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Technical Service Report
Report No. 431-81-804-8
To From Date
E. L. SoneS C. B. Herrin April 8, 1981
Conoco Inc.
Research and Development Department Analytical Research Section Ponca City, Oklahoma
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Subject
PURGEABLE PRIORITY POLLUTANTS IN SAMPLE VOA 4236-93-13 LCCP 002 ANALYTICAL NUMBER 16998
Conclusion
The following priority pollutants were found:
1) methylene chloride 2) chlo roform 3) 1,2 dichloroethane 4) benzene 5) toluene 6) ethyl benzene
1 PPb 0.. 9 ppb 3 ppb 244 ppb 60 ppb 2 ppb.
Other components found in "significant" amounts were butane and hexane and butanol and hexanol.
Expcrimental
The sample was run on the Finnigan 0WA-30 GC/MS/DS using a Tekmar L.SC-2 automatic purge-and-trap apparatus. The conditions were;
Sample Concentrator Purge gas Purge time Desorption time Desorption temperature Sample size Internal standards
G.l s Ch r oma t og r a ph Carrier Column Oven temperature program
Mass Spectrometer Scan 40-250 amu in 4 sec 1000 'n'.o'.is collected.
He @ 40 roft/min 12 min
4 min
L80C 5 ml 1,4 dich1orobutane and bromochloromethane.
He @ 20 mH/min 6 ft, 17o SP 1000 on Carbopak B 30C for 4 min initial hold then 8D-/min up to 180C then hold for 120 min.
SAL 0000881
Technical Service Report No. 631-81-804-8 Page 2
The sample was removed from the cold room and allowed to come to room temperature before it was run. Methanolic solutions of the internal standards were injected into a syringe containing 5 mfi- of sample. Cal ibration was accomplished by dosing boiled-and-sparged Milli-Q water with the internal standards and a blend of EPA Consent Decree volatile standards prepared by Radian Corp. and purchased from Regis Chemical Co. This dosed water was run under the same conditions as the sample, and the data obtained were fed into two of the OWA system libraries. The data from the sample were run through the OWA system automatic quan tification program which employed the two libraries in the reverse search mode. The standard blend did not contain any compounds more volatile than methylene chloride, so a manual search was performed for the five gaseous priority pollutants. None were detected.
Discussion of Results
The sample contained non-priority pollutant components which appeared to be in excess of 10 ppb. These components were forward searched using the NBS library and an automatic search routine. Good matches with ref erence spectra were obtained for the compounds listed in the Conclusion section. Xylenes were not detected. The automatic quantification pro gram gave hits for trichloroethylene and tetrnchloroethylene. These may have been false positives. The spectra were not good enough to make a positive identification. The automatic system also gave a false negative for methylene chloride. The methylene chloride value was calculated manua1ly.
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C. B. Herrin Research Group Supervisor Gas Chromatography Group Analytical Research Section
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SAL 0000138127
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GWA REVERSE SEARCH STATUS RhRL'R T
THE I N IERNAI. STANDARD AREA HAS A DIFFERENCE OF. -100 PERCEIMi Of THE LAST STANDARD INTERNAL STANDARD FOUND FOR LIBRARY: l.I OR ARY V1
CONFOUNDS QUANTITATED BY INTERNAL STANDARD USING PARAMETERS IN 5. IJjRARYUi
Rl I T.R I
EXPECTED BES 1
ENTRY HO SCAN
SCAN
FIT
L J BNARY PEAKS UR I TV ENTRY MO FOUND
PEAKS QUANT
SATURA`
r KS
a <
1.
,? J. L
215
993
6/2
14
1 ll
F44
24 7
998
LSI
I3
OSS
258
964
307
i. 0 13
l 1
0 o
NUMBLY OF COMPOUNDS IDENTIFIED
0
DATA PKGCLSSiNC OF G 1.9313 COMPLETED ON 4/06/01 19.33:17
SAL 000088129
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DATA- St. 73 3 3 T 1 03/36/31 IS: 34 00 SAMPLE LCCF002 SUDMiT i/O BY: ELS
ANALYST C13 H
AMOUNT-AREA (HGHTJ R REF. AMNT / iREF AREA HGhT ) x REfP FACT) PESP. FAC. FROM LIBRARY ENTRY
NO NAME 1 HROMDCHLGROMETHANE <INTERNAL STANDARD) 3 CHLORGMETHANE 3 01OHLDRGDIFLUORQMETHANE 4 HR' 300METHANE 3 VINYL CHLORIDE 6 CHLOROETHANE 7 METHYLENE CHLORIDE 3 IP, ICHLOHOFLUORQMETHAME 9 l-DICHLGROETHYLENt:
10 1.1-DICHLOROETHANE :i J TRANS-1,2-DICHLOROETHYLENE 13. CHLOROFORM 13 1, 3--DICHL0RETHANE 14 1,1,I-TRICHLOROETHANE ID CARBON TETRACHLORIDE 16 BF.OMGDICHL.OROMETHANE
NO H/L SCAN
TIME REF
RRT MF.TH
ILL
215 14.31
1 3 . 000 A BB
FT i FOUND
3 ml v FOUND ! FOUND
3 NG I FOUND
ALL FOUND
NO : F OUND
0 NO. FOUND
Npv found
1 ; ACT FOUND
; ; FOUND
; j 247 1 6 40 1 1. 149 A 1?U
i 9- 258 17: 25 41 !. 200 A BB
HL ' POUND
i i i r POUND
LIN FOUND
ARF.A(HGHT) AMOUNT
138019.
100. OOO UC/L
7.1 UT 96. 05
3155. 797
0. 347 UG/L. 2. 264 UG/L.
0. 21 3. .14
",AL 000SB.I30
: ;-jP-l i GAN TAF- CT: I C CNT'GUND ANAL. , 3 1 5
GUAnTITA'" 1 Oh REPORT
FILE: GL?3 i O
f A- 01. ?3J 3. f I Od.'26/Si 15: CM: 00 SAMPLE: L.CCP002 SUBMITTED BY. ELS
ANALYST- CBH
AMOUNT "AREA < HGHT > * REF. AMNT/( REF. AREA ' MGHT ) REBP. FAC. FROM LIBRARY ENTRY
RESP.FACT!
no name
1 1/A~DICHLOROBUTANE <INTERNAL STANDARD) P 1; 2--DICHLQR0PR0PAME
TRANS-1, 3-D! CHLOROPROFEME 4 TR I CIIL GR OETHYLENE 3 BENZENE 6 CIS-1 . 3-DICHLDROPROPENE 7 1. ; , 2-TRICHLOROETHANE 3 DID20M0CHL0R0METHANE 9 BROMOFORM .5 0 1,1,2, 2-TETRACHLOROETHYLENE 11 1 < 1/2/ 2-TETRACHL0R0ETHANE 1.2 TOLUENE A3 CHLOROBENZENE :. * ETHYLBENZENE
NO r-i / e SC AN
T1I ME REF
RR 7 ME:th
1 55 440 29: 42 1 .1. 000 A BB
NOT FOUND
uJ NOT FOUND
A 30 \ ) */0t3o
30.3 21: 4 a 331 22- 2t
!. 0 734 A BE < 0 752 A BB
J NOT FOUND ; M . ` FOUND
met FOUND
5v- r FOUND
1. 0 L i
431 29 06
1 o. 980 A BB
\ ` NC T FOUND
i o 7 3 4/6 32 OB
l -'.I.- i FOUND
i " ,
636 42: 36
O
CD
M
1 1.
A BB
.1 J 44 5 A BB
AREASHGHT) AMOUNT
72ITT
328818
140. coo NG/ML 31 4 1
1008. 2065130.
0. 267 NG / ML. 0. 06 243. 561 NG/ML 54. 65
86. 267352.
5914
o. 025 NG/ML. 0. 0 !
59. 535 NG/ML 13. 36
0
C- ,
306
NG/ML
0. 52
OOOOBBl31 s&t-
i
SAMPLE 0UAN1 I TAT I UN
CJv.'A RE Vi.-.iR SL SEARCH STAUiti RFTiLiR
ir it. i H LLR, ;AL b ' . AR D AREA HAS A DIFFERENCE OF.
PERCENT nr : i in la?
INTERNAL STANDARD FOUND FOR LIBRARY:LIBRARYV?
TANDARD
COMPOUNDS QUANT FI ATKO DY INTERNAL STANDARD USING PARAMETERS IN I.J0RARYV2
R L.P OFT
EXPECTED BEST
ENTRY NCI. SCAN
SCAN
FIT
LIBRARY PEAKS PUR ITY ENTRY NO. FOUND
PEAKS QUANT
SATUhQ' PEAKS
J
438
4 '10
989
476
1
1
1
0
L*.
321
323
993
6
4
1
J
0
5
32=?
331
1000
483
5
1
1
o
10
429
431
921
33
10
1
1
o
A` C->-
47 5
476
996
641
12
1
3
0
14
634
635
997
198
14
1
J
0
number OF COMPOUNDS IDENTIFIED
6
DATA PROCESSING OF GL9313 COMPLETED ON 4/06/81 20 48:27
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