MIDWEST RESEARCH INSTITUTE
SURFACE WIPE TEST MONITORING FOR THE TOXICANT ANALYSIS CENTER
TASK 48
FINAL REPORT
August 3, 1983
MRI Project No. 4901-A48
EPA Prime Contract No. 68-01-5915
Prepared for:
U.S. Environmental Protection Agency
Office of Pesticides and Toxic Substances
Field Studies Branch
401 M Street, S.W.
Washington, D.C. 20460
Attn: Dr. Frederick Kutz, Project Officer
Mr. O^n Herjyem, Task Manager
MIDWEST RESEARCH INSTITUTE 425 VOLKER BOULEVARD. KANSAS CITY MISSOURI 64110 • 816753-7600
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SURFACE WIPE TEST MONITORING FOR THE TOXICANT ANALYSIS CENTER
by
Paul H. Cramer
John E. Going
TASK 48
FINAL REPORT
August 3, 1983
KRI Project No. 4901-A48
EPA Prime Contract No. 68-01-5915
U.S. EnvironTTtfll Protection Agency
L4b"T". Poom 2^04 PM-211-A
401 M Street. S.W.
Washington, DC 20460
Prepared for:
U.S. Environmental Protection Agency
Office of Pesticides and Toxic Substances
Field Studies Branch
401 M Street, S.W.
Washington, B.C. 20460
Attn: Dr. Frederick Kutz, Project Officer
Mr. Dan rieggem, Task Manager
MIDWEST RESEARCH INSTITUTE 425 VOLKER BOULEVARD, KANSAS CITY, MISSOURI 64110 • 816 753-7600
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DISCLAINER
This document has been reviewed and approved for publication by the
Office of Toxic Substances, Office of Pesticides and Toxic Substances,
U.S. Environmental Protection Agency. Approval does not signify that the
contents necessarily reflect the views and policies of the Environmental
Protection Agency, nor does the mention of trade names or commercial products
constitute endorsement or recommendation for use.
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PREFACE
This report presents the results obtained from the first and second sam-
plings on MRI Project No. 4901-A, Task 48, “Surface Wipe Test Monitoring for
the Toxjcant Analysis Center,” for the U.S. Environmental Protection Agency
(EPA Prime Contract No. 68-01-5915). Samples were collected and analyzed by
Midwest Research Institute. The MRI task manager was Mr. Paul Cramer; sample
analyses were performed by Ms. Kay Turman, Mr. Jon Onstot, Ms. Carolyn Thornton,
and Dr. Lloyd Petrie. Mr. Cramer prepared this report.
Approved:
James L. Spigarelli, Director
Analytical Chemistry Department
August 3, 1983
MI
INSTITUTE
E. Going
Manager
l] .i
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CONTENTS
Preface . . . . iii
Figures vii
Tables . . . . . . ix
1. Introduction 1
2. Summary 2
3. Sample Collection 4
Surface wipe test procedure . . . . 6
Field quality assurance procedures. 6
4. Analytical Protocol 8
Organics 8
Metals 13
5. Results and Discussion . . . . 15
Organics . . . . 15
Metals 30
Appendices
A. Chromatograms and mass spectra for samples analyzed for
priority pollutants A-i
B. Extracted ion current plots for samples analyzed for
herbicides B-i
C. Extracted ion current plots and mass spectra for samples
analyzed for tetrachlorodibenzodioxin isomers C-i
D. Chromatograms and mass spectra for samples analyzed for
priority pollutants during the second sample period D-1
E. Extracted ion current plots for samples analyzed for
herbicides during the second sampling period E-1
F. Extracted ion current plots for samples analyzed for
tetrachlorodibenzodioxin isomers during the second
sampling period F-i
V
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FIGURES
Number Page
1 Floor plan for building 1105 5
vi i
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TABLES
Number Page
1 Sampling Points at TAC . . . 4
2 Sample Information 9
3 GC/MS Parameters for Priority Pollutant Analyses . . . . . 11
4 GC/MS Parameters for Herbicide Analyses . . . 12
5 CC/MS Parameters for TCDD Analyses 12
6 Sample Analysis Results for Priority Pollutants. . . 16
7 Priority Pollutant Data 17
8 Major Peak Tentative Identification Summary 21
9 Surrogate Compound Recoveries 25
10 Priority Pollutant Compound Recoveries - Hood Spikes . . . . 26
11 Priority Pollutant Compound Recoveries - Method Spikes . . . 28
12 Herbicide Compound Recoveries 30
13 Sample Analysis Results for Metals, pg/rn 2 31
14 Sample Analysis Results for Selected Toxic Metals, pg/rn 2 . . 32
15 Toxic Metal Recoveries 34
16 Metal QA Results - Bench Spikes 35
17 Metal QA Results - Filter Spikes 36
ix
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SECTION 1
INTRODUCTION
Laboratories in the Toxicant Analysis Center (TAC) at Bay St. Louis,
Mississippi, were previously monitored for the presence of hazardous chemi-
cals during the completion of Task 20, “Analysis of Air and Wipe Samples for
Dioxin and Other Highly Toxic Substances.” To further ensure the safety of
Environmental Protection Agency (EPA) employees and other personnel at TAC,
Midwest Research Institute ( IRI) was instructed by EPA to assess the extent
of surface contamination a second time in selected areas in Building 1105 at
TAC. By the use of an industrial hygiene technique known as wipe sampling,
MRI was to collect and analyze samples twice during the 1982 calendar year
for selected hazardous chemicals.
On March 15, 1982, a pre-sampling site survey of EPA labs at TAC was con-
ducted by Dr. Aubry Dupuy and Mr. Milas Blaylock of TAC and Dr. John Going
and Mr. Paul Cramer of HRI. A total of 26 sampling locations were identified
where surface wipe samples would be taken for subsequent extraction and analy-
sis for the presence of EPA semivolatile priority pollutants (PP), selected
herbicides (2,4-D and 2,4,5-T), and tetrachlorodibenzodioxins (TCDD). Tenta-
tive identification of major peaks in the chromatographic runs of the sample
extracts would also be completed by computerized library searches. An addi-
tional three sampling locations were identified for possible surface wiping
and analysis for selected metals.
Samples were collected at TAC by MRI personnel on April 6, 1982, and
again on September 30, 1982, and were subsequently analyzed for the designated
hazardous chemicals. The remainder of this report presents the summary, sam-
ple collection and analysis protocols, and results for the first and second
samplings at TAC during the calendar year 1982.
1
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SECTION 2
SUMMARY
On April 6, 1982, 30 wipe samples were taken from 15 laboratories in
Building 1105. In addition, four field blanks were taken to ensure that any
compounds detected did not result from the sampling methods used. Three field
spikes were also performed to give a measure of compound losses incurred from
transportation and extraction procedures. An identical sampling scheme was
implemented again on September 30, 1982.
Analyses of the extracts obtained from the two sets of 30 field samples
indicated that no toxic organic compounds, with the exception of various
phthalates, were present. The estimated limits of detection for semivolatile
EPA priority pollutants and selected herbicides ranged from 2 to 1,000 pg/rn 2 .
The estimated limit of detection for TCDD isomers was 25 ag/rn 2 .
The average recoveries for five surrogate compounds used in the field
spiking studies to assess compound losses during transportation and sample
workup ranged from 61 to 109% for both sampling periods. Extraction efficien-
cies for 90% of all priority pollutants ranged from 50 to 150%. Compounds
with poor stability or high volatility exhibited poorer recoveries. Hood stir-
face spiking experiments conducted at HRI with priority pollutants and se-
lected herbicides gave average recoveries ranging from 1 to 77%, with the more
volatile compounds showing poorer recoveries.
Tentative identification of nonpriority pollutant contaminants in the
wipe extracts indicated that most of the compounds were associated with the
construction of the materials being wiped. The tentative identifications were
made by computerized library searches of the National Bureau of Standards
(NBS) mass spectra library.
Analysis of five filter Leachates for metals showed some contamination
in the atomic absorption laboratory (Room E-504). An aqueous wipe of an AA
vent funnel (made of metal) showed levels of 17 pg/rn 2 for As, 42 pg/m 2 for
Cd, 47 pg/rn 2 for Hg, and 390 pg/rn 2 for Pb for the first sampling. The second
sampling showed considerably lower levels. A wipe of a nearby benchtop in
the same laboratory also showed detectable levels of Cd and Pb at 18 pg/rn 2
and 55 pg/rn 2 , respectively, for the first sampling. The second sampling
showed CD at 7.3 pg/rn 2 and Pb at 130 pg/rn 2 . In a metals preparation lab (Room
E-503), one hood wipe showed a level of Pb at 18 pg/rn 2 for the first sampling.
The second sampling showed a low level of Cd in one hood (3.6 pg/rn 2 ) and mer-
cury at 74 and 43 pg/rn 2 in each hood. Detection limits for all 28 metals
ranged from 0.8 to 10,000 pg/rn 2 . The higher detection limits were caused
by high background levels of some metals in the filters.
2
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The leaching process for the metals analysis yielded average recoveries
for both samplings between 80 and 110% for the 250 pg/rn 2 level, except Ca.
For the 50 pg/rn 2 levels, average recoveries ranged from 75 to 125%, with the
exception of Ca and Na. Laboratory bench wipes showed lower recoveries. At
the 250 pg/rn 2 level, average recoveries were between 52 and 91%, except for
Al, Ca, Fe, Na, and Zn. The 50-pg/rn 2 level showed average recoveries from 8
to 80% except for Al, Ca, Fe, Na, Mg, P, and Zn; these elements were present
in filters at high and varying amounts and caused high recoveries.
3
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SECTION 3
SAMPLE COLLECTION
Sampling was conducted on April 6 and on September 30, 1982.
the sampling sites by room number, type of wipe, and analytes
Figure 1 presents the pertinent portion of the floor plan for
TABLE 1. SAMPLING POINTS AT TAC
Type and number
of wipes
Field
Field
Room number
Hood
Bench
Refrigerator
Wall
blank
spike
Analytes
E502
2
1
Herbicides
E503
2
Metals
E504
E506
1 a
2 b
1
1
1
1
Metals
PP ’s
E508
2
PP’s
E510
1
1
Herbicides
E514
1
1
1
PP’s
E516
1
PP’s
E520
1
1
PP’s
D418
2
1
1
PP’s
D42O
2
PP’s
D421
1
PP’s
A120
1
TCDD
A122
1
TCDD
A124
3
1
1
1
TCDD
Total wipes
21
3
4
2
4
3
a Wipe of AA vent funnel.
b Includes one glove box wipe.
lists
est.
1105.
Table 1
of inter—
Building
4
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£502 J [ 503
[ 504 I , —
E506 [
E508
[ 510 -
________ 0
I- )
£5 14
[ 516
£520
DTD
418 420
‘ I
0
-ø
0
U
__I_
Figure 1. Floor plan for Building 1105.
;ii
U i
‘D” Corridor
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SURFACE WIPE TEST PROCEDURE
The wipe tests were done in accordance with Chapter VI, Section C.3 of
OSHA’s Industrial Hygiene Field Operations 1anual. The procedure used in ob-
taining a surface wipe sample is given below.
1. A sample jar containing four precleaned filters was removed from the
sample transportation container.
2. The sample jar was labeled with the appropriate sample designation
and the custody sheet completed for that sample.
3. The filters (Whatman No. 42, 7 cm) were moistened with pesticide
grade dichioromethane for organic samples. For metals, the filters
were wetted with deionized water.
4. The wetted filters were removed from the sample jar and placed on
the surface to be wiped with a pair of prerinsed metal tongs. For
metal samples, tongs with tips wrapped in prerinsed Teflon® tape
were used.
5. One quadrant of a 400-cm 2 area was wiped with one filter, the filter
was folded in half with the exposed side in, and it was placed back
in the sample jar.
6. The remaining three quadrants were wiped with the other three filters
and folded over the first filter.
7. The stack of filters was folded in half again and placed, angle first,
into the original sample jar.
8. The sample jar was sealed tightly and replaced in the sample shipping
container containing blue ice.
After completion of all sampling, the samples were returned to MRI’s ana-
lytical laboratories via air freight, where all samples were logged in and
placed in cold storage (4°C) until analysis.
FIELD QUALITY ASSURANCE PROCEDURES
Field quality assurance procedures for organic samples consisted of ob-
taining three field blanks and three field spikes. Filter blanks were gener-
ated in the field by opening the sample jar containing a set of blank filters,
wetting the filters with dichioromethane, and then resealing the sample jar
and treating it as a normal sample. Filter spikes were made in the field dur-
ing the first sampling by spiking blank filters in sample jars with 20 pg each
of the surrogates d 8 -naphthalene, d 12 -chrysene, 13 C 6 -pentachlorophenol, d 6 -
3, 4 ,3 ’, 4t -tetrachlorobiphenyl, and dieldrin. During the second sampling, 20
pg of dg-riaphthalene and 13 C 6 -pentachlorophenol were used, but only 10 pg of
d 12 -chrysene, d 5 -3,4,3’ ,4’-tetrachlorobiphenyl, and dieldrin were used.
6
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Field quality assurance procedures for the wipes taken for metals con-
sisted of obtaining a field blank. The field blank was generated in the field
by opening the sample jar containing a set of blank filters, wetting the fil-
ters with deionized water, and then resealing the sample jar and treating it
as a normal sample.
7
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SECTION 4
ANALYTICAL PROTOCOL
Samples collected at TAC were extracted for analysis within 7 working
days after collection. Table 2 gives the sample ID number, the quality assur-
ance sample ID number, sample type, dates of extraction, and dates of analysis
for each of the samples collected at TAC during both sampling periods.
ORGANI CS
Sample Preparation Procedures
All samples collected for organics were Soxhlet extracted for 4 hr with
300 ml of pesticide grade dichloromethane. The extracts were reduced in vol-
ume by Kuderna-Danish evaporation to approximately 5 ml and further reduced
to a volume of 1 ml by evaporation under a stream of prepurified nitrogen
using a modified micro-Snyder column. Samples for tetrachlorodibenzodioxin
analysis were evaporated to dryness and the residue redissolved in 100 iii of
dichioromethane or hexane. The extracts were then stored in a freezer until
GC/MS analysis.
Extracts to be analyzed for the methyl esters of 2,4-0 and 2,4,5-T were
split into two 1/2-nil samples and half of each sample was subjected to a meth-
ylation procedure. Ethereal diazomethane solution used in the methylation
procedure was made by dissolving 2.3 g of KOH in 2.3 ml of water in a 40-nil
vial with a Teflon®-lined screw cap. The solution was cooled in an ice bath
and 25 ml of diethyl ether was added. Then 1.5 g of N-methyl-N’-nitro-N-
nitrosoguanidine was added in small portions over a period of a few minutes
and the solution was vigorously shaken after each addition. The ether layer
was decanted into another vial and stored in a freezer until use.
Extracts were methylated by adding 1 ml of the ethereal diazomethane,
mixing the resulting solution and allowing it to stand for 30 mm. At the
end of 30 mm, the ether and unused diazomethane was evaporated i.mder a stream
of nitrogen. The methylated extract was adjusted to 0.5 ml and stored in a
freezer until analysis.
Sample Analysis Procedure
Analysis of the filter extracts for priority pollutants was conducted by
full-scan GC/MS. Parameters used in the analyses of samples from both sam-
pling periods are given in Table 3.
8
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TABLE 2. SAMPLE INFORMATION
Sample
identification
numbera
QA
identification Set
numbers Dates of
Set 1 Set 2 Type of wipe extraction
1
Set
2
Dates of
extraction
Dates of
analysis
Dates of
analysis
E502—R11-4901A48 41 48 Refrigerator 4/13/82 4/27/82 10/5/82 1/7/83
E502-Hh1-4901A48 40 52 Hood 4/13/82 4/27/82 10/6/82 1/7/83
E502-H21-4901A48 39 46 Hood 4/13/82 4/27/82 10/6/82 1/7/83
E503-H11—4901A48 18 5 Hood - metals 4/15/82 4/16/82 11/16/82 11/24 182
E503-H21—490 1A48 19 7 Hood - metals 4/15/82 4/16/82 11/16/82 11/24/82
E503—FBK-49011A48 22 23 Field blank - metals 4/15/82 4/16/82 11/16/82 11/24/82
E504-H1 1-4901A48 17 3 Hood - metals 4/15/82 4/16/82 11/16/82 11/24/82
E504-B1 1-4901A48 21 21 Bench - metals 4/15/82 4/16/82 11/16/82 11/24/82
E506-H11-4901A48 38 44 Hood 4/13/82 4/23/82 10/5/82 11/4/82
E506-H21-4901A48 37 42 Hood 4/13/82 4/23/82 10/6/82 11/5/82
E506-R11-4901A48 36 40 Refrigerator 4/13/82 4/22/82 10/6/82 11/4/82
E506-W1l-4901A48 35 38 Wall 4/12/32 4/22/82 10/6/82 11/5/82
E508—H11-4901A48 34 36 Hood 4/12/82 4/22/82 10/5/82 11/4/82
E508-1121-4901A48 33 34 Hood 4/13/82 4/22/82 10/6/82 11/4/82
E510-H1 1 -4901A48 32 32 Hood 4/12/82 4/27/82 10/5/82 1/7/83
E51O-B11-4901A48 10 30 Bench 4/12/82 4/27/82 10/6/82 1/10/83
E514-H11—4901A48 9 28 Hood 4/12/82 4/21/82 10/5/82 11/4/82
E514-FBK-4901A48 20 9 Field blank 4/12/82 4/19/82, 10/5/82 11/9/82,
4/26/82 1/6/83
E514-FSp-4901A48 27 11 Field spike 4/12/82 4/19/82 10/5/82 11/4/82
E516-H1 1-4901A48 8 26 Hood 4/12/82 4/21/82 10/6/82 11/4/82
E520-H11-4901A48 7 24 I [ ood 4/12/82 4/20/82 10/6/82 11/4/82
E520-R11-4901A48 6 22 Refrigerator 4/12/82 4/20/82 10/5/82 11/5/82
D418—H11-4901A48 5 20 Hood 4/13/82 4/20/82 10/6/82 11/5/82
D418-H2 1-4901A48 4 18 Hood 4/13/82 4/20/82 10/6/82 11/9/82
D420-Hh1-4901A48 3 16 Hood 4/13/82 4/20/82 10/5/82 11/5/82
D420-H21-4901A48 2 14 Hood 4/13/82 4/20/82 10/6/82 11/4/82
D420-FBK-4901A48 28 13 Field blank 4/13/82 4/21/82, 10/6/82 11/9/82,
4/27/82 1/6/83
D420-FSp-4901A48 29 15 Field spike 4/12/82 4/21/82 10/6/82 11/5/82
D421-BL1—4901A48 1 12 Bench 4/14/82 4/19/82 10/6/82 11/5/82
A120—Hl1-4901A48 11 10 Hood 4/14/82 4/29/82 10/5/82 12/9/82
(continued)
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TABLE 2 (concluded)
QA
Sample
identification
numbera
identification
numbers
Type of wipe
Set
1
Set
2
Dates of
extraction
Dates of
analysis
Dates of
extraction
Dates of
analysis
Set 1 Set
2
A122-R11-4901A48
12 8
Refrigerator
4/14/82
4/28/82
10/6/82
12/9/82
A124-H11-4901A48
13 6
Hood
4/14/82
4/28/82
10/6/82
12/9/82
A124-H21-4901A48
14 4
Hood
4/14/82
4/28/82
10/5/82
12/9/82
A124-H31-4901A48
15 2
Hood
4/14/82
4/29/82
10/6/82
12/9/82
A124-W11-4901A48
16 1
Wall
4/14/82
4/29/82
10/6/82
12/9/82
A124-FBK-4901A48
30 17
Field blank
4/14/82
4/29/82
10/6/82
12/9/82
A124-FSp-4901A48
31 19
Field spike
4/13/82
4/22/82
10/6/82
11/4/82
DT1-HSp-4901A48
23 41
Herbicide hood spike
4/14/82
4/26/82
10/5/82
1/7/83
DT2-HSp-4901A48
24 43
Herbicide hood spike
4/14/82
4/27/82
10/6/82
1/7/83
PP1-HSp-4901A48
25 45
Priority pollutant hood spike
4/14/82
4/20/82
10/6/82
11/5/82
PP2-llSp-4901A48
26 47
Priority pollutant hood spike
4/14/82
4/20/82
10/6/82
11/4/82
LH1-HSp-4901A48
49 35
Low level metal hood spike
4/15/82
4/16/82
11/16/82
11/24/82
LH2—HSp-490 1A48
48 33
Low level metal hood spike
4/15/82
4/16/82
11/16/82
11/24/82
HN1-HSp-4901A48
47 37
High level metal hood spike
4/15/82
4/16/82
11/16/82
11/24/82
11t12- IISp-4901A48
46 39
High level metal hood spike
4/15/82
4/16/82
11/16/82
11/24/82
th l-FSp-4901A48
45 25
Low level metal ilter spike
4/15/82
4/16/82
11/16/82
11/24/82
LM2—FSp-4901A48
44 27
Low level metal filter spike
4/15/82
4/16/82
11/16/82
11/24/82
IIHI-FSp-4901A48
43 29
High level metal filter spike
4/15/82
4/16/82
11/16/82
11/24/82
11H2-FSp-4901A48
42 31
High level metal filter spike
4/15/82
4/16/82
11/16/82
11/24/82
PIS1-FSp-4901A48
50 49
Method spike
4/15/82
4/21/82,
4/27/82
10/5/82
11/9/82,
1/7/83
MS2-FSp-490 1A48
51 51
Method spike
4/15/82
4/21/81,
4/27/82
10/5/82
11/9/82,
1/7/83
MS3-FSp-4901A48
52 50
Method spike
4/15/82
4/21/82,
4/27/82
10/5/82
11/9/82,
1/7/83
a The sample identification numbers followed the general format of room number, wipe location and wipe number,
and 1RI project number. Wall, bench, and refrigerator wipes were designated by W, B, and R, respectively.
b QA identification numbers were nondescriptive numbers randomly assigned to each sample in that laboratory
personnel could not be aware of the type of sample with which they were working.
I - ’
0
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TABLE 3. GC/MS PARANETERS FOR PRIORITY POLLUTANT ANALYSES
Parameter
1st Sampling period
2nd Sampling period
Instrument
Varian 311-A
Finnigan 4000
Capillary column
30 m SE—54 fused silica,
0.25 mm ID, 0.25 pm
film thickness
15 m DB-5 fused silica,
0.25 mm ID, 0.25 pm
film thickness
Temperature program
50°C for 4 mm, then
10°C/mm to 325°C
40°C for 4 mm, then
10°C/mm to 325°C
Column head pressure
10 psi He
8 psi He
Injector
On-column J&W
On-column J&W
Mass range
40-475 amu
40-475 amu
Scan time
1.25 sec
1 sec
Resolution
1,000
1,000
Emission current
1 mA
0.2 mA
Ion source voltage
70 eV
70 eV
Electron multiplier
-1,400 V
-1,650 V
voltage
Three criteria were used to confirm compou.nds in the filter extracts for
which an external standard had been run. For an analyte to be confirmed,
(1) three ions had to coelute (2) with the proper intensity ratio and (3) in
the correct retention time window.
For tentative identification of the five most intense peaks with an in-
tensity of at least 10% of the internal standard (d 10 -anthracene) in a given
chromatographic run, computer searches of the NBS mass spectral library were
made using the complete mass spectra of the compounds. No further attempt
was made to identify a given compound.
Analysis of selected extracts for the methyl esters of 2,4-D and 2,4,5—T
was conducted on a Varian 311-A GC/MS system using selected ion monitoring to
enhance the sensitivity of the analysis. GC/IIS parameters used in the herbi-
cide analysis are given in Table 4.
Selected ion monitoring was also used to analyze selected extracts for
TCDD isomers. GC/HS parameters used in the TCDD analysis conducted on a
Varian 311-A are given in Table 5.
Quality Assurance Procedures
In addition to the quality assurance procedures carried out in the field
via spikes and blanks, additional fortification experiments were carried out
at MRI. A total of seven fortification experiments were conducted by spiking
bench surfaces and filters in Soxhiet extractors with solutions of the ana-
lytes. Duplicate bench spiking experiments were conducted with 20 pg each of
the surrogate compounds and priority pollutants. Similar bench spiking ex-
periments were conducted in duplicate with the acid forms of 2,4-D and 2,4,5-T
11
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TABLE 4. GC/MS PARMIETERS FOR HERBICIDE ANALYSES
Parameter
1st Sampling period
2nd Sampling period
Capillary column
30 m SE—54 fused silica,
15 m DB-5 fused silica,
0.25 mm ID, 0.25 pm
0.25 mm ID, 0.5 pm
film thickness
film thickness
Temperature program
50°C for 2 mm, then
10°C/mm to 325°C
40°C for 2 mm, then
10°C/mm to 325°C
Column head pressure
10 psi He
8 psi He
Injector
On-column J&W
On-column J&W
Ions monitored
188, 199, 233, 234, 236,
268, 270
188, 199, 233, 234, 236,
268, 270
Resolution
1,000
1,000
Emission current
1 mA
2 mA
Ion source voltage
70 eV
70 eV
Electron multiplier
-1,450 V
-2,000 V
voltage
TABLE
5. GC/NS PARAIIETERS FOR
TCDD
ANALYSES
Parameter
1st Sampling period
2nd Sampling period
Capillary column
30 m SE-54 fused silica,
0.25 mm ID, 0.25 pm
film thickness
15 in DB-5 fused silica,
0.25 mm ID, 0.25 pm
film thickness
Temperature program
50°C for 2 mm, then
10°C/mm to 325°C
70°C for 2 mm, then
10°C/mm to 325°C
Column head pressure
10 psi He
8 psi He
Injector
On-column J&W
On-column J&W
Ions monitored
320, 322, 324, 328
320, 322, 324, 328
Resolution
1,000
1,000
Emission current
1 mA
2 mA
Ion source voltage
70 eV
70 eV
Electron multiplier
-2,000 V
-2,000 V
voltage
12
-------
(20 pg each). In all cases the bench surface was wiped according to the sam-
pling procedure and the filters extracted and analyzed according to the ana-
lytical protocol. Extraction efficiencies were also determined in triplicate
for all analytes by spiking blank filters with 20 pg each of the analytes and
then extracting the filters according to the analytical protocol.
In all cases, a nondescriptive quality assurance identification number
(see Table 2) was used to identify the samples during preparation and analysis
procedures. Thus, the laboratory personnel were not aware of the type of sam-
ple (field sample, blank, or spike) with which they were working.
Analysis of the organic sample extracts by GC/HS included spiking each
extract with 20 pg of d 10 -anthracene as an internal standard for quantitation.
Analytical standards of the analytes were used as external standards to deter-
mine retention time windows and response factors. The GC/MS was optimized
according to state-of-the-art techniques to provide the highest practical sen-
sitivity and selectivity.
1ETALS
Sample Preparation Procedures
Samples were prepared for metal analysis using the EPA extraction proce-
dure for lead on air sampling filters, Federal Register , 43(194), October 5,
1978, p. 46260. The filters were leached with 6 ml of warm 3 N Baker Ultrex®
nitric acid for 30 mm. After allowing the sample to cool, the acid leachate
was decanted off the filter and the beaker and filter rinsed with a few milli-
liters of deionized water and allowed to stand for another 30 mm. The first
rinse was then decanted off the filter and combined with the acid leachate.
This process was repeated, and all of the liquid fractions were then combined
and weighed before analysis.
Sample Analysis Procedures
The elemental concentrations in the filter leachates were determined
using a Jarrell-Ash 1odel l155A ICP emission spectrometer interfaced to a
Digital Equipment Corporation PDP 11/23 computer. The following instrument
settings were used:
Forward power: 1.15 kw
Reflected power: 2.0 W
Observation height: 18 mm
Nebulizer type: Fixed cross flow
Coolant gas flow: 18 liters/mm Ar
Sample gas flow: 0.5 liters/mm Ar
Solution uptake: 1.6 ml/min
Quality Assurance Procedures
In addition to the field blank, duplicate reagent blanks and filter
blanks were analyzed by ICP to establish background levels for the 28 metal
analytes.
13
-------
Four filter spikes were also prepared to test the effectiveness of the
acid leaching process. Samples were prepared by adding a fortification solu-
tion directly to the filters before the sample preparation. Duplicate samples
were fortified at the 250 pg/rn 2 level, and at the 50 pg/rn 2 level. The effec-
tiveness of the wiping process was also tested by preparing four wipes at
known concentrations. An aqueous solution of the metals was poured on clean
laboratory benches and allowed to air dry. Then damp Whatman No. 42 filters
were wiped over the area in the same manner as a field sample. Duplicate sam-
ples were generated at the 50 pg/rn 2 and 250 pg/rn 2 levels.
Analysis of the filter leachates by ICP-AES included calibration of all
elemental channels with a reagent blank and a 10 pg/g calibration standard
(equivalent to 200 pg/rn 2 ). Compensation for spectral interferences was made
using correction factors in the computer calculation software.
14
-------
SECTION 5
RESUlTS AND DISCUSSION
ORGANI CS
Appendices A through C contain figures from the GC/MS analyses conducted
on the samples from the first sampling at TAC. Appendices D through F con-
tain those from the second sampling. Specifically, reconstructed ion chro-
matograms (RIC) for each of the samples and for representative standards ana-
lyzed by full scan GC/IIS are shown in Figures A-i through A-44 in Appendix A
for the first set of samples. The second set of samples analyzed for priority
pollutants are shown in Figures D-l through D-77 in Appendix D. Following
each RIC are figures of the full mass spectra of the tentatively identified
peaks which were over 10% of the internal standard intensity. Figures B-i
through B-14 in Appendix B show the extracted ion current plots (EICP) for
the samples and standards for the first set analyzed by GC/MS-SIM for the
methyl esters of 2,4—D and 2,4,5-T. The second set of samples analyzed for
herbicides are shown in Figures E-1 through E-13 in Appendix E. Figures C-I
through C-b in Appendix C show the EICPs for the standards and samples from
the first set analyzed by GC/MS-SIN for tetrachlorodioxin isomers. Figures
for the second set are shown in Figures F-i through F-iO in Appendix F.
Sample Analysis Results
GC/NS analysis of the dichioromethane extracts from the filter wipes
taken at TAC during both sampling periods showed no detectable levels of any
semivolatile priority pollutants except di(2-ethyihexyl)phthalate (DEHP), di-
n-octyl phthalate (DOP), diethyl phthaiate (DEP), and butylbenzyl phthalate
(BBP). The presence of phthaiates, however, is normally associated with plas-
ticizers used in wall coatings and various plastics and does not necessarily
indicate that surface contamination is present from use of that particular
chemical in a laboratory. A summary of the samples containing priority poi-
lutant phthaiates is given in Table 6. Sample Wli-49OiA48 was a wall wipe
from Room E506. This sample contained levels of phthalates considerably
higher than the field blanks, probably because of the use of plasticizers in
the wall coatings.
Instrumental detection limits for all semivolatile priority pollutants
using full scan GC/NS are given in Table 7. Detection limits were estimated
assuming a GC/MS signal of 1,000 area counts as the minimum detectable signal,
using a 1-IJ1 injection volume, a 1-mi extract volume, and a wipe area of 0.04
m 2 . A 100% extraction and wiping efficiency was also assumed. Detection
limit differences between the first and second analyses are a result of using
different mass spectrometers and analytical conditions.
is
-------
TABLE 6. SAMPLE ANALYSIS RESULTS FOR PRIORITY POLLUTANTS
Diethyl
(p
Sample Set I
phthalate
g/m 2 )
Butylbenzyl hthalate
(pg/rn 4 )
Di(2-ethylhexyl)phthalate
(pg/rn 2 )
Di—n-octylphthalate
(pg/rn 2 )
Set
1 Set
2
Set
2
Set
1
Set
2
Set
I
Set
2
D418-Hh1-4901A48
<
9
<
3
K
12
70
K 10
130
K 6
< 2
D418-H21-4901A48
<
9
<
3
<
12
50
K 10
85
K 6
K 2
D420-H21—4901A48
<
9
10
<
12
30
40
70
K 6
K 2
D420-FBK—4901A48
<
9
<
3
<
12
65
K 10
110
< 6
K 2
D421—B11-4901A48
<
9
<
3
<
12
80
300
170
20
< 2
E506-HI1-4901A48
<
9
<
3
K
12
35
330
60
< 6
< 2
E506-1121-4901A48
<
9
K
3
<
12
70
230
370
< 6
< 2
E506-R11-4901A48
<
9
10
<
12
65
30
330
K 6
< 2
E50 6-W11-490 1A48
K
9
<
3
<
12
250
1,430
680
1,200
490
E508-Hh1-4901A48
K
9
K
3
K
12
20
50
50
K 6
< 2
E508-1121-4901A48
K
9
K
3
K
12
75
50
120
K 6
< 2
E514-H11-4901A48
<
9
<
3
K
12
10
< 10
20
K 6
< 2
E514-FBK-4901A48
<
9
<
3
K
12
15
40
35
K 6
< 2
a’
E516-Hh1-4901A48
<
9
<
3
<
12
60
< 10
90
K 6
< 2
E520-H11-4901A48
<
9
<
3
<
12
60
50
100
K 6
K 2
E520-R11-4901A48
<
9
<
3
<
12
30
60
70
K 6
< 2
-------
Instrumental
limit of
m/z
ion
Retention
Amount
detectiona
used to
Compound quantitate
Scan
No.
time (mm)
injected
(ng)
( ig/m 2 )
Set 1 Set 2
Set 1
Set 2
Set 1 Set 2
d 10 -Anthracene
188
883
1,084
18:24
18:04
20
b
b
bis(2-Chloroethyl)ether
93
283
405
5:54
6:45
20
26
5
o-Chlorophenol
128
285
402
5:56
6:42
20
25
6
Phenol
94
292
405
6:03
6:45
20
28
4
m-Dichlorobenzene
146
294
419
6:07
6:59
20
15
5
j -Dichlorobenzene
146
302
428
6:17
7:08
20
14
5
o-Dichlorobenzene
146
325
455
6:46
7:35
20
16
5
bis(2-Chloroisopropyl)ether
121
351
484
7:19
8:04
20
77
3
Hexachioroethane
117
360
496
7:30
8:16
20
56
13
N-Nitroso-di-n-propylamiue
130
369
505
7:41
8:25
20
49
13
Nitrobenzene
77
380
515
7:55
8:35
20
12
2
Isophorone
138
411
551
8:34
9:11
20
44
12
o-Nitrophenol
139
422
559
8:47
9:19
20
35
9
2,4-Dimethyiphenol
122
445
582
9:16
9:42
20
27
5
bis(2-Chloroethoxy)methane
93
450
594
9:22
9:54
20
21
2
1,2,4—Trichlorobenzene
180
459
604
9:34
10:04
20
16
6
2,4-Dichiorophenol
162
462
597
9:37
9:57
20
37
7
d 8 -Naphthalene
136
462
607
9:37
10:07
20
5
2
Naphthalene
128
464
610
9:40
10:10
20
6
2
Hexachiorobutadjene
225
492
642
10:15
10:42
20
29
16
—Chloro-rn-cresol
142
567
711
11:49
11:51
20
28
7
Hexachiorocyclopentadiene
237
587
747
12:14
12:27
20
25
5
Trichiorophenol
196
606
762
12:37
12:42
20
26
10
2-Chloronaphthalene
162
617
779
12:51
12:57
20
9
3
Acenaphthylene
152
671
839
13:59
13:57
20
6
2
Dimethylphthalate
163
679
849
14:09
14:09
20
8
3
2,6-Dinitrotoluene
165
685
854
14:16
14:14
20
32
10
Acenaphthene
154
694
867
14:27
14:27
20
8
3
(continued)
-------
TABLE 7 (continued)
Instrumental
limit of
m/z
ion
Retention
Amount
detectiona
used to
Compound quantitate
Scan
No.
time (mm)
injected
(ng)
( ig/m 2 )
Set 1 Set 2
Set 1
Set 2
Set I Set 2
2,4-Dinitrophenol 184 715 888 14:54 14:48 200 39 13
2,4-Dinitrotoluene 165 734 910 15:17 15:10 20 24 7
-Nitrophenol 139 742 911 15:27 15:11 100 50 10
Fluorene 166 759 942 15:49 15:42 20 7 3
4-Chiorophenyl phenyl ether 204 766 951 15:57 15:51 20 9 4
N-Nitroso-diphenylamine 169 766 951 15:57 15:51 20 103 45
Diethylphthalate 149 771 955 16:04 15:54 20 9 3
4,6-Dinitro—o-cresol 198 783 968 16:19 16:08 100 29 11
1,2-Diphenylhydrazine 105 784 973 16:20 16:13 20 18 8
4-Bromophenyiphenyl ether 248 827 1,020 17:14 17:00 20 18 12
Hexachlorobenzene 284 838 1,034 17:27 17:14 20 15 11
Pentachiorophenol 266 869 1,064 18:06 17:44 20 26 17
‘ 3 C 6 -Pentachlorophenol 272 868 1,064 18:05 17:44 20 25 24
Phenanthrene 178 879 1,080 18:19 18:00 20 5 2
Di-n-butylphthalate 149 980 1,197 20:25 19:57 20 5 2
Fluorant..hene 202 1,033 1,255 21:31 20:55 20 2 2
Pyrene 202 1,058 1,286 22:02 21:26 20 4 2
Benzidine 184 1,060 1,361 22:15 22:41 20 110 82
t)ieldrin 263 1,089 1,324 22:41 22:04 20 91 26
d 6 -Tetrachlorobipheny l 298 1,098 1,333 22:52 22:13 20 7 30
Butylbenzylphthalate 149 1,170 1,416 24:22 23:36 20 12 4
‘ 1 12 -Chrysene 240 1,218 1,470 25:22 24:30 20 5 32
Chrysene 226 1,221 1,474 25:26 24:34 20 14 10
3,3’-Dich lorobenzidine 252 1,227 1,482 25:36 24:42 20 13 23
Di(2-ethylhexy l)phthalat.e 149 1,253 1,515 26:06 25:15 20 10 3
Di-n-octyl phthalate 149 1,330 1,603 27:42 26:43 20 6 2
Benzo [ kjfluoranthene 252 1,350 1,621 28:07 27:01 20 3 2
Benzola]pyrene 252 1,387 1,660 28:54 27:40 20 12 6
Dibenz [ a,h]anthracene 278 1,515 1,807 31:34 30:07 50 4 4
Benzo [ ,h,iJpery1ene 276 1,539 1,831 32:04 30:31 50 4 3
(continued)
-------
TABLE 7 (concluded)
Instru mental
limit of
m/z ion
Retention
Amount
detectiona
Compound
used to
quantitate
Scan
No.
time (mm)
injected
(ng)
(pg/rn 2 )
Set 1 Set
2
Set 1
Set 2
Set 1 Set 2
a-BIIC
183
830
1,024
17:30 17:05
10
250 21
y-BHC
183
868
1,064
18:05 17:42
10
250 25
-BHC
181
869
1,069
18:05 17:48
10
250 25
-BHC
183
903
1,101
18:49 18:21
10
250 36
Fleptachior epoxide
355
1,024
1,250
21:20 20:50
10
120 60
Dieldrin
79
1,090
1,324
22:42 22:03
20
180 10
p,p’-DDE
246
1,092
1,327
22:45 22:07
20
50 13
p,p’-DDD
235
1,138
1,375
23:42 22:55
60
40 6
Endrin
345
1,143
1,384
23:48 23:05
20
70 240
Aldrin
262
1,160
1,201
24:10 20:01
10
250 65
1Ieptachlor
272
1,161
1,160
24:11 19:19
10
27 35
Endosulfan I
195
1,162
1,294
24:15 21:33
20
1,000 115
Endosulfan sulfate
272
1,165
1,411
23:55 23:21
60
160 50
p,p’-DDT
235
1,170
1,417
24:22 23:38
60
40 8
a Not corrected for wiping efficiency.
b GC/PIS internal standard.
-------
In the analysis of selected extracts for the herbicides 2,4—D and 2,4,5-T,
no detectable levels were found in any samples except sample E502-H21-4901A48
during the second sampling. This sample contained 1.3 pg/rn 2 of 2,4-D. The
detection limits were 0.1 and 0.2 pg/rn 2 for 2,4-D and 2,4,5-T, respectively,
based on 1,000 area counts as the minimum detectable signal, a 1-pi injection
size, 1-ml extract volume, and a 0.04 in 2 wipe area. A total of five wipes
from Rooms E502 and E510 were analyzed by GC/NS-SIN for the herbicides. Field
blanks taken in Rooms E514 and D420 and a method blank of the methylation pro-
cedure were also analyzed for the methyl esters of 2,4-D and 2,4,5—T. Neither
of the methylated herbicides was detected in any of the blank samples.
No detectable levels of any tetrachioro—isomers of polychiorinated di—
benzo- -dioxins were found in extracts of wipes from the dioxin analysis lab-
oratories. Since workers at TAC use significant amounts of 2,3,7,8— 37 C1-TCDD,
m/e 328 was also scanned in the GC/NS-SItl analysis of the extracts. External
standards used in the analysis consisted of 10 to 100 pg each of 1,2,3,4-TCDD
and 2,3,7,8- 37 C1-TCDD. No internal standard was used. Since 10 pg of both
TCDD standards could be detected with GC/MS-SIM, the estimated detection limit
for those compounds calculates to be 25 ag/rn 2 allowing for a 1—pi ln,iection
from a 100-pl extract volume resulting from a surface wipe of 0.04 m’. How-
ever, after the analysis of a few extracts the noise level of the ions moni-
tored increased to obscure a 10-pg standard. A 100-pg standard, however
could always be seen, thus a more realistic detection limit was 250 ng/m
Analysis of sample A124-W11-4901A48, a wall wipe taken in Room A124 dur-
ing the first sampling period, showed a very large m/e 328 peak at the reten-
tion time of 37 C1-TCDD (see Figure C-9, Appendix C). Reanalysis of the ex-
tract by full scan NS, however, showed that the 328 ion was associated with
triphenyiphosphate, a chemical used as a plasticizer in lacquers and varnishes
Figure C-li in Appendix C shows a reconstructed ion chromatogram of sample
A124-W11-4901A48 run in the full scan mode. The mass spectra of the peak in
question is given in Figure C-12, and again in Figure C-13, Appendix C, com-
pared with the library mass spectra of triphenylphosphate. Further evidence
of the presence of organophosphates in the dioxin laboratory wipe comes from
the only other wall wipe taken at TAC, sample E506-Wl1-4901A48, which con-
tained octyldiphenylphosphate. Analysis of the wall wipe taken in Room A124
during the second sampling also showed a large m/e 328 peak but in this in-
stance chromatographic separation between the compound in question (presumably
triphenyiphosphate) and 2,3,7,8- 37 C1-TCDD was achieved (see Figure F-9, Appen-
dix F).
Other compounds also tentatively identified in the filter extracts from
both samplings are listed in Table 8 and are cross referenced to their com-
plete mass spectra. Generally, most of the peaks identified were miscella-
neous phthalates from plastics and paints or hydrocarbons from oils or greases
found on laboratory surfaces.
20
-------
TABLE 8. MAJOR PEAK TENTATIVE IDENTIFICATION SUMMARY
a Nolecular Spect um
Sample RT(min)/RRT weight Spectrum Tentative identification fit
Spectrum
purity
First Sampling
Second Sampling
A124-Wl1-4901A48
22:25/1.22
326
Figure C-12
Triphenyiphosphate
801
727
E506-H21-4901A48
27:00/1.48
390
Figure A-8
Di-iso-octylphthalate
591
535
E506-R11-4901A48
14:48/0.81
220
Figure A-IO
2,6-Bis(1,1-dimethylethyl)-
4-methyl-phenol
812
812
E506—H11-4901A48
24:37/1.35
25:22/1.39
412
366
Figure A-5
Figure A-6
Bis(2-ethylhexyl)nonanedioate
Bis(2—butoxyethyl)phthalate
678
649
523
649
E506-W1l-4901A48
25:06/1.36
25:11/1.36
29:25/1.59
31:03/1.68
272
362
390
330
Figure A-12
Figure A-13
Figure A-14
Figure A-IS
Dibutylheptanedioate
Octyldiphenylphosphate
Di-iso-octylphthalate
Dicyclohexylphthalate
701
895
894
815
204
821
716
510
E508-1121-4901A48
E514-H11—4901A48
20:34/1.12
22:33/1.23
2:32/0.14
256
284
114
Figure A-18
Figure A-19
Figure A-21
Hexadecanoic acid
Octadecanoic acid
2(2-Butynyloxy)ethanol
848
863
552
644
675
552
E520-R11-4901A48
15:57/0.87
17:14/0.94
19:37/1.07
20:43/1.13
21:48/1.19
254
240
282
506
296
Figure A-25
Figure A-26
Figure A-27
Figure A-28
Figure A-29
Hexamethyldodecane
lleptadecane
Eicosane
Hexatriacontane
Tetramethyiheptadecane
721
709
834
738
672
573
665
691
563
545
E506-H11-4901A48
6:05/0.34
6:46/0.37
24:39/1.37
120
120
366
Figure D-4
Figure D-5
Figure D-6
Methylethylbenzene
1,2,3-Trimethylbenzene
Bis(2-butoxyethyl)phthalate
d
981
786
d
933
679
E506-H21-4901A48
3:09/0.17
3:27/0.19
19:59/1.11
24:03/1.33
26:21/1.46
116
98
256
326
390
Figure D-8
Figure D-9
Figure D-1O
Figure D-11
Figure D-12
4-Hydroxy-4-methyl-2-pentanone
2-Hexenal
Hexadecanoic acid
Triphenylphosphate
Diisooctylphthalate
981
885
944
933
700
970
795
769
796
581
(continued)
-------
TABLE 8 (continued)
a Molecular Spect um
Sample RT(min)/RRT weight Spectrum Tentative identification fit
Spectru
purity
E506-R11-4901A48
3:10/0.18
116
Figure
0-14
4-Hydroxy-4-methyl-2-pentanone
978
966
3:29/0.19
98
Figure
D-15
2-Hexenal
890
809
8:09/0.43
98
Figure
0-16
2-Cyclohexen-1-ol
913
703
20:38/1.14
256
Figure
0-17
Molecular sulfur
971
950
27:09/1.5
296
Figure
D-18
2,6,10,14-Tetramethyiheptadecane
942
811
E506-W11-4901A48
3:29/0.19
24:14/1.34
98
100
Figure
Figure
D-20
0-21
2-}Iexenal
1-Ethenyloxybutane
889
789
801
358
24:22/1.35
28:14/1.56
362
390
Figure
Figure
0-22
D-23
Octyldiphenyiphosphate
Diisooctyl phthalate
915
947
797
834
E508-H1]-4901A48
3:24/0.19
202
Figure
D-25
tert-Dodecanethiol
885
756
E508-1121--4901A48
3:27/0.19
6:04/0.34
6:44/0.37
19:57/1.11
202
120
120
256
Figure
Figure
Figure
Figure
0-27
D-28
D-29
0-30
tert-Dodecanethiol
1-Ethyl-2-methylbenzene
1,2,3-Trimethylbenzene
Hexadecanoic acid
863
996
995
993
730
920
939
813
E514-H11—4901A48
21:51/1.21
3:26/0.19
298
98
Figure
Figure
0-31
0-33
Nonadecanoic acid
2-Hexenal
869
904
709
831
E516-H 1 1-4901A48
1:58/0.11
3:12/0.18
3:30/0.19
92
116
98
Figure
Figure
Figure
0-35
0-36
0-37
Toluene
4-Hydroxy-4--methyl-2-pentanone
2-Hexenal
990
980
890
954
967
805
E520-H11—4901A48
1:59/0.11
3:32/0.2
8:02/0.45
92
98
98
Figure
Figure
Figure
D-39
D-40
D-41
Toluene
2-Hexenal
1-Cyclohexen-1-ol
988
894
934
954
805
679
E520-R11-4901A48
3:32/0.2
18: 14/1.01
19:19/1.07
20:19/1.13
21:18/1.18
24:50/1.38
98
254
182
240
296
490
Figure
Figure
Figure
Figure
Figure
Figure
D-43
0-44
0-45
0-46
D-47
D-48
3,3’-Oxybis-l-propeue
Octadecane
1,1,1-Trifluoro-2,4—heptanedione
lleptadecane
Heneicosane
17-Pentatriacontane
851
961
978
974
954
957
719
789
856
822
808
688
0418-H11-4901A48
3:13/0.18
3:31/0.19
116
202
Figure
Figure
0-50
0-51
4-Hydroxy-4-methyl-2-pentanone
tert-Dodecanethiol
964
865
953
732
(continued)
-------
TABLE 8 (concluded)
Sample
a
RT(min)/RRT
Molecular
weight
Spectrum
Tentative identification
Spect um
fit
Spectru
purity
D418-1121-4901A48
3:04/0.17
3:21/0.19
4:12/0.23
5:15/0.29
8:01/0.44
116
202
98
96
98
Figure
Figure
Figure
Figure
Figure
D-53
D-54
D-55
D-56
D-57
4—Hydroxy-4-methyl-2-pentanone
tert-Dodecanethiol
2-Cyclohexen-1-o].
2-Cyclohexen-1-one
2-Cyclohexen-1-ol
963
879
976
969
962
946
748
864
947
735
D420-Hl1-4901A48
2:01/0.11
92
Figure
D-59
Toluene
989
947
D420-H21-4901A48
3:12/0.18
3:30/0.19
116
202
Figure
Figure
D-61
D-62
4-Hydroxy-4-methyl-2-pentanone
tert-Dodecanethiol
964
866
950
728
D421-B11-4901A48
2:00/0.11
3:34/0.20
8:09/0.45
92
98
98
Figure
Figure
Figure
D-64
D-65
D-66
Toluene
2-Hexenal
2-Cyclohexen-1-ol
991
892
889
950
806
688
D420-FBK -4901A48
3:21/0.19
202
Figure
D-68
tert-Dodecanethiol
885
757
a Retention time (min)/relative retention time to deuterated anthracene.
b Spectrum fit is a value mathematically derived from matching peaks from the unknown spectrum to the library
spectrum and indicates the degree of similarity between the two spectra. Values over 700 are generally
considered good.
c Spectrum purity is a value mathematically derived which indicates the absence of interfering mass peaks in
the unknown spectrum compared to the library spectrum. Values over 700 are generally considered good.
d Manual interpretation.
-------
Quality Assurance Results
Individual recoveries of surrogate compounds used to fortify filter sam-
ples in the field ranged from 52 to 125% as seen in Table 9. Recoveries
slightly lower than extraction efficiencies were seen for the more volatile
compounds such as d 8 -naphthalene and ‘ 3 C 6 -pentachloropheaol, while virtually
quantitative recoveries were seen for dieldrin, d 6 -tetrachlorobiphenyl, and
d 12 -chrysene. These results indicate that small losses occurred during trans-
portation and handling and, in general, volatile compounds will suffer some
losses as a result of transportation processes. Bench (hood) wipe experiments
with the surrogate compounds gave a similar recovery pattern. d 6 -Naphthalene
showed a very poor average recovery indicating that compounds with similar
volatility may not be recovered by the wipe method. Average recoveries for
the less volatile compounds ranged from 40 to 60%. Extraction efficiencies
(method spikes) for all surrogate compounds averaged greater than 80%.
Recovery studies with semivolatile priority pollutants included hood
spiking experiments and extraction efficiency determinations. The results of
these experiments are shown in Tables 10 and 11, respectively. The average
recoveries for these compounds for both samplings ranged from 1 to 77% and
followed a pattern similar to that shown by the surrogate compounds. Extrac-
tion efficiencies generally were greater than 40% with the exception of the
very volatile priority pollutants and compounds which probably did not recov-
er because of their poor stability.
In general, the recovery experiments showed that the wipe procedure will
indicate gross contamination by nonvolatile organics. For volatile compounds,
such as hexachioroethane, naphthalene, etc., or acidic compounds, such as o-
nitrophenol, pentachlorophenol, etc., the procedure is less effective and will
yield low results. The loss may be due to ineffective collection by the wipe
or volatilization during collection and preparation. The detection limits in
Table 7 do not include this factor.
For the herbicides 2,4-0 and 2,4,5-T, the wipe procedure was not effec-
tive as shown by the recoveries given in Table 12. Although the acid form of
the herbicides extract from filter paper to some degree, they apparently can-
not be wiped from a bench surface with dichioromethane. Although a GC/HS
limit of detection was 0.1 and 0.2 ig/m 2 for 2,4-0 and 2,4,5-T, respectively,
the method detection limit would be 10 to 20 . g/m 2 based on an average 1% re-
covery from the wiping and extraction processes. Thus although the wipe pro-
cedure was not effective for the herbicides, the use of SIN in analyzing the
extracts still gave a reasonable method detection limit.
No bench spiking experiments were performed with dioxins in this task.
Experiments performed in Task 20, however, indicated that approximately 60 to
90% of TCDD isomers could be recovered from a bench spike.
24
-------
TABLE 9. SURROGATE COMPOUND RECOVERIES
d 8 —Naphthalene
Sample Set I Set 2
Percent
recovery
‘ 3 C 6 -Pentachlorophenol
Set 1 Set 2
Dieldrin
d 6 -Tetrachlorobiphenyl
d 12 -Chrysene
Set 1
Set
2
Set
1
Set
2
Set
I
Set 2
Field spikes
E514-FSp-490 1A48
D420-FSp-4901A48
A124-FSp-4901A48
Average recovery
76
73
58
69
52
52
54
53
68
68
71
69
85
79
59
74
108
123
125
119
108
99
91
99
101
99
85
95
114
100
105
106
102
102
108
104
106
84
84
91
Hood spikes
PP1-HSp-4901A48
PP2-HSp-49011A48
Average recovery
3
5
4
12
8
10
24
40
32
4b
57
52
35
60
47
72
79
76
33
58
45
70
76
73
34
60
47
70
83
76
Method spikes
IISI-FSp-4901A48
tiS2-FSp-4901A48
tlS3-FSp-4901A48
Average recovery
54
87
76
72
97
95
84
92
90
93
88
90
93
97
93
94
84
114
75
91
94
106
90
97
89
113
103
102
91
96
89
92
79
97
94
90
100
101
85
95
-------
TABLE 10. PRIORITY POLLUTANT COIIPOUND
RECOVERIES - HOOD
SPI S
Percent recovery
Hood spike
Hood spike
Average
No. 1
Compound Set 1 Set 2
No. 2
recovery
Set 1 Set 2
Set I Set 2
bis(2-Chloroethyl)ether 0 7 0 4 0 6
o-Chlorophenol 0 11 0 16 0 14
Phenol 0 20 0 25 0 23
m-Dichlorobenzene 4 2 5 6 4 4
2-Dichlorobenzene 4 2 5 4 4 3
o-Dichlorobenzene 3 4 5 7 4 6
bis(2-Chloroisopropyl)ether 0 5 0 < 1 0 3
Hexachioroethane 4 2 7 2 5 2
N-Nitroso-di-N-propylamine 0 20 0 17 0 19
Nitrobenzene 3 18 3 17 3 17
Isophorone 13 31 19 38 16 35
o-Nitrophenol 0 21 0 26 0 24
2,4-Dimethylphenol 3 17 4 29 3 23
bis(2 -Chloroethoxy)metharie 9 29 14 34 11 32
1,2,4-Trichlorobenzene 6 16 10 18 8 17
2,4-Dichiorophenol 6 32 0 41 3 37
Naphthalene 7 22 11 23 9 22
Hexachiorobutadjene 4 13 10 13 7 13
E-Chloro-rn—cresol 10 47 23 57 16 52
Hexachiorocyclopentadiene 3 15 6 18 4 16
Trichiorophenol 14 47 30 58 22 52
2-Chloronaphthalene 10 44 17 51 13 48
Acenaphthylene 14 52 24 63 19 57
Dimethylphthalate 25 58 40 70 32 64
2, 6 -Dinitrotoluene 22 52 41 60 31 56
Acenaphthene 13 54 25 63 18 59
2,4-Dinitrophenol 21 29 38 35 29 32
2,4-Dinitrotoluene 29 58 47 71 38 64
-Nitropheno1 4 32 7 37 5 35
Fluorene 23 62 40 74 31 68
4-Chiorophenyl phenyl ether 24 62 43 71 33 66
N-Nitroso-diphenylainine 29 59 49 71 39 65
Diethylphthalate 31 64 52 76 41 60
4 , 6 -Dinitro—o-cresol 27 47 53 51 40 49
1,2-Diphenyihydrazine 26 46 51 49 38 47
4-Bromophenyl-phenyl ether 26 63 47 75 37 69
Hexachlorobenzene 29 66 52 76 40 71
Pentachlorophenol 16 52 30 61 23 56
Phenanthrene 30 67 53 76 41 72
Di-n-butylphthalate 37 72 64 80 50 76
Fluoranthene 36 71 65 79 50 75
(continued)
26
-------
TABLE 10 (concluded)
Percent
recovery
Hood spike
Hood spike
Average
Compound
No.
1
No.
2
recovery
Set 1 Set
2
Set
1
Set
2
Set 1
Set
2
Pyrene
32
71
57
80
44 76
Benzidine
0
79
0
201
0 140
Butylbenzylphtha late
35
69
61
94
48 82
Chrysene
32
71
56
82
44 76
3,3 t -Dichlorobenzidine
12
65
37
135
24 100
Di(2-ethylhexyl)phthalate
50
71
87
101
68 86
Di-ri-octylphthalate
36
74
61
83
48 79
Benzo [ k]fluoranthene
33
74
57
79
45 77
Benzo [ a]pyrene
37
71
63
83
50 77
Dibenz [ a,h]anthracene
32
74
58
81
45 78
Benzo [ ,h,i]pery1ene
33
75
58
79
45 77
27
-------
TABLE U. PRIORITY POLLUTANT COMPOUND RECOVERIES - tIETHOD SPIKES
Method
No.
Compound Set 1
spike
1
Method
No.
Percent
spike
2
recovery
Method
No.
spike
3
Average
recovery
Set 1 Set 2
Set 2
Set
1
Set
2
Set 1
Set 2
bis(2-Chloroethyl)ether 14 84 99 84 89 73 67 80
o-Chlorophenol 0 88 74 88 74 82 49 86
Phenol 20 93 59 84 82 73 54 83
rn-Dichlorobenzene 18 71 69 78 49 58 45 69
p-Dichlorobenzene 17 82 246 88 NSa 66 132 /9
o-Dichlorobenzene 18 75 74 82 55 65 49 74
bis(2-Ctiloroisopropyl)ether 15 88 73 89 67 166 52 85
Hexachioroethane 18 79 20 86 NS 63 19 76
N-Nitroso-di--N-propylamine 50 90 76 93 71 81 66 88
Nitrobenzene 43 83 89 89 82 80 71 84
Isophorone 127 75 217 79 NS 72 172 75
o-Nitrophenol 39 84 102 92 87 87 76 88
2,4-Dimethylphenol 40 64 55 69 81 67 59 67
bis(2-Chloroethoxy)methane 140 88 206 94 NS 86 173 89
1,2,4-Trichlorobenzene 84 89 226 90 NS 82 155 87
2,4-Dichlorophenol 56 89 116 87 86 78 86 85
Naphthalene 54 87 87 91 73 83 71 87
Hexachlorobutadiene 34 83 90 91 74 78 66 84
-Ch1oro-rn—cresol 94 85 108 97 101 89 101 90
Hexachiorocyclopentadiene 112 76 217 83 NS 74 164 78
Trichiorophenol 83 90 87 96 82 89 84 92
2-Chloronaphthalerie 78 93 89 97 77 90 81 93
Acenaphthylene 157 90 228 95 NS 88 192 91
Dimethyiphlhalate 200 82 284 98 NS 86 242 89
2,6-Dinitrotoluene 63 80 114 95 93 82 90 86
Acenaphthene 96 94 105 97 81 88 94 93
2,4-Dinitrophenol 101 88 108 105 104 97 104 97
2,4-Dinitrotoluene 245 86 287 103 NS 96 266 95
-Nitrophenol 96 98 90 80 97 78 94 85
(continued)
-------
TABLE 11 (concluded)
Percent
recovery
Method
spike
Method
spike
Method
spike
Average
No.
Compound Set 1
1
No.
2
No.
3
recovery
Set 1 Set 2
Set 1
Set 2
Set 2
Set 1
Set 2
Fluorene 97 95 99 98 87 91 94 95
4-Chlorophenyl phenyl ether 167 94 204 97 NS 92 185 94
N-Nitroso-diphenylainine 170 97 217 101 24 95 137 98
Diethylphthalate 149 91 210 99 NS 88 180 93
4,6-Dinitro-o-cresol 103 93 113 103 106 93 107 96
1,2-Diphenylhydrazine 103 87 114 88 101 112 106 96
4-Bromophenyl-phenyl ether 108 94 105 129 95 97 103 107
Hexachlorobenzene 226 96 246 99 NS 110 236 102
Pentachiorophenol 93 92 95 102 95 92 95 95
Phenanthrene 145 97 203 101 NS 97 174 98
Di-n-butylphthalate 90 100 126 101 95 98 104 100
Fluoranthene 82 96 92 100 97 96 90 97
Pyrene 99 96 113 101 97 95 103 97
Benzidine 0 35 0 40 0 34 0 36
Butylbenzylphthalate 84 111 94 103 68 103 82 106
Chrysene 248 99 279 102 NS 96 264 99
3,3’-Dichlorobenzidine 27 120 29 54 72 63 43 79
Di(2-ethylhexyl)phthalate 94 136 111 121 88 121 98 126
Di-n-octylphthalate 144 100 206 108 NS 106 175 105
Benzo [ k]fluoranthene 170 93 241 96 NS 91 205 93
Benzo [ a]pyrene 99 94 99 97 102 93 100 95
Dibenz [ a,h]anthracene 101 92 99 94 97 91 99 92
Beuzo [ g,h,i}perylene 117 95 178 96 NS 91 147 94
a NS - Not spiked.
-------
TABLE 12. HERBICIDE COMPOUND RECOVERIES
Sample
Percent
recovery
2,4-D
2
,4,5—T
Set
1
Set 2
Set 1 Set
2
Hood spikes
DT1-HSp-4901A48
2
< 1
3
< 1
DT2-HSp-4901A48
4
< 1
4
< 1
Average recovery
3
< 1
3
< 1
Method spikes
MS1-FSp-4901A48
47
6
60
9
FIS2-FSp-4901A48
68
6
56
8
MS3-FSp-4901A48
78
4
58
3
Average recovery
64
5
58
7
METALS
Sample Analysis Results
Results of the ICP-AES analysis of the five field samples taken at TAC
are shown in Table 13. Also shown are the results of the analysis of two re-
agent blanks and two filter blanks. Values preceded by a “less than” symbol
are the detection limit for that element. The detection limits for the two
sample sets were determined in slightly different ways as the result of in-
ternal changes in the instrument operating procedures. Detection limits for
the first set were based on three times the standard deviation(s) of 10 repli-
cate analyses of one of the field samples. The dilution factor was 48.4.
Detection limits for the second set were based on three times the standard
deviation of 10 replicate analyses of a fortified reagent blank. Determining
on random error about a measurable analyte signal has proven to provide more
realistic detection limits for those analytes. Due to large Ca interferences
on the Se analysis channel, the detection limits for Se were raised above the
3S levels. Duplicate values shown for aluminum and iron resulted from moni-
toring two wavelengths. Data for the four toxic metals of specific interest
to personnel at TAC have been summarized in Table 14.
The blank filter leachates were found to contain some elements in amounts
significantly greater than the reagent blanks. The elements Al, Ca, Fe, Na,
and Zn were not of special interest in this analysis and were found in amounts
low enough so as to not interfere with the detection of high (> 500 g/m 2 )
levels in any of the wipes. For the 24 elements listed in Table 12, 12 ele-
ments were found in the field blank at a higher concentration than in the lab-
oratory filter blanks and two of those elements, Ca and Na, were present in
the filters in varying amounts. Hood wipes from Room E503 contained signifi-
cant levels of Ca, Fe, Al, Mg, and Na and varying amounts of Ba, Cr, Mn, Ni, F,
30
-------
TABLE Ii SAJIPLE ANALYSIS RESULTS FOR IIETALS.
E50 3-F 8R- OSQJ-Illi- C303 OIl- FS04-lIIl-- 1504-Oil-
tie.
-------
TABLE 14
SANPLE ANALYSIS
RESULTS FOR SELECTED
TOXIC P1ETALS pg/rn 2
Element
Rea8ent
blank I
Set I Set
2
Reagent
blank 2
Set I Set 2
Fflter
blank I
Set 1 Set
2
Filter
blank 2
Set I Set
2
E503-FBK-
4901A48
Set I Set
2
E503- 111 1- E503- 1 121-
490 1A48 490 1A48
Set I Set 2 Set I Set
2
E504iIII-
490 1A48
Set I Set 2
E504-BII-
490 1A48
Set 1 Set
2
As
<6 2 <44
(6 2 <44
(6 2 <44
<6 2 (44
<6 2 <44
<6 2 <44
<6 2 <64
Il <44
<6 2 <44
Cd
<1.0 <2
5
<1.0 <2.5
(1 0 <2
5
<1 0 <2
S
<1 0 <2
5
<1 0 3 6 <1 0 <2
5
42 S
18 7
3
hg
-------
Se, Sb, Ti, Zn, and Pb above the levels found in the field blank. Hood wipes
from the AA laboratory, Room E504, were of a metal vent funnel over an AA
spectrometer flame assembly (sample E504-Hll-4901A48) and of a lab bench sur-
face (E504-B11-49olA48). The bench wipe contained high levels (> 1,000 pg/rn 2 )
of Na, Ca, and K and also moderate levels of Fe, Zn, Sn, Al, Ni, P, and Cr.
Of the metals of particular interest to personnel at TAC, the bench wipe con-
tained an average of 13 pg/rn 2 of Cd and 92 pg/rn 2 of Pb for both samplings.
The wipe of the AA vent funnel provided more interesting results. The ex-
tremely high levels of Cr, Fe, and Ni can probably be attributed to the metals
used in the construction of the funnel and to the condition of the funnel when
it was wiped (i.e., acid pitted). Other metals present at elevated levels,
such as Co, Cu, Mn, Zn, and Pb, may or may not have been caused by the mate-
rials used in the construction of the funnel. The presence of some metals,
such as As, Cd, Hg, and Mo, may have been the result of the types of samples
analyzed at that particular instrument.
Quality Assurance Results
The results of the fortification experiments conducted to determine the
efficiency of the wiping and leaching processes are shown in Table 15 for the
metals of specific interest to TAC. The results for the remainder of the
metals analyzed for by ICP-AES are shown in Tables 16 and 17. The recoveries
for all elements were calculated taking into consideration the average amounts
found in the blank filters. However, the values for some elements, particu-
larly Al, Ca, Fe, Na, and Zn, varied considerably between different filters,
and led to erroneously high or low percent recoveries in the fortified samples.
In general, the laboratory bench fortification (Table 16) showed lower
recoveries than the filter spikes. At the 250-pg/rn 2 level, recoveries were
between 33 and 106% except for Al, Ca, Fe, Na, and Zn. The 50 pg/m 2 level
showed recoveries between 0 and 97%, except for the same metals. These ele-
ments all had high recoveries because of presumably their presence in the
filters in varying amounts. For the selected metals of interest to TAC, an
average recovery of 52% was achieved at the 50-pg/rn 2 level and an average re-
covery of 62% was achieved at the 250-pg/rn 2 level.
The leaching process yielded average recoveries (Table 17) between 80
and 110% for both samplings for the 250-pg/rn 2 level with the exception of Ca.
The Ca value was high most likely because of the variation of filter blank Ca
contained in the batch of filters used. For the 50-pg/rn 2 level, the leaching
process was not as successful, showing average recoveries between 75 and 95%
with the exception of Al, Ca, Fe, Na, and Se. All of these elements showed
high recoveries because of their presence in the filter blanks. For the se-
lected metals of interest to TAC, an average 85% leaching efficiency was ob-
tained for the 50-pg/rn 2 level and a 90% efficiency was obtained for the
250-pg/rn 2 level.
33
-------
TABLE 15. TOXIC KETAL RECOVERIES
Element
As Cd
Sample Set 1 Set 2 Set 1 Set
percent recovery
Hg
Pb
2
Set
1
Set 2 Set 1 Set 2
Bench spikes
50 pg/rn 2 level a
Ltll-HSp-4901A48 61 < 88 74 70 17 < 70 78 52
Lt12-HSp-4901A48 54 < 88 60 50 14 < 70 58 < 44 a
Average 57 < 88 67 60 15 < 70 68 48
250 pg/rn 2 level
HH1-HSp-4901A48 78 56 89 72 62 32 65 60
1ft12-HSp-4901A48 70 50 81 70 48 22 63 67
Average 74 53 85 71 55 27 64 63
Filter spikes
50 pg/rn 2 level
4> Ltll-FSp-490 1A48 79 96 81 91 79 85 70 83
LM2-FSp-4901A48 80 114 82 94 80 92 68 87
Average 79 105 81 92 79 88 69 85
250 pg/rn 2 level
11111-FSp-4901A48 92 91 93 92 91 91 82 84
H112-FSp-4901A48 91 92 95 92 93 87 84 84
Average 91 91 94 92 92 89 83 84
a Detection limit for analyte higher than spiking level.
-------
TABLE 16. METAL QA RESULTS - BENCH SPIKES
250 hg/rn 2
Bench wipe
50 Jg/m 2 Bench wipe
LMI-HSp-
LFI2-HSp-
Illh l-HSp-
HM2-HSp-
Element
(wavelength
[ A])
4901A48
4901A48
4901A48
4901A48
Set 1 Set
2
Set 1 Set
2
Set 1 Set 2
Set 1 Set
2
Al (3082)
Al (2373)
99 124
100 121
93
94
151
152
145
148
a
a
107
109
a
a
B
81 48
71
35
38
64
31
83
Ba
49 82
40
75
55
69
51
97
Be
Ca
86 72
171 92
80
160
69 b
-
50
133
43 b
26
62 b
Co
90 69
85
68
76
37
60
58
Cr
69 75
62
75
71
68
56
126
Cu
Fe (2599)
Fe (2714)
Mg
87 71
88 137
96 168
97 86
79
89
81
88
71
142
165
105
76
114
106
95
102 b
b
b
-
91
85
71
102 b
b
b
-
Mn
89 71
81
70
77
62
60
92
Mo
65 47
63
33
14
0
19
0
Na
196 +a
÷a
+a
+a
+a
+a
a
Ni
P
83 71
81 101
78
75
72
106
74
85
70
a
57
67
84
a
Sb
64 53
56
48
41 <
72
46
93
Se
91 NDC
85
NDC
79
58
Sn
39 43
33
40
16
J{_ C
27
c
Ti
63 53
61
45
50
16
48
30
Ti
54 52
47
44
7
ND’
a
Y
Zn
83 69
97 114
76
87
66
122
69
125
40
a
56
72
58
a Recovery over 200% because of high variance in filter background level for these
elements.
b Negative recovery caused by high variance in filter background level for Ca.
( -B
c Not determined because of interference.
-------
TABLE 17 METAL QA RESULTS - FILTER SPIKES
250 .ig/m 2 Filter spike
IDI1-FSp- 11M2-FSp-
50 Jg/m 2
LFI1-FSp-
Filter
spike
LM2-FSp-
Element
(wavelength
[ A])
4901A48
490 1A48
4901A48
4901A48
Set
1 Set 2 Set 1 Set 2
Set 1 Set 2 Set
1 Set 2
0 ’
Al
(3082)
102
93
103
91
120
94
121
98
Al
(2373)
102
89
104
87
121
97
122
97
B
90
95
91
103
73
121
75
112
Ba
70
94
70
93
58
92
54
94
Be
Ca
94
189
93
+a
112
9 b
—
+a
93
+a
81
+a
94
+a
Co
99
93
94
92
81
95
82
95
Cr
88
93
88
92
77
95
78
97
Cu
93
93
95
92
80
92
80
96
Fe
(2599)
108
76
107
78
105
100
108
82
Fe
(2714)
99
93
99
93
99
101
102
91
Mg
95
96
96
87
90
89
91
94
tIn
92
93
94
93
80
94
81
95
Mo
86
89
90
88
73
94
74
93
Na
110
91
108
76
139
29
155
194
Ni
89
92
88
91
76
93
77
93
p
93
81
96
88
91
110
93
134
Sb
91
94
93
91
80
90
77
66
Se
100
99
101
53
109
38
107
142
Sn
87
91
91
89
68
92
68
84
Ti
87
92
89
91
77
83
77
84
Ti
93
105
94
90
79
93
82
126
Y
87
91
89
90
76
92
77
93
Zn
97
93
97
87
91
91
89
96
a Recovery over 200% because of high variance in filter background level for Ca.
b Negative recovery caused by high variance in filter background level for Ca.
-------
APPENDIX A
CHROMATOGRAMS AND MASS SPECTRA FOR SAMPLES ANALYZED
FOR PRIORITY POLLUTANTS
A-i
-------
Figure A—i.
Priority pollutant composite standard — 20 ng.
1
D 10 -Anthrocene
200
400
600
800
1000
1200
1400
1600
SC H
4:
10
8:2U
12:30
16:40
20:50
25:00
29:
10
33:20
TIME
>
I
1
‘ 3
1
-------
Figure A—2. Priority pollutant pesticide standard.
>
D 0 —Anthracene
I - ‘ I I • •
200 400 600 800 1000 1200 1400 1600 SCAM
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
-------
Figure A—3. RIC for solvent blank.
D 1 0 —AnIhracene
200
400 600 800 1000 1200 1400 1600 SCAN
4:10
8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
> . .
4-
0
*
C
-------
D 1 0 —Anthracene
) nonanedloate
DEHP
Bis—(2—butoxyethyl)phthalate
200 400 600 800 1000 1200 1400
4:10 8:20 12:30 16:40 20:50 25:00 29:10
1600 SCAN
33:20 TIME
Figure A—4. RIC for sample E506—Hhl—4901A48.
>‘.
(J1.
C
-------
129.2 -I
Figure A—5. Mass spectrum for compound
tentatively identified as bis(2—
ethylhexyl)nonanedioate.
>‘
.4-
a)
a-
C
112.3
4 1’
C.— •) 1 u •
ib.
7U.2
C.
-I
241.4
1 1.2 259.4
193.4
iii ___ I I ___ i iii I I I ______
I I •I I • I 1 I III’I I I I I • i • I
50 100 150 200 250 m/z
-------
149.2
Figure A—6. Mass spectrum for compound tentatively identified as
bis(2—butoxyethyl)phthalate.
>-
56.2 193.2
— 101.3
‘ J. 3
85.2
176.2
133.2
luuIIII I 11111111 1 11 1 1 11 III IlIllIllIllIll I 1 1 1 11u1 1 1 1 1 14 11 1 1 1 1J 1 1 t llI I
4U 60 80 100 120 140 160 180 rn/z
-------
D 10 —Anthracene
Figure A—7. RIC for sample E506—H21—4901A48.
Di—iso—octylphthalate
DEHP
200 400 E00 800 1000 1200 1400 1600 SCAN
4:10 8:20 12:30 16:40 28:50 25:00 29:10 33:20 TIME
-------
26
.4
Figure A—8. Mass spectrum for compound tentatively identified as di—iso—octylphthalate.
56.2
2
2
2
>-
.t
‘ .0
4
50
ii
150
250 m/z
-------
D 1 0 —Anthracene
Figure A—9. RIC for sample E506—R1l—4901A48.
2, 6—Bis(1 , 1—dimethylelhyl )—
4—methyl—phenol
200 400 600 800 1000 1200 1400 1600 SCAN
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
>
0 C
-------
.3
Figure A-b. Mass spectrum for compound tentatively identified as
2, 6—bis(1 , b-dimethylethyl)—4—methyl—phenol.
150
>.,
4-
I •
C
4-
C
3
2
C- -
uk
m/z
-------
200 400 600 800 1000 1200 1400
4:10 8:20 12:30 16:40 20:50 25:00 29:10
1600 SCAN
33:20 TIME
Figure A—il. RIC for sample E506—Wll—4901A48.
0 ctyldphenylphosphate
>
.4-
l’ )
4-
C
Dibutyheptanedioate
Di - i so-oc ty lphtha late
DOP
D 10 -Anthracene
Dicyclohexylphthalate
-------
1
3
>-
.4-
C I
.4-
C
2
Figure A-12. Mass spectrum for compound tentatively identified as
dibutyiheptanedloate.
125.2
101.2
1-
40
113.1
II
80
II
—- — I
1
133.2
L 1 1
.2
120
160
>
-4 -
C
QI
.4 -
C
im/z
4
255.3
-
- 4’ .4
.4
.4
5
240 260
280
320
340
360
380
420 m/z
-------
Figure A—13.
Mass spectrum for compound tentatively identified as octyldiphenyiphosphate.
24.5 I
112.3 125.2
141.2 15 .2
170.2
II.
>
4 -
4 ) ’
4-
C
40
48..? 65. 7?’. 2
I .
60 80
.3
100
120
140
160
183.3 199.3 215.2
180
>-
.4-
a ’
.1-
C
200
I
220 m/z
240 260 280
10
‘.5
320
340
360
380
4
m /z
-------
149.2
Figure A—14. Mass spectrum for compound tentatively
identified as dl—iso—octylphthalate.
>
4-
.1-
C
35. 1
56 3
71 .2 8 .2 97.2 112.3 132.2 16 .2 207.2 29.4
I i i .••j •I • 1 • I • I • I • I J I • I • I•I’J•I•
I-
U i 50 100 150 200 250 I m/z
4-
C
4-
279.4
289.4 307.5
418.6
I • I • • I • I • I • I • I • •
300 350 400 450 500 m/z
-------
Figure A—15. Mass spectrum for compound
tentatively identified as
dicyclohexylphthala te.
—
5 .3
123.2
> .
0 ’
0
a-
C
• Ci7 )
58
1’
m/z
-------
D 1 0 -Anthracene
Figure A—16. RIC for sample E508—Hhl—4901A48.
1200
25:00
1600 SCAN
33:20 TIME
>.
4)
C
600
12; 30
1400
29: 10
4:10 8:20
-------
Hexadecanoic odd
Figure A—17. RIC for sample E508—H21—4901A48.
Octadecanoic acid
D 10 —An hracene
I - — -r — •- I I - - J - - T- _ I
20U 40U 600 800 1000 1200 1400 1608 SCAN
4:10 8:20 12:38 16:40 20:58 25:00 29:10 33:20 TIME
-------
1
Figure A—18.
Mass spectrum for compound tentatively identified as hexadecanoic acid.
73.2
85.2
0 ’ ‘)
j( . .
I.
11
3
5
: >-
I
¼0
4.-
C
50
150
250 m/z
-------
5
Figure A—19. Mass spectrum for compound tentatively identified as octadecanoic acid.
2
73.2
83.2
2
4
227.4
50 1
150
250 m/z
-------
D 1 0 -Anthracene
Figure A—20. RIC for sample E514—Hhl—4901A48.
2 —( 2 —Butynyloxy) ethanol
200
400
600
800
1000
1200
1400 1
600 SCAN
4:10
E::2 0
12:
30
16:40
20:50
25:00
2 :
10 3
3:20 TIME
>-
a-
C
-------
Figure A—21. Mass spectrum for compound tentatively identified as
2—( 2—bu tynyloxy) ethanol.
60
1
5
>‘
I’ .) 41
a-
C
1
7
30
40 50
80 rn/i
-------
D 10 —Anthracene
Figure A—22. RIC for sample E516—H1l—4901A48.
200 400 600 800 1000 1200 1400
4:10 8:20 12:30 15:40 20:50 25:00 29:10
1600 SCAM
33:20 TIME
>
-------
D 1 o— Anthrace ne
Figure A—23. RIC for sample E520—Hhl—4901A48.
200 408 600 800 1000 1200 1408 1600 SCAN
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
>‘
N ) ,it
4-
C
-------
D 10 -Anthracene
Figure A—24. RIC for sample E520—Rll—4901A48.
Heptadecane
Hexamethyldodecane
E i cosane
Hexatriacontane
Tetrame thyl heptade cane
DEHP
200 400 600 800 1000 1200 1400
4:10 8:20 12:30 16:40 20:50 25:00 29:10
1600 SCAN
33:20 TIME
N)
LI ’
4-
C
-------
9
Figure A-25.
2
Mass spectrum for compound tentatively identified as
hexamethyldodecane.
2
100 150
N.)
0 ’
50
nVz
-------
56.2
Figure A—26. Mass spectrum for compound tentatively identified as heptadecane.
35.0
71.2
85.2
>
.4-
•1 •
I-
4-
C
9 . 2
113.2
127.2
24 i 3
141.2 155.2 169.3 183.3
_____________ ___________ H ___________ U ___________ I 9 i .
I • —j -• I • I I •I I I • ( • I • I I’ I •I I •
50 100 150 200 m/z
-------
56.2
Figure A—27. tiass spectrum for compound tentatively identified as elcosane.
35. U
71.2
ou.
>..
t )
co
4-
C
99.2
4 4 _ —
I I .
127.2
155.2 258.4
183.3 211.3
i,LI,, 1 •H,L4 _ 1 1 HIL 1 h1 LH .H 1 JL 1 . 1 iLHL
50 100 150 200 250 m/z
-------
56.2
Figure A—28. Mass spectrum for compound tentatively identified as hexatriacontane.
34.9
712
85.2
I)
4-
C
113.2
127.2
141.2
-- - 262.4
1b 197 ‘
I, jl j.I
50 100 200 250 nVz
-------
56.2
Figure A—29. Mass spectrum for compound tentatively identified as
tetramethyiheptadecane.
34.9
71.2
85.2
>-
.4-
‘ -
0
4-
C
99.2
113.2
127.2
155.2
183.3 296.4
211.3 239.3
I • •‘ I , I 1 I • I• I
50 100 150 200 250 300 nVz
-------
D i 0-Anthracene
Figure A—30. RIC for sample D418—Hll—4901A48.
>.
.4-
.4-
‘ I I I I I I
2@O 400 600 800 1008 1200 1400 1600 SCAN
4:10 8:20 12:38 16:40 20:50 25:00 29:10 33:20 TIME
-------
D 10 —Anthracene
Figure A—31. RIC for sample D418—H21—4901A48.
200 400 600 800 1000 1200 1400 1600 SCAM
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
>-
4-
( -i . )
N.)
4-
C
-------
D 10 —Anthracene
Figure A—32. RIC for sample D420-H1l—4901A48.
200
400
600
880
1000
1200
1408
1600
SCAt
4:10
8:20
12:30
16:40
20:50
25:00
29:10
33:20
TIME
C
-------
D 1 —Anthracene
Figure A—33. RIC for sample D420—H21—4901A48.
208
480
608
800
1000
1280
1480
1608
SCAN
4:10
8:20
12:30
16:40
20:50
25:80
29:10
33:20
TIME
>..
.t
C
-a-
C
-------
D 1 0 -Anthracene
Figure A-34. RIC for sample D421—Bll—4901A48.
DEHP
U ’
.1-
C
I I I I I I I
2UC’ 400 600 800 1000 1200 1400 1600 5CAH
4:10 12:30 16:40 20:50 25:00 29:10 33:20 TIME
-------
D 1 0 —Anthracene
Figure A—35. RIC for field blank sample
E514—FBK—4901A48.
2 U 40U 600 800 1000 1200 1400 1600
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
-------
D 10 -An hracene
Figure A—36. RIC for field blank sample
D4 20-FBK-4 901A48.
208
400
600
800
1000
1200
1400
1600
SCAN
4:10
8:20
12:30
16:40
20:50
25:00
29:10
33:20
TIME
>-
I
-------
Dó-Tetrachlorobiphenyl
Figure A—37. RIC for field spike sample E514—FSp—4901A48.
D 0 -Anthracene
Dieldrin
D 1 2 —Chrysene
D 8 — Nophthalene
‘ 3 C—Pentachlorophenol
200 400 600 800 1000 1200 1400 1600 SC H
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
>.‘
.t
a,
.4-
C
-------
Dó—Tetrach orobiphenyI
Figure A—38. RIC for field spike sample D420—FSp—4901A48.
D 8 - Naphthalene
1 3 C—Pentachlorophenol
Die Idrin
D 10 -Anthracene
D 1 2 —Chrysene
200 400 600 800 1008 1200 1400
4:10 8:20 12:30 16:40 20:50 25:00 29:10
1600 SCAN
33:20 TIME
>-
C
-------
D -TetrachtorobiphenyI
Figure A—39.
RIC for field spike sample Al24—FSp—4901A48.
D 0 -Anthracene
Dieldrin
D 12-Chrysene
D8— Naphthalene
13 C—Pentachlorophenol
200
400
608
800
1000
1200
1400
1600
SCAN
4:
10
8:20
12:30
16:40
20:58
25:00
29:10
33:20
IDE
>‘
I ‘
.1-
C
-------
D 10 —Anthracene
Figure A—40. RIC for priority pollutant hood
spike sample PP1—HSp—4901A48.
I
200 400
600
800 1006 1200
1400 1600 SCAN
4:10 8:20
12:30
16:40 20:50 25:00
29:10 33:20 TIME
>.-
:x .t
C
1
1219
1094
1029
975
834
1166
J.J
1%
I’ ..
-------
Figure A—41. RIC for priority pollutant hood spike sample PP2—HSp—4901A48.
D 10 -Anthracene
1480
29:10
1608 SCAH
33:20 TIME
>-
:
I tn
. C
F ) 4)
C
408
8:20
600
12:30
800
16:40
1008
20:50
1200
25:00
-------
1354
Figure A—42. RIG for priority pollutant method spike sample MS1—FSp—4901A48.
1222
D 1 O-Ar thracene
767 1554
838
>..
.t
. . C
L..) W
.1-
1097
457 671
978 1169
244 r JiL _______ b T — — I - J
200 400 600 800 1000 1200 1400 1600 SCAN
4:10 8:20 12:30 16:40 20:50 25:00 29:10 33:20 TIME
-------
1353
Figure A— li. ]. KIC I or 1 riorILy poihildilL method spike arnpEe MS2—FSp—4901A48.
1224
D 0 -Anthrocene
5 7
>‘
4-
— C
a) -
.4-
C
C
J 671 1101
382
11 ?2
11 L iL . , I. I - — 4 - i, I
200 400 600 800 1000 1200 1400 1600 SC IH
4:10 20 12: U 16:’1 0 20:50 25:00 29:10 3?:20 TIME
-------
1513
Figure A—44.
RIC for priority pollutant method spike sample MS3FSp—4901A48.
456
Lii
612
‘ Ii
711
1097
1218
1169
1386
‘ I
I
I
I
I
I
200
400
600
800
1000
1200
1400
4:10
8:20
12:30
16:40
20:50
25:00
29:10
1600 SCAN
33:20 TIME
>.
I - f l C)
. 1-
C
1030
978
364
288
164
J
-------
APPENDIX B
EXTRACTED ION CURRENT PLOTS FOR SAfiPLES ANALYZED
FOR HERBICIDES
B-i
-------
Figure B—i. EICPs for methylated 2,4—D and 2,4 1 5—T standaid — 1 ng each.
nVz
234
1350 SCAM
17:23 TIME
188
199
233
D 1 0-Anthrocene
270
I •• I I
10130
12:52
2,4,5—1 \
/ \
1050 1100 1150
13:31 14:10 14:48
1200
15:2?
1300
16:44
-------
Figure B—2. EICPs for sample E502—R1l—4901A48.
m/z
188
199 -
2331
!23411 •1 I .. 1
JI .J
II 111,111 I 11111111 I IlliJi
270 Ij
I UJIIJIIJ I I u
1000 1050 1100 1150 1200 1258 1300 1350 SCAN
12:52 13:31 14:10 14:48 15:27 16:05 16:44 17:23 TIME
D 10 —Anthracene
Jul.1 1 .’ • I • I I 111111111 •
-------
Figure B—3.
EICPs for sample E502—Hhl—4901A48.
I . . . I I I I I I I I I I I I I I IIIIJII I I I
I Illij Ill • ililtiliri III• IIII IU . .
I I I
I
I I I
1000 1050 1100 1130 1200 1250 1300 1350 SCAN
12:52 13:31 14:10 14:48 15:2? 16:05 16:44 17:23 TIME
188
199
D 10 —Anthracene
234
270
-------
Figure B—4. EICPs for sample E502—H21—4901A48.
I i.u.i....j.uuuj...ru.u..u.iu.i.ru. II
III uI.I..I...IIIIIIIrIIIII...Ju,u.
1 ’ ,.
L .PJ
270
I I I I I I I I 1 I I . . . i
I
I •
I
I
I
I
• I
1000
1850
1100
1150
1280
1250
1300
1350
SCAN
12:52
13:31
14:10
14:48
15:2?
16:05
16:44
17:23
TIME
188
1 i9
L
m/z
U,
D 1 0 —Anthracene
-------
Figure B—5. EICPs for sample E510—Hll—4901A48.
188
1 39
233
0” ‘--I
I I I I • I I I I I I I I I I j
268.
270
_ IiIIIlIII I • I I I I • I I I
10130 1050 1100 1150 1200 1250 1300 1350 SCAN
12:52 13:31 14:10 14:48 15:27 16:05 16:44 17:23 TIME
D 10 -Anthracene
H:.
-------
Figure B—6. EICPs for sample E510—Bll—4901A48.
188
199
233
234
• I I 111 ..,. . . ., 1I.tu ... • u•••1 I I I i
1 1 1 1( 1 1 1 1 I I I I uhh I II IhhhIThThII IP •
I I • Jr . 1 Ii .. I
27i1 -
1111111.. I uIIuIuIIIIIIIIui, III.I I
1000 1050 1100 1150 1200 1250 1300 1350 SCAN
12:52 13:31 14:10 14:48 15:27 16:05 16:44 17:23 TIME
D 10 —Anthrocerie
I I 1 ‘ I I 11111111 IlhhulI,1h 1h111 I
-------
Figure B—7. EICPs for method blank sample.
235
270
IJIuJI IUUI UIEI JUIU ( I I I I I I
I I
I. IIIIII I • IrIlIllIll.. II
- I-—..
1000 1050 1100 1150 1200
12:52 13:31 14:10 14:48 15:27
I
1250 1300 1350 SCAN
16:05 16:44 17:23 TIME
m/z
188
199
233
D 1 0 —Anthracene
-------
188
199
233
234
236 -
••••I... . I
. u•Jr11I•uIIlIrIIulII. I
I
I I I
1000 1050 1100 1150 1200 1250 1300 1350 SCAN
12:52 13:31 14:10 14:48 15:27 16:05 16:44 17:23 TIME
m/z
Figure B—8. EICPs for field blank sample E514—FBk—4901A48.
D 10 —Anthracene
270
-------
I— I !
I I I • I I I • I •
1050
1100
1150 1200 1250 1300 1350 SCAM
12:52 13:31
14:10
14:48 15
:27 16:05 16:44 17:23 TIME
Figure B—9. EICPs for field blank sample D420—FBk—4901A48.
m/z
cD
D 10 —Anthracene
188
199
233
234
268
270
-------
Figure B—b. EICPs for hood spike sample DT1—HSp—4901A48
m/z
D 1 -Anthracene
188
199
233
234
270
1’
12:52
1100
14: 10
1150
14:48
1280 1250 1308
15:27 16:05
1358 SCAN
17:23 TIME
16:44
-------
Figure B—li. EICPs for hood spike sample DT2—HSp—49OlA48.
1050 1100 1150 1200 1250 1300
13:31 14:10 14:48 15:27 16:05 16:44
m/z
I-
D 1 0 —Anthracene
188
199
233
234
2b
270
A
2,4,5-T
1000
12:52
1350 SCAN
17:23 TIME
-------
Figure B—12.
EICPs for 2,4—D and 2,4,5—T method spike sample HS1—FSp—4901A48.
188
199
234 -
1000
12:52
m/z
D 1 0 —Anthracene
236
U I
A
270
1050
13:31
1100 1150 1200 1250 1300
14:10 14:48 15:27 16:05 16:44
1350 SCAN
17:23 TIME
-------
Figure B—13. EICPs for 2,4—D and 2,4,5—T method spike sample MS2—FSp—4901A48.
188
199
233
D 10 —Anthracene
234
236
270
1000
12:52
1050 1100 1150 1200 1250 1300
13:31 14:10 14:48 15:2? 16:05 16:44
1350 SCAN
17:23 TIME
-------
Figure B—14. EICPs for 2,4—D and 2,4,5—T method spike sample MS3—FSp—4901A48.
m/z
188
1 S9
D 10 -Anthrocene
270
1000
12:52
1050 1108 1150 1200 1250 1300
13:31 14:10 14:48 15:27 16:05
1350 SCAN
17:23 TIME
16:44
-------
APPENDIX C
EXTRACTED ION CURRENT PLOTS AND MASS SPECTRA FOR SAMPLES
ANALYZED FOR TETRACHIOROD I BENZOD IOXIN I SOMERS
C-i
-------
Figure C—i. EICPs for TCDD standard — 10 pg each.
1128
1134
1143 1149 1158
1106
1178 1187 1195
I — — — — — .;_ -I— - - --— - — —1
1125
1 ,2,3,4—TCDD
1185
1144 1158 1164 1174 1180
1151
1192 119?
— I ____ — — I— —— I
1122
1148 1169 1176 1183
s /
1200 SC t1
24:00 Tir1E
m/z
320 -
324 -
328
2,3, 7,8- 37 C1—TCDD
—— —I I — I — — I —1— ——..—T —I I
1
1100
22:00
1120 1140 1160 1180
22:24 22:48 23:12 23:36
-------
Figure C—2. EICPs for TCDD standard — 20 ng each.
320
1,2
1142
1139
11
1166
1
1100 1120 1140 1160 1180 1200 SC t4
22:00 22:24 22:48 23:12 23:36 24:00 TIME
m/z
,J’.
324
328
-------
Figure C-3. EICPs for TCDD standard — 100 pg each.
1114
7
1108 , —______._.._J1j J1 1 4 ____ 1L75_JL83 1188 1194
I —— — — —I —I —
1113
\
1147 1152 115? 1163 1171 1183 1188 1195
1 3 1108 1
—
I— — I — I — — I — — — I —
1 126
2,3,7 8 37 C 1 TCDD
1112 1117 / 1165 1176 1182 1196
I - — — I -
I—
—
I
1120
1140
1160
1180
1200
SCA 1
22:03 22:24
22:48
23:
12
23:36
24:00
TIME
m/z
1
,2,3,4—TCDD
1145
1153
1163
320
322
324
328
-------
Figure C—4. EICPs for sample A120—Hll—4901A48.
1130
1115
1110
—— - -I— —--_I • —I • I— ‘— ——I
1100
1120
1140
1160
1180
1200
SCAN
22:00
22:24
22:48
23:12
23:36
24:00
TIME
m/z
U i
—
I— — —
320
322
324
I——— —l ———I—
1122
—I—
— I
IPI
1108 ,r—- \ 1128 1150 11 - _____ 1183 J
1116
1169
—.-——-- ——------—-
—
-------
Figure C—5. EICPs for sample A122—Rll—4901A48.
1
1111
1120
22:24
1141
— — — — — —1- ‘ I —‘ — -t— — — 1 —
1146
1139
1174
1104 1109 1115 1128 _____
____ . ——I— — I —I—— . — I •— ———— —•1—
1174
1159
( \ 1128 1133 / 0
1109 1140
‘ 1146 115
1100
22:00
— ____ __ ______ .L —
1200 SCAN
24:00 TIME
1180
23:36
m/z
1
1175 1
320
,.I 4.
328
1110
I — I I • I
1151
-1 — — — — — -r — — ——
1140 1160
22:48 23:12
-------
Figure C—6. E ICPs for sample A124—Hl1--4901A48.
320
322
0
-.4
‘pa
1186
324 - 1111
/ - _—-/\ ‘ p
/ v ’ s
‘ — _ 1
— I • 1 __________
1126
1173
1105 1146 t_
328 / 1133 —‘ \ 1151
.___, •r - ._J /
I — I I I
1100 1120 1140 1160 1180 1200 SCAN
22: 130 22:24 22:48 23:12 23:36 24:00 TIME
1106
1
-------
Figure C—7. EICPs for sample A124—H21—4901A48.
—
I
I
1125
I
1 ?
I I
1100 1120 1140 1160 1180 1200 SCAN
22:00 22:24 22:48 23:12 23:36 24:00 TIME
1
1
320
I1
1156
. 1’)
‘JA .
328
-------
Figure C—8. EICPs for sample A124—H31—4901A48.
_______________________ — I I ——‘———————.t—
I I -
L J
“‘I
1’
i I
floe 1144 f l53_ 174 11861196
1100 1120 1140 1160 1180 1200 SCAN
22:00 22:24 22:48 23:12 23:36 24:00 TIME
320
322
1
I — 1157 1174
1121 1145 / -
1126 1136 / 1
324 1104 / \/\ /\\ / •\i / \ 1167 / 1186 1192
- ---
I—
-------
Figure C—9. EICPs for sample A124—Wll—4901A48.
— --
111 1 iL .12
1100 1120 1140 1160 1180
22:00 22:24 22:48 23:12 23:36
1200 SCAN
24:00 TIME
320
m/z
cD
322
——— I — — —I— ————• I ———•——— — I —I
1184
)hb
-------
Figure C-lO. EICPs for sample A124-FBk—4901A48.
— I — ‘ — —1——— — — ; -_ _- — — — — — —
m/z
1
320
322 -
1
1132 1193
1105 1119 \. 1138 1144 1160 116?
324
-r —i—
1181 1186
1100
22:00
/‘
1118 1123
1120
£_ • 4.
1140
22:42
1150
23: 12
1180
23:36
-r
1200 SCAN
24:00 TIME
-------
Figure C—li. RIC for sample Al24—Wll—4901A48.
100.0-
RIC
200
4:10
I I • I
877
400 600 800 1000
8:20 12:30 16:40 20:50
-------
Figure C—12. Mass spectrum for compound tentatively identif led as triphenyiphosphate.
7?. 1
2?’. 8
34.1 65.0
48.8 71.2
42.51 ilL... ii .
94. 1
112.2
83.1
i .Iii ..i i.i.,li. •. I
129. 1
18• 1 199.2
>. .
C -
4)’
C
>-
4-
C
4)
.1-
C
• I TV T T
40 60 80 100 120
170. 1
141.1
IIIi. .I.i.,i
215. 1
.. 1
.-I-T-VTV I I
140 160 180 200
I.
..1
m/z
.1
259.2
340
3.33.8
240 260
280
320
360
380
420 m/z
-------
Eigure C—13.
Library mass spectrum of triphenyiphosphate compared with sample peak.
I t l
.111 Ii l .
100
J.I thu , . ..i I
, . III I i. ,tt
- -
150 200
I .
250 300 350
SAMPLE
>‘
a,
.1-
C
>-
C
a,
.1-
C
SAMPLE MINUS LIBRARY
>-
a-
C -
a)
a-
C
50
rn/i
-------
APPENDIX D
CHROMATOGRANS AND MASS SPECTRA FOR SAMPLES ANALYZED FOR
PRIORITY POLLUTANTS DURING TilE SECOND SAMPLING PERIOD
D- 1
-------
Figure D—l. Priority pollutant composite standard — 20 ng.
>-
I —
tn
z
‘U
I-
z
icUo
16:40
sc
1 1 1 W
25 C )
-------
Figure D—2. Priority pollutant pesticide standard.
>-
I-
z -
u - I
I.-
z
T 1 LiiiJL
508 1000 1500 2008 SC t1
8:20 16:40 25:00 33:20 TINE
-------
Figure D—3. RIC for sample E506—Hll—4901A48.
PO—Anthracene
U)
z
z
Methylethylbenzene
.2, 3-Trlmeihylbeniene
Bs (2-butoxyethyl) phihalate
DEHP
OBP
I 5013
25:00
2000 SC(ItI
33:20 TIPIE
8:20
-------
Figure D—4. Mass spectrum for compound tentatively identified as a methylethylbenzene.
tIlej.
100.@ -
>-
I —
In
z o .o.
I L ,
I —
z
120.1
77.1 91.1
I ii 1 .... 1 ...Ji
WIZ 40 70 120
-------
Figure D—5. Mass spectrum of compound tentatively identified as l,2,3—trimethylbenzene.
I i0. 0
Z 50.0
C’
40.8
59.0 p55.1
Iv%/Z
78
80
SO
II
ItO 120
-------
Figure D—6.
Mass spectrum for compound tentatively identified as bis(2—butoxyethyl)phthalate.
ioo.o
$0.0
117.1
II
I 3,3. 2
wz
80
120 140
160 180
-------
Figure D—7. RIC for sample E506-H21—4901A48.
DEHP
5,
U,
z
z
Ilsooctyl pkthalate
Ilexadecanoic acid
1000
16:40 25:00
2000 SC dI
33:20 huE
8:20
-------
Figure D—8. Mass spectrum for compound tentatively identif led as 4—hydroxy—4—methyl—
2—pentanone.
Z 50.0-
59.0
lot. 1
41.Ci
38.31 98.1
iI.1— IJI 1
M/Z 40 50 60 70 80 90
-------
Figure D—9. Mass spectrum for compound tentatively identified as 2—hexanal.
100.0
50.0
Q
‘4
73.1
?. 1
M/Z
60 70
80
-------
Figure D—lO.
I —
Mass spectrum for compound tentatively Identified as hexadecanoic acid.
100.0
.0
‘9
2
2
2
wz 50
150
250
-------
Figure D—ll. Mass spectrum of compound tentatively identified as triphenylphosphate.
21 J. 1
233. I
220 240
260 280
300 320
£5.
57. 1
u i
t’)
>-
I-
( ‘ I
NVZ 40 60
100.0-
51.0
2
120
140
I n
z: 50.0
‘U
I .-
z
160
326. 1
200
-------
Figure D—12. Mass spectrum of compound tentatively identified as diisooctylphthalate.
112. I
143.0
>-
50.0- 57.1
83. 1
41.0
121.1
I I , ii
50 100 150
wz
250
-------
Figure D—13. RIC for sample E506—Rll—4901A48.
I ’M3.e•
2—Hexencil
Molecular Sulfur
>-
I —
— DIO—Anthrocene
U,
I— . z
uJ
I-
DEIIP
— 4 —Hydroxy—4-methyl-2-pentanone
2—Cyclohexen— 1-ol V 2 6 . o. 14-Tetramethyiheptodecane
5130 1000 1500
‘800 SCcni
8:20 16:10 25:00 33: i3 TilIE
-------
Figure D—14. Mass spectrum for compound tentatively identified as 4—hydroxy—4—methyl—
2—pen tanone.
too.ci-
Z50.O
59.1
41.1
39.O 56.1 . -‘ 98.1
II I .... ... _ LL _ .. . . _ j.I
W /Z 40 50 6 70 80 90 IOU
-------
Figure D—15.
Mass spectrum for compound tentatively identified as 2—hexanal.
1 O. 0
I — .
I /I
Z ‘ ci .(3
I
a’
0
97. 1
wz
40
60
-------
Figure D—16. Mass spectrum for compound tentatively identified as 2—cyclohexen—1—ol.
I€to. o
50.0
-0
51.0
cj
I3
-------
Figure D—17. Mass spectrum for compound tentatively identified as molecular sulfur.
tj:i
z 50.0
50
I I
150
250
-------
Figure D—18. Mass spectrum for compound tentatively identified as 2,6,10,14 —tetra—
methyiheptadecane.
43.1 71.2
5,
‘.0 -
Z 50.0
85.2
98.9
127. 2
141.2
r’LL !... 1 ’tL ,..‘Lr . .’
40 0 1Q 13 120 140 l 0 I s O
-------
Figure D—19.
I 8 .
RIC for sample E506—W1l—4901A48.
He xe no I
Octy ldpkeny lphosphate
Ii ,
z
U,
I . - .
z
010 -Anthracene
Ikooctyl phihalate
cjcj
8:20
I 5 1 i0
25:00
20130 sc i:
33:20 TIlIE
16:40
-------
Figure D—20.
Mass spectrum for compound tentatively identified as 2—hexenal.
I ’ . ,
>-
I-
U’
Z 50.8
U i
I —
z
.0
78.9
M/Z
40
cu
9’)
-------
Figure D-21.
Mass spectrum for compound tentatively identified as 1—ethenyloxybutane.
227.1
hl,i.1 i
243.1 25 .I
100.0
>-
I —
Z 50.0
M/Z
I00.0
>-
I-
U’
Z 50.0
Lu
I .-
z
40
120 140 169 180
271.2
2 I3
299.2
280
320
.35 . 2
340
WZ2 ’!10
240
300
3 I)
-------
Figure D—22. Mass spectrum for compound tentatively identified as octyldiphenyiphosphate.
100.0
>-
I-
Z
— 94.0
41.0
55.0 77.0
65. 1 83 1 170.2
. !jJ i !.. , csL!k . u: isk. . “.‘. , . , 1 . . . ±. . . :L .IJ ! .
‘ a) Wç/Z 40 60 20 100 120 140 160 180 200
ioo.o 25’.O
>-
I-
in
1 50.0
362.2
215.1 232.1 • 263.1 1
1 ± . . , 1 .. ,c . _
t4/Z 220 240 260 280 300 320 340
-------
Figure D—23. Mass spectrum for compound tentatively identified as diisooctyl phthalate.
I 4. . U
ioc .o•
>-
I —
50.0
43.8
57. 1
I 71.1 279.2 --
I . ±.1 .II I ‘ . 20 .l • • 26 .2 29.3
M/Z 50 I O U I 4) 200 L5U 301’
-------
Figure D—24.
•I 0 .
z
z
RIC for sample E508—H1l—4901A48.
10 -Anlhrocene
lert-Doclecanethiol
500
8:20
BBP
1000
lc:40
2000 s’: ii
33:20 huE
25:00
-------
Figure D-25. Mass spectrum for compound tentatively identified as tert—dodecanethiol.
100.0
a’
U)
z 50.0
z
.0
M/Z 40
€0
SO U
-------
Figure D—26. RIC for sample E508—H21—4901A48.
100.0-
- ilexodecanoic acid
In
z
ILl
I—
z
DiO-Anlhrocene
(ert-Dodeconethiol
Nonadecanoic cicici
j— 1—EIhyi—2—methyIb nzene
/ DEHP
- f 1 1.2,3-Trimethylbenzene
-
500 1000 1500 2000 rdi
16:40 25:00 33:20 huE
-------
Figure D—27.
Mass spectrum for compound tentatively identif led as tert—dodecanethiol.
IOC1.O
1
t )
0,
60
70
tJ
-------
Figure D—28. Mass spectrum for compound tentatively Identified as l—ethyl—2—methylbenzene.
I@0.0
>-
I —
50.0
0
51.
40
60
80
90
110 12’)
-------
Figure D—29. Mass spectrum for compound tentatively Identif led as l,2,3—trimethylbenzene.
100.
>-
I-
50.0
1
0
1
wz
80
II
ItO
120
-------
Figure D—30. Mass spectrum for compound tentatively identified as hexadecanoic acid.
100. ci -
43.1
68.0
>-
In
Z 50.0-
U i
129.2 256.2
85 2
157.2
185.2
143.1 I
I 199.2 227.2
L . 1 2 I .
I I —i I..J I .I.I.I•—• T•
M/Z 100 150 200 250
-------
Figure D—31.
Mass spectrum for compound tentatively Identif led as nonadecanoic acid.
I
ij
5cL@
L
M/Z 50
ISO
-------
Figure D—32. RIC for sample E514—1-Ll1—4901A48.
ieo.o-
D 10-An Ibracene
5,
(4
2 —Hexenol
DE HP
1 - r - . I - .JLJ U I I I I I U
500 1000 15 ’JO 2000 ECAII
0:20 16:40 25:00 33:20 TitlE
-------
Figure D—33.
t€iO.Ci
In
z
z
Mass spectrum for compound tentatively identified as 2—hexenal.
M/Z 40
6 )
fl
90
-------
Figure D—34. RIC for sample E516—Hhl—4901A48.
Totuene
DlO-An hrocene
Z 2-Hexenol
4-tlydroxy-4-melhyl -2-pentonone DE
SBP
I k.
I I •
500 1000 15ñ0 20i:io si:hll
8:20 16:40 25:00 33:20 TitlE
-------
Figure D—35. Mass spectrum for compound tentatively identified as toluene.
I 013.0
50.0
0 \
3 .9
M/Z
60
70 80 90
-------
Figure D—36. Mass spectrum of compound tentatively identif led as 4-hydroxy—4—
methyl—2—pentanone.
100.0
Lfl
Z 50.0-
59.1
101.1
41.1
3.2
1 J 1 . _ , iii I
M/Z 40 50 60 70 80 90 100
-------
Mass spectrum for compound tentatively identified s 2—hexenal.
Figure D-37.
5:J
0 ,
In
z
z
I
73.2
M/Z
40
60
-------
Figure D—38. RIC for sample E520—Hll—4901A48.
Toluene
2-Hexenol
‘ .0
Z Di 0 -Anthracene
z
t-Cyc ohexen-I--oI
DE HP
i BB [
500 1000 1500 2000 S(0
8:20 I :40 25:00 3 3:20 TIME
-------
FIgure 39.
1 ø.O
5o.o
Mass spectrum or compound tentatively i’dent fied as toluene.
.9
M/Z 40
60
‘0
-------
Figure D—40. Mass spectrum of compound tentatively identif led as 2—hexenal.
1UO.O
2
-N
U ,
z
U i
I —
z
I
M/Z
40
F.fl
80
90
II
-------
Figure D—41.
Mass spectrum for compound tentatively identified as 1—cyclohexen—1—ol.
I CtO. 0
50.0
51.1
68.1
.0
55.0
2
53. I
57. I
65.0
63. 1
M/Z
40
60
.3’)
-------
Figure D—42.
RIC for sample E520—Rl1—4901A48.
‘nfl.
>-
I —
z
‘U
I-
z
1. I. I—Trirluoro-2.4-hepianedione
Ocladecai
‘win
8:20
1500
25:00
Uoci LHtI
33:20 TIME
16 :40
-------
Figure D—43.
Mass spectrum for compound tentatively identified as 3,3’—oxybis—l—propene.
5,
1 .iU. U
wz
70
.3’)
-------
Figure D—44. Mass spectra for compound tentatively identified as octadecane.
100.0
43.0
71.1
5o.0
85. 1
112.9
12 .2 11.2 155.2 • • 9.2
M/Z I ‘30 1 5 13 200 250
-------
Figure D—45.
U
5 3.o
Mass spectra for compound tentatively identified as 1,1,1—trifluoro—
2, 4—heptanedione.
?1. I
85.1
Ii
99.2
I
.2
wz
1’
150
-------
Figure D—46. Mass spectrum for compound tentatively identified as heptadecane.
o
>-
I-
Z 50.
0
9 :’
L
M/Z 50
150
-------
Figure D—47. Mass spectrum for compound tentatively identif led as henelcosane.
100.0
- ‘S
z
U i
z
Z .4
M/Z 50
250
-------
Figure D—48. Mass spectrum for compound tentatively identified as 17—pentatriacontene.
100.0 57.1
43.13
‘C 71.1
‘I ,
Z 50.0 -
w
83.1 97.2
111.1
125.2
liii i 3 1 153.2 163.3
L- - 1 [ . . . . . ,• I I .. . .. . . iJ L .1, LI. i.., .
40 io 10’) I . u 14u IbJ
-------
Figure D—49. RIC for sample D418—H11—4901A48.
D i —Anthracene
I . ; ’ >-
In
2 tert-Dodeconeth lol
DEHP
— 4-Hydroxy—4-methyl-2-pentonone
BBP
I
I i j - , L 1
5 1 )13 15 ( 10 2In3t) S( III
8:2 ’ ) 1 :40 25:00 33:0 TItlE
-------
Figure D—50. Mass spectrum for compound tentatively identified as 4—hydroxy—
4—methyl—2—pentanone.
42.9
>-
50.0-
59.0
1.0
38.91 . o - i 98.1
— •.••
M/Z 4’) 50 6’) ?0 - 90 I0 ’3
-------
Figure D—51. Mass spectrum for compound tentatively identified as tert—dodecanethiol.
l i x ’. c i
>-
40
70
90
-------
Figure D—52. RIC for sample D418—H21—4901A48.
1’X . Ci-
icr I - I ode canet h lo I
>-
I.-
z
z
— D 10 -Anthrocene
—4-Hydroxy-4—meihy l-2-pentanone
r 2-Cyctohexen— 1-01
/ 2 -Cyclohexen-I-one
/ f
( BBP
JL L÷Jf -, 4
I C’O ) I 5’3U 2OU’ S i: tl
8:20 IE:4 0 25:00 33:0 TitlE
-------
Figure D—53. Mass spectrum for compound tentatively Identified as 4—hydroxy—
4-me thyl-2-pentanone.
1 O. ‘3
. /1
SE. 1
M/Z
40
50
70
90
-------
Figure D—54. Mass spectrum for compound tentatively identified as tert—dodecanethiol.
I(I(I.0’
5:J
Lfl
50.0
z
0
.0
M /Z
6 ’) 70
90
-------
Mass spectrum for compound tentatively identified as 2—cyclohexene—l—ol.
Figure D—55.
ICICi. 0
>-
C ’
67.1
M/Z
60
-------
Figure D—56.
Mass spectrum for compound tentatively identif led as 2—cyclohexen--l—one.
100.0
In
Z 5 3.O
z
U i
.0
96.0
M/Z
40
-------
Figure D—57. Mass spectrum for compound tentatively identified as 2—cyclohexen--1—ol.
O 3. 0
(J1
50.0
“3. I
68, 1
55 0
1
53.’!
5 1.0
57.0
I
ES. 1
E3.0 Ii
M/Z
40
50
70
30
-------
Figure D—58. RIC for sample D420—Hll—4901A48.
1 J.Ci-
D1O—Anlhrocene
>-
‘ - Il
z
Toluene
5i )0 I1.iC, 1500 2000 SC I
3:20 11:40 25: 0 ’ ) 33: 0 TI LE
-------
Figure D—59. Mass spectrum of compound tentatively identified as toluene.
100.0
>-
I —
0 ’
Q
tvVZ
40
E.43
go
-------
Figure D—60. RIC for sample D420—H21—4901A48.
1LJL L .
5 : ,
0 \
I - ’
z
z
thioI
-Hyrdoxy-4-methyl —2--pentonone
DEI-tP
15C’C’ 2000 S At
2 5:fl0 33:20 TItlE
-------
Figure D—61. Mass spectrum for compound tentatively identified as 4—hydroxy—4—
methyl—2—pentanone.
43.0
In
a’ Z r 1
U i , - ,.
z
59. 1
10 1.1
41.1
. tII. 1,.. . ... . I IiL rr T _ ’,r 1 I
M/Z 4u 50 t0 70 80 100
-------
Mass spectrum for compound tentatively identified as tert—dodecanethiol.
Figure D—62.
1C’C .U
5:,
C ’
>-
I-
5O.U
M/Z
40
60
80 9t )
-------
Figure D—63. RIC for sample D421—Bll—4901A48.
2— Flexenol
U
Toluene
D1O-Anthrocene
2—Cyclohexen- 1-01
DE IIP
BBP
-r — i -‘
50’ ) 1000 15110 20’u3 9:iiII
:3:20 16:40 25:00 33:20 TIME
-------
Figure D—64. Mass spectrum of compound tentatively identified as toluene.
I M3.
9
M/Z
40
60
qc I
-------
Figure D—65. Mass spectrum of compound tentatively identified as 2—hexenal.
1CU).0
50.0
a’
C’
57.0
wz
40
70
90
II
-------
Mass spectrum of compound tentatively identified as 2—cyclohexen—1—ol.
Figure D—66.
I O 3. 0
0
5:’
0 ’
Z 50.0
w
I-
z
51.0
tvVZ
41-i
70
80
-------
Figure D—67.
RIC for field blank sample D420—FBK—4901A48.
toO.
D 0 —Anthracene
0 ’
>-
I - .
z
canethIoI
DEHP
SCAN
T hE
25: C
-------
Figure D—68.
Mass spectrum for compound tentatively identified as tert—dodecanethiol.
103.0
I n I )
C ’
.0
69. I
79. ’
7 ? .l
“V IZ
00
-------
Figure D—69. RIC for field blank sample E514—FBK—4901A48.
—a Di -AnIhroceoe
z
U i
I-
z
DEHP
500 1000 1500 2000 SC II
3:20 1E:40 25:00 33:20 huE
-------
Figure D—70. RIC for field spike sample A124—FSp—4901A48.
DIO—Anthracene
D 8 — Nophiholene
>-
z.
LU
I-
z
-Do-1etrochIorobphenyI
\ DI2-Chry5ene
13 C-PentochIorophenoL \ \
D eldr n—.., \
1 L - _____ LL
500 1000 1500 2000 SCAI
8:20 1E:40 25:00 3:2i TitlE
-------
Figure D—71.
RIC for field spike sample D420—FSp—4901A48.
D, —Anthracene
I O.
>-
I.-
In
z
U i
I—
z
D8—Naphlhalene
‘ 3 C-Pentochlorophenol
—D 12 -Chrysene
500
S: 20
1000
16:40
1500 000 C’itI
25:1)0 33:20 TitlE
-------
Figure D—72. RIC for field spike sample E514-FSp—4901A48.
10 -Anthracene
D - Naphiholene
>-
I —
tn
z
w
z
13 C—Pentachlorophenol
1000 1500
25:00
Sc itil
3I :0 TitlE
500
8:20
-------
Figure D—73. RIC for priority pollutant hood spike sample PP1—HSp—4901A48.
5 :,
>-
I - .
In
z
lOC ) 15’iO
1 :4I 25:00
2000 SC II
33:20 TIME
8:20
-------
Figure D—74. RIC for priority pollutant hood spike sample PP2—HSp—49OlA48.
I
>-
‘ -4 I-
(‘I
z
U i
I-
z
10 —Anthracene
I 5€$3
25: I)
5 1J0 I’3U
:2CI 16:40
SI ,RtI
33:20 TIIIE
-------
Figure D-75.
RIC for priority pollutant method spike sample MS1—FSp—4901A48.
>-
I —
z
‘U
z
- DiO—Anthracene
1000
16:40 25:08
2000 si:, ’t
33:20 TitlE
3:2 ’ )
-------
Figure D—76.
RIC for priority pollutant method spike sample MS2—Hsp—4901A48.
D i Q -Anthrocene
500
8:20
1
-I
I5CJ 21) SCAH
25:C 33:2. titlE
100.0-
>-
I-
z-
I
-
.0
-------
Figure D—77. RIC for priority pollutant method spike sample MS3—FSp—4901A48.
>-
I —
z
uJ
I-
z
20
L5C )
25:00
2000 Sti tII
33:2’) TitlE
l :4CI
-------
APPENDIX E
EXTRACTED ION CURRENT PLOTS FOR SAMPLES ANALYZED FOR
HERBICIDES DURING THE SECOND SAMPLING PERIOD
E—1
-------
Figure E—1. EICPs for methylated 2,4—D and 2,4,5—1 standard — 1 ng each.
M/Z
I80
‘99
233
234
238
268
270
AN
TitlE
1ö31
[ \D)onraene
txl
-------
Figure E—2. EICPs for sample E502—R11—4901A48.
M/Z 1038
- Dp 0 —An hrocene
188 -
l 0l -i 1 - 4 —r 93 t —
1002
• F • •
• • • • • • • • •
234
I I I I J I I I I I I I I I I J
1077
2361 1______________________________________
2681 912 _____________________________________
270
I I I I I I I I I I I I I I I
803 950 1080 1Q50 1103 SCAtI
13:47 14:33 15:19 16:05 16:51 111W
-------
Figure E—3.
EICPs for sample E502—Hll—4901A48.
I • I • • I
I • • I • • I • • I
‘0 o
16:05
188
233
is
23 1 -
236
• I • • I • • • • l•
268
270
980
13:47
I - - - — I
850 1000
14:33 15:19
itco SCAN
16:51 TUIE
-------
Figure E—4. EICPs for sample E502—H21—4901A48.
tv%/Z
188
*99
J\D o —Anlhrocene
233
231
236
262
2701
9C0 *099
13:17 15:19
U — — — U —
*002
*095
u o SCAN
*6:5* TuE
950
*4:33
*650
*6:05
-------
Figure E—5.
EICPs for sample E510—H1l—4901A48.
M/Z
188
199
233
I • I • I •
234 -
F 1
• I • • I • I •
236
268
270 -
I • I • • I
I • • • I • • I
1680
IS: 19
D 10 -Anlhracene
I • — I • •— • I • • I
1 1C3 SCAN
18:5! TitlE
900
13:47
90
14:33
1050
16:05
-------
Figure E—6.
EICPs for sample E510—Bl1—4901A48.
M/Z
lee
199
n3
Ii
r h
234
236
I . I . I
270
I I I I •1
50
11:3)
1600
15:19
900
13:47
I - — - I
1050 llt 0 StAll
16:05 16:51 TIIIE
-------
Figure E—7. EICPs for field blank sample E514—FBk—4901A48.
M/z 1049
189 /\D ,O_An hracene
9J8 - 9 0 973 1003 1029 1Q! l0 I “-_..,.. _IV3 1Q89
1013
233
I 1 • I • I • • • • I • • • •
234
• I I I I I I I J I I I I
236
I I I I I I I I I I ‘
260
I I I 1 I • I I I
210
I I I • I I I ( I I I
9C3 850 1080 1050 1103 SCAN
13:47 14:33 15:19 16:05 16:51 TitlE
-------
Figure E—8. EICPs for field blank sample D420—FBk—4901A48.
M/Z t 15
188 1 /\0 10 _Anthracene
I • • . •
1077
233
I I I I I I I I I I I
234
I — I I • I I
236
I I I I I I I I I I I I I I I I I
268
I I I I I I I I I
270
I I I I I I I I I J I I I I u • I
960 950 1050 IICO StAll
13:47 14:33 15:19 16:05 16:51 TI1IE
-------
Figure E—9. EICPs for hood spike sample DT1—HSp—4901A48.
tv%IZ
lBS
‘99
233
234
236
263
270
TitlE
o34
1 t racene
t;i
0
:05
-------
Figure E—lO.
EICPs for hood spike sample DT2—HSp—4901A48.
tvVz
‘Be
‘99
233
234
236
269
270 -
903
13:47
I • I • . I ’ •
4
I\
I050
16:05
l,’4
950
‘4333
15:19
1103 SCAfl
16:51 TitlE
-------
Figure E—ll.
EICPs for method spike sample tlSl—FSp—4901A48.
r i
wz
188
‘99
233
234
236
268
270
f 4T
I • I —
icso
,6 0
I6 05
900
‘3:47
- I
950 1090
11:33 1519
itbo SCAN
16:51 TItlE
-------
r i
Figure E—12.
EICPs for method spike sample MS2—FSp—4901A48.
1036
f\\DIo —Anthrocerie
I9 J
wz -
188
199
233 -
234 -
236.
269
270 -
I . . I I
I
1
-t I
T
I
.
I
.
I
.
I
.
1I’
I J
,
I
9 A
.i” ,
]
I
.
.
L1I
I I
.
I
I — I I I
I94
1019
I I 2 i 1.5T.
1050
16:05
I ICO SCAH
16:51 TitlE
900
1147
I I
950 lc80
14:33 15:19
-------
Figure E—13. EIPCs for method spike sample 14S3—FSp—4901A48.
WZ Ø34
1 /\ iOnthracene
‘99
233
234
236
269
270
SCAN
($:5t huE
-------
APPENDLX F
EXTRACTED ION CURRENT PLOTS FOR S ANPLES ANALYZED FOR
TETRACHLORODIBENZODIOXIN ISOMERS DURING TEE
SECOND SAMPLING PERIOD
F—i
-------
Figure F—i.
EICPs for TCDD standard — iO pg each.
14 /Z
328
322
324
328
I .2.34-TCDD
‘ - x l
2, 3,7,8— 37 C1--TCDD
1
1288
17:42
1258 1388 1358 1488
18:26 19:11 19:55 20:39
1458 1588 SCAt ]
21:23 22:88 TIME
-------
Figure F—2.
EICPs for TCDD standard — 50 pg each.
M/Z
320
322
324
328
1200
17:42
I I
1 .2 ,3 ,4- ICOD
U )
2, 3, 7, 8- 37 C I— ICDD
1250 1300 1350 1400 1458
18:26 19:11 19:55 20:39 21:23
1500 SCAN
22:08 T itlE
-------
Figure F—3.
EICPs for TCDD standard — 100 pg each.
M/Z
320
3n -
324
328
1200
17:42
1295
I?
I, 2. 3. 4-TCDD
1317
A
I I I
111111 I I • I I J I I I I I
1363 1381
2, 3. 7, 8- 37 C I-TCDD
1250
18:26
1358
19:55
1480
20:39
1450
21:23
1580 SCAN
22:08 TIME
1388
19:11
-------
Figure F—4. EICPs for sample A120—H1l—4901A48.
M/Z
320 -
I I V I J I I I I I I I I I I I V I I I I I J
322
I I I I I I I I I J I I I I J I I I I I I I I J I I I I J
U i
324
I I I I J V I I I I I I I I I I IIhIhII, 1 1 1
328 -
I I I I I I I I I I I I I I I J I I I I I I I I I
12 O 1250 1300 1358 1480 1450 1508 SCAH
17:42 18:26 19:11 19:55 20:39 21:23 22:08 TitlE
-------
Figure F—S. EICPs for sample A122—Rl1—4901A48.
14/Z
320
322
324
328
1508 SCAN
22:08 TIME
-------
Figure F—6. EICPs for sample A124—111l—4901A48.
1:
PvVZ
320
322
324
328
-4
1200
17:42
1400
20:39
1450
21:23
1500 scatI
22:03 TIME
18:26
-------
Figure F—7. EICPs for sample A124—H21—4901A48.
1233
1218
£
1473 ( 1 14/Ill
1382
..• 4!\ 4k J\A AAA’ 1 I\]lA
1404 1428
1283 1385 1329 1346 14
1252 1268
-J I
1200
17:42
wz
320 -
322
324
328 -
I—
I 4 9
1 1431
I I’ 6 ,j
--I ——
1479
A J i
1216
— — — .a a — I — _ I — 1
1250 1380
18:26 19:11
—-I
—t
1350 1480
19:55 28:39
1450 1588 SC4 H
21:23 22:08 TIME
-------
Figure F—8. EICP for sample A124—H31-4901A48.
P
¼0
M/Z
320
322 -
324
328
1491
1200 1250
17:42 18:26
1350 1400 1450
19:55 20:39 21:23
SCAN
22:88 T itlE
-------
Figure F—9.
EICP5 for sample Al24-Wl1—4901A48.
1’
0
tvVZ
320
322
324
328
I .
1290 1250 1309
17:42 18:26 19:11
1350
19:55
SCAN
22:88 111€
20:39
21:23
-------
Figure F—b. EICPs for field blank sample Al24—FBk—49OlA48.
wz
32
I I I I II II IpI I I I I I I I I I I I - ——
322 -
• I I I I I I I I I I I • I I I I I I I I I I
‘•Il
324
I I I I 1 I I I I I I I I I 1111111111 I
328
I I I I I I I I I I I I I I I I I I I I I I 1
1288 1258 1388 1358 1400 1450 1508 SCAM
17:42 18:26 19:11 19:55 28:39 21:23 22:08 TIME
-------
TABLE 10. PRIORITY POLLUTANT COIIPOUND
RECOVERIES - HOOD
SPI S
Percent recovery
Hood spike
Hood spike
Average
No. 1
Compound Set 1 Set 2
No. 2
recovery
Set 1 Set 2
Set I Set 2
bis(2-Chloroethyl)ether 0 7 0 4 0 6
o-Chlorophenol 0 11 0 16 0 14
Phenol 0 20 0 25 0 23
m-Dichlorobenzene 4 2 5 6 4 4
2-Dichlorobenzene 4 2 5 4 4 3
o-Dichlorobenzene 3 4 5 7 4 6
bis(2-Chloroisopropyl)ether 0 5 0 < 1 0 3
Hexachioroethane 4 2 7 2 5 2
N-Nitroso-di-N-propylamine 0 20 0 17 0 19
Nitrobenzene 3 18 3 17 3 17
Isophorone 13 31 19 38 16 35
o-Nitrophenol 0 21 0 26 0 24
2,4-Dimethylphenol 3 17 4 29 3 23
bis(2 -Chloroethoxy)metharie 9 29 14 34 11 32
1,2,4-Trichlorobenzene 6 16 10 18 8 17
2,4-Dichiorophenol 6 32 0 41 3 37
Naphthalene 7 22 11 23 9 22
Hexachiorobutadjene 4 13 10 13 7 13
E-Chloro-rn—cresol 10 47 23 57 16 52
Hexachiorocyclopentadiene 3 15 6 18 4 16
Trichiorophenol 14 47 30 58 22 52
2-Chloronaphthalene 10 44 17 51 13 48
Acenaphthylene 14 52 24 63 19 57
Dimethylphthalate 25 58 40 70 32 64
2, 6 -Dinitrotoluene 22 52 41 60 31 56
Acenaphthene 13 54 25 63 18 59
2,4-Dinitrophenol 21 29 38 35 29 32
2,4-Dinitrotoluene 29 58 47 71 38 64
-Nitropheno1 4 32 7 37 5 35
Fluorene 23 62 40 74 31 68
4-Chiorophenyl phenyl ether 24 62 43 71 33 66
N-Nitroso-diphenylainine 29 59 49 71 39 65
Diethylphthalate 31 64 52 76 41 60
4 , 6 -Dinitro—o-cresol 27 47 53 51 40 49
1,2-Diphenyihydrazine 26 46 51 49 38 47
4-Bromophenyl-phenyl ether 26 63 47 75 37 69
Hexachlorobenzene 29 66 52 76 40 71
Pentachlorophenol 16 52 30 61 23 56
Phenanthrene 30 67 53 76 41 72
Di-n-butylphthalate 37 72 64 80 50 76
Fluoranthene 36 71 65 79 50 75
(continued)
26
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