VOLUME 7

APPENDIX G

ANALYTICAL DATA (CONTINUED)

G.4 VOHAPS DATA
lb
APPENDIX G.4

VOHAPS DATA

. ’

CASE NARRATIVE

Analysis of Samples for the Presence of

Volatile Analytes by

High-Resolution Gas Chromatography 1 Low-Resolution Mass Spectrometry

METHOD 8260

Date : August 24, 1998

Client ID : Pacific Environmental Services

TLI Project Number : 46297

This report should only be reproduced in full. Any partial reproduction of this report requires permission from

Triangle Laboratories, Inc.

Triangle Laboratories, Inc.

801 Capitota Drive RO. Box 13485

Durham, NC 27713-4411 Research Triangle Park, NC 27709-3485

919-544-5729 Fax Y 919-544-5491
K

Triangle Laboratories, Inc. August 24,1998

Case Narrative 46297

Objective: Analysis of four VOST tube pairs ( T-V-l-l-A&-B, T-V-1-2-A&-B, T-V-1-3-A&-B,

T-V-1-4-A&-B) for a client specified list of volatile compounds, using Method 8260.

Method:

Eight VOST tube pairs were received at Triangle Laboratories, Inc. on July 25, 1998 on ice at

6°C in good condition. The samples were stored in a refrigerator at 4°C prior to ‘analysis. The

VOST tube sample pairs were analyzed according to the guidelines of Methods 8260 and 5040.

EPer client request, the compounds 1,3-butadiene, vinyl bromide, methyl-t-butylether (MTBE), nhexane, 1,2-epoxybutane, iso-octane, and ethyl acrylate were additional target compounds. A one

point calibration was analyzed for these additional compounds and the resulting response factor

used for quantitationz The internal standards and surrogate standards were added in the amount

of 0.25 micrograms (up) immediately prior to analysis by GUMS. The internal standards are

pentafluorobenzene, 1,4-difluorobenzene, and chlorobenzene-ds and 1,4-dichlorobenzene-&. The

surrogate standards reported are dibromofluoromethane, toluene-ds, and 4-bromofluorobenzene.

The results reported relate only to the items tested.

The GClMS analysis conditions are listed below:

Purge and trap: Tekmar LSC-2000

Purge: 11 min.

Desorb Temperature: 250 c

Desorb Time: 4 min.

GC Conditions:

Column: 30 m x 53 mm x 0.3~ J&W DB624

0 C hold .5 min. 10 C/mm t o 4X, 6 C/mm to 9OC, hold 1.5 min.

50 C/mm to 200C.

MS Conditions:

Instrument:

Scan:

Interface:

VG-TRIO-1 Lab Base data system

35-350 amu at .6s/scan

Jet Separator, 200 C

Report:

Enclosed with the case narrative are copies of the sample identification index, the project

summary sheets, client paperwork, sample log-in sheets, and log book pages. A sample

identification index summarizes the client sample name, TLI sample number, and analytical file

name for each sample and blank. The project summary lists the amounts for detected analytes in

gray. The estimated detection limits will be listed in parentheses when the target analytes are not

detected.

The data are reported as quantitation reports, chromatograms. interim reports, and spectra of

detected target. The quantitation report header lists the TLI project number, analysis method,

2 . 2
Triangle Laboratories, Inc.

Case Narrative

August 24,1998

46297

instrument sample tile name, client sample name, client project number, TLI sample number,

calibration tile, date received, and analysis date. The response factors used for all calculations are

from the calibration file listed in the header. All initial and continuing calibration data are located

in the back of the data package. The amount is reported in total ug for the VOST tubes. The

retention time (RT) will be listed for all internal standards and analytes which are detected. If a

target analyte is not detected, it will be flagged with a “U” and a detection limit will be listed.

Estimated detection limits are calculated for all analytes which were not found in the samples by

using an area of 2000. The estimated detection limits reported are the average detection limits

achievable over time on an instrument type. The actual detection limit for a given compound on a

given day may vary from the estimate reported. The quantitation limit for all analytes is half of

the low point of the initial calibration. Below this point the calibration cannot be considered to be

linear. Any amount reported at a level below the quantitation limit will be flagged with a “J” and

should be considered estimated. If any compounds are found at a level above the upper

calibration range, the analyte will be flagged with an “E” and the amounts reported should be

considered estimated. If any target analytes found in the laboratory blanks are detected in the

associated samples, they will be flagged with a “B” on each sample topsheet. All analytes are

quantitated against the internal standard preceding them on the target analyte list. Surrogate

standards are quantitated against the internal standard with the matching internal standard

reference number. For example, toluene-ds has 2 in the IS Ref column and would be quantitated

against the internal standard which has IS2 listed in the flag column. If an internal standard area is

above or below the quality control limits as defined by the continuing calibration, it will be flagged

with “High” or “Low” in the flag column.

Results:

The VOST tube pairs were analyzed ten days outside the fourteen day sampling to analysis

holding time. The VOST tubes were analyzed separately per client request.

The surrogate percent recoveries~‘met all quality con,trol criteria for all sample and blank analyses

with the exception of samplesp-V-1-l-A and T-V-l-2-A.

16.~$ mj/,

&ccL-,c gAnrr go _ / ~0 $

The area for internal standard met quality control criteria for all sample and blank analyses with

the exception of sample T-V-l-3-B. In this sample the area of pentafluorobenzene was high in

comparison to the one point calibration standard.

Sample T-V-l-2-A was analyzed one minute outside the instrument’s twelve hour tune time

cnterla. ‘0 tyke o~ padcfi &E blN~fl c~a 590~~~~~ lu~rib.~)

No data was collected for sample T-V-1-4-A, due to GC oven shutting off and not ramping,

during the acquisition.

The laboratory blanks contained several target analytes at amounts below the quantitation limit.

The target analytes in the laboratory blank should not be considered as truly present in the native

samples unless found at a level at least five times the amount found in the associated blank. In the

event that the amount of a target analyte found in the samples is twenty times the amount found in

the associated blank, the contribution from the blank can be considered negligible.
* Triangle Laboratories, Inc.

Case Narrative

Sample Calculations:

Response Factor (RF) = [area analvte) x (amt IS)

(area IS) x (amt analyte)

Amount (ug) = (area anaivte in samule) x (amt IS1

(area IS) x (avg icaI RF)

August %I,1998

46297

amt IS = amount of internal standard = 0.25 ug

ical = initial calibration

The data in this package has been judged to be valid according to the guidelines of Methods 8260

and 5040 except as noted above. Should you have any questions, please feel free to contact our

Project Scientist, Deb. Smith, at (919) 5445729, ext. 267.

For Triangle Laboratories, Inc.,

Report Preparation: Quality Control:

Valgena Respass

Report Preparation Chemist

v

Penny A. Brock

Report Preparation Chemist

The total number of pages in this data package is 28. 3

4
Triangle Laboratories, Inc.

Sample Identification Index for Project: 46297

T-V-I-l-AT

T-V-I-I-B TC

T-V-1.2-AT

T-V-l-2-B TC

T-V-l-3-A T

T-V-l-3-B TC

T-V-1-4-B TC

VOSTBLK081798

VOSTBLK081898

VOSTBLKO81998

214-l-6A

214-l-6B

214-l-7A

214-l-78

214-l-8A

214-l-88

214-l-9B

VOSTBLKO8179

VOSTBLKO8189

vOSmLKo8199

FX883

FX879

FX895

FX880

H!N713

FX882

FX881

FX878

FX894

HW705
Client ID:

Triangle Laboratories, Inc.

Project Summary for Project 46297

T-V-l-1-A T-V-l-I-B T-V-1-2-A T-V-l-2-B T-V-l-3-A

T T C T T C T

( )-Estimated Detection Limit Page 1

Triangle Laboratories, Inc. Savar v3.7

801 Capitola Drive * Durham, North Carolina 27713 Printed: 18:0456 W24J9.3

I’hone: (919) 5445729 . Fax: (919) 5445491

lo 6
Client ID:

Triangle Laboratories, Inc.

Project Summary for Project 46297

T-V-1-1-A T-V-1-1-B T-V-I-2-A T-V-I-2-B T-V-l-3-A

T TC T TC T
Client ID:

Triangle Laboratories, Inc.

Project summary for Project 46297

T-V-l-3-B T-V-l-4-B VOSTBLKO81 voSTBLKo81 VOSTBLKOSl

T C T C 798 898 998

Filename : FX882 FX881 FX878 FX894 w7O5

TLIId : 214-l-88 214-I-98 VOSTBLK08179 VOSTBLKO8189 VOSTBLKD8199

Matrix : VOST VOST VOST VOST VOST

Units : “g ug “g ug ug

ChlOlWD3h~lW ~~~.~~~~~~~: ~:~~~,~~~~~~~ (0.001) ((j-jjl) ~:~~~~~~~~~~

Vinyl Chloride (0.001) (0.001) (0.001) (0.001) (0.001)

Bromomethane ~,~~~~~~~~~~~,~~~~~~ ~~,~~~~~~~ (0.001) (OsQl) (0.001)

Chloroethane (Osm) (O.all) (0.001) (O.oill) (0.001)

Trichlorofluoromethane (0.001) (0.001) (0.001) (0.001) (0.001)

I,]-Dichloroethene (0.001) (0.001) (0.001) (0.001) (0.001)

Metbylene chloride ~~~~~,~~~~~~~~~~,~~~ ~~~~~~~~~~~ (0.001) @ml) ~~~~:~~~~~~~~~~~

trans-1,2-Dichloroetene (0.001) (0.001) (O.aol) (0.001) (0.001)

l,l-Dichloroethane (0.001) (0.001) (0.001) (0.001) (0.001)

cis-l,Z-Dichloroethene (0.001) (0.001) (0.001) (0.001) (0.001)

Chloroform (0.001) (0.001) (0.001) (Osxll) (0.001)

l,l,l-Trichloroethane (0.001) (0.001) (0.001) (0.001) (0.001)

Iodomethane (0.001) (0.001) (0.001) (0.001) (0.001)

Carbon disuifide ~~~~~~~~ (0.001) (0.001) (0.001) (0.001)

Acetone ~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~~ mm (0.006) (0.004)

Ally1 chloride (0.001) (0.001) (0.001) (0.001) (0.001)

Acrylonitrile (0.016) (0.016) (0.016) (0.021) (0.006)

Vinyl acetate (0.002) (0.002) (0.002) (O.cQ2) (0.001)

2-Butanone (0.004) ww @.cw (0.005) (0.003)

Carbon tetrachloride (0.001) (0.001) (0.001) (0.031) (0.001)

Benzene (0.001) ((jW1) ~~~~~~~~~~~~~~~~~~~ ~~~~~~~~~~~~~~~~~ (0.001)

1,2-Dichloroethane (O.GQl) (0.001) (0.001) (0.001) (0.001)

Trichloroethene (0.001) (0.001) (0.001) (Osm) (0.001)

1,2-Dichloropropane (0.001) (0.001) (O.cQl) (0.001) (OOOl)

Bromodichloromethane (0.001) (0.001) (Osxil) (O.col) (0.001)

cis-1,3-Dichloropropene (0.001) (0.001) (O.GfH) (0.001) (0.001)

Toluene :~~~~~-rl~~~~~~~~~~ ~~L~~~~:ii~~~i~~~~~iiii’“:::“:i -i-8i:~-j,ilri-:iiri~~~~~~~:;..~..~~ lGiE~~~~~Sii~~~iSi:‘i;..-‘:;‘i ~~:,:::ia~~,i:--i,,,~:~~~~~~.~~:~~~~:.:~

,:~~~~~~~~~~~:~~::~~~~:~:~~~~~~~~ ~:~~~~~~~~~~~~~~~:~:~:~~~~~~~~.~~~:~:~:~~~~~~~~~ ~~~:~:~~:~:~:~~~~~~~~~~~:~:~:~~~~~~~~~~~:~~~~~~- -~~~~~~~~~~~~~~~~~~~~m~~~~:~~~~~~~~~~~

trans-1,3-Dichloropropene (0.001) (0.W) (0.001) (0.002) (0.001)

l,l,ZTrichloroethane (0.002) (0.002) (0.001) (0.002) (0.001)

Methyl methacrylate (0.006) (O.@w (0.006) (0.007) (0.002)

4-Methyl-2-pentanone (0.005) (0.005) m-w (0.~) (0.001)

Tetrachloroethene (0.001) (0.001) (0.001) (0.001) (0.001)

Dibromochloromethane (0.001) (0.001) (0.001) (0.001) (0.001)

1,2-Dibromoethane (0.002) (0.001) (0.001) (0.002) (0.001)

Chlorobenzene (0.001) (0.001) (0.001) (0.001) (0.001)

( )-Estimated Detection Limit Page 3

Triangle Laboratories, Inc. savar v3.7

X01 Capitola Drive - Durham, North Carolina 27713 hinted: 18:04% a3,24,98

Phone: (WU) W-5729 * Fax: (919) 5445491

8 8
Client ID:

Triangle Laboratories, Inc.

Project Summary for Project 46297

T-V-l-3-B T-V-l-4-B VOSTBLKOSI Vo!sBLKO81 VOSTBLKO81

TC Tc 798 898 998

Filename : FX882 FX881 FX878 FX894 Hw705

TLIId : 214-l-88 214-l-9B VOSTBLK08179 VGSTBLKO8189 VOSTBLK08199

Matrix : VOST VOST VOST VOST VOST

Units : “g “g ug “g %

Ethylbenzene

m-/p-Xylene

o-Xylem

SlyEXle

Bromoform

2-Hexanone

Cumene

1,1,2,2-Tetrachloroethane

(0.001) (O.cm)

(O.cOl) (0.001)

(0.001) (0.001)

(0.001) (0.001)

(0.003) (0.002)

(0.006) (0.006)

(0.001) (0.001)

(0.003) (0.002)

(0.001)

(0.001)

(0.001)

(0.001)

(0.003)

(0.006)

(O.Oix)

(0.003)

(O.crJl) (0.001)

(oJJJ*) ~~~~~~~~~~

(O.col) (0.001)

(0.001) (0.001)

ww (0.001)

(0.008) (0.002)

(0.001) ~~~~~~~~~~~~~

ww (0.001)

,‘- ( )-Estimated Detection Limit Page 4

Triangle Laboratories, inc. savar v3.7

801 Capitola Drive * Durham, North Carolina 27713 Printed: 18:04:S6 08,*4,9g

I’hww (W) 5445729 . Fax: (919) %&519,
Client ID:

Triangle Laboratories, Inc.

Project Summary for Project 46297

T-V-1-1-A T-V-1-1-B T-V-l-2-A T-V-l-2-B T-V-l-3-A

TC TC T T C T

Filename :

TLIId :

Matrix :

Units :

1,3-Butadiene

Vinyl bromide

MTBE

n-H‘ZXalle

1,2-Epoxybutane

Iso-Octane

Ethyl acrylate

FX883 FX879 FX895 FX880 Hw713

214-l-6A 214-l-68 214-l-7A 214-l-78 214-1-8A

VOST VOST VOST VOST VOST

% ug “g “g ug

(0.001) (0.001) (0.001) (0.001) (0.001)

(0.001) (OSKN) (O.GQl) (0.001) (0.001)

(0.001) (Osnll) (0.001) @ml) ~~~~~~~~

i~.~~~~~~~.~.~.~~~~~~~~~~~ ~~~~~~~~~~~~~~~I”“‘: ~~~,~~~~~~~““:i” ~~~~~~~~~~~~~~ ~~~~~~~~~~ :~ii~.~~l~~~;~~~~: :~~i-.~::~~~.~::::~~~:~~~~ :::::::~ii:~::.i:l:::::i:::~~~:: :.~~:i,:.:.:~~:::~:~.:.::i:....r.~..........~....~

(omo) (0.011) (0.015) (0.010) (0.011)

(0.001) (0.001) (0.001) (0.001) (0.001)

(0.002) (0.003) (0.004) (0.002) (0.001)

Triangle Laboratories, Inc.

( )-Estimated Detection Limit

801 Capitola Drive * Durham, North Carolina 27713

Phone: (911)) 5445729 * Fax: (919) 544-5491

Page 1

Printed: 183439 08/24/98
Client ID:

Triangle Laboratories, Inc.

Project Summary for Project 46297

T-V-l-3-B T-V-l-4-B VOSTBLKO81 VOSTBLKO81 VOSTBLKOBI

T C T C 798 898 998

Filename : FX882 FX881 FX878 FX894 HJv7@5

TLIId : 214-l-88 214-l-9B VOSTBLKO8179 VOSTBLK08189 VOSTBLK08199

Matrix : VOST VOST VOST VOST VOST

Units : “g ug w ug “g

1,3-Butadiene (O.Wl) (0.001) (0.001) (0.001) (0.001)

Vinyl bromide (0.001) (O.cm) (0.001) (O.cQl) (0.001)

MTBE (0.001) (0.001) (O.cm) (0.001) (0.001)

Il-HIZWW ‘~~ii:.BI~~~~~~~~~~ ~~~~~~~~~~~~~~ (0.001) (O,-Jl) ~~~~~.~~~~~

1,2-Epoxybutane (0.011) (0.011) (0.011) (0.020) (0.017)

ISO-OCtVW (0.001) (O.M)l) (0.001) (O.M)l) (0.001)

Ethyl acrylate (0.003) (0.003) (0.002) (0.W (0.001)

1.l ( )-Estimated Detection Limit Page 2

Triangle Laboratories, Inc. savar “3.7

x(11 Capitola Drive * llurhum, North Carolina 27713 Printed: 1834~39 08/24/98

I’hone: (919) S&5729 * Fax: (919) 5445191