Document YDb8LeXEXBn4BaGnvX1yQ3bgO
Technical Service Report
Report No. 430-81-834-9
Conoco inc.
Research and Development Department Analytical Research Section
Ponca City, Oklahoma
To E.L.Sones
From
C. B. Herrin
Date
Apri1 7, 19 81
Subject
LUIRGEABLE P KIOKITY POLLUTANTS I.N .SAMPLE VOA 4236-93-3 VCM 10 LANALYTICAL NUMBER 16997
Cone 1 us ion
Methylene chloride was resent at less than two ppb. Ethyl benzene and 1,2 dichloroethane were detected but they were below the quantification threshold. No other pr ority pollutants were detected.
Expe riment a1
The sample was run cn t e Finnigan OWA-30 GC/MS/DS using a Tekmar LSC-2 autOmanic purge--and-tra ' apparatus. The conditions were:
Sample Concentrat Purge gas Purge time Desorption tide Desorpt ion ton por \turc Sample size Internal stancard
He @ 40 m2,/min 12 min 4 min 180D C 5 m2. 1,4 dichlorobutane bromochloromethane
and
Gas Chromatograph Carrie r Column Oven temperature
program
He @ 20 m2./min 6 ft, 1% SP 1000 on Carbopak B 30C for 4 min initial hold then 8/min up to 180C then hold for 120 min.
Mass Spectrometer Scan 40-250 anu i a 4 sec 1000 scans col lee ted.
Methanol ic. solutions of t he internal standards were injected into a syringe containing 5 m2, ol: `amp In. The spiked sample was then immediately injected into the purge cell,
Calibration was acc qmplished by d- mug boiled-and-sparged Milli-Q water with the internal sst andards and a blend of EPA Consent Decree volatile standards prepared by Radian Corp. and purchased from Regis Chemical Co. This standard blend was run under the same conditions as the sample, and the data obtained we re fed into two of the 0WA system libraries. The sample was run, and the 0WA system automatic quantification program which employed the two li raries in the reverse search mode was used.
3106 ,0001 VN/C
Tcchnic.il Service Report No. 430-81-839-0 Page 2
Discussion of Result;;
A hit was obtained f o r methylene chloride. The spectrum was observed manually to confirm he identification. The value for methylene chloride on the quantificatio re port is in error due to a software bug. The correct value was ca cul ated to be 1.7 ppb. The standard blend did not contain any compound more volatile than methylene chloride. A manual search was performed for the five gaseous priority pollutants. None was detected.
C"
f-fer/'in
C. B. Herrin Research Group Super va sor Gas Chromatography Ghoup Analytical Research Sect ion
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UNKNOWN SAMPLE QUANT I TAT I Oi
OWA REVERSE SEARCH STATUS REPORT
THE. - INTERNAL STANDARD AREA HA^ A DIFFERENCE OF: -tOO PFRCENT OF THE LAST STAND* INTERNAL STANDARD :OU|MD FOR LIBRARY: LIBRARYV1
COMPOUNDS QUANTITATED BY INTERNAL STANDARD USING PARAMETERS IN LIBRARYV1
REPORT EXPECTED BEST
LIBRARY PEAKS
PEAKS
SATURATED
ENTRY NO. SCAN
SCAN
IT
PURITY ENTRY NO. FDUND
QUANT
PEAKS
1
212
215
?97
657
7 161
164
?96
COMPOUND PASSED RE /ER SET SEARCH BUT WAS BELOW MINIMUM AREA FOR ION QUAN1
13
256
259
779
32
13
I
0
0
NUMBER OF COMPOUNDS IDENT I Fie D
3
DATA PROCESSING OF GL933D :om PLETED ON 4/02/81 14:41:00
VVc 0000131U
N L GAN TARGE T FGflPPUND ANAL >'Si'
IT ATION RE?OH
i Li: :,L9:
a ' , ^ 'o'L. 933D. s To /& i l T C
AMPLE. VCM 1 uRmr TED BY
AN A'. YS
FOUNT--AREA(HGHT & REF. l FAC. FROM ;,.iDHAR v-
YEN v j |r r
nam:: i -1 r- iCHLURDBUT /Nr: INTEKMAI.
1. 2-LUCHLCRur`FOPANE TRANS--; , S-DiCHL ir-;.
TRICHLOROETHYLENE BENZENE
CIS-1,3-DICHLOR PR 1,1,2-TRICHLOROETHANE DIBROMDCHLOROMETHANE BRGMOFQRM i, 1,2, 2-T'ETRACHLOR0E7 HYLENE 1, 1,2, 2-'TETRACHL0R0T|HALE TOLUENE CHLOROBENZENE ETHYL BENZENE
STANDARD)
NO N/E SCAN
r IriE OFF
i 55 442 OF - DO
MOT FOUND
r NOT FOUNT
NOT FOUND
TOT FOUND
TOT FOUND
7 NOT FOUND
T NOT FOUND
V NOT FOUND
10 hot found
: ' MOV FOUND
> T wn r FOUND
nOT FOUND
NOT YjOND
-:RT METH '00 a BD
area<hght) "'5267
amount
y.io
25. 000 IMG/ML *iOO
vvc 00l3li2
. NKNGWN SAMPLE GU ANT I TAT I 0?.
OWA PFA'EPS'.-. SEARCH STATUS REPORT
r\>F: I NT ORNAt... STANDARD AREA MAE A DIFFERENCE GF
-69 PERCENT OF THE LAST STANDA
INTERNAL STANDARD r CJUND FOR LIBRARY: LIBRARYV2
COMPOUNDS QUANTITATED T, iTERNAL STANDARD USING. PARAMETERS IN LIBRARYV2
REPORT
EXPECTED BEST
ENTRY NO. SCAN
SCAN
L. iBRARY purif < entry no
PEAKS
found
PEAKS
quant
SATURATED
peaks
1
433
442
?86
4I7
llio
COMPOUND PASSED RE PR
SEAR CM BUT WAS BELOW MINIMUM AREA FOR ION QUANT
. +
6 u Ll
`,'D _> C
V68
.1 <*
Oo
NUMBER OF COMPOUNDS IDENT1 i, iC,.J
DATA PROCESS INC OF 5L933D COMPLETED ON 4/0*/Sl 3. 2D 29
VVC 000013113