyca concentration which can reliably ba quantified. Tha precision of tha determination of the analyte concentration at the LOQ is normally on tha order of 100%. Tha LOQ la normally determined experimentally by adding a known amount of analyte to the sample matrix and measuring tha percent recovery at the LOQ. In soma cases, whan there Is insufficient sample quantity, or for convenience, an LOQ will be determined using other methods. These methods should be clearly described in this report.
Further Information
The general area of Quality Assurance/Quality Control, along with much of the terminology described above, la very complex. The following references may provide further Information which may be useful in understanding the validity of the results reported in this study.
ggffl aeeitdexd Preetiee P4210-S3 entitled "Intreleboretory Quality Control Procedures and a Discussion on Reporting Low-Level Data".
A8TM CeAsi-d PractlCM D2777-77 entitled 'Determination of Prod,ton and Bias of Methods of Committee D-L9 on Water".
An artlela " Aneiwetcal Chemistry. authorad by 29 wall-known environmental aclanclaea. This artlela was fundad by a (rant froa tha Environmental Protscclon Agsney and acknowledges 24 additional selantlsta In Industry and government who wars lnwolvad In Che rawlaw of cho artlelo. lea citation la: 'Principles of Environmental Analysis*. L. H. Kslch, at. al.. Anal. Chan. 1983, 55, 2210 - 221S.
an era Part Hi ancltlsd 'Guldalinaa Establishing Tsat Procedural for cha Analysis of Pollutants Under tha Clsan Vatar Act; Final Aula and Inearln Final Aula and Proposed Aula*. This docuasnt lneludas daealla of EPA'a 600-tarlea analysis aschoda. A currant copy of those nethods can ba found In cho October 26, 19(4 Fadaral Aaglscar.
QAQCTE:MH
HONS 024490
Analyte Extraction Terminology
This faction describes commonly used terminology and phrases which are used in conjunction with analyte extraction. This information aay be helpful in understanding some details of how analytes In your samples were isolated for instrumental analysis. Instrumental Analysis Terminologies are given in the following section of this report.
Sample - Terminology used to reference the material which you submit for analysis. Samples may be solid, liquid, and in some cases, gases. In general, when a sample Is received for analysis, it is logged into ehe ESC sample login book and proper chain*of-custody documents ere maintained in the event this information aay be required for litigation purposes.
Analyte - Terminology used to reference specific compounds or formulations of compounds. When an analysis is requested for a certain analyte within a certain sample matrix, normally some type of extraction process Is required.
Extraction - This terminology refers to the step which Isolates the analyte of interest into an appropriate solvent. Extraction is required for several reasons. In many cases, the concentration of the analyte is below the level of detection of the instrument which will be used for analysis. Therefore, extraction Involves- re* moving the analyte of Interest from a relatively large volume of sample and placing It into a relatively small volume of sol vent. This places the analyte in the solvent at a concentration which can easily be detected by the analytical instrument.
A second reason that oxtractlon is required, is that the eemple aay not ba approprlata for direct Instrumental analysis of the analyte of Interest. This can ba easily understood for analytss In soils. Vary few analytical instruments allow soils to bo directly Inserted into the instrument. Therefore some type of Isolation step <1. o. extraction) is required In order to piece the analyte in an appropriate matrix for inatruaontal analysis.
Whan the analyte of Interest is present at sufficient concentra tion, and the sample matrix can be directly Inserted into the analytical instrument, the sample, or cho diluted aample, can be directly analysed. However, this case reprasanca a minority of sample analyses which ESC Is ssksd to perform.
(continued)
HONS 024491
Pago 2, Analyte Extraction Terminology
Matrix - Terminology used to reference the aejor components of a sample. In
eat eases, major components are not of direct Interest except as
they affect the types of extraction steps and other isolation
*
procedures which must be used to isolate the analyte from the sample
matrix. For the majority of environmental samples which ESC Is asked
to analyze, the matrix is normally water or soil. However, many
environmental matrices contain relatively high levels of organic
compounds which nay lnterfer with the instrumental analysis of the
analyte of interest. Therefore, depending upon the analyte of
Interest, the required level of detection, and the amounts and types
of ocher organic materials which may lnterfer with the instrumental
analysis, extraction methods must be developed which are very
specific for a given sec of samples. In order to deal with almost
a limitless sec of matrices, analytes, extraction methods and instru
mental methods, an organized approach to sample extraction, followed
by instrumental analysis, has been developed at ESC.
Extract - Termlnolocr used to identify the analyte-containing solvent which was obtained from the extraction of a certain matrix.
Extract Clean-up - Terminology used to identify chemical steps which are required in order to reduce Che concentration of organic compounds which may be extracted with the analyte of interest. These coextree ted compounds may be at such high levels and/or produce responses so chat they lnterfer with the Instrumental analysis of the analyte in the extract.
Extractable Compounds - Terminology which refers to the ability of a compound to be isolated from the sample matrix and placed into the extract solvent. When the sample matrix is primarily soil which contains lietle organic matter, most organic compounds are extractable com pounds. However, when the sample matrix is primarily water, only chose compounds which are hydrophobic are extractable compounds.
Standard Extraction Method - Terminology used to reference an organized description of the steps involved in isolating an analyte from a given matrix. These methods are assigned short names which can also be used as computer file names for these methods. The names of specciflc Standard Extraction Mochoda which aro used in this study are llatod in the final report in the section entitled "Details". In addlelon, copiss of those Standard Extraction Methods are shown in a sapareta saetion of this raport. Standard Extraction Methods also Include details of sample clean-up. If required.
Extraction Flow Sheet Terminology used to roforenco a graphic description of a Standard Extraction Method. This flow shoot Is filled out by the analyst in the laboratory and serves as a detailed record of what occurred in the sample extraction step. Flow sheets of In dividual sample extractions may ba included in a section of ehls
report.
(continued)
HONS 024492
Page 3, Analyte Extraction Terminololgy
Surrogate Standard* (SS) - Ona Important alaaanc In cha extraction of an analyte from a aatrlx, la eh* determination of whae parcanc of eha analyte waa actually extracted from cha aacrlx. For aethods which involve liquid/liquid extraction of vaear with an organic solvent, or liquid/solid extraction of soil* with an organic solvent, it la laparaclve ehac dace be obtained which gives ehe analysis requestor information concerning whae percentage of the analyte was isolated in the excrace during the extraction step. Surrogate Standards serve chls iaportant purpose.
The philosophy on the use of Surrogate Standards is as diverse as the analyses who use thea. If coat were no object, analyte recovery information could be obtained by the use of standards addition analy sis aechods. However, since aany samples require extensive labor eo isolate an analyte into an extract, standards addition analysis aothode are coo costly for aost studies. (A standards addition ana lysis requires each sample to bo extracted and analyzed ec least three tines.) Surrogate Standards give the same type of information, with only one analysis bolng required.
A "Surrogate* Standard is a compound which Is chosen to behave exactly as the analyte. It is a surrogate for chat analyto and thus information obtained for this surrogate can be assumed to else apply to the analyte of interest. For the analysis of regulated analytes, it is iaportant that when data is generated chat shows that the analyte is not present, that we can also show chat if the regulated analyte were present in the sample matrix, it would have been detected. This is especially true when complex extraction and instrumental analysis steps are Involved in chls determination. Therefore, when an extraction is performed, a known amount of a Surrogate Standard is added to the sample before any extraction steps take place. Uhen Che extract is Chen analyzed for the analyte of Interest, the amount of the Surrogate Standard is also determined. From this information one can document, for each saaple, what recoveries were measured for chls Surrogate Compound. Froa this, one can describe some level of confidence on the data generated for the analyte of Interest.
A detailed discussion on how Surrogate Standards are chosen is be
yond the scope of this section on Analyte Extraction Terminology.
ESC normally uses two types of Surrogate Standards. The first is
when the surrogate is exactly the same as the analyte of interest,
exeept that the naturally occurring carbon, hydrogen, or halogen
Atoms in the analyte have been replaced with non-narurally occurring
Isotopes. These surrogates can be expected to act exactly as the
native analytes. One good example of chls type of surrogate is the
2.3.7.8-TCDD surrogate in which ell carbon atoms are carbon*13 or all
chlorine atoms are chlorine-37.
(continued)
HONS 024493
Pag* 4, Analyte Extraction Terminology
Tho socond type of Surrogata Standard la ona which doaa not haw* cha same chaalcal structure aa th* analyta of ineeresc, but la known, or assumed to act chemically identical to tha analyta of intaraat during tha extraction and clean-up atapa. Examples of chla type of surrogataa are deuteratad compounds which aay be added to a aatrix in which any chroaatographabla aaterlal* are to b* identified. Thia approach can only b* applied to GC/MS analyaaa, einee cha aurrogataa can be differentiated from cha native coapounda froa chair different aaaa apactra. Since it la not known before aaapla extrac tion and extract analyala what analytea aay be present, aurrogataa auat be chosen thae could not possibly be present in the saaple. In addition, since only liquid/liquid or liquid/solid extraction would b* involved, with no clean-up (since clean-up would teaova coapounda in which tha requester la interested) any hydrophobic deuteratad coepound could serve as a surrogate. Normally, pheool-dS, 2-CL-phenol-dA, CL2-benzene-dA, pyrene-dlO and chrysene-dl2 are used as Surrogate Standards for the analysis of a vide variety of hydro phobic aaterlala in environmental saaplee.
A sub-set of this second type of Surrogate Standards are the surrogates which are used in the capillary GC/EC analysis of Aroclor formulations. Since aass spectromecrlc detection is not used, surrogates which contain unique isotopes cannot be dis tinguished from their native counterparts. Therefore, ocher com pounds are used as Surrogate Standards since they have been ob served to act exactly as the polychlorinated biphenyls (PCBs) in the Aroclor formulations. Any halogenated compound can be used which acts exactly as PCBs in th* extraction and clean-up step. ESC normally uses CLS-benxene and 2,4,6-CL3-biphenyl for this pur pose.
Native Analytes - Terminology which references the analytes of interest which contain naturally-occurring isotopes of carbon, hydrogen, halogens, etc.
Native Spike - Terminology which references the Addition of known amount of native analytea to tha sampla matrix. Normally, at least one sample will be spiked with th* native analyte at tha reported level of de tection (low native spike) end at 10 time* the level of decoction (high native spike). Recoveries of the native analytea provide fur ther documentation on th# quality of tha analyses performed. For semple seta which contain mors than 10 samplas, cho frequency of low and high native spikes la 10% of cho number of samplos. (continued)
HONS 024494
Pago 5, Analyta Extraction Terminology
Method Blank Terminology which refers Co a sample which Is known Co concain nona of chs analytes of Inearasc. For vaear analysaa, chi 1* nor* aally Burdick and Jackson Brand Water, da-tonizad, or dlscillad wacar. For soil, ic aay ba soil which has baan previously analyzed and known co concain nona of cha analyeas of inearasc. All axcrac* don scaps, using randomly salaecad glatsvara, solventj. and all surrogaea spiking solutions muse ba usad. This provides docuaancation ehae cha analyeas of inearasc vara noc lnadvercandy praaanc in axtracclon glassware and solvancs usad in cha analysis. A ainiaua of ona aachod blank ausc ba ganaracad with aach sac of samples. For saapla saes concalnlng aora chan 10 saaplaa. aachod blanks ara ganar acad ac a frequency of 10% of cha nuaber of saaplaa.
Duplicate Analyses - Terminology usad to indicate cha duplicate axcracclon and duplicate extract analysis of a saapla. This provides docuaenclon on cha precision of an analysis. Normally cha precision of environ mental analysaa of homogeneous samplos la on cha order of 30%. A ainiaua of ona duplicate analysis la requirsd for aach saapla sac. For saapla sees containing aora chan 10 saaplaa, duplicate analysaa ara gaoaratad at a frequency of 10% of eho nuaber of aaaplaa.
Further Info cion
Tho general area of Analyte Bxcraccion, along with auch of cha terminology described above, la vary coaplex. The following references aay provide further information which may bo usoful In understanding axtracclon funda mentals and terminology.
40 CTI Part 13% entitled "Culdellnes Establishing Teat Procedures for the Analysis of Pollutants Under tho Cloan Water Act; Final Rule and Interim Final Rula and Proposed Rule". This docuaanc Includes da calls of t?A's 600-series analysis methods. A currant copy of chess methods can ba found in the October 26, 196* Federal Raglacar.
Itittat of gorfc for -
Laboratory Frami which 1, umd In
conjunction with EPA'a Superfund Site studies. A currant copy aay ba obtained
by contacting:
Joan F. Fisk, Project Officer Analytical Supporc Branch Hazardous Response Supporc Division
USEPA Washington, D. C. 20460
ANEXTE;MH
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Instrumental Analysis Terminology
This sscclon describes coMonly ussd terminology and phrasss which ara used in conjunction with extract analysis. This Information say ba helpful in understanding some details of how instrumental analyses of sample extracts were performed. The previous section of this report describes terminology associated with analyte extraction.
Sample Extract - Terminology used eo describe the solvent containing ehe analyte of Interest which is obtained from some type of sample extraction step. Detailed information on how this extract is pre pared can be found in the Standard Extraction Methods and flow sheete associated with the methods. Summerlee of these method# which were used for this project can ba found In a separate section of this report.
Internal Standard (IS) - Terminology used to reference e compound which is added to the eemple extract and standard solutions of the enalytee of interest (Mediately before instrumental analysis. The purpose of the internal standard Is to provlds data whleh can be used to correct for verletlone In Injectod volumes of extract end standard solutions whleh may occur during instrumental analysis. The internal standard muse not bo prossne in the sample extract. Typical Internal standards used in mass spectromacric analyses ara benzene-d6, naphehalene-dS, anthracene-dlO end chrysene-dl2. These dauearacad compounds produce unique mass spectra and ara not prssent In naturally*occurring samples. A commonly used internal standard for CC/EC analysis is hexsehlorobenzene.
Internal Standard Quantitation Hotbed - Terminology which refers to e method of daea analysis. This msthod requires that a known amount of an lneemal standard be added to the temple extract prior to instru mental analysis. Responses of all analytes ere calculated relative to ehe internal standard using the following relationship:
(Analyte Area) RR - Relative Response - ..............................................................
(Internal Standard Area)
If different volumes of the sample extracts end standard solutions are injected, these differences are reflected by differences in the internal standard area. In addition, if instrument sensitivity changes, these changes are also reflected in changes In the Inter nal standard area. The calculation of the relative response cor rects for those types of fluxuaclona.
In order to determine the analyte concentratlon-Reletlve Response relationship, analyte Relative Response Factors srs calculated using the following relationship for data obtained from the analysis of standard solutions:
(continued)
MOMS 024496
Pap 2, Instrumental Analysis Terminology
(Intamal Standard
(Analyta Araa) Concentration)
RRF - Ralatlva Response Factor - ..................................................................................
(Internal Standard (Analyta
Araa)
Concentration)
When Identical amounts of the internal standard are added to both extracts and standard solutions, the Internal standard concentration tern in the above equation can be eliminated. Uhan this Is done and Relative Response Is substituted for the ratio of analyte area to internal standard area, ehe RRF equation becomes:
RRF - RR/(Analyte Concentration)
Analyte concentrations in the extracts are calculated from the folloving equation:
Analyte extract Concentration - RR/RRF
In order to obtain the concentration of the analyte In the sample, the following equation is used:
(Analyte Extract Concentration ) (Extract Volume) Analyte Sample Concentration - ...........................................................................
(Amount of Sample Extracted)
The area terms in the above equations nay be total Ion areas, FID peak areas, EC peak areas, or extracted ion areas. The details of how the internal standard quantitation method is applied to specific methods are described in the various Instrumental Standard Analysis Methods.
The following equation shove what calculations should bo made to
correct for analytical bias:
(Analyte Semple Concentration)
Analyte Sample Concentration - ................................................................
(Corrected for Analytical Bias)
(Assumed Analyte Recovery)
The Assiaed Analyte Recovery can be obtained from an average of surrogate recoveries or native analyte recoveries, measured for the ample in question. MOTE!! Mo data reported In this study Include any correction for surrogate standard recovery. It Is the responsi bility of the person requesting the analyses to apply appropriate recovery corrections, If he/she feels that such corrections are
warranted.
External Standard Quantitation Method - Terminology which refers to a method
of data analysis. This method requires that a known amount of the
analyte standard be analysed under the same conditions as the
sample extract. In order to determine ehe analyte concentration-
Analyte response relationship, Response Fseeors are obtained from
the following relationship:
(concinuad)
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Page 3, Instrumental Analysis Terminology
RJ - Response Factor - (Analyte Area)/(Analyte Concentration)
Analyte concentrations In cho extracts are calculated from cho fol lowing equation:
Analyte Extract Concentration - (Analyte Area)/RF
In order co obtain cho concentration of cho analyte In the sample. cho following equation la used:
(Analyte Extract Concentration) (Extract Volume)
Analyte Sample Concentration - ................................................................................ (Amount of Sample Extracted)
The area terma In the above equatlona may be total ion areas, FID peak areas, EC peak areas, or extracted Ion areas. The details of how the external standard quantitation method Is applied to specific methods are described In the various Instrumental Standard Analysis Methods.
The following equation shows what calculations should be made to correct for analytical bias:
(Analyte Sample Concentration)
Analyte Sample Concentration - ........................................... -......................
(Corrected for Analytical ftlas)
(Assumed Analyte Recovery)
The Assumed Analyte Recovery can be obtained from an average of surrogate recoveries or native analyte recoveries, measured for the ssmpls la question. MOTS! I Mo data reported in this study include any correction for surrogate standard recovery. It Is the responsi bility of the person requesting the analyses to apply appropriate recovery corrections. If he/she feels that such corrections are warranted.
Standard Analysis Methods - Terminology used to reference an organized description of the steps involved In the instrumental analysis of a sample or a sample extract. These methods are assigned short names which can also be used as computer file names for these methods. The names of specific instrumental Standard Analysis Methods which are used In this study are listed in the final repore In the section entitled "Details*. In addition, copies of these Standard Analysis Methods are shown in a separate section of this report. Flow sheets of the Standard Analysis Methods are usually also provided In this section.
Analysis Flow Sheet - Terminology used to reference a graphic description of a Standard Analysis Method. This flew sheee gives specific
information on how extracts and standards are analyzed and what
types of data reduction aeehods are used. (continued)
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page 4, Inatrumental Analysis Tttrni.nology Further Information
Th* ganttral area of Extract Analysla, along with ouch of tha tarnlnology described bov, la vary conplx. References provided In tha pravloua aactlon antltlad 'Analyte Extraction Tarnlnology* nay provide further Information which nay ba uaeful In understanding Instrumental analysis fundamentals and terminology. INANTE:MH
HONS 024499