United States
Environmental Protection
Agency
Office of Mobile Source Air Pollution Control
Emission Control Technology Division
2565 Plymouth Road
Ann Arbor, Michigan 48105
EPA 460/3-82-008
August 1982
&EPA
Air
Filter Extraction Procedures and
Results for Various EPA/ECTD
Particulate Samples
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EPA 460/3-82-008
Filter Extraction Procedures and Results
for Various EPA/ECTD Particulate Samples
by
Mary Ann Warner
Southwest Research Institute
6220 Culebra Road
San Antonio, Texas 78284
Contract No. 68-03-2884
Task Specification 9
EPA Project Officer: Robert J. Garbe
Task Technical Officer: Thomas M. Baines
Prepared for
ENVIRONMENTAL PROTECTION AGENCY
Office of Mobile Source Air Pollution Control
Emission Control Technology Division
2565 Plymouth Road
Ann Arbor, Michigan 48105
August 1982
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This report is issued by the Environmental Protection Agency to report
technical data of interest to a limited number of readers. Copies are
available free of charge to Federal employees, current contractors and
grantees, and nonprofit organizations - in limited quantities - from
the Library Services Office, Environmental Protection Agency,
2565 Plymouth Road, Ann Arbor, Michigan 48105.
This report was furnished to the Environmental Protection Agency by
Southwest Research Institute, 6220 Culebra Road, San Antonio, Texas,
in fullfillment of Task Specification 9 of Contract No. 68-03-2884.
The contents of this report are reproduced herein as received from
Southwest Research Institute. The opinions, findings, and conclusions
expressed are those of the author and not necessarily those of the
Environmental Protection Agency- Mention of company or product names
is not to be considered as an endorsement by the Environmental Protec-
tion Agency.
Publication No. 460/3-82-008
11
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FOREWORD
This project was conducted for the U.S. Environmental Protection Agency
by the Department of Emissions Research, Southwest Research Institute. The
work was carried out between April 1981 and June 1982 under EPA Contract No.
68-03-2884, Task Specification Number 9. It was identified within South-
west Research Institute as Project 05-5830-009. The scope of work defined
by EPA is located in Appendix A of this report. The EPA Project Officer
was Mr. Robert J. Garbe, and the Task Technical Officer was Mr. Thomas M.
Baines, both of the Characterization and Technical Applications Branch,
Emission Control Technology Division, Environmental Protection Agency,
2565 Plymouth Road, Ann Arbor, Michigan. The Southwest Research Institute
Project Manager was Charles T. Hare, and the Project Leader and Principal
Investigator was Mary Ann Warner.
111
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ABSTRACT
This report describes filter extractions and benzo(a)pyrene analyses
performed for the Emission Control Technology Division of the Environmental
Protection Agency. Pallflex filters measuring 20x20 inches were soxhlet-
extracted in methylene chloride to remove organic soluble material. Some
of the extracts were analyzed for benzo(a)pyrene, and some underwent Ames
bioassay. Percent extractables and benzo(a)pyrene concentrations in the
extracts are reported. Part of the effort also went into splitting and
recombining extracts with the necessary extra drying and weighing steps.
IV
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TABLE OF CONTENTS
Page
FOREWORD iii
ABSTRACT iv
LIST OF TABLES vi
I. INTRODUCTION 1
II. ANALYTICAL PROCEDURES AND INSTRUMENTATION 2
III. SUMMARY OF RESULTS 10
APPENDIX
A. Scope of Work, Contract 68-03-2884, Task Specification 9
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LIST OF TABLES
Table Page
1 Extraction Data for Filters Received from EPA 11
2 Extraction Data for Volvo TD100A (Dual Fuel) and
Volvo TD100C (Diesel) Filters 12
3 Extraction Data for Volkswagen Rabbit Diesel Filters
Collected under an Alternate Fuel Study 15
4 Extraction Data for Two Ford Escorts and Two VW
Rabbits using Several Combinations of Fuel and
Catalysts 16
5 Extraction Data for a Mack EM6-300 Heavy-Duty
Diesel Engine using Alternate Fuels 17
VI
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I. INTRODUCTION
The purpose of work directive number 9 of EPA Contract No. 68-03-2884
was to perform soxhlet extractions and BaP analyses on diesel particulate
samples collected from various sources. Selected samples were also to be
sent to Microbiological Associates (formerly EG&G Mason Research Institute)
for Ames bioassay. The initial scope of work (found in Appendix A) called
for the extraction of 239 filters, analysis of 49 samples for benzo(a)pyrene,
and the shipment of 82 extracts for Ames bioassay. This was altered during
the program at the request of the Project Officer. A total of 146 filters
were extracted (37 from EPA, 109 from Southwest Research Institute's
Emissions Laboratory), 21 extracts were analyzed for benzo(a)pyrene, and
17 were shipped for Ames bioassay. As a substitution, extra sample work-
up involving the combination and splitting of extracts was performed.
Additionally, extracts from 52 pre-extracted filters were combined to form
aggregate samples. Tables 1 through 5 in Section III describe the treatment
of each, extract or filter during sample processing.
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II. ANALYTICAL PROCEDURES AND INSTRUMENTATION
Particulate-loaded filters were extracted in a soxhlet apparatus with
methylene chloride as the solvent. The extracts were filtered, concentrated
under vacuum, transferred to preweighed glass vials, and weighed. Whenever
possible, two filters were extracted in one soxhlet. Some extracts were
also combined to form composite samples, and subsequently split up as
required. Several extracts were analyzed for the presence of benzo(a)pyrene
using a high pressure liquid chromatograph. The method closely follows
the analytical procedure developed by General Motors Research Laboratories
for measuring benzo(a)pyrene in organic extracts of automotive exhaust.(1)
The analytical system consists of a Perkin-Elmer Series 2 Liquid Chromato-
graph, Model 650 Fluorescence Detector, and Model 150B Xenon Power Supply.
The detection limit of this system is 0.5 yg benzo(a)pyrene per filter.
Analytical Procedure for Solvent Extraction of Particulate Filters
LARGE SOXHLET EXTRACTION OF ORGANIC SOLUBLES FROM 20x20 PALLFLEX FILTERS
(Condensed Procedure)
Check extraction schedule and obtain filters.
Put solvent and Teflon boiling chips in pot: 400 mSL measured with graduated
cylinder.
Fold filter and place in soxhlet.
Label boiling pot with filter and test number, solvent, and extraction date.
Hook-up hoses to condenser, turn on water.
Turn on heaters to large soxhlets to 100%.
Swarin, S.J., "Liquid Chromatographic Determination of Benzo(a)pyrene
in Diesel Exhaust Particulate: Verification of the Collection and
Analytical Methods," General Motors Research Laboratories report
GMR-3127 prepared for presentation to the Fourth International Sym-
posium on Polynuclear Aromatic Hydrocarbons, Columbus", Ohio, October 4,
1979, and for publication in "Polynuclear Aromatic Hydrocarbons,"
Raven Press, 1979.
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Record filter data in log book.
Extract for 8 hours - Extractions started by 9 a.m. are completed at 5 p.m.
Filter extracts of 20x20 filters through 47 mm Pallflex filters.
Roto evaporate extract to about 20 m£.
Transfer extract to 30 mH beaker.
Blow down solvent in desiccator to 2-3 mH.
Transfer extract to preweighed sample vial. NOTE: SAMPLE VIALS SHOULD NOT
BE TOUCHED WITH BARE HANDS; FINGERPRINTS MAY CAUSE WEIGHING ERRORS. USE
TWEEZERS OR WEAR GLOVES WHEN HANDLING.
Dry extract in desiccator.
Weigh vial with cap on.
Record weight in log book.
Calculate percent extractables.
Make a copy of data in log book and give to Mary Ann Warner.
The organic solubles extraction procedure is a very precise method
requiring careful, repetitive lab technique. It is necessary in this
involved procedure that each step is carried out in a precise and repro-
ducible fashion. If a spillage or other accident occurs while handling a
sample, the problem should be recorded in the log book. In this way unex-
plained irregularities in the results can be traced to the extraction
process.
Special attention also needs to be directed to the bookkeeping required
for the extractions. An extraction schedule is posted weekly designating
which filters are to be extracted. Each soxhlet needs to be labeled with
filter and test number, solvent and extraction date. When the extractions
are finished, the beaker used in the blowdown step should also be labeled
with filter and test number, solvent and extraction date. The weighed
sample bottles should be numbered and this number recorded in the log book.
After the final weighing, the sample vial should also be labeled. On a
daily basis the filters extracted need to be recorded in the log book.
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The purpose of the soxhlet extraction is to remove organic sellable
material from exhaust particulate collected on filters. Several safety
precautions need to be taken when working with diesel exhaust products.
The concentrated exhaust products should be treated as potentially hazardous
compounds. The following safety precautions are recommended:
1. The soxhlets are set up under a vented hood in case vapors escape
from the extractors. Any other step which involves open containers of
solvent (sample transfer, filtration, etc.) should be carried out under the
hood. Avoid breathing solvent vapors. When the desiccator is opened, a
high concentration of solvent vapor is usually emitted. In this case, the
door to the desiccator should be opened wide and the vapors allowed to
vent into the hood. When the vapor concentration has decreased, work can
be continued with the desiccator.
2. Where reasonable, protective clothing should be worn (lab coat
and plastic gloves). However, plastic gloves should not be allowed to con-
tact the particulate or organic extractables.
3. If extract spills on the skin, immediately wash off with soap and
water. Otherwise, wash hands thoroughly after working with the extracts
and before eating or drinking.
LIST OF EQUIPMENT
Extraction
soxhlet - 55/50 top joint, 24/40 bottom joint
condenser - 55/50 joint
500 m£ flat bottomed boiling pot - 24/40 joint
six position heating mantle
Teflon boiling chips
drying tubes filled with molecular sieve and silica gel
Filtration
Millipore all glass filtration apparatus:
300 mJJ, cup
vacuum adapter with glass frit - 40/35 joint
1 H filter flask - 40/35 joint
clamp
vacuum source
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Concentration
Buchler flash evaporator with cold finger condenser
1 £ round bottom flask
steam bath
hot plate
vacuum source
Drying
desiccator box
gas manifold with curved syringe needles
dry zero nitrogen
aluminum blocks
weighing vials
Accessories
glass petri plates
Teflon squeeze bottles with solvents
transfer pipets plus rubber bulbs
beakers
large and small tweezers
vacuum grease (for condenser hose only)
Chemicals
Extraction
Burdick and Jackson glass distilled cyclohexane, methylene chloride,
acetonitrile
Concentration
isopropyl alcohol, dry ice
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WASHING PROCEDURES
Glassware
See attached procedure.
Teflon Boiling Chips^
Used boiling chips are washed with methylene chloride in the sonic
bath. They are placed in a petri dish, covered with methylene chloride
and sonicated for about 15 min. The methylene chloride is discarded and
fresh solvent is added. The chips are again sonicated for 15 min. The
solvent is discarded. If particulate remains on the chips, they are
rinsed with methylene chloride until clean. The clean chips are dried
under the hood and placed back in the bottle.
Weighing Vial
New vials are rinsed in methylene chloride, air dried and stored in
trays. Used bottles are solvent rinsed and washed as glassware. Before
using again they are rinsed in CH2C12, air dried and stored in trays.
Once the weighing vials have been cleaned do not touch with hands as
fingerprints will add weight to the vials. Wear gloves or use tongs
when handling vials.
LARGE SOXHLET EXTRACTION PROCEDURE
Extraction of 20x20" Pallflex Filters
1. Several (8-10) Teflon boiling chips are dropped into a round,
500 mJi, flat bottomed flask. The desired Burdick and Jackson glass distilled
solvent is added to the flask (400 m£ of cyclohexane, methylene chloride or
acetonitrile) using a 500 mf, graduated cylinder. 20x20 filters can be found
in Tedlar bags in the freezer in the shop. Remove the needed filters and
cross through the corresponding filter numbers on the bag. Purge the bag
with dry zero nitrogen (same cylinder used to dry organic extracts in the
chem lab) and then heat seal the bag. Place bag back in the freezer and
lock the freezer. The person weighing filters can help locate filters if
they can not be found.
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2. The 20x20 filter is then folded as shown below. The filter is
usually folded three times before it is placed in the paper envelope.
The filter needs to be folded to a smaller size to fit into the
soxhlet below the solvent level. Clear an area and lay out a terry towel
to work on. Only metal tweezers should be allowed to contact the filter
in the folding process. Do not touch with hands or gloves.
Soxhlet extractor ^s assembled. Some solvent in the Teflon squeeze bottle
should be squirted on the joint to prevent sticking. Slight twisting of
the joint will distribute the solvent around the joint. No Vacuum grease
should be used. The soxhlet is secured to the stand over the multiple
extraction heater so that the flask sits evenly on the heater. Boiling
pots are labeled with filter and test number, solvent and extraction date.
3. Water hoses on the condenser are connected so that water flows
from the bottom to the top of the condenser. A small amount of vacuum
grease may be used on the hose connectors so that the hoses will slip on
and off the condenser. If too much grease is used, however, the hoses
may pop loose.
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4. A drying tube packed with fresh molecular sieve and silica gel
(kept in the chem lab oven) and a Teflon connector is placed on top of each
condenser. A supply of drying tubes should be kept on hand in the oven.
When the indicator changes from dark blue to pale blue or clear the
desiccant needs to be changed.
5. The heater and condenser water are turned on. The heater control
is turned to 100%.
6. Once a week the cycling rates should be checked.. This is done by
timing each soxhlets1 cycling period three times after the boiling rate has
stabilized (about 2 hours). The soxhlets should cycle at least every 15
minutes for a desired rate of 4 cycles/hour. (Timing is done by first
allowing the soxhlet to fill with solvent. One cycle is timed from the
point at which solvent begins siphoning until the soxhlet fills again and
starts siphoning).
7. The large soxhlet extraction is run for 8 hours (9 am - 5 pm) .
8. To shut the system down after 8 hours, the heater is turned off.
After the solvent stops boiling (15-30 minutes) the cooling water is also
shut off.
Concentration of Extract
1. The next day the boiling pots should be placed in the desiccator
to prevent condensation of moisture. The solvent remaining in the soxhlet
is poured into the waste container.
2. If the filter is extracted with only one solvent, the filter is
removed to a glass petri dish with large tweezers and placed in the desiccator
or under the hood until dry. The filter is discarded. If the filter is
extracted sequentially, the filter is left in the soxhlet until extracted
with the last solvent. Then the filter is removed with large tweezers to
a glass petri dish and placed in the desiccator or under the hood until dry.
The filter is discarded.
3. The pan with approximately 1-1 1/2" of deionized water is heated
on the hot plate to 40 °C for methylene chloride and to 80° for cyclohexane
and acetonitrile.
4. Isopropyl alcohol is added to the cold finger condenser until it
is half full. Small chunks of dry ice are slowly added to the alcohol (one
at a time, otherwise the alcohol boils over) , until the mixture is about 2"
from the. top. It may be necessary to place a towel on top of the cold
finger to prevent splashing.
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5. Filtration - All extracts are filtered through a 47 mm Pallflex
filter as follows: Filtration apparatus and filter acee washed with solvent.
The solvent is discarded. The pressure relief valve on the vacuum pump
should be fully opened to provide minimum vacuum on the filtration apparatus.
The extract plus boiling chips are poured into the filter funnel keeping
the liquid level less than half full. Solvent is used to wash the
boiling pot and filter funnel three times. Vacuum is turned off as soon
as all the liquid is filtered to prevent moist air from being drawn through
the filter flask containing the extract.
6. The filtered extract is poured into a prewashed 1000 m£ round
bottom flask with washings. The flask is attached to the roto- evaporator
so that the flask is submerged about 1/2" in the pan of heated deionized
water. The vacuum is connected to the condenser. The pressure relief
valve is closed so that maximum vacuum is pulled (as close to 76 cm Hg
as possible).
7. The vacuum pump and roto- evaporator are turned on and allowed to
run (approximately 20-40 minutes) until there is only about 20 m£ of sample
remaining in the flask. If the entire amount of solvent is evaporated by
mistake, solvent is drained back into the 1000 m& flask with washings and
re-evaporated to approximately 20 m£. The carbon in the vapor filter should
be changed about once a month. The micron filters should also be serviced
monthly by sonicating the filter frit in methylene chloride for about
30 minutes.
8. The concentrated extract is transferred to a 30 mil beaker with
washings. The extract is further concentrated by blowing dry zero nitrogen
over the sample in the desiccator until the volume is reduced to 2 or 3 m&.
(The nitrogen flow should be maintained at a rate that does not blow sample
out of the beaker or vial). The contents are again transferred with washings
to a preweighed sample bottle. NOTE: SAMPLE VIALS SHOULD NOT BE TOUCHED WITH
BARE HANDS; FINGERPRINTS MAY CAUSE WEIGHING ERRORS. USE TWEEZERS OR WEAR GLOVES
WHEN HANDLING. The extract is completely dried in the desiccator (1-2 hours).
Sometimes the sample will appear oily or wet. The extract can be weighed
several times to determine if the sample is losing weight to solvent evaporation.
If the weight remains stable, the sample is dry and the weight can be recorded.
Wooden bottle trays or plastic tubing should not be used in the desiccator as
they may contaminate the samples. The molecular sieve and silica gel desiccant
should be changed when the indicator turns pale blue or clear. The lifetime
of the desiccant can be prolonged if the gas exit valve is closed off overnight.
This prevents moist room air from backing up into the desiccator.
9. After the final weighing, the vials are sealed with Teflon tape
and labeled.
10. Ames extracts are sealed in a nitrogen purged Tedlar bag and stored
upright in dry ice. All other extracts are stored upright (to prevent
leakage) in trays.
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III. SUMMARY OF RESULTS
The data reported for this work assignment included percent organic
extractables (as a fraction of total particulate collected), and in some
cases, micrograms of benzo(a)pyrene per milligram of extract. The results
are found in Tables 1 through 5. Some samples required additional analyses
not included in this program. These additional data and the Ames data are
found in the final reports of the respective projects. The reports are
footnoted in Tables 1 through 5.
10
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TABLE 1. EXTRACTION DATA FOR FILTERS RECEIVED FROM EPA
Sample Description
Batch 1
8-20 x 20 filters
10 filter socks
from salt mine
Batch 2
19-20 x 20 filters
Sample Date
Number Received
81-0010
81-0020
81-0030
81-0040
81-0050
81-0060
81-0070
81-0080
10 socks*
(unnumbered)
81-0440
81-0450
81-0460
81-0500
81-0510
81-05-20
81-0560
81-0570
81-0580
81-0590
81-0660
81-0670
81-0680
81-0690
81-0700
81-0710
81-0720
81-0730
81-0740
4-8-81
4-8-81
4-8-81
4-8-81
4-8-81
4-8-81
4-8-81
4-8-81
4-8-81
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-62-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
5-26-82
Total Extract Percent
Particulate Particulate Weight Extract-
Weight (mg) Weight (rag) (mg) ables
550
330 1230 110.971 9.02
350
1040 1040 171.283 16.47
230
460 1230 73.376 6.00
540
30 1030 39.095 3,80
none provided — 29657.3
610
720 2150 746.070 34.70
820
330
280 920 68.760 7.47
310
220
360 1230 647.821 52.67
420
230
460
450 1380 218.936 15.86
470
400
340 1120 140.719 12.56
380
60
50 170 25.537 15.02
60
*• •*
Ames BaP
Date Ug BaP/mg
Required Shipped Required Extract
yes 5-20-81 yes 0.0201
yes 5-20-81 yes 0.0330
yes 5-20-81 yes 0.0155
yes 5-20-81 yes <0.07
yes 5-20-81 yes not measurable
yes no —
yes no —
yes no —
yes no
yes no
yes no —
*Socks extracted in pairs and extracts combined.
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TABLE 2. EXTRACTION DATA FOR VOLVO TD100A (DUAL FUEL) AND VOLVO TD100C (DIESEL) FILTERS*"
Sample Analysis
b b
Filter A Filter B
(5830.6-P20-) (5830.6-P20-)
48 — )
67 — J
68 — j
202 — -j
203 — I
204 — j
50
51
196 — -j
197 — \
198 — j
M
136 — )
137
138 — )
127 ~ "I
128 -- V
129 -- )
145 — \
146 — \
147 -- )
184 — •)
185 ™ (
186 " j
Total Part. Total Ext.
Weight (mg) Weight (mg)
VOLVO TD100A
241.4 38.303
19001 41.591
81.5 17.278
77.3 15.837
289.3 33.749
VOLVO TD100A
257.3 126.318
247.9 126.014
VOLVO TD100A
288.8 44.731
413.1 34.658
Ames BaP
Percent Date yg BaP/mg Sample0
Extractables Required Shipped Required Extract Processing
TRANSIENT METHANOL AND CATALYST
15.87
21.88
21.20
20.49
11.67
C
C
C
f~*
C
NO — YES 0.0055 C
C
C
C
C
C
TRANSIENT ETHANOL
C
49.09
50.83
C
C
NO — YES 0.0017
C
C
C
TRANSIENT ETHANOL AND CATALYST
C
15.49
8.39
C
NO — YES 0.0921 C
C
c
c
VOLVO TD100A TRANSIENT METHANOL
15 -- }
1
4 5
9 10 (
11 12 ;
657.4 501.469
E & C
76.28 YES 5-13-81 YES 0.0061 E & C
E & C
E & C
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TABLE 2 (CONT'D). EXTRACTION DATA FOR VOLVO TD100A (DUAL FUEL) AND VOLVO TD100C (DIESEL) FILTERS
Sample Analysis
Filter A Filter Bb
(5830.6-P20-) (5830.6-P20-)
Total Part.
Weight (mg)
Total Ext.
Weight (mg)
Ames BaP
Percent Date yg BaP/mg Sample0
Extractables Required Shipped Required Extract Processi
VOLVO TD100C TRANSIENT DIESEL
311
333 334 \
335 336 (
337 338 )
238
- \
213
214 — '
219 — |
220 — (
l—i 1
u> 221 — )
232
225 — i
226 — I
227 — j
208 — 1
209 — >
210 — )
244
161.1
901.7
743.5
463.9
438.8
367;9
230.1
390.1
753.1
56.267
276.459
VOLVO TDlOOA
678.983
155.754
27.334
299.095
49.422
100.508
627.469
E & C
34.82 YES 5-13-81 YES 0.0168 E & C
E & C
30.66 E & C
d
STEADY STATE METHANOL
91.32 \ C
33.57
6.23
C
C
C
C
C
C
81.30 \ YES 5-13-81 YES 0.0043 C
21.48
25.76
83.32
C
C
C
C
C
C
C
VOLVO TDlOOA STEADY STATE ETHANOL AND WATER
290
295
304
232
308
298
292
307
1057.3
145.5
146.2
367.9
117.0
202.0
1274.6
118.1
1029.645
58.911
32.936
299.095
17.590
37.831
925.677
16.402
97.38
40.49
22.53
81.30
15.03
18.73
72.62
13.89
C
C
5-13-81 C
p
YES and YES 0.0064 n
5-18-81 '-
C
C
C
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TABLE 2 (CONT'D). EXTRACTION DATA FOR VOLVO TD100A (DUAL FUEL) AND VOLVO TDlOOD (DIESEL) FILTERS
Sample Analysis
Filter Ap Filter BP
(5830.6-P20-) (5830.6-P20-)
247
254
271
277
264
262
249
252
272
265
259
278
273
263
Total Part.
Weight (mg)
842.9
383.5
671.3
97.6
780.6
534.8
428.9
373.4
1207.2
908.4
1129.6
339.0
245.0
318.3
135.1
456.4
672.1
447.8
158.3
163.0
158.0
149.8
Total Ext.
Ames BaP
Percent Date yg BaP/mg
Weight (mg) Extractables Required Shipped Required Extract
VOLVO TD100A
779.919
21.104
8.325
64.805
25.925
16.635
243.940
18.922
9.542
7.210
22.462
VOLVO TD100C
303.526
133.437
'21.642
109.444
42.238
65.478
390.951
11.422
64.262
57.353
46.120
STEADY STATE METHANOL AND CATALYST0
92.53
5.50
1.24
66.40
3.32
3.11
56.88
5.07
0.80
0.80
» YES 5-13-81 YES 0.0011
2.00
STEADY STATE DIESELd
89.54
54.46
6.80
81.00
9.25
9.74
87.30
7.22
YES 5-13-81 YES 0.0032
39.42 NO — NO
36.30 NO — NO
30.79 NO ~ NO
340
349
357 358
347
354 355
351 352
344
359
324
310
330
Additional information on these filters can be found in EPA report EPA 460/3-81-023.
Filter nubmers in both Filter A and Filter B columns indicate that two filters were extracted per soxhlet.
~C-combined, E-extracted
Ames bioassay will be performed on the extracts from each individial modal cycle in addition to the
composite sample.
C
C
C
E & C
C
C
C
E & C
E & C
E & C
E & C
E & C
E & C
E & C
E & C
E & C
E & C
ESC
E & C
E
E
E
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TABLE 3. EXTRACTION DATA FOR VOLKSWAGEN RABBIT DIESEL FILTERS COLLECTED UNDER AN ALTERNATE FUEL STUDY6
SAMPLE ANALYSIS
r>
AMES
BaP
FILTER A
(5830.3-P20-)
78
79
101
102
90
92
80
103
94
82
en ®^
48
49
57
58
69
70
72
73
98
^\J
99
107
108
111
112
TOTAL PART.
FILTER B WEIGHT (mg)
(5830.3-P20-)
593.6
449.5
788.0
653.1
91 846.0
93 590.6
606.4
984.6
851.0
I
~ [ 1238.2
— )
.
~ | 1654.6
~~ [ 1356.6
— '
~~ I 1747.8
— '
— )
( 1182.8
— 1
— )
f 1437.5
— )
~~ | 1656.8
~~ I 1510.1
TOTAL EXTRACT
WEIGHT (mg)
144
116
122
74
230
144
145
127
140
180
245
184
263
296
298
241
192
PERCENT
EXTRACTABLES
24.3 [
25.9 '
15.5 1
11.4 '
27.2 »
24.4 I
23.9
12.9
16.4
14.6
14.8
13.6
15.0
25.0
20.7
14.6
12.7
DATE DATE
REQUIRED SHIPPED REQUIRED SHIPPED
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
-b-
aAdditional information on these filters can be found in EPA Report, EPA 460/3-82-002.
^Various analyses performed under another task of this project and published in above
mentioned report.
cC-combined, E-extracted, S-split
SAMPLE
PROCESSING'
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
E&S
E&S
E&S
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
E, C&S
-------
TABLE 4. EXTRACTION DATA FOR TWO FORD ESCORTS AND TWO VW RABBITS
USING SEVERAL COMBINATIONS OF FUEL AND CATALYST3
Filter Ab
(5830.11-P20-)
9
11
13
15
25
27
37
39
41
43
(6619-P20-)
17
19
77
79
Filter Bb
(5830.11-P20-)
10
12
14
16
26
28
38
40
42
44
(6619-P20-)
18
20
78
80
Total
Part.
Weight (mg)
160.6
270.5
198.3
227.3
177.4
325.6
2807.5
Total
Extract
Weight (mg)
46.559
47.955
50.955
58.718
52.485
54.060
30.619
Percent
Extrac tables
28.99
17.73
25.72
25.83
29.59
16.60
1.09
Samp'.
Procesi
E,C
E,C
E,C
E,C
E,C
E,C
E,C
(6619.3-P20-)
57
59
(6619.3-P20-)
58
60
198.6
56.305
28.35
E,C
Additional information on these filters will be published in the final report of another phase of
this project: Contracts 68-03-2884, Task Specifications 11 and 12 and 68-03-3073, Work Assignments
1 and 3.
Benzo(a)pyrene and Ames analyses not required on this Work Assignment.
C Filter numbers in both Filter A and Filter B columns indicate that two filters were extracted per
soxhlet.
E-extracted, C-combined
-------
TABLE 5.
EXTRACTION DATA FOR A MACK EM6-300 HEAVY-DUTY DIESEL
ENGINE USING ALTERNATE FUELS**
Sample Analysis
Filter Ab
Total
Part.
Filter Bb Weight (mg)
Total
Extract
Weight (mg)
Percent
Extractables
Ames
Date
Req ' d Shipped
BaP
yg/BaP
Req'd Sample
(5830.14-P20-)
13
15
19
21
17
40
42
43
45
47
22
24
25
27
29
31
33
34
36
38
(5830.14-P20-)
14
20
16)
18 /
41
44
46 \
48 j
23
26)
28 /
30
32
35
37 I
39 /
625.8
330.8
601.1
1224.0
1031.5
559.7
663.0
1374.0
855.1
403.1
1157.2
542.5
FUEL 509
133.028
66.871
118.703
230.601
FUEL 510
773.070
386.898
389.045
754.077
FUEL 511
129.543
71.888
264.663
126.768
FUEL 517
21.26
20.21
19.75
18.84
74.95
69.13
58.68
54.88
873.5
438.0
692.2
1371.4
119.248
58.837
114.419
218.856
13.65
13.43
16.53
15.96
Yes 6-29-82 Yes 0.0631
Yes 6-29-82 Yes 0.0099
Yes 6-29-82 Yes 0.2045
Yes 6-29-82 Yes 0.1425
Yes 6-29-82 Yes 0.2969
Yes 6-29-82 Yes 0.0361
Yes 6-29-82 Yes 0.0750
Yes 6-29-82 Yes 0.0479
Sample
Processingc
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
E,C
Additional information on these filters will be published in the final report of another phase of this
project: Contract 68-03-2884, Task Specification 14.
^Filter numbers in both Filter A and Filter B column indicate that two filters were extracted per soxhlet.
CE-extracted, C-combined
-------
APPENDIX A
SCOPE OF WORK
Contract 68-03-2884
Task Specification 9
-------
SCOPE OF WORK
The purpose of this task is to provide ECTD with extraction and BaP
analysis support. This will consist of- a number of work elements,'
including: performing soxlet extractions on a given set of filters,
determining the proportion that is solvent soluble organic, performing
BaP analysis, mixing the appropriate filter extracts to form a sample,
taking the sample to dryness, shipping the sample under dry ice to ECTD's
Ames test contractor, EG and G Mason Research. The exact instructions.for
each sample may vary and will be given upon sending the samples to SwRI,
Most Ames Test Samples will consist of a combination of extracts from
two or more filters. Under most conditions, the filters can be extracted
in groups, providing the apparatus is adequately large. There will be
some specific cases where this may not be done; for example, when individual
BaP or Ames Test analyses must be done. The following is a Table of the
expected sample requirement:
Project
SDSB-H.D.
Diesel Baseline
SDSB-Misc.
TAEB-Trap Testing
TAEB-Misc.
CTAB-L.D. Diesel
Organics
CTAB-Volvo
CTAB-H.D. Diesel
Malfunction
CTAB-Synthetic
Fuels (VW)
CTAB-Misc.
TOTAL
No. of
Ames Samples
3
10
15
10
12
8
10
10
82
Estimated No.
of Filters
21
20
45
25
24
56
28
20
20
239
Estimated No.
of BaP Analyses
0
10
0
0
0
8
14
10
7
Time Frame
Required.198:
Jan-March
Jan-March
Jan-Dec.
Jan-Dec.
Sept-Jan.
Jan-April
Feb-May
Feb-Dec,
Jan-Dec.-
49
The reporting requirements shall consist of: 1) monthly progress letters
outlining the progress of the work as well as the resulting data, and
2) a final letter report briefly outlining the conduct of the task.
A-2
------- |