EPA-600/R-94-141
August 1994
FINAL REPORT
CHARACTERIZATION OF EMISSIONS FROM CARPET SAMPLES
USING A 10-GALLON AQUARIUM AS THE SOURCE CHAMBER
Prepared by:
Zhishi Guo and Nancy Roaehe
Acurex Environmental Corporation
4915 Prospectus Drive
P.O. Box 13109
Research Triangle Park, NC 27709
EPA Contract No. 68-DO-0141
Technical Directives No. 93-111 and 93-170
EPA Project Officer: Mark A. Mason
U.S. Environmental Protection Agency
Air and Energy Engineering Research Laboratory
Research Triangle Park, NC 27711
Prepared for:
U.S. Environmental Protection Agency
Office of Research and Development
Washington, D.C. 20460
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TECHNICAL REPORT DATA
{Please read Instructions on the reverse before comple I I |||| II |||| |||l ||||[| 1 1II
1, REPORT NO. 2,
EPA-60Q/R-94-141
3 11IIIIIIIIII [III IIII11 III il
FB94-210002
4. TITLE AND SUBTITLE
Characterization of Emissions from Carpet Samples
Using a 10-Gallon Aquarium as the Source Chamber
S, REPORT DATE
August 1994
6. PERFORMING ORGANIZATION CODE
7. AUTHOH(S)
Zhishi Guo and Nancy Roache
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
A cur ex Environmental Corporation
P. 0. Box 13109
Research Triangle Park, North Carolina 27709
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-DO-0141, Tasks 93-111
and 93-170
12, SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Air and Energy Engineering Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final; 10/92 - 6/93
14. SPONSORING AGENCY CODE
EPA/600/13
15. supplementary notes AEERL pro:)ect offlcer is MarkA< Mason, Mail Drop 54, 919/541-
4835.
16. abstract rep0rj; discusses part of a Phase I carpet bioresponse study sponsored
by EPA. The study evaluated emissions from carpet samples that had previously
been reported to show toxic effects on experimental mice. The report describes the
major findings of only the chemical characterization work conducted at the Indoor
Source Characterization Laboratory of EPA1s Air and Energy Engineering Research
Laboratory. All other results (animal testing, microbial testing, chemical analysis
by sample extraction, and pesticide analysis) are reported separately. The experi-
mental system used in this study, developed by Anderson Laboratories, was identi-
cal to that used by EPA's Health Effects Research Laboratory in carpet bioresponse
testing. Duplicate tests were conducted for each of three samples received from the
Consumer Product Safety Commission: two previously used carpet samples plus
mock (empty bags) samples. An emissions characterization team from the Contrac-
tor evaluated the experimental system and concluded that the test system developed
by Anderson Laboratories was not suitable for carpet chemical emissions character-
ization because of poor reproducibility, non-uniform thermal conditions, and emis-
sions from the source chamber itself. A 1-hour bake cycle prior to the dynamic mode
is not typical of indoor air characterization methods.
17. KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Pollution
Carpets
Emission
Chemical Composition
Pollution Control
Stationary Sources
13 B
he
14G
07D
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS {This Report)
Unclassified
21. NO. OF PAGES
127
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 <9-73}
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ABSTRACT
As part of Phase I of the carpet bioresponse study sponsored by the U.S. Environmental
Protection Agency (EPA), a study was conducted to evaluate the emissions from carpet samples that
had previously shown toxic effects on experimental mice as reported by Anderson Laboratories Inc.,
Dedham, MA in 1992, This document describes the major findings of the chemical characterization
work conducted at the Indoor Source Characterization Laboratory of EPA's Air and Energy
Engineering Research Laboratory (AEERL). All other results (animal testing, microbial testing,
chemical analysis by sample extraction, and pesticide analysis) are reported separately.
The experimental system used in this study was first developed by Anderson Laboratories and
was identical to the system EPA's Health Effects Research Laboratory (HERL) used in carpet
bioresponse testing. Duplicate tests were conducted for each of three samples received from the
Consumer Product Safety Commission (CPSC): two carpet samples plus mock samples (one empty
bag and one bag of computer paper).
Toxicologists from HERL evaluated the carpet sample emissions data and concluded that the
analytical results did not make a compelling case for a toxic exposure.. The emissions characterization
team from Acurex Environmental Corporation evaluated the experimental system and concluded that
the test system developed by Anderson Laboratories was not suitable for carpet emissions
characterization because of poor reproducibility, unusually highihermal conditions, and spurious
emissions from the source chamber itself. The 1-h bake cycle prior to the dynamic mode is not
typical of indoor air characterization methods.
iii
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TABLE OF CONTENTS
Section Page
ABSTRACT ill
LIST OF TABLES viii
LIST OF FIGURES xi
1.0 INTRODUCTION 1
2.0 MATERIALS AND METHODS 3
2.1 DESCRIPTION OF CARPET SAMPLES TESTED . 3
2.1.1 Sample Source 3
2.1.2 Installation 4
2.1.3 Determination of Sample Area and Volume 5
2.2 EXPERIMENTAL SYSTEM 5
2.3 PREPARATION OF THE SOURCE CHAMBER 9
2.4 AIR SUPPLY AND HUMIDITY CONTROL 9
2.5 AIR FLOW AND PRESSURE CONTROL , 10
2.6 TEMPERATURE CONTROL 10
2.7 TEST OF AIR MIXING IN THE EXPOSURE CHAMBER . 13
2.8 AIR SAMPLING AND ANALYSIS FOR ORGANIC COMPOUNDS 13
2.8.1 Sorbents 13
2.8.2 Sampling Procedure 14
2.8.3 Analytical Instruments 15
2.8.4 Analysis 16
2.9 AIR SAMPLING FOR ANALYSIS OF CARBONYL COMPOUNDS . 18
2.10 SAMPLING AND ANALYSIS OF AEROSOLS 18
3.0 RESULTS 20
3.1 EXPERIMENTAL SUMMARY 20
3.2 MONITORING RESULTS OF EXPERIMENTAL CONDITIONS 21
3.2.1 Air Mixing in the Exposure Chamber 21
3.2.2 Air Pressure in the Exposure Chamber 22
3.2.3 Temperature , 22
3.2.4 Humidity 30
3.2.5 Air Flow Rate 31
3.3 SAMPLE WEIGHT LOSS AFTER EXPERIMENT 32
3.4 QUALITATIVE ANALYSIS OF ORGANIC COMPOUNDS 32
3.5 QUANTITATIVE ANALYSIS OF ORGANIC COMPOUNDS 36
3.5.1 TVOCs and Grouped VOCs 36
3.5.2 Individual Compounds 45
(continued)
V
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TABLE OF CONTENTS
Section • Page
3.6 PARTICLE COUNTING 51
3.7 MISCELLANEOUS OBSERVATIONS . . > 53
4.0 DATA QUALITY REVIEW 55
4.1 DATA QUALITY OBJECTIVES 55
4.2 TEMPERATURE 55
4.2.1 Sensor Calibration 55
4.2.2 Temperature Control 56
4.3 RELATIVE HUMIDITY 56
4.3.1 Calibration of Humidity Probes . . 56
4.3.2 Humidity Measurement 56
4.4 AIR FLOW RATE MEASUREMENTS 61
4.4.1 Sampling Flow Rate 61
4.4.2 Chamber Air Flow Rate 61
4.5 GC ANALYSIS 65
4.5.1 Detection Limit and Quantification Limit 65
4.5.2 Daily QC Check 67
4.5.3 Accuracy 67
4.5.4 Precision 67
4.5.5 Completeness of ST032 Sorbent Samples 72
4.6 IDENTIFICATION OF INDIVIDUAL COMPOUNDS 72
4.7 QUANTIFICATION OF INDIVIDUAL COMPOUNDS 73
4.8 EFFECTIVENESS OF CHAMBER CLEANING 73
4.9 PARTICLE COUNTING 76
4.10 AUDITS 77
4.11 CONCLUSIONS ON DATA QUALITY REVIEW . 77
5.0 DISCUSSION OF RESULTS . 79
5.1 COMPARISON OF INITIAL TVOC CONCENTRATIONS IN THE SOURCE
CHAMBER 79
5.2 COMPARISON OF AVERAGE TVOC CONCENTRATION IN THE SOURCE
CHAMBER DURING THE EXPOSURE PERIOD 79
5.3 CALCULATION OF TOTAL AMOUNT OF TVOC ELUTED FROM THE SOURCE
CHAMBER DURING AN EXPOSURE 81
5.4 ESTIMATION OF THE PERCENTAGE OF TVOC EMITTED DURING ONE-HOUR
STATIC HEATING PERIOD 83
5.5 THE CHANGES OF TVOC COMPOSITION DURING THE TEST 84
(continued)
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TABLE OF CONTENTS (concluded)
Section Page
5.6 EMISSIONS OF INDIVIDUAL COMPOUNDS 91
5.6.1 Acetic Acid 91
5.6.2 Benzene 91
5.6.3 Naphthalene 91
5.6.4 BHT 91
5.7 CONCENTRATION CHANGES OF INDIVIDUAL COMPOUNDS DURING THE
TEST 91
5.8 MOST ABUNDANT VOLATILE ORGANIC COMPOUNDS IN THE CARPET
EMISSIONS AS SAMPLED ON MULTI-SORBENT TRAPS 93
6.0 CONCLUSIONS 97
7.0 REFERENCES 99
APPENDIX A—SAMPLING SUMMARY 100
APPENDIX B—TEMPERATURE DATA 108
APPENDIX C—CALIBRATION DATA FOR TEMPERATURE AND HUMIDITY PROBES . . 112
vn
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LIST OF TABLES
Table Page
2-1. INSTALLATION SUMMARY 4
2-2. CALCULATED SAMPLE AREA AND VOLUME . 5
2-3. LOCATIONS OF TEMPERATURE SENSORS 12
2-4. DESCRIPTION OF ANALYTICAL SYSTEMS 15
3-1. EXPERIMENTAL SUMMARY 20
3-2. DISTRIBUTION OF ST032 SORBENT TRAPS 21
3-3. CONCENTRATIONS OF SFfi TRACER GAS MEASURED IN DIFFERENT LOCATIONS 21
3-4. TVOC CONCENTRATIONS AT DIFFERENT MOUSE PORT . 22
3-5. TEMPERATURE RANGES AT 12 LOCATIONS FOR ALL THE TESTS (IN °C) 23
3-6. MEASURED RELATIVE HUMIDITY FOR INLET AIR 30
3-7. THE INLET AND OUTLET FLOW RATES BEFORE TESTING STARTED 31
3-8. THE OUTLET FLOW RATES MEASURED DURING THE EXPERIMENT . 31
3-9. THE CHANGE OF INLET AIR FLOW DURING AN EXPERIMENT . 32
3-10. THE WEIGHT CHANGES OF SAMPLES AFTER TEST 32
3-11. INDIVIDUAL COMPOUNDS IDENTIFIED IN THE THREE SAMPLES 35
3-12. CLASSES OF COMPOUNDS IDENTIFIED IN THE THREE SAMPLES 36
3-13. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 1 (SAMPLE A) . . 38
3-14. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 2 (SAMPLE B) . . 39
3-15. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 3 (SAMPLE B) . . 40
3-16. CONCENTRATIONS OF TVOCs AND GROUPED VOCS FOR TEST 4 (SAMPLE C) . . 41
3-17. CONCENTRATIONS OF TVOCs AND GROUPED VOCS FOR TEST 5 (SAMPLE C) . . 42
3-18. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 6 (SAMPLE A) . . 43
3-19. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 1
(SAMPLE A) 46
3-20. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 2
(SAMPLE B) 47
3-21. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 3
(SAMPLE B) . 48
3-22. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 4
(SAMPLE C) 49
3-23. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 5
(SAMPLE C) 50
3-24. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 6
(SAMPLE A) 51
3-25. PARTICLE CONCENTRATIONS IN THE EXPOSURE CHAMBER . 53
4-1. DATA QUALITY OBJECTIVES . 55
4-2. MEASURED RELATIVE HUMIDITY FOR INLET AIR . 60
4-3. EC I DETECTION AND QUANTIFICATION LIMITS 66
4-4. EC II DETECTION AND QUANTIFICATION LIMITS 66
(continued)
viii
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LIST OF TABLES
Table Page
4-5. DAILY QC CHECK STATISTICS 67
4-6. DETERMINATION OF ACCURACY FOR TOLUENE 67
4-7. DUPLICATE SAMPLES STATISTICS 70
4-8. COMPARISON OF DUPLICATE SAMPLES—TVOC 70
4-9. COMPARISON OF DUPLICATE SAMPLES—ACETIC ACID 71
4-10. COMPARISON OF DUPLICATE SAMPLES—NAPHTHALENE 71
4-11. COMPARISON OF DUPLICATE SAMPLES—BHT 72
4-12. ZERO-CHECKING RESULTS FOR PARTICLE COUNTER 76
5-1. AVERAGE TVOC CONCENTRATIONS IN THE EXPOSURE CHAMBER 81
5-2. THE AMOUNT OF TVOC ELUTED FROM THE SOURCE CHAMBER DURING EACH
EXPOSURE 83
5-3. PERCENTAGE OF TVOCs EMITTED BEFORE DYNAMIC MODE STARTED 84
5-4. TEN MOST ABUNDANT COMPOUNDS IN THE EMISSIONS FROM SAMPLE A ... 93
5-5. TEN MOST ABUNDANT COMPOUNDS IN THE EMISSIONS FROM SAMPLE B 94
5-6. TEN MOST ABUNDANT COMPOUNDS IN THE EMISSIONS FROM SAMPLE C 94
5-7. THE CHANGE OF TOP TEN LIST DURING TEST 1 (SAMPLE A) 95
5-8. THE CHANGE OF TOP TEN LIST DURING TEST 6 (SAMPLE A) 96
A-l. SAMPLING SUMMARY FOR EXPERIMENT I 101
A-2. SAMPLING SUMMARY FOR EXPERIMENT 2 102
A-3. SAMPLING SUMMARY FOR EXPERIMENT 3 103
A-4. SAMPLING SUMMARY FOR EXPERIMENT 4 104
A-5. SAMPLING SUMMARY FOR EXPERIMENT 5 . 105
A-6. SAMPLING SUMMARY FOR EXPERIMENT 6 106
A-7. SUMMARY OF DNPH SAMPLE IDS SENT TO RTI 107
B-l. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 1 109
B-2. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 2 109
B-3. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 3 110
B-4. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 4 110
B-5. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 5 111
B-6. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 6 Ill
C-l. CALIBRATION OF THERMOCOUPLE 1 113
C-2. CALIBRATION OF THERMOCOUPLE 2 113
C-3. CALIBRATION OF THERMOCOUPLE 3 113
C-4. CALIBRATION OF THERMOCOUPLE 4 ... 114
C-5. CALIBRATION OF THERMOCOUPLE 5 114
C-6. CALIBRATION OF THERMOCOUPLE 6 114
C-7. CALIBRATION OF THERMOCOUPLE 7 115
(continued)
ix
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LIST OF TABLES (concluded)
Table Page
C-8. CALIBRATION OF THERMOCOUPLE 8 115
C-9. CALIBRATION OF THERMOCOUPLE 9 115
C-10. CALIBRATION OF THERMOCOUPLE 10 . . 116
C-ll. CALIBRATION OF THERMOCOUPLE 11 116
C-12. CALIBRATION OF THERMOCOUPLE 12 . . 116
C-13. CALIBRATION OF HUMIDITY PROBE 1 . 117
C-14. CALIBRATION OF HUMIDITY PROBE 2 117
x
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LIST OF FIGURES
Figure Page
2-1. THE EXPERIMENTAL SYSTEM. . 6
2-2. SAMPLING LOCATIONS IN THE EXPOSURE CHAMBER 8
2-3. THE AIR HUMIDIFYING SYSTEM 11
3-1. TEMPERATURE PROFILES FOR TEST 4; AIR TEMPERATURE ON DAY 1 24
3-2. TEMPERATURE PROFILES FOR TEST 4; AIR TEMPERATURE ON DAY 2 25
3-3. TEMPERATURE PROFILES FOR TEST 4; SAMPLE SURFACE TEMPERATURE ON
DAY 1 26
3-4. TEMPERATURE PROFILES FOR TEST 4; SAMPLE SURFACE TEMPERATURE ON
DAY 2 27
3-5. TEMPERATURE PROFILES FOR TEST 4; CHAMBER PANEL TEMPERATURE ON
DAY 1 28
3-6. TEMPERATURE PROFILES FOR TEST 4; CHAMBER PANEL TEMPERATURE ON
DAY 2. . . 29
3-7. REPRESENTATIVE CHROMATOGRAMS FROM TEST SOURCES 34
3-8. OBSERVED TVOC CONCENTRATIONS VS. EXPONENTIAL DECAY (EXPOSURE 1,
TEST 1) 44
3-9. PARTICLE COUNTING DATA FOR SAMPLE A IN TEST 1 52
4-1. RESULTS OF TEMPERATURE CONTROL; CHAMBER BOTTOM PANEL 57
4-2. RESULTS OF TEMPERATURE CONTROL; CHAMBER AIR 58
4-3. RESULTS OF TEMPERATURE CONTROL; AIR IN THE EXPOSURE CHAMBER. ... 59
4-4. CALIBRATION OF MASS FLOW CONTROLLERS (1) FLOW RATE = 150 mL/MIN. . 62
4-5. CALIBRATION OF MASS FLOW CONTROLLERS (2) FLOW RATE = 400 mL/MIN. . 63
4-6. CALIBRATION OF MASS FLOW CONTROLLERS (3) USED AT TWO FLOW RATES. 64
4-7. GC DAILY QC CHECK RESULTS (1) ENVIROCHEM I/LIQUID TOLUENE STANDARD.68
4-8. GC DAILY QC CHECK RESULTS (2) ENVIROCHEM ILLIQUID TOLUENE STANDARD69
4-9. CHAMBER BACKGROUND: AQUARIUM 3. 74
4-10. CHAMBER BACKGROUND: AQUARIUM 4. . 75
5-1. INITIAL TVOC CONCENTRATIONS IN THE SOURCE CHAMBER 80
5-2. AVERAGE TVOC CONCENTRATIONS DURING EXPOSURE PERIODS 82
5-3. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE A, TEST 1. 85
5-4. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE A, TEST 6. 86
5-5. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE B, TEST 2. 87
5-6. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE B, TEST 3. 88
5-7. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE C, TEST 4. 89
5-8. THE CHANGE OF TVOC COMPOSITION DURING EXPOSURES; SAMPLE C, TEST 5. 90
5-9. CONCENTRATION CHANGES FOR THREE COMPOUNDS DURING EXPOSURES THE
TESTS OF SAMPLE A. .... 92
XI
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SECTION 1
INTRODUCTION
In 1992, researchers at Anderson Laboratories of Dedham, MA distributed data indicating
irritancy and toxicity to mice exposed to emissions from heated carpet samples collected from sites
with a history of indoor air complaints. The detailed chemical and physical parameters associated with
their experiments, however, were unknown. The Indoor Air Branch of the U.S. Environmental
Protection Agency's (BPA's) Air and Energy Engineering Research Laboratory (AEERL) collaborated
with the EPA Health Effects Research Laboratory (HERL), Pulmonary Toxicology Branch, in an
attempt to systematically reproduce Anderson Laboratories' test method and to provide an independent
corroboration of Anderson's test results. EPA/AEERL conducted a thorough chemical, physical, and
microbial characterization of the test sources (two carpets and an empty chamber), and HERL provided
a comprehensive toxicity screen. This report documents the findings of chemical characterization of
emissions from source samples tested and the physical characterization of the test method as performed
by Acurex Environmental Corporation under EPA Contract No. 68-DO-0141, Technical Directive Nos.
93-170 and 93-111.
Chemical characterization of emissions from carpet samples is an essential step in establishing
a correlation between observed toxic effects, if any, and the causative agent or agents. The study
goals, reported herein, were limited to answering the following questions:
• Are any known toxic compounds observed as emissions from the carpet samples? And, if
so, in what concentrations?
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* Are any known toxic compounds observed as emissions from the source chamber itself?
And, if so, in what concentrations?
• Are qualitative and quantitative changes observed over the course of an experiment?
It should be emphasized that the analytical results reported in this document should be
considered exploratory and preliminary for the following reasons: (1) the source chamber used in
Phase 1 experiments (i.e., the 38-L aquarium) is not a conventional apparatus for source
characterization, (2) the source chamber itself is a pollutant emitter, (3) in the source chamber, the
carpet samples are heated unevenly to high temperatures not representative of indoor environments,
and (4) the experimental conditions are difficult to control. Therefore, the results reported are not
likely to occur in normal carpet use,
Because of the limited amount of time given for the analysis of Phase 1 data, only the data
that answer the specific questions given in the test plan and restated above have been addressed.
2
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SECTION 2
MATERIALS AND METHODS
2.1 DESCRIPTION OF CARPET SAMPLES TESTED
2.1.1 Sample Source
All tested carpet samples were received by an independent party (Acurex Environmental Task
Lead) to ensure that the research teams were not aware of which tests had carpet in the chamber and
which did not. Carpet samples were placed in blinded aquariums prior to testing, and the content code
that revealed which experiments contained carpet was not given to the research team until after all data
had been analyzed. The samples from the Consumer Product Safety Commission included two types
of carpets and mock samples (empty bags). The two carpet samples collected by CPSC for EPA were
from carpets that had previously been tested by Anderson Laboratories and had been shown to produce
biological effects on laboratory animals when they were exposed to the emissions from heated carpet.
Each of the samples (carpets and empty bags) were received at least 48 hours prior to testing in the
aquarium systems. The carpet samples received from CPSC were packaged in single-layer, heat-sealed
o if
Tedlar bags with three, 0.093 in (1 -ft ) sections per bag. Each section was tagged with a bag and
section number. There were three bags of carpet per box. The first set of samples was used in the
EPA/AEERL chamber to determine chemical emissions, and the second set was used in the
EPA/HERL chamber for bioresponse testing. The remaining bags' contents were subdivided into
separate heat-sealed Tedlar bags for distribution to Research Triangle Institute (RTI)/Analytical and
Chemical Sciences (ACS) for pesticide evaluation, RTI/Center for Environmental Analysis (CEA) for
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microbial evaluation, and the EPA's Atmospheric Research and Exposure Assessment Laboratory
(AREAL) for headspace, supercritical fluid extraction (SFE), and soxhlet extraction.
2,1,2 Installation
One day prior to testing, the carpet samples were removed from the sealed Tedlar bags and
each section was weighed and measured before being sealed in the test aquarium. Each section was
rolled so that two diagonal corners met and were tied together with a nylon tie. The rolled sections
were placed in a clean, background tested aquarium with two sections on the bottom and one section
on top of the other two in a pyramidal fashion. Such sample layout created many dead spaces in the
source chamber. The aquariums were sealed and covered with duct tape to conceal the contents from
the laboratory personnel conducting the experiments. Table 2-1 gives a summary of the test sources as
received from CPSC. Each test system was tested for leaks by pulling 7 L/min zero-grade air through
the system and measuring the inlet and outlet flow through the system. The difference of these two
measurements was not to exceed 10 percent. After the systems were tested for leaks, each aquarium
was sealed at both its inlet and outlet with a 14/23 sealed ball and socket joint and placed in the
appropriate laboratory on the heating devices (heat off) for testing the next day.
TABLE 2-1. INSTALLATION SUMMARY
Experiment ID
Date Source Received
Date Source Installed
Source/Bag Identifications
1
03/05/93
03/08/93
Sample A1/1292, 1410,1747
2
03/09/93
03/10/93
Sample B Empty Bag/1768
3
03/19/93
03/22/93
Sample B Empty Bag2/! 399
4
03/23/93
03/24/93
Sample C3/1274, 1925, 1488
5
03/26/93
03/29/93
Sample C/1508, 1340, 1916
6
03/30/93
03/31/93
Sample A/1899, 13784, 1499
1 Sample A: Dark pink, low pile, SBR backing, basically new with some household dirt.
2 Experiment 3's empty bag contained computer paper.
3 Sample C: Indoor/outdoor dark blue with gray flecks, urethane backing, glue and plywood on
backing, sections marked with an unknown marker source, samples contained large amounts of
sand.
4 Section 50 in bag 1378 was noted to have an -200 cm2 area of water stain on the backing.
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2.1.3 Determination of Sample Area and Volume
The carpet samples received were not exactly squares or rectangles. To calculate the actual
sample area with better accuracy, the lengths of each side and one diagonal were measured. The
diagonal divides the quadrilateral into two triangles, and the area of each triangle was calculated from
Heron's formula:
Area of Triangle = [s (s - a) (s - b) (s - c)]0 5
where a, b, and c are the lengths of the three sides and s = (a + b + c)/2.
The calculated sample area and volume (area multiplied by thickness) are given in Table 2-2.
The approximate area of sample in contact with the heated chamber panel (as measured after loading)
in the chamber is also given.
TABLE 2-2. CALCULATED SAMPLE AREA AND VOLUME
Test
Sample
Section
Total
Contact
Total
ID
Bag Number
Numbers
Area (cm2)
Area (cm2)
Vol. (cm3)
1
1410 •
60, 47, 21
2950
520
3540
2
1768
N/A
N/A
N/A
N/A
3
1399
N/A
N/A
N/A
N/A
4
1925
27, 56, 65
2890
N/A1
1730
5
1508
5, 42, 21
2870
370
1720
6
1378
45, 12, 50
2960
520
3550
1 Not measured.
2.2 EXPERIMENTAL SYSTEM
The experimental system for chemical characterization (Figure 2-1) consisted of four following
functional parts: (1) the air supply system, (2) the source chamber (i.e., the aquarium), (3) heating and
insulation devices for the source chamber, and (4) the exposure chamber. Teflon tubing with 1 -cm ID
was used to connect the air supply, the source chamber, and the exposure chamber. The experimental
set-up and operational conditions were similar to those used for bio-response studies conducted by
5
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Humidified
Zero-Grade Air
Source Chamber
(Aquarium)
Exposure
Chamber
Heating Pads & Insulation
Figure 2-1. The experimental system.
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EPA/HERL except that no experimental animals were put in the exposure chamber. Instead, the
mouse exposure ports (PI, P2, P6, and P7 in Figure 2-2) were used to collect air samples.
Each of the six tests consisted of four one-hour exposure periods and took two days to
complete. The following is a brief discussion of the test procedure:
* Step 1. The day prior to testing, CPSC supplied sources were placed into the source
chamber.
* Step 2. On day 1, the initial static mode, the source chamber was sealed, then heated to
and maintained in desired temperature ranges. There was no air flow through the chamber
during this stage. The samples were baked under such static conditions for about one
hour.
* Step 3. During the first one-hour dynamic mode (i.e., the first exposure period), the
source chamber was connected to the exposure chamber and humidified zero-grade air was
pulled through the system with a vacuum pump for one hour.
* Step 4. During the two-hour static mode between two exposures, after the first exposure,
the air flow was cut off and the source chamber was disconnected from the exposure
chamber and sealed again. The source chamber was allowed to stay in the static mode for
two hours with the heating system on,
* Step 5. During the second one-hour dynamic mode (the second exposure period), the
same procedure as in step 3 was followed.
* Step 6. During the experimental pause overnight, after the second exposure, the air flow
was again cut off, the source chamber disconnected from the exposure chamber, sealed,
and the heating system turned off. On the second day, steps 2 through 5 were repeated to
complete the third and fourth exposure periods.
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P6
P7
Air from
P3
O
P4
O
P5
O
To Pump
Aquarium
P1
P2
Figure 2-2. Sampling locations in the exposure chamber.
8
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2.3 PREPARATION OF THE SOURCE CHAMBER
The source chambers used were 10-gal (38-L) glass aquariums made by All Glass Aquarium
Co., Inc., Franklin, Wl, and purchased from a local store. Side and bottom panels were 3-mm thick
glass plates and the top was 5-mm thick. The outside dimensions of the aquarium were
20 by 10 by 12.5 in (50.8 by 25.4 by 31.8 cm). Four aquariums were used in the six tests.
The aquariums were first prepared by removing the plastic rim using a hot air gun and a knife.
Excess silicone adhesive was removed with razor blades and precision knives. The aquariums were
then baked overnight at test temperature conditions with a 7 L/min laboratory air flush to remove
excess adhesive vapors. Before a test, the aquarium was washed with a Liquinox detergent solution
and rinsed with deionized water. The aquarium was air dried or dried with a low lint tissue wipe for
immediate use.
In all tests, the aquarium was turned on its side so that the pedestal was facing the wall and
designated the "back panel," and the opening was facing the exposure chamber and designated the
"front panel." The two largest panels (12.5 by 20 in) then became the top and the bottom. The front
panel (i.e., the 10- by 20- by 0.19-in glass cover) has two 0.5-in ID nylon bulkhead fittings in
diagonal corners 3 in from each side. An additional 0.25-in ID nylon bulkhead fitting was added for
temperature measurement. The cover was attached to the aquarium with duct tape (the Original Brand
B-600, Manco Inc., Westlake, OH) and covered with the same type of duct tape to conceal the
contents.
2.4 AIR SUPPLY AND HUMIDITY CONTROL
The air supply used in the tests was zero-grade compressed air, which is a synthetic blend of
nitrogen and oxygen from Air Products & Chemicals, Inc. (APCI), Research Triangle Park, NC. The
Certificate of Zero Grade Air provided by APCI indicated that both total volatile organic compound
(TVOC) and water contents were certified to less than 0.1 ppm.
-------
The air humidiflcation was achieved by passing part of the air flow through an impinger—a
1,000-mL flask containing about 600 mL of deionized water (Ion Pure mixed bed/Millipore water
system), as seen in Figure 2-3. Two mass flow controllers (Tyian Model FC-260) were used for flow
control, and Weathertronics Model 1GIA humidity probe was used to monitor the relative humidity.
The desired humidity of 50% ± 10% was achieved by adjusting the ratio of the dry/wet air flows. The
actual dry/wet flow ratio was about 1:1.
2.5 AIR FLOW AND PRESSURE CONTROL
The air flow through the experimental system was driven by the positive pressure from the air
supply and a vacuum pump downstream from the exposure chamber. To keep the inside pressure
close to the ambient atmospheric pressure, the air flow from the gas cylinder was set to a rate higher
than the air flow through the exposure chamber. This ensured that excess air was constantly released
in the room through a T-tube between the humidifier and the source chamber. A typical flow balance
was as follows:
Humidified air from air supply 9-10 L/min
Outlet air flow of exposure chamber 7 L/min
Air flow for two sorbent tube samples 0.3 L/min
Air flow for particle counter 0.7 L/min
Excess air flow 1-2 L/min
For each exposure, the air flow rates were measured at two locations with a precalibrated rotameter:
the inlet flow of the source chamber and the outlet flow of the exposure chamber.
The pressure inside the exposure chamber was measured by HERL during all the tests with a
magnehelic (Dwyer Instrument Co.) pressure gauge.
2.6 TEMPERATURE CONTROL
The main goal of temperature control was to create temperature profiles in the source chamber
as close as possible to those found in Anderson Laboratories' experimental systems. Based on the
10
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To
Chamber
Figure 2-3. The air humidifying system.
11
-------
actual measurements at Anderson Laboratories (January 4, 1993), the targeted operational parameters
were set to the following:
Bottom outside surface of the source chamber 70 ± 5 °C
Air in source chamber 37 ± 3 °C
Air in exposure chamber 24 ± 2 °C
The temperature inside the source chamber was created and maintained by two heating pads
outside the aquarium: a Sunbeam model E12107 pad under the bottom and a Sunbeam model HT-1
pad on the top. The heating intensity could be adjusted by the heating pad control systems.
During an experiment the temperature was continuously monitored at 12 locations (Table 2-
3). The position descriptions such as "left," "right," "front," and "back" were defined assuming the
observer was standing near the exposure chamber and facing the source chamber. Temperature data
from the 12 locations were collected by Cole-Palmer Model 92800-00 Scanning Thermocouple
Thermometer at a frequency of one reading every minute and logged by a computer.
TABLE 2-3. LOCATIONS OF TEMPERATURE SENSORS
Sensor ID
Sensor Type
Location
1
Air
Inside the aquarium
2
Air ,
Room air
3
Air
Exposure chamber (front)
4
Air
Exposure chamber (back)
5
Surface
Left glass panel of the aquarium (outside/center)
6
Surface
Right glass panel of the aquarium (outside/center)
7
Surface
Top glass panel of the aquarium (outside/center)
8
Surface
Bottom glass panel of the aquarium (outside/center)
9
Surface
Back glass panel of the aquarium (outside/center)
10
Surface
Front glass panel of the aquarium (outside/center)
11
Surface
Carpet sample (backing side)
12
Surface
Carpet sample (fiber side)
12
-------
Surface temperatures were measured with K-type, fast-response surface thermocouples and air
temperature with Teflon-coated, K-type thermocouples.
2.7 TEST OF AIR MIXING IN THE EXPOSURE CHAMBER
Imperfect air mixing may affect the transport of emissions from the source to each of the
experimental animals. To test whether exposures at the four ports were equivalent, the air mixing
pattern in the exposure chamber was characterized by using SF6 tracer gas. The results of this
experiment are presented in Section 3.2.1. A calculated amount of SF6 was injected into the source
chamber without a carpet sample. With an air flow rate of 7 L/min, the tracer concentrations were
measured at the four exposure ports with a Briiel & Kjasr (B&K) Type 1302 Multi-gas Monitor. The
optical filter used for measuring SF6 was UA 0988, which has the center wavelength of 10.6 pm with
a half-power bandwidth of approximately 0.4 ^m. A detection limit of 5 ppb is reported by the
manufacturer.
The results from the analysis of duplicate sorbent tubes collected at different exposure chamber
ports help to validate the mixing of the source chamber emissions. These results are found in Sections
3 and 4.
2.8 AIR SAMPLING AND ANALYSIS FOR ORGANIC COMPOUNDS
2.8.1 Sorbents
The relatively low levels of volatile organic compound (VOC) emissions from carpet samples
required preconcentration prior to chemical analysis. ST032 multibed sorbent traps were used for this
purpose. ST032 traps (T.R. Associates Inc.) are fabricated of 6 mm OD by 203 mm long silanized
borosilicate glass tubing sequentially packed with a fritted glass disk, 290 mg of 20/30 mesh silanized
glass beads, 85 mg of 20/35 mesh Tenax TA, 170 mg of 35/60 mesh Ambersorb XE-340, and 48 mg
of 80/100 mesh activated charcoal. This sampling media allows quantification of volatile and
semivolatile compounds ranging from C4 to C16 with a satisfactory collection and desorption
efficiency.'
-------
Before use, sorbent tubes were conditioned in sets of six using the Enviroehem Model
785 Sorbent Tube/Trap Conditioner, The tubes were connected to the conditioner, and a
heating sleeve was placed over each respective tube. A purge flow of ca. 50-60 mL/min of
UPC nitrogen gas was begun 5 min prior to the heating of the sorbent tubes. The tubes were
then heated to 350 °C. The tubes were allowed to remain at this temperature and under the
nitrogen purge flow for 20-25 min. After this period, the heat was turned off and the tubes
were allowed to cool to 50 °C at which time they were removed from the desorber using lint-
free nylon gloves and placed in their respective vials. The vials were then placed in their
appropriately labelled PTFE bags and sealed using an impulse bag sealer. To evaluate the
"cleanliness" of the conditioned tubes, one tube from each set of six was randomly chosen
and desorbed/run on the GC under the same conditions as a sample would be. If the total
mass resulting from the GC run was less than 40 ng, then that tube and the other five tubes in
the set of six were considered as having passed QC.
2.8.2 Sampling Procedure
Immediately before each one-hour exposure period, three air samples were drawn
directly from the source chamber to determine the accumulated organic pollutant
concentrations that resulted from heating under the static mode. For tests 1-3, static chamber
samples were collected at a volume of 0.1 L using a Samplair vacuum pump. This volume
was determined to be inadequate for quantitative analysis by gas chromatography, since the
peaks were below the detection limit of the instrument Therefore, 1-L samples were
collected using mass flow controllers for tests 4-6. This volume was the largest that could be
justified without jeopardizing the integrity of the static chamber emissions. The dilution of
14
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the static air containing the accumulated carpet emissions in the source chamber was less than
10 percent.
During each exposure, the time-concentration dependence was monitored by
sequentially taking samples from the mouse ports in the exposure chamber by using an air
pump at a flow rate of either 50 mL/min or 150 mL/min to collect sorbent trap samples. The
sampling flow rate was controlled by a mass flow controller.
When the sampling was completed, the trap was put back in the glass vial and sealed
in Teflon bags. The samples were stored in a freezer at approximately -10 °C until analysis
(up to 21 days).
2.8,3 Analytical Instruments
Two gas chromatograph (GC) systems were used in this work. Table 2-4 describes
both analytical systems.
TABLE 2-4. DESCRIPTION OF ANALYTICAL SYSTEMS
Analytical Systems
Envirochem I (EC I)
Envirochem II (EC II)
GC
GC column
Multitube desorber
Concentrator
Flame ionization detector
(FID)
Hewlett-Packard (HP)
model 5890, series II
J&W Megabore DB-5
Envirochem model 8916
Unacon model 810
HP model 19231-60010
Mass spectrometric detector Not equipped
HP model 5890
J&W Capillary 0.32 mm
DB-5
Envirochem model 8916
Unacon model 810
HP model 19231-60010
HP model 597 (MSD)
15
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2.8.4 Analysis
The primary identification of individual compounds from the sources used in this
study was the responsibility of RTI/ACS. However, Acurex Environmental provided backup
identifications from samples collected for analysis using the HP MSD on EC II. Compound
identification was done using an electronic database search of the NBS 43K mass spectral
library and the NIST/EPA/NIH mass spectral library for personal computers. Further manual
review of the data was performed using the Alderman 8-Peak Compound Index EPA/NIH
Spectra Data Base to verify computer library searches and to identify compounds not found
during the search.
The analytical results for specific VOCs will be reported at the following three levels:
* Level 1. A compound in samples that has previously been analyzed as a standard
by the laboratory, and a retention time and mass spectra exist that match the
sample compound as reviewed by the analyst.
* Level 2. A compound that has not been previously identified by a match with
retention time of a known standard but has a good library match as reviewed by
the analyst. The concentration will be reported "as toluene."
* Level 3. The compound is not individually identified by MS but is confirmed as a
class such as alkanes or isomers of a compound. These compounds will be
reported as the class name and the concentration reported "as toluene."
The initial list of identifications from RTI was given to the HERL to mark any
compounds that had known toxic effects. The following compounds were requested by
HERL for quantitation and evaluation of their behavior over the course of the experiments:
1. Methylene chloride
16
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2. Perchloroethylene
3. Benzaldehyde
4. Methylnaphthalene
5. Acetic acid
6. Benzene
7. Naphthalene
8. Butylatedhydroxytoluene (BHT)
All of these compounds were evaluated first for their maximum concentrations and
feasibility of quantitation over the duration of the study. Methylene chloride was noted as a
system contaminant and therefore was eliminated from the list, Perchloroethylene was found
only in trace amounts in Sample A. Benzaldehyde coeluted with another compound and was
difficult to identify and quantify. Methylnaphthalene was identified by RTI; however, this
particular compound could not be identified in the retention time range by Acurex
Environmental. 4-pheylcyclohexane (4-PCH) was also added to this list of compounds
because it is a known carpet emission. On the MSD system, 4-PCH was identified by ion
extraction from a coeluting siloxane compound and found in trace amounts in both carpet
samples and none in the empty chamber. Acetic acid, benzene, naphthalene, and BHT were
all found in quantifiable concentrations throughout all of this study. These compounds
comprise the major focus of the individual compound analysis for this study.
Quantitative analysis was made by using both GC systems with FID. All
concentrations were based on the response factor for toluene and reported at the following
three levels: (1) TVOCs; (2) TVOCs divided into three groups—molecular weight C12; and (3) selected individual organic compounds,
17
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Quantification of individual compounds required retention time correlation of known
marker compounds (toluene and alkanes) between the MSD/FID output from EC II and the
FID output from EC I. Manual review of the chromatograms for matching peak shapes and
patterns was also performed to ensure the best match to the identified compound,
2.9 AIR SAMPLING FOR ANALYSIS OF CARBONYL COMPOUNDS
DNPH-Silica Sep-Pak cartridges purchased from Waters were used to sample
formaldehyde and other carbonyl compounds from chamber air. The effective reagent, 2,4-
dinitrophenylhydrazine (DNPH), in the cartridge reacts with the aldehydes and ketones to
form hydrazone derivatives. DNPH samples were taken from one of the mouse ports of the
exposure chamber at a sampling flow rate of 400 mL/min for the duration of the dynamic
mode.
The DNPH cartridge samples collected were then sent to RTI/ACS for extraction and
subsequent reverse-phase HPLC analysis. The analytical results will be reported separately by
RTI in a Final Report.
2.10 SAMPLING AND ANALYSIS OF AEROSOLS
The instrument used for monitoring particle concentration was a model 8010
PortaCount portable counter (TSI, Inc.). Designed to count individual airborne particles, this
instrument is based on a miniature, continuous-flow condensation nucleus counter (CNC) and
is sensitive to particles having diameters as small as 0.02 }im, but insensitive to variations in
particle size, shape, composition, and refractive index. In this work, the instrument was
operated in the "Count Mode," in which the instrument directly counts the aerosol drawn
through the sample port and gives the concentration in particles per cubic centimeter (P/cm3).
The instrument can measure particle concentration between 0 and 5 x 105 P/cm3. The
18
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counting results can be taken either manually from its display or automatically through a
computer.
Air samples were taken from the top of the exposure chamber through sampling port
P4 (see Figure 2-2). The sampling flow rate was 0.7 L/min. For comparison purposes, the
particle concentrations in the laboratory air were also measured before and after each
exposure period.
19
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SECTION 3
RESULTS
3.1 EXPERIMENTAL SUMMARY
A total of six tests were conducted for the three samples received from CPSC with each being
tested in duplicate. Four aquariums were used in the six tests. This was necessary because of the test
schedule and breakage. An experimental summary is given in Table 3-1.
TABLE 3-1. EXPERIMENTAL SUMMARY
Test 1
Test 2
Test 3
Test 4
Test 5
Test 6
Experiment ID
1
2
3
4
5
6
Chamber ID
AQ2
AQ4
AQ4
AQ3
AQ4
AQ1
Sample ID
A
B
B
C
€
A
Test start date
03/09
03/11
03/23
03/25
03/30
04/01
Test finish date
03/10
03/12
03/24
03/26
03/31
04/02
A total of 148 ST032 sorbent traps and 30 DNPII cartridges were taken during the six tests
for chemical analysis. This number excludes field blanks, laboratory blanks and background samples.
A detailed sampling scheme is given in Appendix A. Table 3-2 shows the distribution of ST032 traps
All the DNPH cartridges were sent to RTI for analysis of carbonyl compounds and the results will be
reported by RTI in a separate report.
20
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TABLE 3-2. DISTRIBUTION OF ST032 SORBENT TRAPS1
Number of Traps
Purpose
Analyzed by
14
Qualitative analysis
RTI
26
Qualitative analysis
Acurex Environmental
99
Quantitative analysis
Acurex Environmental
1 Nine traps were lost before or during analysis.
3.2 MONITORING RESULTS OF EXPERIMENTAL CONDITIONS
3.2.1 Air Mixing in the Exposure Chamber
The air mixing in the exposure chamber was determined prior to Test 1. Normal air flow was
maintained during the test, SF() tracer gas was introduced into the source chamber at a constant rate.
After equilibrium was established, the tracer concentrations were measured at five locations, and the
results are given in Table 3-3. The difference of average concentrations between the two mouse ports
was less than 10 percent.
TABLE 3-3. CONCENTRATIONS OF SFfi
TRACER GAS MEASURED
IN DIFFERENT LOCATIONS (IN mg/m3)
Sampling Location
Mean
RSD (%)
Manifold between aquarium and exposure chamber
9.94
2
Inside the aquarium
9.72
2
Mouse port 1 of exposure chamber'
8.56
4
Mouse port 2 of exposure chamber2
9.29
2
Center of exposure chamber
9.72
1
Mouse port 1 is marked "PI" in Figure 2-2.
2 Mouse port 2 is marked "P2" in Figure 2-2.
3 This sampling port is marked"P4" in Figure 2-2.
Sampling of duplicate volume sorbent traps at different mouse ports confirms the mixing of
the effluent from the source chamber in the exposure chamber. Table 3-4 gives a summary of the
21
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results from three selected duplicate analyses. A complete report of all duplicate samples is presented
in Section 4 of this document.
TABLE 3-4. TVOC CONCENTRATIONS AT DIFFERENT MOUSE PORT
(Concentration unit: jig/m3)
Sample ID
Mouse Port
TVOC Cone.
Mean
RSD
3105
Port 1
164
3106
Port 2
200
182
14%
3315
Port 1
2470
3316
Port 41
2750
2610
8%
3522
Port 1
2320
3523
Port 41
2070
2200
8%
1 Mouse port 4 is marked "P7" in Figure 2-2.
3.2.2 Air Pressure in the Exposure Chamber
The air pressure inside the exposure chamber was measured before the first sample testing
under experimental air flow condition (7 L/min). The source chamber was empty and unheated.
Slight negative pressure was observed inside the exposure chamber. The pressure difference between
laboratory air and exposure chamber was in the range of 0.050-0.075 in of water (0.09-0.14 mm Hg).
This measurement was performed during all mouse exposures by the bioassay laboratory and remained
constant throughout the study.
3.2.3 Temperature
The temperature ranges for all the six tests are given in Table 3-5. An example of temperature
profiles for a complete test is graphically shown in Figures 3-1 through 3-6, The average temperatures
measured at 12 locations (see Section 2.6 for description) during each test are given in Appendix B.
22
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TABLE 3-5. TEMPERATURE RANGES AT 12 LOCATIONS FOR ALL THE TESTS (IN °C)
Thermocouple Location
Mean
Ranj
ge
Air in source chamber
41
36-
46
Laboratory air
23
21 -
24
Air in exposure chamber (front port')
27
23 -
29
Air in exposure chamber (back port )
25
23-
26
Left panel of source chamber
44
39 -
50
Right panel of source chamber
43
38-
48
Top panel of source chamber
48
44-
54
Bottom panel of source chamber
72
66 —
76
Back panel of source chamber
46
37-
52
Front panel of source chamber
32
29-
36
Sample backing (inward)3
50
40-
57
Sample fiber (outward)3,4
68
59-
72
1 Marked "P3" in Figure 2-2.
2 Marked "P5" in Figure 2-2.
3 Excluding Test 2 and Test 3 (no carpet sample).
4 Temperature of sample surface in contact with heated chamber bottom.
23
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First
Exposure
Second
Exposure
50 100 150~ 200 250 300 350 400 450
Elapsed Time (min)
Source Chamber Exposure Chamber P3
Exposure Chamber P5
Figure 3-1. Temperature profiles for Test 4; Air temperature on Day 1.
24
-------
Elpased Time (min)
Source Chamber Exposure Chamber P3
Exposure Chamber P5
Figure 3-2. Temperature profiles for Test 4; Air temperature on Day 2.
25
-------
Elapsed Time (min)
Carpet Fiber Carpet Backing
Figure 3-3. Temperature profiles for Test 4; Sample surface temperature on Day 1.
26
-------
80
70
~ 60
O
o
2 50-
3
£5
&. 40-
0
30
20
10
Third
I Fourth
Exposure
| Exposure
0 50 100 150 200 250 300 350 400 450 500
Elapsed Time (min)
Carpet Fiber
Carpet Backing
Figure 3-4, Temperature profiles for Test 4; Sample surface temperature on Day 2,
27
-------
Elapsed Time (min)
Bottom Panel Top Panel
Figure 3-5, Temperature profiles for Test 4; Chamber panel temperature on Day 1.
-------
o
Q
CD
L_
cd
CD
CL
E
0)
80
70
60
50
40
30
20
10
1
1 /
Third
! Fourth
1 11
Exposure
" i
{Exposure
i i i 1 r ¦
i
0
50 100
150 200 250 300 350
Elapsed Time (min)
400 450 500
Bottom Panel Top Panel
Figure 3-6. Temperature profiles for Test 4; Chamber panel temperature on Day 2.
29
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3,2,4 Humidity
The desired relative humidity for humidified air was 50 percent. The actual measured
humidity varied between 41 and 59 percent (Table 3-6). Deviations from the target value are all
within 10 percent with an average deviation of 2.3 percent.
TABLE 3-6. MEASURED RELATIVE HUMIDITY FOR INLET AIR
Date Time Test ID Exposure ID Measured RH (%)
03/09/93 08:45 1 1 43.1
03/09/93 14:06 1 2 48.6
03/10/93 09:00 1 3 51.5
03/10/93 14:09 1 4 45.3
03/11/93 08:55 2 1 49.7
03/11/93 13:59 2 2 48.8
03/12/93 06:39 2 3 52.4
03/12/93 13:22 2 4 47.6
03/23/93 08:30 3 1 51.3
03/23/93 13:38 3 2 59.3
03/24/93 08:56 3 3 50.2
03/24/93 13:30 3 4 49.9
03/25/93 08:15 4 1 50.2
03/25/93 13:15 4 2 50.2
03/26/93 14:00 4 3 47.9
03/26/93 07:50 4 4 , 52.4
03/30/93 08:48 5 1 52.4
03/30/93 14:27 5 2 48.8
03/31/93 08:36 5 3 52.0
03/31/93 15:02 5 4 54.5
04/01/93 08:12 6 1 50.6
04/01/93 13:12 6 2 49.3
04/02/93 07:26 6 3 54.5
04/02/93 12:33 6 4 49.5
30
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3,2.5 Air Flow Rate
Before the start of each experiment, the inlet and outlet flow rates were measured to make sure
the difference between the two flow rates was within 10 percent (Table 3-7).
During an experiment, the outlet flow was checked prior to each exposure. Results in Table
3-8 shows that the outlet flow was well controlled. The inlet flow, however, had more substantial
changes during the experiment (Table 3-9). This may have been caused by the increased leakage in
the source chamber as a result of continuous heating. Experiment 4 was an extreme case, in which the
inlet flow was reduced by 68 percent after four exposures.
TABLE 3-7. THE INLET AND OUTLET FLOW RATES BEFORE TESTING STARTED (L/min)
Experiment ID
Outlet Flow (L/min) Inlet Flow (L/min)
Percent Difference
1
7.20
6.70
6.9
2
7.28
6.73
7.6
3
7.25
6.70
7.6
4
7.20
6.75
6.3
5
7.14
6.90
3.3
6
6.90
6.35
8.0
TABLE 3-8. THE OUTLET FLOW RATES MEASURED DURING THE EXPERIMENT (L/min)
Experiment ID
Exposure 1
Exposure 2
Exposure 3
Exposure 4
1
7.08
7.08
6.45
6.95
2
6.98
6.95
7.04
6.84
3
7.09
6.95
7.01
6.88
4
6.98
6.99
6.95
6.90
5
6.76
6.65
7.14
7.01
6
6.83
6.84
7.07
7.11
31
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TABLE 3-9.
THE CHANGE OF INLET AIR FLOW DURING AN EXPERIMENT (L/min)
Experiment ID
Flow After
Exposure 2
Percent
Reduction1
Flow After
Exposure 4
Percent
Reduction1
1
N/A
N/A
6.11
9
2
6.49
4
5.95
12
3
N/A
N/A
5.79
14
4
N/A
N/A
2.17
68
5
6.03
13
5.9
14
6
5.04
21
4.85
24
1 Percent reduction was calculated based on the initial inlet flow rate (Table 3-7) to 100%.
N/A = data not available.
3.3 SAMPLE WEIGHT LOSS AFTER EXPERIMENT
The samples were weighed before and after the test. The change of sample weights is shown
in Table 3-10.
TABLE 3-10. THE WEIGHT CHANGES OF SAMPLES AFTER TEST
Test ID Weight Before Test (g) Weight After Test (g) Weight Change (g)
1 764 742 -22
4 544 539 -5
5 533 525 -8
6 807 804 -3
3.4 QUALITATIVE ANALYSIS OF ORGANIC COMPOUNDS
The qualitative analysis of the heated emissions from each of the sources tested in this study
proved to be a challenge. More than two hundred compounds existed in the carpet emissions.
Automated library searches with the NBS 43 K mass spectral library were of limited success for most
of the samples because of the number of compounds (up to 300) detected in each of the sources tested.
Therefore, each ion chromatogram was manually scanned and evaluated for the major emissions from
each of the study sources. The specific compounds requested by HERL were given the highest
32
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priority for in-depth evaluations. A comprehensive identification of the emissions from each of the
sources will be reported by RTI/ACS in a separate report. The correlation of findings from both
laboratories (RTI/Aeurex Environmental) were ensured by the analysis of an even n-alkane standard
that was prepared by Acurex Environmental for daily QC checks for all three analytical systems. An
early evaluation of each laboratory's identifications of the source emissions showed no disagreement.
Among more than 200 peaks in the chromatograms, about 15% have been identified and confirmed by
interlaboratory comparison so far, another 70% were tentatively identified, and the remaining 15%
remained unknown. Figure 3-7 shows a typical chromatogram from each of the tested sources. These
chromatograms are typical of static chamber emissions from the sources used in this study. Test 2,
Sample B shows a typical emissions spectrum from an empty aquarium with a TVOC value of 1,200
pg/nr from a 0.1-L volume sample. Tests 5 and 6 show representative emissions from the carpet
sources with TVOC values greater than 6,000 pg/m3 from 1-L samples.
Table 3-11 gives the list of compounds identified by Acurex Environmental from each of the
test sources. All compounds listed in this table are considered Level 2 identifications with the
exceptions of toluene and styrene which are Level 1. Table 3-12 shows the classes of compounds
found in the emissions from each of the sources.
33
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20-
10-
o"
400-
0
400-
200-
03160CJ
Teat 2 Sample B
A/.
—tJ*.
¦ I in
I I M I II I I M II I I t I I II I I I I! I I I I I I I I I I I I I I I M I I I I I I I I I I I I I I I I i I 1 I I I I I I I 1 I I M
0413004
Test 5 Sample C
¦fJUaMiBKJi
i-i j ,.i,
A* •*»*T^V« f' • ( V
I I 1 I I I I I I I I I I I I [ t I I I I 1 1 I I t i I I i I I I I I I I I I I 1 1 I I I I I [ I I I I I I I I I II I 1 I I I i I I I I I I I I I
040
003
Te3l 6 Sample A
ji u . , . ,I i li jjkiM.it K 1 i.il
I
11 111 11 I ] II I I I I I I I I I I I j II 1 I I I 111 I I I 11 I j II I I I 11 11 II I I II III I 11 I I 11 II 11 11 I t I
0 8 16 24 32 40 48 56 64 72
Figure 3-7. Representative ehromatograms from test sources.
34
-------
TABLE 3-11. INDIVIDUAL COMPOUNDS IDENTIFIED IN THE THREE SAMPLES
Compound Name
Sample A
Sample B
Sample C
Acetone +
Isopropanol +
Benzene
Acetic acid +
Toluene +
Hexanal +
Ethylbenzene +
m,p-Xylene +
N,N-Dimethyl-acetamide +
Styrene +
o-Xylene +
a-Pinene +
Benzaldehyde +
Decane +
Trimethylbenzene +
Limonene +
Acetophenone
Terpene +
Undecane +
n-Dodecene
Camphor +
Naphthalene +
Dodecane +
Dodecamethylcyclohexasiloxane +
4-Phenylcyclohexene +
Butylatedhydroxytoluene +
Hexadecane +
Butanoic acid +
2,3-Dihydro-1,1,3-trimethyl-3-phenyl-1 H-indene
+
+
+
+ —"
+
+
+
+
+
+
4
+
+
+
+
+
+
+
+
+
+
-------
TABLE 3-12. CLASSES OF COMPOUNDS IDENTIFIED IN THE THREE SAMPLES
Class Name
Sample A
Sample B
Sample C
Alkanes
+
-
+
Alkenes
+
-
+
Cyeloalkanes
+
-
+
Cycloalkenes
+
-
+
Oxygenated hydrocarbons
+
+
+
Substituted benzene
+•
+
+
Siloxanes
+
+
+
Substituted phenol
+
-
+
3.5 QUANTITATIVE ANALYSIS OF ORGANIC COMPOUNDS
3.5.1 TVPCs and Grouped VOCs
TVOC concentration data are presented in Tables 3-13 through 3-IS. Before the start of air .
flow through the source chamber for each exposure of each experiment, static chamber samples were
collected to determine the maximum concentration for that exposure. For any given experiment,
during exposures 1 and 3, the time-concentration dependence was monitored by sequentially collecting
samples at 0-5 min, 5-20 min, 20-40 min, and 20-60 min. The sampling flow rate was consistent at
150 mL/min for all six experiments. During exposures 2 and 4, simultaneous 60-min samples were
collected to represent the average concentration of the VOCs from the carpet emissions. The flow rate
for the 60-min samples varied from 150 mL/min for experiments 1, 2 (exposure 2), 3, and 4
(exposure 2) to 50 mL/min for experiments 2 (exposure 2), 4 (exposure 4), 5 and 6. After analysis of
the first set of samples, the sample volume of the 60-min sample was determined to be too large for
the amount of volatiles detected on the sorbent. Therefore, the flow rate was reduced to 50 mL/min.
The mass flow controllers used for air sampling were calibrated individually. The flow rates used
were close to each other but not exactly the same; this was not considered a problem. In addition,
TVOCs in each sample is divided into three groups based on the retention times of alkane markers.
Group 1 includes the light compounds with retention time less than octane, group 2 includes the
36
-------
compounds in the intermediate range with a retention time between and including octane through
dodecane, and group 3 includes the heavier compounds with retention times greater than dodecane.
Quantification limits and detection limits are given in Section 4,5.1.
Figure 3-8 is an example of decaying pattern of TVOC concentrations during an exposure.
<"2
Hie dotted line in the figure is the simple first-order decay (i.e., exponential decay) curve. The
difference between the two curves is an indication of continuous TVOC emissions during the exposure
period (see Section 5.4 for further discussion).
37
-------
TABLE 3-13. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 1
(SAMPLE A)
(Concentration unit: ng/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
TVOC
C12
1
1
1
1
1
2977
2979
2980
2982
2985
0.10
0.75
2.20
2.98
5.80
static
0 to 5
5 to 20
20 to 40
20 to 60
8790
7610
3010
1820
1380
7310
5200
1290
437
281
1070
1730
1060
737
526
434
681
665
644
569
2
2
2
2
2999
3001
2995
2997
0.10
0.10
9.05
8.76
static
static
0 to 60
0 to 60
2810
BQL
1890
1580
BQL
BQL
261
222
918
424
715
618
665
456
915
744
3
3
3
3
3
3
3055
3058
3059
3047
3048
3049
0.10
0.10
0.80
2.20
3.00
6.00
static
static
0.2 to 5.3
5.3 to 20.3
20.3 to 40.3
20.3 to 60.3
2300
2040
2570
1730
1320
1190
BQL
BQL
841
292
120
86.9
503
582
1030
706
456
404
721
509
698
728
742
696
4
4
4
3033
3034
3065
0.10
9.20
8.90
static
0 to 60.3
0 to 60.3
BQL
1650
1560
ND
90.7
81.5
589
566
552
734
992
921
ND = Not detected
BQL = Below quantification limit
38
-------
TABLE 3-14. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 2 (SAMPLE B)
(Concentration unit: pg/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
TVOC
(-12
1
3030
0.10
static
BQL
BQL
ND
42.2
I
3006
3.00
20.2 to 45.2
86.8
BQL
14.3
42.4
1
3007
5.90
20.2 to 60.2
90.8
BQL
17.1
46.7
2
3101
0.10
static
BQL
ND
BQL
BQL
2
3103
0.10
static
BQL
ND
BQL
BQL
2
3105
9.00
1 to 61
164
43.6
31.4
87.8
2
3106
8.80
1 to 61
201
54.5
39.4
106
3
3147
0.10
static
BQL
ND
BQL
BQL
3
3129
0.76
2.8 to 7.8
1030
475
294
251
3
3118
2.20
7.8 to 22.8
243
83.0
57.7
99,2
3
3117
2.96
22.8 to 42.8
78.6
ND
15.3
57.4
3
3115
6.00
22.8 to 62.8
83.9
BQL
16.1
54.7
4
3109
0.10
static
BQL
ND
ND
ND
4
3112
3.30
0.6 to 67.4
162
BQL
32.4
100
4
3113
3.40
0.6 to 67.4
129
BQL
28.5
75.5
ND = Not detected
BQL = Below quantification limit
39
-------
TABLE 3-15. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 3 (SAMPLE B)
(Concentration unit: jig/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
TVOC
CL2
1
3233 ,
0.10
static
BQL
BQL
346
2040
1
3229
0.76
1 to 6
1400
679
341
377
1
3231
2.27
6 to 21
466
227
114
125
1
3209
2.99
21 to 41
BQL
BQL
BQL
BQL
1
3210
6.02
21 to 61
110
33.9
19.1
57.7
2
3237
0.10
static
BQL
ND
ND
BQL
2
3221
0.10
static
BQL
ND
ND
152
2
3222
9.05
0.3 to 60.3
112
31.6
18.4
61.8
2
3225
8.76
0.3 to 60,3
117
38.5
19.4
59.8
3
3256
0.10
static
BQL
ND
BQL
242 ¦
3
3257
0.10
static
BQL
ND
BQL
ND
3
3261
0.74
0.2 to 5.3
210
BQL
38.1
79.5
3
3249
2.25
5.3 to 20.2
74.4
BQL
10.7
30.2
3
3250
2.99
20.2 to 40.2
27.7
ND
ND
12.4
3
3252
5.95
20.2 to 60.2
55.3
BQL
10.1
24.7
4
3253
0.10
static
BQL
ND
ND
ND
4
3240
8.90
1.3 to 61.3
75.5
18.5
13.4
43.8
4
3228
8.90
1.3 to 61.3
71.5
20.5
11.4
39.8
ND = Not detected
BQL = Below quantification limit
40
-------
TABLE 3-16. CONCENTRATIONS OF TVOCs AND GROUPED VOCS FOR TEST 4
(SAMPLE C)
(Concentration unit: |Jg/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
TVOC
00
u
V
C8~C12
V
n
1
3287
1.00
static
12000
2730
8270
1030
1
3289
0.75
1.5 to 6.5
9240
1820
6660
765
1
3291
2.26
6.5 to 21.5
5590
609
4140
843
1
3305
2.97
21.5 to 41.5
4070
218
2960
892
1
3306
6.02
21.5 to 61.5
3180
161
2180
836
2
3281
1.00
static
7580
367
5630
1590
2
3282
0.99
static
6100
435
4820
844
2
3285
8.60
0.7 to 60.7
1890
148
1530
218
3
3318
1.00
static
7220
836
5430
954
3
3319
0.99
static
7300
797
5400
1110
3
3327
5.96
20.3 to 60.3
1180
121
808
260
4
3330
1.00
static
5840
304
4550
985
4
3315
3.09
0.4 to 61
2470
89.0
1760
619
4
3316
3.03
0.4 to 61
2750
92.9
1810
844
41
-------
TABLE 3-17. CONCENTRATIONS OF TVOCs AND GROUPED VOCS FOR TEST 5
(SAMPLE C)
(Concentration unit: ng/m3)
Exposure
ID
Sample
ID
Sampling
Vol, (L)
Sampling
Period (min)
TVOC
A
O
00
Cg~Cj2
>C12
1
3369
1.00
static
6500
723
4780
986
1
3372
0.74
0.3 to 5.3
7040
728
5420
879
1
3373
2.24
5.3 to 20.3
4260
304
3310
634
1
3383
2.97
20.3 to 40.3
3220
139
2430
646
1
3384
6.02
20.3 to 60.3
2770
88.5
2000
680
2
3387
0.99
static
7070
532
5680
841
2
3388
0.98
static
7730
600
6010
1100
2
3354
3.02
0.3 to 60,2
3180
90.1
2370
719
2
3355
2.89
0.3 to 60.2
1010
695
261
54 .3
3
3501
1.02
static
4950
485
3680
777
3
3502
1.01
static
5030
518
3770
731
3
3505
0.75
0.4 to 5.4
4100
339
3070
680
3
3507
. . 2.29
5.4 to 20.4
2740
93.3
2000
642
3
3508
3,02
20.4 to 40.4
2210
46.1
1560
606
3
3509
5.99
20.4 to 60.4
1880
29.6
1220
627
4
3349
0.98
static
4250
205
3300
729
4
3510
2.83
0.3 to 60.3
2020
30.5
1350
629
4
3358
2.78
0.3 to 60.3
2030
44.4
1420
569
42
-------
TABLE 3-18. CONCENTRATIONS OF TVOCs AND GROUPED VOCs FOR TEST 6
(SAMPLE A)
(Concentration unit: jig/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
TVOC
cCg
c8~c12
C,2
1
3549
1.00
static
9220
2210
5600
1420
1
3552
0.80
0 to 5
5690
1140
3450
1090
1
3553
2.27
5.8 to 20.8
3500
503
2060
932
1
3555
2.98
20.8 to 40,8
2390
191
1370
829
1
3556
6.04
20.6 to 60.7
2280
176
1160
935
2
3558
0.99
static
4740
531
3060
1140
2
3559
0.99
static
4920
423
3150
1340
2
3522
3.23
0.4 to 60.4
2320
180
1110
1030
2
3523
2.89
0.4 to 60.4
2070
161
1030
879
3
3587
1.00
static
3460
515
1750
1180
3
3586
1,00
static
3350
457
1730
1150
3
3584
0.76
0.2 to 5.2
2390
358
1110
920
3
3593
2.25
5.2 to 20.2
1930
134
871
918
3
3594
2.99
20.2 to 40.2
1910
102
815
988
3
3595
5.97
20.2 to 60.2
1820
73.0
749
994
4
3569
0.99
static
4150
550
2180
1410
4
3600
3.27
2.2 to 62.2
2030
143
750
1130
4
3601
3.06
2.2 to 62.2
1970
155
748
1060
43
-------
Elapsed Time (min)
s— Observed TVOC Decay Exponential Decay
Figure 3-8. Observed TVOC concentrations vs. exponential decay (Exposure 1, Test 1).
44
-------
3.5.2 Individual Compounds
The quantitative analysis of individual compounds for the source emissions was limited to the
specific compounds selected by HERL as possible irritants or toxicants.
Four individual compounds were quantified for all the samples. They are as follows:
Acetic acid (AA)
Benzene (Benz)
Naphthalene (Naph)
Butylatedhydroxytoluene (BHT)
The results are presented in Tables 3-19 through 3-24. Note that the abbreviation BQL in the tables
means that compound was identified in the sample but its quantity is below quantification limit,
whereas ND means that compound was not detected in the sample.
45
-------
TABLE 3-19. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 1
(SAMPLE A)
(Concentration unit: (ig/m3)
Exposure
ID
Sample
ID
Sampling
Vol, (L)
Sampling
Period (min)
AA
Benz
Naph
BHT
1
2977
0.10
static
90.2
ND
BQL
242
1
2979
0,75
0 to 5
58.3
ND
25.7
362
I
2980
2.20
5 to 20
27.7
ND
21.1
316
1
2982
2.98
20 to 40
16.6
ND
17.5
322
I
2985
5.80
20 to 60
7.33
ND
15.5
295
2
2999
0.10
static
ND
ND
BQL
332
2
3001
0.10
static
ND
ND
ND
239
2
2995
9.05
0 to 60
14,8
ND
20.0
413
2
2997
8.76
0 to 60
12.9
ND
17.3
360
3
3055
0.10
static
ND
ND
ND
344
3
3058
0.10
static
ND
ND
ND
290
3
3059
0.80
0.2 to 5.3
BQL
ND
17.8
373
3
3047
2.20
5.3 to 20.3
8.30
ND
16.8
369
3
3048
3.00
20.3 to 40.3
10,0
ND
15.4
363
3
3049
6.00
20.3 to 60.3
8.32
ND
14.5
347
4
3033
0.10
static
ND
ND
ND
431
4
3034
9.20
0 to 60.3
11.1
ND
15.2
401
4
3065
8.90
0 to 60.3
4.87
ND
15.4
411
ND = Not detected
BQL = Below quantification limit
46
-------
TABLE 3-20. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 2
(SAMPLE B)
•3
(Concentration unit: pg/m )
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
AA
Benz
Naph
BHT
1
1
1
3030
3006
3007
0.10
3.00
5.90
static
20.2 to 45.2
20.2 to 60,2
ND
ND
ND
ND
ND
ND
ND
ND
ND
BQL
13.0
14.9
2
2
2
2
3101
3103
3105
3106
0.10
0.10
9.00
8.80
static
static
1 to 61
1 to 61
ND
ND
BQL
1.0
ND
ND
ND
ND
ND
ND
ND
ND
108
BQL
26.5
31.5
3
3
3
3
3
3147
3129
3118
3117
3115
0.10
0.76
2.20
2.96
6.00
static
2.8 to 7.8
7.8 to 22.8
22.8 to 42.8
22.8 to 62.8
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
BQL
60.5
27.5
11.9
14.7
4
4
4
3109
3112
3113
0.10
3.30
3.40
static
0.6 to 67,4
0.6 to 67.4
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
30.6
20.8
ND = Not detected
BQL = Below quantification limit
47
-------
TABLE 3-21. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 3
(SAMPLE B)
(Concentration unit: (ig/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
AA
Benz
Naph
BHT
1
3233
0.10
static
ND
ND
ND
ND
1
3229
0.76
1 to 6
ND
ND
ND
121
1
3231
2.27
6 to 21
ND
ND
ND
95.7
1
3209
2.99
21 to 41
ND
ND
ND
ND
1
3210
6.02
21 to 61
ND
ND
ND
22.6
2
3237
0.10
static
ND
ND
ND
BQL
2
3221
0.10
static
ND
ND
ND
BQL
2
3222
9.05
0.3 to 60.3
ND
ND
ND
19.3
2
3225
8.76
0.3 to 60.3
ND
ND
ND
17.0
3
3256
0.10
static
ND
ND
ND
BQL
3
3257
0.10
static
ND
ND
ND
BQL
3
3261
0.74
0.2 to 5.3
ND
ND
ND
21.5
3
3249
2.25
5.3 to 20.2
ND
ND
ND
11.4
3
3250
2.99
20.2 to 40,2
ND
ND
ND
4.02
3
3252
5.95
20.2 to 60.2
ND
ND
ND
9.34
4
3253
0.10
static
ND
ND
ND
BQL
4
3240
8.90
1.3 to 61.3
ND
ND
ND
14.2
4
3228
8.90
1.3 to 61.3
ND
ND
ND
13.4
ND = Not detected
BQL = Below quantification limit
48
-------
TABLE 3-22. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 4
(SAMPLE C)
(Concentration unit: ng/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
AA
Betiz
Naph
BHT
1
1
1
1
I
3287
3289
3291
3305
3306
1.00
0.75
2.26
2.97
6.02
static
1.5 to 6.5
6.5 to 21.5
21.5 to 41.5
21.5 to 61.5
BQL
29.8
46.9
20.1
7.92
245
161
51.0
14.1
8.77
BQL
BQL
BQL
BQL
BQL
14.9
14.4
19.7
21.9
21.9
2
2
2
3281
3282
3285
1.00
0.99
8.60
static
static
0.7 to 60.7
ND
ND
ND
ND
BQL
BQL
BQL
BQL
BQL
14.9
BQL
5.70
3
3
3
3318
3319
3327
LOO
0.99
5.96
static
static
20.3 to 60.3
16.7
16.2
3.60
BQL
BQL
BQL
BQL
BQL
BQL
10.4
11.3
2.64
4
4
4
3330
3315
3316
1.00
3.09
3.03
static
0.4 to 61
0.4 to 61
13.9
3.93
9.18
BQL
ND
ND
BQL
BQL
BQL
14.6
16.2
20.1
ND = Not detected
BQL = Below quantification limit
49
-------
TABLE 3-23. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 5
(SAMPLE C)
¦3
(Concentration unit: pg/m )
Exposure Sample Sampling Sampling
ID ID Vol. (L) Period (min) P BHT
1
3369
LOO
static
ND
212
13.1
19.8
1
3372
0.74
0.3 to 5.3
ND
170
BQL
14.9
1
3373
2.24
5,3 to 20.3
ND
52.2
5.00
12.8
1
3383
2.97
20.3 to 40.3
ND
25.9
4.50
17.0
1
3384
6.02
20.3 to 60.3
ND
BQL
4.20
17.9
2
3387
0.99
static
ND
BQL
7.80
11.0
2
3388
0.98
static
10.5
BQL
9.80
20.5
2
3354
3.02
0.3 to 60.2
ND
ND
5.00
21.2
2
3355
2.89
0.3 to 60.2
5.10
ND
1.20
ND
3
3501
1.02
static
ND
ND
7.30
10.8
3
3502
1.01
static
ND
ND
BQL
11.9
3
3505
0.75
0.4 to 5.4
8.90
ND
BQL
BQL
3
3507
2.29
5.4 to 20.4
ND
ND
4.70
16.0
3
3508
3.02
20,4 to 40.4
4.10
ND
4.00
14.2
3
3509
5.99
20.4 to 60.4
ND
ND
2.10
15.1
4
3349
0.98
static
BQL
ND
BQL
10.5
4
3510
2.83
0.3 to 60.3
ND
ND
3.70
15.8
4
3358
2.78
0.3 to 60.3
ND
ND
5.50
12.1
ND = Not detected
BQL = Below quantification limit
50
-------
TABLE 3-24. CONCENTRATIONS OF SELECTED INDIVIDUAL COMPOUNDS FOR TEST 6
(SAMPLE A)
(Concentration unit: fJg/m3)
Exposure
ID
Sample
ID
Sampling
Vol. (L)
Sampling
Period (min)
AA
Benz
Naph
BHT
1
1
1
1
1
3549
3552
3553
3555
3556
1.00
0.80
2.27
2.98
6.04
static
0 to 5
5.8 to 20.8
20.8 to 40.8
20.6 to 60.7
58.4
108
99.9
44.8
24.8
ND
ND
ND
ND
ND
43.6
30.5
23.9
27.0
24.0
597
470
404
356
337
2
2
2
2
3558
3559
3522
3523
0.99
0.99
3.23
2.89
static
static
0.4 to 60.4
0.4 to 60.4
49.4
57.2
30.8
24.1
ND
ND
ND
ND
35.1
36.2
24.6
20.0
515
591
428
386
3
3
3
3
3
3
3587
3586
3584
3593
3594
3595
1.00
1.00
0.76
2.25
2.99
5.97
static
static
0.2 to 5.2
5.2 to 20.2
20.2 to 40.2
20.2 to 60.2
28.0
29.2
18.7
17.0
10.2
11.8
ND
ND
ND
ND
ND
ND
27.5
26.7
21.2
18.7
20.7
20.4
457
460
395
383
381
379
4
4
4
3569
3600
3601
0.99
3.27
3.06
static
2.2 to 62.2
2.2 to 62.2
24.2
20.9
20.4
ND
ND
ND
30.5
18.2
18.0
586
434
446
ND = Not detected
3.6 PARTICLE COUNTING
The average particle concentrations during exposure periods are summarized in Table 3-25.
An example of particle concentration profile is shown in Figure 3-9. Without carpet sample in the
source chamber, the particle concentration was about 30 P/em3 (Test 3). The particle concentration
with carpet samples were not much higher than the empty chamber except Test 4, which had the
highest concentration of 740 P/cm3. This high reading, however, may have been caused by the
51
-------
Elapsed Time (min)
Figure 3-9. Particle counting data for Sample A in Test 1.
52
-------
intrusion of laboratory air. During that test, the most serious air leak occurred—the humidified air
flow entering the source chamber reduced by 68 percent by the end of the test (see air flow data in
Table 3-5).
TABLE 3-25. PARTICLE CONCENTRATIONS IN THE EXPOSURE CHAMBER (IN P/cm3)
Test ID
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Test 1
50
N/A1
20
N/A1
Test 2
N/A2
N/A1
N/A3
N/A1
Test 3
30
30
40
20
Test 4
60
630
740
70
Test 5
30
60
50
40
Test 6
N/A3
60
30 140
1 Not measured.
Data lost due to computer problem.
3 Instrument flooding problem.
N/A = data not available.
For comparison purposes, the particle concentrations in the laboratory air were also measured
during each test, and they varied from 1,000 to 10,000 P/cm3.
3.7 MISCELLANEOUS OBSERVATIONS
Sample A, the dark pink low pile carpet, was noted to have a variety of dirt spots on the
samples used for Test 1. The Sample A subset of carpet used for Test 6 was observed to have a large
yellow water stain on one section. During this test, condensation filled the exposure chamber during
the first exposure. This phenomenon was not observed by HERL during animal testing.
Sample C, the indoor/outdoor dark blue carpet, was adhered to the inside of the Tedlar bag
from the glue on the backing of the carpet. Slivers of plywood were attached to the glue. The Tedlar
bags contained about 2.0 mL of sand in one bag. The carpet sections were also marked with an ID
No. on the carpet. The source of these makings was not identified but became a part of the test.
Condensation was again observed in the AEERL system and not in the HERL system during Test 4.
53
-------
The bottom of the chamber cracked from the heat during the first exposure of Test 5. The
chamber was repaired with duct tape and the sampling continued.
54
-------
SECTION 4
DATA QUALITY REVIEW
4,1 DATA QUALITY OBJECTIVES
Data quality objectives as outlined in the test plan are summarized in Table 4-1. In addition,
objectives for temperature control were described in Section 2.6,
TABLE 4-1. DATA QUALITY OBJECTIVES
Measurement Accuracy Precision Completeness
Temperature ± 1°C N/A 85%
Airflow 10% 15% 85%
Relative humidity 10% 15% 85%
Carpet area 10% 15% 85%
Sampling period 5% N/A 90%
GC analysis 15% 15% 90%
Aerosol zero-ehecking <200 P/cm3 N/A 90%
4.2 TEMPERATURE
4.2.1 Sensor Calibration
The thermocouples were calibrated before Test 1 and after Test 6. The temperature medias
used were as follows: iee/water mixture (0 °C), boiling water (100 °C), and warm water (temperature
was determined by an NIST standard thermometer). The calibration data are given in Tables C-l
through C-l2 in Appendix C, The absolute errors varies from 0 to 0.9 °C—all are within the ± 1 °C
55
-------
accuracy objective. The standard deviations for repeated measurements are also satisfactory—ranging
from 0.0 to 0.11 °C.
4.2,2 Temperature Control
Figures 4-1 through 4-3 show the temperature control results for the three key locations in the
experimental system—the outside surface of the source chamber bottom, the air in the source chamber,
and the air in the exposure chamber. All data are the average temperature during the exposure
periods. The air temperature in the exposure chamber is the average of two sampling locations.
For chamber bottom temperature measurements, three out of 24 data points exceeded the
70 ± 5 °C range, 71 percent of average temperature for chamber air exceeded the 37 ± 3 °C range.
Overall, the air temperature was 4 °C higher than the 37 °€ target.
For the temperature measurements in the exposure chamber, nine out of 24 data points
exceeded the 24 ± 2 °C range.
4.3 RELATIVE HUMIDITY
4.3.1 Calibration of Humidity Probes
Humidity probes were calibrated before and after the testing period. Two humidity standards
were used: saturated NaCl solution and saturated LiCl solution. The calibration data are given in
Appendix C (Tables B-13 and B-14). Results show that the responses of the two sensors shifted only
0.5 percent relative humidity (RH).
4.3.2 Humidity Measurement
The desired RH for humidified air was 50 percent. The actual measured RH varied between
41 and 59 percent (Table 4-2). The deviations from 50 percent RH are all within 10 percent.
56
-------
90-
80
75
70-
-b a-
~
~
© 60
>
55-
~
' I—| D ~ O
^ ~ ~
••E3--0-
~ o
a a
~
50-
0
5 10 15 20
Serial Number of Exposures
25
Figure 4-1. Results of temperature control; Chamber bottom panel.
57
-------
60
O
Q
m
i—
3
+¦»
10
j—
o>
a.
E
m
50
45
40
0 35
O)
cd
0 30
>
25-
20
o o
~
o ^ ~
~
~
o
~
O r~i
n ~ O ~ ~
-Q-
xr_Q._S-
"O O"
~ o
0
10 15 20
Serial Number of Exposures
Figure 4-2. Results of temperature control; Source chamber air.
58
-------
35
30
~
~
25
"~ °"a D"
a
o
D O
~
..Q.-Q..-0 q-'O-
~
~
~ P
~
~
a> 20
>
<
15
0
10 15 20
Serial Number of Exposures
25
Figure 4-3. Results of temperature control; Air in the exposure chamber.
59
-------
TABLE 4-2. MEASURED RELATIVE HUMIDITY FOR INLET AIR
Date
Measured
RH (%)
Deviation
from 50% RH
03/09/93
43.1
+6.9%
03/10/93
51.5
+1.5%
03/10/93
45.3
-4.7%
03/11/93
49.7
-0.3%
03/11/93
48.8
-1.2%
03/12/93
52.4
+2.4%
03/12/93
47.6
-2.4%
03/23/93
51.3
+1.3%
03/23/93
59.3
+9.3%
03/24/93
50.2
+0.2%
03/25/93
50.2
+0.2%
03/25/93
50.2
+0.2%
03/26/93
47.9
-2.1%
03/26/93
52.4
+2.4%
03/30/93
52.4
+2.4%
03/30/93
48.8
-1.2%
03/31/93
52.0
+2.0%
03/31/93
54.5
+4.5%
04/01/93
50.6
+0,6%
04/01/93
49.3
-0.7%
04/02/93
54.5
+4.5%
04/02/93
49.5
-0.5%
Average1
2.3%
1 Average was made on absolute values.
60
-------
4.4 AIR FLOW RATE MEASUREMENTS
4.4.1 Sampling Flow Rate
Three sampling flow rates requiring mass flow controllers were used in the experiment: 50,
150, and 400 mL/min. Mass flow controllers were fully calibrated and checked daily. Figures 4-4
and 4-5 show the calibration results for the seven mass flow controllers that had been used to sample
at only one rate setting, and Figure 4-6 shows the results for the three mass flow controllers that had
been used at varied sampling flow rates. All the flow rates were within 10 percent of the target rates.
There were only three flow rates exceeding 5 percent of the desired rate.
4.4.2 Chamber Air Flow Rate
The inlet/outlet flows were all well balanced before the start of each test, and the differences
of the two flow rates were all within 10 percent (see Table 3-7).
The outlet flow rates measured during the tests were also satisfactory (see Table 3-8). The
difference between the desired rate (7 L/min) and those observed ranged from 0.1 to 8 percent.
Because of the continuous heating, the chamber became progressively leakier during the test
period. In two out of six cases, the inlet flow decreased by more than 15 percent at the end of the
test. The worst case occurred in Test 4, in which the flow reduction was as high as 68 percent. Note
that this may not be a data quality problem but rather a problem with the experimental method.
To evaluate the effect of laboratory air intrusion on pollutant concentrations in the
experimental system, laboratory air samples were taken during the testing period. These samples have
been analyzed, and the analytical results were not considered an important factor to the final results of
this study.
61
-------
180
0
CO
cc
£
o
U-
140
130
120
10 15
Calibration Sequence
Controller A-4
Controller B-3 —¦
—* Controller B-4
Controller C-3 ~
Controller C-4
Figure 4-4. Calibration of mass flow controllers (1) Flow rate = 150 mL/min.
62
-------
500
475
450
425
400
375
+10%
-10%
I i 1
r
300
0
10 15
Calibration Sequence
20
Controller A-1 Controller A-2
Figure 4-5. Calibration of mass flow controllers (2) Flow rate =
63
400 mL/min.
-------
200
150-
j loo-
ts
cr
o
50-
+ 10%
•10%
+ 10%
-10%
0-
0
10 15 20
Calibration Sequence
30
Controller A-3 — Controller B-1 Controller B-2
Figure 4-6. Calibration of mass flow controllers (3) Used at two flow rates.
64
-------
4.5 GC ANALYSIS
4.5.1 Detection Limit and Quantification Limit
The Method Detection Limit (MDL) is the smallest amount qualitatively found in a sample
analysis. The Method Quantification Limit (MQL) is defined as the smallest amount that can be
accurately quantified in a sample analysis. The detection and quantification limits for each of the
instruments used for analysis for this project were determined from the variability in the field blanks
collected during the sampling. A field blank is described as a sorbent trap that has been removed
from the storage vial, placed on the sampling system, leak-checked, and then returned to the storage
vial. The field blank then follows the path of the samples to analysis. Because of a noted system
contamination from methylene chloride, all chromatograms would have the area counts for methylene
chloride subtracted before any further analysis of the data.
A total of six field blanks were analyzed by EC I and eleven analyzed by EC II. Detection
limits for TVOC and specified compounds were determined by the following:
MDL = MeanFB + 3 (STD)
where Mean = average ng of the background from the field blank minus MeCl2.
Quantification limits for TVOC and specified compounds were determined by the following:
MQL = MeanFB + 10 (STD)
Tables 4-3 and 4-4 give a complete breakdown of detection limits and quantification limits for both
analytical systems.
65
-------
TABLE 4-3. EC I DETECTION AND QUANTIFICATION LIMITS
Compound
Mean (ng)
RSD
MDL (ng)
MQL (ng)
TVOC
40
16
87
197
Toluene
1.4
0.5
2
6
Benzene
13
4
24
48
4PCH
29
3
10
33
C12
2
1
5
13
TABLE 4-4. EC II DETECTION AND QUANTIFICATION LIMITS
Compound
Mean (ng)
RSD
MDL (ng)
MQL (ng)
TVOC
50
21
114
262
Toluene
2
0.5
3
6
Benzene
6
6
25
67
4PCH
2
0.2
0.6
6
C12
5
3
14
37
Because of the lack of any system background in the retention time region of 4PCH, the
detection limit for 4PCH was determined by the variability in the lowest concentration standard used
for GC response calibration.
MDL = 3(STD)loweststd
MQL = 10 (STD) lowest std
66
-------
4.5.2 Daily QC Check
Liquid toluene standards (106 and 280 ng/jjL) were used for daily QC check. Table 4-5
summarizes the results and Figures 4-7 through 4-8 show the QC chart.
TABLE 4-5. DAILY QC CHECK STATISTICS
Envirochem I Envirochcm II
Total no. of injections 57 14
No. of injections with error > 15% 6 1
4.5.3 Accuracy
The accuracy of the instruments were estimated by making gas standard injections. The
standard used was 165 ppm toluene. Results are summarized in Table 4-6.
TABLE 4-6. DETERMINATION OF ACCURACY FOR TOLUENE
Envirochem I
Envirochem II
Total no. of injections
32
41
No. of injections with error > 15%
• 5
3
4.5.4 Precision
The precision of the GC results was measured by comparing duplicate samples. Table 4-7
summarizes the results of the duplicate samples that were collected over the course of this study.
Several duplicates were lost because of instrument malfunctions, changes in analysis protocol, and
concentrations that were below the quantification limits for the instrument. Tables 4-8 through 4-11
give the precision estimates for TVOCs and individual compounds.
67
-------
100-
80-
60-
40-(
, D Upper Limit (15%)
«f; ^ ..... ,, , [ „ t i „ „„ . ,,,, 4 ( __ _
D ° rP EtFtP m CD __ _ S ctP cy-1 ~ tP cFn
a —d.,—.............. crB .~ pj-3 o q it?...
u O ~ ~ ~ ~
g z.
~20i Lower Limit (-15%)
-40-
-60-
-80*
~
-100-J 1 1 I ~
0 20 40
Injection Sequence Number
Figure 4-7. GC daily QC check results (1) Envirochcm I/Liquid Toluene standard.
68
-------
/
100-
80-
60-
40-
20_, Upper Limit (15%)
~
0-j q----- -p. n z: Q "d""
n r-i D ^ ~ o
..o J= 9. ...S. _ Jz
o
Lower Limit (-15%)
-60-
-80-I
-100-
0 5 10 15
Injection Sequence Number
Figure 4-8. GC daily QC check results (2) Envirochem II/Liquid Toluene standard.
69
-------
TABLE 4-7. DUPLICATE SAMPLES STATISTICS
Pairs
Total no. of duplicates collected 23
Total no. lost 6
No. with error > 15% for TVOC 2
TABLE 4-8. COMPARISON OF DUPLICATE SAMPLES—TVOC
Sample ID
Cone. Mg/m3
Sample ID
Cone, pg/m3
Mean conc.
RSD (%)
2995
1890
2997
1584
1737
12
3055
2300
3058
2041
2170
8.4
3034
1649
3035
1554
1602
4
3105
164
3106
200
182
14
3112
162
3113
129
145
16
3222
112
3225
117
115
4
3240
76
3228
72
74
4
3281
7583
3282
6101
6842
15
3318
7222
3319
7301
7262
1
3315
2468
3316
2751
2610
8
3387
7068
3388
7728
7398
6
3354
3181
3355
1013
2097
73
3510
2016
3358
2033
2024
1
3558
4739
3559
4929
4831
3
3522
2323
3523
2073
2198
8
3587
3457
3586
3350
3404
2
3600
2025
3601
1967
1996
2
RSD = Relative standard deviation
70
-------
TABLE 4-9. COMPARISON OF DUPLICATE SAMPLES—ACETIC ACID
Sample ID Cone. Mg/m3 Sample ID Cone, ng/ra3 Mean conc. RSD1 (%)
2995
15
2997
13
14
10
3034
11
3065
5
8
55
3318
17
3319
16
16.5
2
3315
4
3316
9
7
57
3558
49
3559
57
53
10
3522
31
3523
24
28
17
3587
28
3586
29
28.6
3
3600
21
3601
20
20.7
1.7
1 Three out of eight pairs have RSD >15%.
TABLE 4-10. COMPARISON OF DUPLICATE SAMPLES—NAPHTHALENE
Sample ID
Conc. pg/m3
Sample ID
<2
Conc. pg/m
Mean conc.
RSD1 (%)
2995
20
2997
17
19
10
3034
15.2
3065
15.4
15.3
1
3387
8
3388
10
9
16
3354
5
3355
1.2
3
88
3510
3.7
3358
5.5
5
28
3558
35.1
3559
36.2
35.7
2.3
3522
24
3523
20
22
15
3600
18.2
3601
18.0
18.1
0.6
1 Three out of eight pairs have RSD > 15%.
71
-------
TABLE 4-11.
COMPARISON OF DUPLICATE SAMPLES—BHT
Sample ID
Cone, pg/m3
Sample ID
Cone. |Ag/m3
Mean conc.
RSD1 (%)
2995
413
2997
360
386
10
3055
344
3058
290
317
12
3034
401
3065
411
406
2
3105
27
3106
32
29
12
3312
31
3113
21
26
27
3222
19
3225
17
18
9
3240
14
3228
13
13.5
4
3318
10.4
3319
11.3
10.8
6
3315
16
3316
20
18
15
3387
11
3388
20
16
43
3510
16
3358
12
14
19
3558
515
3559
591
553
10
3522
428
3523
386
407
7
3587
457
3586
460
458
0.4
3600
434
3601
446
440
2
1 Three out of 11 pairs have RSD > 15%.
4.5.5 Completeness of ST032 Sorbent Samples
The total number of planned observations was 138, and the number of valid observations was
101. This gives the completeness of 73 percent.
4.6 IDENTIFICATION OF INDIVIDUAL COMPOUNDS
The identification of individual compounds required both electronic and manual evaluation of
the results as presented in Section 2 of this report, RTI was designated as the primary source for
compound identification because of the availability of a high resolution GC/MS system. Acurex
Environmental provided backup to RTI with the EC II GC system that split the effluent from the
column to an MSD and an FID. This provided both qualitative and quantitative evaluation of the
compounds. To ensure comparable responses for all three analytical systems, a standard containing
72
-------
the even n-alkanes (Cg~C20), toluene, and 4PCH was utilized for the purpose of establishing a
retention time correlation and response factor database between the three analytical systems used in
this study, Sorbent traps were spiked with this standard and analyzed on all systems. RTI spiked a
series of sorbent traps with their system to verify the comparability of spiking systems for the purpose
of daily QC checks of their MS system.
4.7 QUANTIFICATION OF INDIVIDUAL COMPOUNDS
The quantification of individual compounds required correlation of marker retention times
from the RTI MS output and Acurex Environmental MSD output to the FID output from EC I.
Manual interpretation of the FID chromatogram from EC I and total ion chromatogram (TIC) from
EC II MSD and RTI MS to match peak shapes and patterns was also performed. For the prominent
emissions/peaks this process proved successful as reported in Table 4-11, results of duplicate analysis
for BHT. The evaluation of compounds found in low concentrations or compounds that showed poor
chromatography, such as acetic acid (Table 4-9), was more difficult and required extensive manual
interpretation of the GC data.
4.8 EFFECTIVENESS OF CHAMBER CLEANING
One question asked in the test plan was, "Is there any memory of carpet emissions in a
cleaned, reused aquarium?" Five different aquariums, AQ0-AQ4, were used in this study including
those used by HERL. The most repeated use of an aquarium was three times each by AQ3 and AQ4.
Figures 4-9 and 4-10 show the TVOC profiles of duplicate 3-L samples collected from heated empty
chambers after cleaning. The MSD analysis identifies siloxanes, toluene, and BHT as the major
emissions from a cleaned chamber. The differences in the TVOC emissions from each use can be
attributed to differences in air supply or poor cleaning. As mentioned previously, the zero-grade air is
¦3
certified to contain less than 0.1 ppm THC. This can be equated to -400 jig/m toluene. RTI
identified 4PCH in the empty chamber experiments (Tests 2 and 3). This was not confirmed by
Acurex Environmental's evaluation of the chamber emissions.
73
-------
HERLTest2 AEERLTest4 HERLTestS
Repeated use of source chamber
Figure 4-9. Chamber background: Aquarium 3.
74
-------
AEERL Test 2 AEERLTest 3 AEERLTest 5
Repeated use of source chamber
Figure 4-10, Chamber background: Aquarium 4.
75
-------
4.9 PARTICLE COUNTING
The particle counter used requires factory calibration. The last calibration was made before
the tests started (February 8, 1993), and the calibration remains valid for one year.
During the testing period, zero-checking was made each day to ensure that there were no leaks
in the instrument or in the sampling line. All the zero-checks passed the 200 P/cm3 objective with
typical values below 10 P/cm3 (Table 4-12).
TABLE 4-12. ZERO-CHECKING RESULTS FOR PARTICLE COUNTER1
(Unit: P/cm3)
Test ID
Exposure 1
Exposure 2
Exposure 3
Exposure 4
1
OK
N/A
OK
N/A
2
N/A
N/A
OK
N/A
3
OK
<20
OK
<10
4
<1
<1
<1
<1
5
<1
<10
<10
N/A
6
<10
<10
<1
<10
1 In early experiments, the actual zero-check readings were not recorded. OK means the check passed
(reading is below 200 P/cm3).
During the testing period, the instrument flooded with newly added 2-propanol several times.
(This instrument requires adding alcohol after use for several hours.) This phenomenon may give
faulty high concentration readings for a period of time. Serious flooding occurred during Exposure 1
of Test 2 and Exposure 1 of Test 6. Consequently, these two sets of particle data were not used.
After the tests were completed, the problem was discussed with a representative of the
manufacturer of the instrument. The manufacturer advised running the instrument for about 10 min
while turning it upside down—an action that the operation manual does not recommend. The
manufacturer stated that the newer model of this instrument no longer has the problem.
76
-------
4.10 AUDITS
Three external audits were performed by the AEERL Quality Assurance (QA) program during
the course of this project. The first was an audit to evaluate the test plan for the study. The second
was a technical systems audit, and the third was audit to examine the analysis and data reduction
procedures as compared to those documented in the laboratory QA Project Plan (QAPP). We have
responded to all comments and correction measures were made.
The first audit of the test plan resulted in the reconstruction of the study test plan into separate
plans for each laboratory. All findings and comments were responded to in an appropriate manner.
The second external audit for the technical systems found only a few problems with the most
serious being "operating procedures of the laboratory are scattered throughout several documents and
some are not available." At the start of this project, the laboratory had an approved QAPP. However,
it did not encompass all the fabricated systems and new equipment that was necessary for this study.
Because of the time restraints placed on this project, each issue was addressed as it surfaced. All of
the concerns that were noted in the audit were amended.
The analysis and data reduction audit pointed out the need for a more standardized data
management process. These issues have been addressed. The data management procedures that
proved to be effective during Phase I of this project will be documented in a SOP format and included
in the laboratory facilities manual. An internal evaluation of custody and document procedures was
also performed by the Acurex Environmental QA staff.
4.11 CONCLUSIONS ON DATA QUALITY REVIEW
All the data quality goals have been achieved except the following.
(1) Average air temperature in the source chamber: Overall, the actual temperature was
4 °C higher than the 37 °C target.
(2) Air temperature in the exposure chamber: 9 out of 24 exposure periods had
temperatures exceeding the 24 ± 2 °C range.
-------
(3) Due to sample loss, the completeness of ST032 sorbent samples was 73%, whereas
the target was 85%.
(4) For the analysis of individual compounds, about one-third duplicate samples showed
relative standard deviations (RSD) greater than the target 15%. Several pairs of
duplicate samples had very large RSD. We recommend that the analytical results for
individual compounds be considered semi-quantitative.
78
-------
SECTION 5
DISCUSSION OF RESULTS
5.1 COMPARISON OF INITIAL TVOC CONCENTRATIONS IN THE SOURCE CHAMBER
After a one-hour heating period without air flow, the peak TVOC concentration in the source
chamber was reached. This peak concentration was determined by directly sampling from the source
chamber before the dynamic mode started. A comparison of peak TVOC concentrations between the
two carpet samples is shown in Figure 5-1. All values in the graph are averages of duplicate tests.
We were unable to quantify the initial concentrations for the mock samples (Tests 2 and 3) because
the sample volumes were too small.
5.2 COMPARISON OF AVERAGE TVOC CONCENTRATION IN THE SOURCE CHAMBER
DURING THE EXPOSURE PERIOD
The calculation of average concentrations found in the source chamber involves the following
two steps: (1) calculating the area under the time-concentration curve by means of integration and (2)
calculating the average concentration. The curve integration can be approximated by:
\ - £ (C, At,)
1=1
where Ac is the area under the time-concentration curve, in (jig m"3 min);
Cj is the concentration for sample i, in (pg m );
79
-------
CO
CO
3
c
.2
»
2
-*—*
c
m
o
c
o
o
10000
8000
6000
4000
2000
Exp 2 Exp 3
Exposure ID
Sample A Sample C
Figure 5-1. Initial TVOC concentrations in the source chamber.
-------
Atj is the sampling period for sample i, in (min); and
N is the total sample number, excluding the overlapping samples.
The average concentration can then be determined from:
1
where Cx is the average concentration during an exposure, in (fjg/in ); and
tx is the exposure period, in (min).
The calculated results are given in Table 5-1 and Figure 5-2.
TABLE 5-1. AVERAGE TVOC CONCENTRATIONS IN THE EXPOSURE CHAMBER (in pg/m3)
Test No.
Exposure 1
Exposure 2
Exposure 3
Exposure 4
1
2740
1740
1280
1600
2
79
182
227
145
3
274
115
63
74
4
4440
1890
2200
2750
5
3480
2100
2500
2020
6
2830
2200
1880
2000
5.3 CALCULATION OF TOTAL AMOUNT OF TVOC ELUTED FROM THE SOURCE
CHAMBER DURING AN EXPOSURE
The total amount of a given pollutant eluted from the source chamber can be calculated from:
WE=CxQtx
where WE is the total mass eluted from the source chamber, in (jag); and
Q is the air exchange flow rate through the system, in (nrVmin).
81
-------
Exp 1
Exp 2 Exp 3
Exposure ID
Exp 4
Sample A
'///,
Sample B
Sample C
Figure 5-2. Average TVOC concentrations during exposure periods.
82
-------
In our case, tx is equal to 60 min and Q = 8 x 10 m /min, which is the sum of the outlet flow rate of
the exposure chamber and the total sampling flow. Table 5-2 gives the results for the six tests. As
VOC emitters, the source strengths for Sample A and Sample C are of the same order, whereas the
source strength of Sample B is about one order of magnitude lower than the other two samples.
TABLE 5-2. THE AMOUNT OF TVOC ELUTED FROM THE SOURCE CHAMBER
DURING EACH EXPOSURE (in ng)
Test ID
Sample ID
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Total
1
A
1320
834
616
769
3539
2
B
38
87
109
70
304
3
B
132
55
30
35
252
4
C
2130
908
1060
1320
5418
5
C
1670
1010
1200
972
4852
6
A
1360
1060
904
958
4282
5.4 ESTIMATION OF THE PERCENTAGE OF TVOC EMITTED DURING ONE-HOUR STATIC
HEATING PERIOD
The total TVOC emitted in one exposure cycle can be divided into two parts: those from
during the one-hour pre-exposure heating period (static mode) and those from the one-hour exposure
period (i.e., dynamic mode). The ratio of the two parts can be calculated from:
Ps = WS0 / (WB + WS1)
where Ps is the percentage of TVOC emitted before the dynamic mode started;
WSq is the amount of TVOC in the source chamber before the start of dynamic mode;
Wg is the amount of TVOC eluted during the dynamic mode; and
WS1 is the amount of TVOC left in the source chamber after the exposure.
83
-------
Since the last term is small, a rough estimation can be made by letting WS1=0. Data in Table 5-2 can
be used as WE, and Wso is the product of initial concentration (see Table 5-1) and the net volume of
the source chamber. The calculated results in Table 5-3 suggest that the majority of the TVOCs were
emitted during the exposure period and only less than one quarter were emitted in the static heating
period. This can be explained by the "vapor pressure effect"—the elevated TVOC concentration in the
air prevented the further emissions from the source. When the air flow started, the chamber air was
diluted allowing more VOCs to be emitted from the source.
TABLE 5-3. PERCENTAGE OF TVOCs EMITTED BEFORE DYNAMIC MODE STARTED
Test No.
Exposure 1
Exposure 2
Exposure 3
Exposure 4
1
23%
12%
12%
N/A
2
N/A
N/A
N/A
N/A
3
N/A
N/A
N/A
N/A
4
20%
27%
25%
16%
5
14%
27%
15%
16%
6
23%
16%
13%
15%
5.5 THE CHANGES OF TVOC COMPOSITION DURING THE TEST
Not only did the average TVOC concentration levels change during the test, but the TVOC
composition also changed. Figures 5-3 through 5-8 show the different trends for the three samples
tested.
For Sample A, the heavier components (>Cj2) were not dominant in the first exposure. In the
last exposures, however, they became the most abundant components. In contrast, the lighter
components followed a decay trend consistently.
For Sample B, the heavier compounds seemed dominant throughout the test. However, the
reasons for differences between the patterns for Test 2 and Test 3 is not known.
84
-------
1200
S2 1000
Exp 1
Exp 2 Exp 3
Exposure ID
Exp 4
C12
Figure 5-3. The change of TVOC composition during exposure; Sample A, Test 1.
85
-------
CO
O)
3
c
o
"S
0
o
o
o
Exp 1
Exp 2 Exp 3
Exposure ID
Exp 4
C12
Figure 5-4, The change of TVOC composition during exposures; Sample A, Test 6.
86
-------
CO
Ui
3
c
o
CO
-4-»
c
C12
Figure 5-5. The change of TVOC composition during exposures; Sample B, Test 2.
87
-------
CO
500
450
400
g> 350
c
_o
"¦tf
CO
k_
c
©
o
c
o
O
Exp 1
Exp 2 Exp 3
Exposure ID
Exp 4
C12
Figure 5-6. The change of TVOC composition during exposures; Sample B, Test 3.
88
-------
Exposure ID
C12
Figure 5-7. The change of TVOC composition during exposures; Sample C, Test 4.
89
-------
Exp 1
Exp 2 Exp 3
Exposure ID
Exp 4
C12
Figure 5-8, The change of TVOC composition during exposures; Sample C, Test 5.
90
-------
For Sample C, the components in the intermediate range (C8~C]2) were most dominant
throughout the test. From Exposure 1 to Exposure 4, the emissions of lighter compounds tended to
decay, but the heavier components remained relatively steady.
5.6 EMISSIONS OF INDIVIDUAL COMPOUNDS
5.6.1 Acetic Acid
Sample A was the strongest emitter of acetic acid among the three samples. The average
concentration in the exposure period varied from 7 to 50 fig/m3. A small amount of acetic acid was
emitted from Sample C, and no acetic acid was emitted from Sample B.
5.6.2 Benzene
Sample C was the only sample that emitted benzene, and benzene was only found in the first
exposure. The average concentration was 36 pg/m for Test 4 and 27 pg/m for Test 5.
5.6.3 Naphthalene
Sample A was the strongest emitter of naphthalene among the three samples. The average
concentration in the exposure period varied from 14 to 24 jig/m . Smaller amounts of naphthalene
were emitted from Sample C (less than 5 pg/m }, and no naphthalene was emitted from Sample B.
5.6.4 BHT
Again, Sample A was the strongest emitter of BHT (300-400 pg/m3) and much stronger than
•j
the other two samples. Concentration levels for Samples B and C were comparable (10-20 pg/m ).
No significant decay of BHT was apparent during the testing of all three samples.
5.7 CONCENTRATION CHANGES OF INDIVIDUAL COMPOUNDS DURING THE TEST
The concentration changes of individual compounds followed different patterns. Figure 5-9
compares the average concentrations of three compounds from Sample A. During a four-exposure
period, the concentration of acetic acid had significant decay (about 50 percent), naphthalene decayed
only slightly, and BHT remained fairly stable.
-------
CO
CD
3-
c
g
"¦4-1
(d
c
0)
o
c
o
O
xz
CL
cd
c6
<
<
500
-400
200
100
Exp-1
Exp-2 Exp-3
Exposure ID
Exp-4
CD
CD
D
300 §
cd
•4-1
c
©
o
c
o
O
l—
X
CD
AA ^ Naph ^ BHT
Figure 5-9. Concentration changes for three compounds during exposures the tests of Sample A.
92
-------
5.8 MOST ABUNDANT VOLATILE ORGANIC COMPOUNDS IN THE CARPET EMISSIONS AS
SAMPLED ON MULTI-SORBENT TRAPS
Tables 5-4 through 5-6 outline the 10 most abundant compounds found in the emissions from
each of the study sources. The compounds were identifications made from the 60 minute samples
taken in the second exposure.
TABLE 5-4. TEN MOST ABUNDANT COMPOUNDS IN THE EMISSIONS FROM SAMPLE A
Experiment 1
Experiment 6
Compound
Cone, (jig/m3)
Compound
Cone, (jig/m3)
Butylatedhydroxytoluene
386
Butylatedhydroxytoluene
407
Toluene
134
Nonanal
108
Nonanal
49
Cj2 Alkene
70
Tri(t-butyl) phenol
48
Siloxane Isomer
65
Cj2 Alkene
40
Siloxane Isomer
63
Cjj Alkene
34
C12 Alkene
55
C|2 Alkene
26
Tri(t-butyl) phenol
55
Siloxane Isomer
24
C12 Alkene
40
n-Hexadecane
27
Siloxane Isomer
35
Isopropanol
26
Unknown
35
93
-------
TABLE 5-5. TEN MOST ABUNDANT COMPOUNDS TN THE EMISSIONS FROM SAMPLE B
Experiment 2
Experiment 3
Compound Cone.
fig/m3
Compound
Cone, pg/m3
Toluene
44
Toluene
21
Butyl atedhydroxytoluene
29
Butylatedhydroxytoluene
18
Siloxanc Isomer
7
Acetone
5
Siloxane Isomer
5
Siloxane Isomer
5
Siloxane Isomer
5
Siloxane Isomer
4
Siloxane Isomer
4
Siloxane Isomer
4
C13 Hydrocarbon coelution
3
Siloxane Isomer
3
Siloxane Isomer
3
Siloxane Isomer
3
Siloxane Isomer
3
CI3 Hydrocarbon coelution
3
Siloxane Isomer
3
Isopropanol
3
TABLE 5-6. TEN MOST ABUNDANT COMPOUNDS IN THE EMISSIONS FROM SAMPLE C
Experiment 4
Experiment 5
Compound
Cone, (pg/m3)
Compound
Cone, (pg/m3)
Siloxane Isomer
89
Cyclic Alkane
178
Cjj Alkene
64
Nonanal
169
Siloxane Isomer
59
C12 Alkane
100
Unknown coelution
57
C12 Alkene
95
Nonanal
53
Alkene
83
Siloxane Isomer
49
Phenol
73
C12 Alkene
42
Cj2 Alkene
69
C|2 Alkene
42
C12 Alkene
68
Unknown
40
Unknown
63
Unknown coelution
39
Unknown
62
94
-------
It should be pointed out, however, that the top ten lists were variable depending on when the
air samples were taken. Tables 5-7 and 5-8 illustrate such changes by comparing the top 10
compounds in the air sample taken from static chamber prior to exposure 1 and those in the 60-minute
sample taken during exposure 2.
TABLE 5-7. THE CHANGE OF TOP TEN LIST DURING TEST 1 (SAMPLE A)
Exposure 1 (Static Chamber)
Exposure 2 (60-min Sample)
Compound
Cone. (|ig/m3)
Compound
Cone. (|ig/m3)
Toluene
3036
Butylatedhydroxytoluene
386
Isopropanol
1980
Toluene
134
Acetone
1241
Nonanal
49
Sulfur Dioxide
527
Tri(t-butyl) phenol
48
C4 Alkene(?)
299
C|2 Alkene
40
Butylatedhydroxytoluene
242
Cj2 Alkene
34
Nonanal
146
Cj2 Alkene
26
Benzene
139
Siloxane Isomer
24
Siloxane Isomer
99
n-Hexadecane
27
Siloxane Isomer
98
Isopropanol
26
95
-------
TABLE 5-8. THE CHANGE OF TOP TEN LIST DURING TEST 6 (SAMPLE A)
Exposure 1 (Static Chamber)
Exposure 2 (60-min Sample)
Compound
Cone, (fig/m3)
Compound
Cone, (ng/m3)
Butylatedhydroxytoluene
597
Butlyatcdhydroxytoluene
407
Nonanal
357
Nonanal
108
Acetone
343
C12 Alkene
70
C12 Alkene
322
Siloxane Isomer
65
Isopropanol
296
Siloxane Isomer
63
Siloxane Isomer
294
Cj2 Alkene
55
C4 Alkene(?)
289
Tri(t-butyl) phenol
55
Ethano!
251
Cj2 Alkene
40
Toluene
232
Siloxane Isomer
35
Siloxane Isomer
232
Unknown
35
96
-------
SECTION 6
CONCLUSIONS
The objective of this study was to characterize the physical parameters of the test system and
the chemical emissions from two specific carpet samples and the empty source chamber under test
protocol conditions. The experimental system used for the physical and chemical characterization was
identical to the system used by HERL in their bioresponse testing. Although the experimental systems
were identical in design and materials, the emissions generated during testing with individual systems
could be different based on the following observations:
• Non-uniform heating of chamber surfaces, chamber air, and carpet samples
• Development of air leakage in chambers during testing
• Emissions of pollutants from the source chamber
• Inadequate temperature control because of low precision manual temperature controls
The study results indicate that environmental conditions could not be precisely controlled or
reproduced. Therefore, there is no assurance that identical systems would produce identical emissions.
More than 200 compounds were emitted by the two carpet samples that were tested. Twenty nine of
the 200 compounds (15 percent) were identified by GC/MSD and confirmed, and another 70 percent
were tentatively identified. Of the 29 compounds that were confirmed, 58 percent were found in both
carpet samples tested and five of the confirmed compounds were observed in all three of the test
samples (two carpets and empty chamber). The majority of the emissions from the empty source
-------
chamber were siloxane isomers with most of the emissions being less than the quantification limits of
the analytical instruments.
Quantitative differences of some of the individual compounds were observed during an
exposure, between the four successive exposure cycles of a single test and between replicate test using
different subsets of the same carpet sample. Although the same flow rate and temperature protocols
were followed throughout this study and replicate subsets of the same carpet samples were tested, no
two exposures produced the same emission profile. During the exposure period, the TVOC
concentration and concentrations of some individual compounds decreased with time but did not
exhibit an exponential decay. Some of the predominant highly volatile compounds observed in the
first exposure were below the detectable limits of the analytical systems in subsequent exposures. The
emissions from these tests were a function of the exposure protocol and the time during the exposure
at which the samples were collected.
No evidence was found to support the hypothesis that the carpet samples could generate a
significant amount of particles under the experimental conditions.
The data reported in this document are representative only of the two carpet samples tested during this
study. The carpet samples evaluated were not new; some of the emissions may have been of
chemicals adsorbed onto the samples during previous use.
98
-------
SECTION 7
REFERENCES
Mason, M., Krebs, K., Roache, N., and Dorsey, J. "Practical Limitations of Multisorbent
Traps and Concentrators for Characterization of Organic Contaminants of Indoor Air,"
Measurement of Toxic and Related Air Pollutants. VIP 25, A&WMA, 1992.
TSI Inc., "Porta Count Operation and Service Manual," March 1991.
Tichenor, B.A. and Guo, Z. "The Effect of Ventilation on Emission Rates of Wood Finishing
Materials, Environmental International. Vol. 17, pp 317-323, 1991.
99
-------
APPENDIX A
SAMPLING SUMMARY
100
-------
TABLE A-1. SAMPLING SUMMARY FOR EXPERIMENT 1
Day 1 Experiment 1
March 9, 1993 HERL 93-17
CPSC 1292/60,47,21 Anderson 921 -924 9303O9.AQ2
Envirochem 1
Envirochem 2
RTI
Exposure 1 temp. 21
8°C
RH 33.9%
BP 30.08 in Hg Dynamic 11:03:50 12:05:29 T & P
Time (min)
Tube ID
Volume
-------
TABLE A-2. SAMPLING SUMMARY FOR EXPERIMENT 2
Day 1 Experiment 2 March 11, 1993 HERL 93-17
CPSC 1768 Anderson 925 - 928
930311.AQ4
Envirocliem 1
Etivirochem 2
RTI
Exposure 1
temp. 20,?°C
RH 29.2%
BP 30.02 in Hg Dynamic 11.03:23 12:03:51 T & P
Time (min)
Tube ID
Volume (L)
Tube ID
Volume (L)
Tube ID
Volume (L)
1.25 SC
3013
lost
.100
3030 3/16
.100
3025
.100
5
3015
lost
.800
15
3016
lost
202
20
3006
3/15
3.0
3005 3/16
3.0
40
3007
3/15
5,9
3010
lost
LB
3027 3/16
LB
3024
LB
3012
lost
FB
3029 3/16
FB
Exposure 2
temp. 22,3°C
RH 29.2%
BP 30.07 in Hg Dynamic 14:29:00 15:34:05 Temp.
1.25 SC
3101
3/8
.100
1.25 SC
3103
3/8
.100
60
3105
3/8
9.0
60
3106
3/8
8.8
3107
3/8
LB
Day 2 Experiment 2
March 12. 1993
930312.AQ4
Exposure 3
temp. 2Q.2°C
RH 52.4%
BP 30.23 in Hg Dynamic 9:27:00.,... 10:36:25 T & P
1.25 SC
3125
lost
.100
3147 3/16
.100
1.25 SC
3126
lost
.100
5
3129
3/15
.7595
15
3118
3/15
2.195
20
3117
3/15
2.96
3114(Lab Air)a
3.1
40
3115
3/15
5.996
3123
lost
LB
3144 3/16
LB
3124
lost
LB
3145 3/16
FB
Exposure 4
temp. 22.2°C
RH 27.5%
BP 30,22 in
Hg Dynamic 13:20:25 14:32:20 Temp,
1.25 SC
3109
3/15
.100
3149
.100
60
3112
3/15
3.3
60
3113
3/15
3.4
3108
lost
LB
3148
LB
102
-------
TABLE A-3. SAMPLING SUMMARY FOR EXPERIMENT 3
Dav 1 Experiment 3
March 23, 1993 HERL 93-19
CPSC 1399 Anderson 940 - 943
930323.AQ4
Envirochem 1
Envirochem 2
RTI
Exposure 1
temp. 21.6°C
RH 41.3%
BP 30.36 in Hg Dynamic 10:38:30 11:52:30 T & P
Time (min)
Tube ID
Volume (L)
Tube ID
Volume (L)
Tube ID
Volume (L)
1.25 SC
3217 (HERL)
.100 3/24
1,25 SC
3233
3/22
.100
3214 3/24
,100
3205
,100
5
3229
3/22
.757
15
3231
3/22
2.27
20
3209
3/22
2.99
3216 3/24
2.99
40
3210
3/22
6.02
60
3208(Lab Air)*
9.09 3/24
3226
3/22
LB
3211 3/24
LB
3204
LB
3227
3/22
FB
3213 3/24
FB
FB
Exposure 2
temp, 23.3 °C
RH 59.3%
BP 30.28 in Hg Dynamic 14:17:30 15:21:20 T & P
1.25 SC
3237
3/22
.100
1,25 SC
3221
3/22
.100
60
3222
3/22
9.05
60
3225
3/22
8.76
3219
3/22
LB
Day 2 Experiment 3
March 24,
1993
930324.AQ4
Exposure 3
temp. 22.1°C
RH 58,4%
BP 30,08 in Hg Dynamic 10:38:45 11:39:35 T & P
1.25 SC
3256
3/22
.100
3244 3/25
.100
1.25 SC
3257
3/22
.100
5
3261
3/22
0.744
15
3249
3/22
2.25
20
3250
3/22
2.99
40
3252
3/22
5,95
3255
3/22
LB
3241 3/25
LB
3258
3/22
FB
3245 3/25
FB
251
3246{Lab Air)*
12.6 3/25
Exposure 4
temp. 22.2°C
RH 61.2%
BP 30.06 in Hg Dynamic 13:49:00 14:53:10 T & P
1,25 SC
3253
3/22
.100
3239
,100
60
3240
3/22
8.9
60
3228
3/22
8.9
3247
3/22
LB
3238
LB
103
-------
TABLE A-4. SAMPLING SUMMARY FOR EXPERIMENT 4
Day 1 Experiment 4 March 25, 1993 HERL 93-20
CPSC 1925/27,56,65
Anderson 944 - 947 930325.AQ3
Envirochem 1
Envirochem 2
1 RTI
Exposure 1
temp. 21.7°C
RH 49.6%
BP 30.18 in Hg
Dynamic 10:54:35 11:55:50 T & P
Time (inin)
Tube ID
Volume (L)
Tube ID
Volume (L)
Tube ID
Volume (L)
1.25 SC
3298 (HERL)
.100
3/26
6.67 SC
3287
3/29
0.997
3299 3/25
1.0
3304
.997
5
3289
4/9
0.748
15
3291
4/9
2,26
20
3305
4/9
2,97
3301 3/26
2.99
40
3306
4/9
6,02
3286
lost
LB
3295 3/26
LB
3303
LB
3309
3/22
FB
3300 3/26
FB
Exposure 2
temp. 21
8°C
RH 46,6%
BP 30.23 in Hg
Dynamic 14:20:50 15:22:10 T & P
6.67 SC
3281 4/8
0,998
6,67 SC
3282 4/12
0.992
60
3283 *
9.04
60
3285 4/8
8,6
3280
3/22
LB
Day 2 Experiment 4 March 26, 1993
930326.AQ3
Exposure 3
temp. 21J
!°C
RH 46.6%
BP 30 23 in Hg
Dynamic 10:49:00 11:51:10 T & P
6.67 SC
3318
4/12
0.999
3311 3/33
0.993
6.67 SC
3319
4/12
0.993
5
3323
lost
0.745
15
3325
lost
2.25
20
3329
lost
2,97
40
3327
4/12
5.96
3317
lost
LB
3310 3/30
LB
3322
3/29
FB
3313 3/30
FB
Exposure 4
temp. 21.
8"C
RH 46,6%
BP 30.23 in Hg
Dynamic 14:14:45 15:17:30 T & P
6.67 SC
3330
4/12
0.999
3333
0.993
60
3315
4/12
3.09
60
3316
4/12
3.03
3324
3/29
LB
3331
LB
104
-------
TABLE A-5. SAMPLING SUMMARY FOR EXPERIMENT 5
Day 1 Experiment 5 March 30, 1993 HERL 93-21
CPSC 1508/5,42,21 Anderson 95?
-961 930330.AQ4
Envirochem 2
Envirochem 2
RTI
Exposure 1
temp.
22.4X
RH 42%
BP 29.88 in Hg Dynamic 11:43:35 12:49:15 T & P
Time (mill)
Tube ID
Volume (L)
Tube ID
Volume (L)
Tube ID
Volume (L)
1,25 SC
6.67 SC
3369
4/13
LOO
3365 4/1
1.00
3353 *
0.99
5
3372
4/13
0.74
15
3373
4/13
2.24
20
3383
4/13
2.97
3364 4/1
2.99
40
3384
4/13
6.02
60
3361 (LA) 4/5
9.08
3367
4/13
LB
3360 m
LB
3357 *
LB
3371
4/13
FB
3363 4/1
FB
1 Exposure 2
temp, 23.6°C
RH 47.1%
BP 29.83 in Hg Dynamic 15:05:15 16:06:45 T&P
6.67 SC
3387
4/14
0.99
6.67 SC
3388
4/14
0,98
60
3354
4/14
3.02
3347 (LA) 4/5
9.01
60
33S5
4/14
2.89
3382
4/13
LB
Day 2 Experiment 5
March 31, 1993
930401. AQ4
Exposure 3 temp.20.8
°C
RH 49.6%
BP29.91 in Hg
Dynamic 10:52:15 11:53:40
T&P
6.67 SC
3501
4/16
1.02
3390 4/3
1.01
6,67 SC
3502
4/14
1,01
5
3505
4/16
0.75
15
3507
4/16
2.29
20
3508
4/16
3.02
40
3509
4/15
5.99
3500
4/13
LB
3389 4/1
LB
3503
4/13
FB
3391 4/1
FB
60
3393 (LA) 4/3
9.162
Exposure 4 temp, 22.7
°C
RH 68.3%
BP 29.56 in Hg Dynamic 14:11:25 15:15:00 T&P
6,67 SC
3349
4/15
0.98
3352 *
0.98
60
3510
4/15
2.83
3395 (LA) 4/3
8.97
60
3358
4/15
2.78
3506
4/13
LB
3348 »
LB
105
-------
TABLE A-6. SAMPLING SUMMARY FOR EXPERIMENT 6
Day 1 Experiment 6 HEEL 93-22 CPSC 1378/45,12,50 Anderson 962-965
9304O1.AQ1
Envirochem 1
Envirochem 2
1 RTI
Exposure 1
temp. 22,3'C
RH 65.8%
BP 29.62 in Hg
Dynamic 10:12:00 11:14:00 T & P
Time (min)
Tube ID
Volume (L)
Tube ID
Volume (L)
Tube ID
Volume (L)
1,25 SC
3543 (HERL)*
0.100
4/2
6.67 SC
3549
4/12
1.00
3545 4/2
1.01
3520 *
1,00
5
3552
4/12
0.80
15
3553
4/12
2.27
20
3555
4/12
2.98
3547 4/2
3.00
40
3556
4/12
6.04
60
3542 4/2
LB
3519 *
LB
3546 4/2
FB
Exposure 2
temp. 23.7"C
RH 40.8%
BP 29.6 in Hg
Dynamic 13:27:00 14:29:25 T & P
6-67 SC
3558
4/12
0.99
6£7 SC
3559
4/12
0.99
60
3522
4/12
3.23
3521 *
8.93
60
3523
4/12
2.89
3554
4/12
LB
Day 2 Experiment 6 April 2, 1993
9304Q2.AQ1
Exposure 3 temp 21.5°C
RH 41.7%
BP 29.72 in Hg
Dynamic 09:12:30 10:14:10
6.67 SC
3587
4/12
1.00
3591 4/12
1,01
6.67 SC
3586
4/12
1.00
5
3584
4/12
0.76
15
3593
4/12
2.25
20
3594
4/12
2.99
40
3595
4/12
5.97
3588
4/12
LB
3597 4/12
LB
3585
4/12
FB
3598 4/12
FB
Exposure 4 temp, 22.2°C
RH 42,2*
BP 29.73 in Hg
Dynamic
12:27:10 13:32:10
6.67 SC
3569
4/12
0.99
3570
0.99
60
3600
4/12
3.27
60
3601
4/12
3,06
3592
4/12
LB
LB
106
-------
TABLE A-7, SUMMARY OF DNPH SAMPLE IDS SENT TO RT1
Test ID Exposure I Exposure 2 Exposure 3 Exposure 4
1
3067
3070 LB
3159
LB
3161
1
3069
3071
3160
3162
2
2775
LB
3165
2779
LB
3166
2
2776
2781
3167
2
2777
3
3186
LB
3185
3184
3183
3
3187
3
31S9
4
3180
LB
3181
3171
LB
3173
4
3178
3172
4
3179
5
3175
LB
3177
3638
3639
5
3188
5
3169
6
3633
LB
3636
3632
LB
3631
6
3634
3630
6
3635
LB = Laboratory blank
107
-------
APPENDIX B
TEMPERATURE DATA
108
-------
TABLE B-l. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 1 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
36.4
41.9
36.3
42.0
Laboratory Air
22.4
22.7
22.0
22.3
Air in Exposure chamber (Port 3)1
23.9
26.0
23.9
27.0
iy
Air in Exposure chamber (Port 5)
23.2
24.2
23.0
24.6
Left Panel of Source Chamber
39.1
44.4
39.1
44.5
Right Panel of Source Chamber
38.5
43.8
38.3
44.0
Top Panel of Source Chamber
44.4
50.9
44.0
50.8
Bottom Panel of Source Chamber
65.9
75.0
70.8
74.8
Back Panel of Source Chamber
37.7
44,3
37.4
44.7
Front Panel of Source Chamber
29.1
32.2
28.6
31.8
Sample Backing (inward)
41.5
46.3
40.3
46.9
Sample Fiber (outward3)
59.0
67.2
62.9
67.1
Marked "P3" in Figure 2-2.
Marked "P5" in Figure 2-2.
Sample surface in contact with heated chamber bottom.
TABLE B-2. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 2 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
43.4
45.6
42.7
43.6
Laboratory Air
22,2
22.4
21.3
22.1
Air in Exposure chamber (Port 3)1
23.3
28.0
27.4
27.9
Air in Exposure chamber (Port 5)2
22.7 •
24.3
23.8
24.0
Left Panel of Source Chamber
45.4
50.3
45.9
46.8
Right Panel of Source Chamber
44.2
47.2
44.0
44.8
Top Panel of Source Chamber
47.6
50.8
47.6
48.4
Bottom Panel of Source Chamber
68.2
69.3
68.4
69.0
Back Panel of Source Chamber
44.6
47.7
44.5
45.4
Front Panel of Source Chamber
34.0
36.1
34.4
34.9
Sample Backing (inward)
41.4
44.3
41.6
42.5
Sample Fiber (outward3)
38.4
42.6
39.6
40.8
Marked "P3" in Figure 2-2.
marked "P5" in Figure 2-2.
Sample surface in contact with heated chamber bottom.
109
-------
TABLE B-3. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 3 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
44.4
41.1
39.8
42.2
Laboratory Air
22.7
23.2
225
22.6
Air in Exposure chamber (Port 3)1
28.1
27.5
24.9
27.2
Air in Exposure chamber (Port 5)
25.7
25.8
23.7
25.3
Left Panel of Source Chamber
44.5
42.7
39.5
42.6
Right Panel of Source Chamber
44.1
42.2
38,7
41.4
Top Panel of Source Chamber
49.9
46.1
45.6
48.8
Bottom Panel of Source Chamber
68.9
67.7
67.7
68.8
Back Panel of Source Chamber
47.0
43.4
40.3
43.3
Front Panel of Source Chamber
34.1
31.9
31.3
32.6
Sample Backing (inward)
43.1
39.6
37.5
40.7
¦j
Sample Fiber (outward )
42.9
39.1
37.5
40.5
Marked "P3" in Figure 2-2,
Marked "P5" in Figure 2-2.
Sample surface in contact with heated chamber bottom.
TABLE B-4. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 4 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
36.4
41.9
36.3
42.0
Laboratory Air
44.4
41.1
39.8
42.2
Air in Exposure chamber (Port 3)1
22.7
23.2
22.5
22.6
Air in Exposure chamber (Port 5)2
28.1
27.5
24.9
27.2
Left Panel of Source Chamber
25.7
25.8
23.7
25.3
Right Panel of Source Chamber
44.5
42.7
39.5
42.6
w~k i /• ri 1
Top Panel of Source Chamber
44.1
42.2
38.7
41.4
Bottom Panel of Source Chamber
49.9
46.1
45.6
48.8
Back Panel of Source Chamber
68.9
67.7
67.7
68.8
Front Panel of Source Chamber
47.0
43.4
40.3
43.3
Sample Backing (inward)
34.1
31.9
31.3
32.6
Sample Fiber (outward3)
43.1
39.6
37.5
40.7
Marked "P3" in Figure 2-2.
Marked "P5" in Figure 2-2.
Sample surface in contact with heated chamber bottom.
110
-------
TABLE B-5. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 5 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
43.2
44.3
42.7
41.6
Laboratory Air
23.0
23.9
22.4
22.4
Air in Exposure chamber (Port 3)'
27.9
28.7
27.3
27.1
Air in Exposure chamber (Port 5)2
25.7
26.5
25.0
24.7
Left Panel of Source Chamber
45.6
47.0
45.0
43.3
Right Panel of Source Chamber
46.0
47.5
45.4
43.6
Top Panel of Source Chamber
48.3
50.0
47.8
45.8
Bottom Panel of Source Chamber
71.4
71.7
71.1
71.6
Back Panel of Source Chamber
49.3
51.4
49.3
47.4
Front Panel of Source Chamber
34,5
36.0
34.2
33.4
Sample Backing (inward)
69.4
69.4
68.7
68.9
Sample Fiber (outward3)
56.3
57.2
56.0
55.7
1 Marked "P3" in Figure 2-2.
2 Marked "P5" in Figure 2-2.
3 Sample surface in contact with heated chamber bottom.
TABLE B-6. AVERAGE TEMPERATURE AT 12 LOCATIONS FOR TEST 6 (IN °C)
Thermocouple Location
Exposure 1
Exposure 2
Exposure 3
Exposure 4
Air in Source Chamber
39.6
39.9
40.1
41.6
Laboratory Air
22.8
23.7
22.3
22.4
Air in Exposure chamber (Port 3)1
26.9
27.8
26.6
26.9
Air in Exposure chamber (Port 5)2
25.5
26.3
24.8
24.9
Left Panel of Source Chamber
44.6
44.3
45.8
47.4
Right Panel of Source Chamber
41.6
41.8
42.7
43.9
Top Panel of Source Chamber
50.9
50.0
51.7
53.9
Bottom Panel of Source Chamber
75.0
75,3
75.9
76.3
Back Panel of Source Chamber
49.2
48.6
49.9
52.3
Front Panel of Source Chamber
30.0
31.0
30.1
30.7
Sample Backing (inward)
71.4
71.7
72.1
72.4
Sample Fiber (outward )
46.4
46.8
46.7
47.8
1 Marked "P3" in Figure 2-2.
2 Marked "P5" in Figure 2-2.
Sample surface in contact with heated chamber bottom.
Ill
-------
APPENDIX C
CALIBRATION DATA FOR TEMPERATURE AND HUMIDITY PROBES
112
-------
TABLE C-l. CALIBRATION OF THERMOCOUPLE 1 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0,0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.4
-0.6
0.04
03/29/93
Ice/Water
0.0
13
0.1
0.1
0.00
03/29/93
Warm Water
46.3
13
45.7
-0.6
0.05
04/08/93
Ice/Water
0.0
16
-0.1
-0.1
0.04
04/08/93
Warm Water
47.8
16
47.4
-0.4
0.06
TABLE C-2. CALIBRATION OF THERMOCOUPLE 2 (UNIT: °C)
Date
Temperature
Media
Actual
Temp,
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.2
-0.8
0.00
03/29/93
Ice/Water
0.0
13
0.2
0.2
0.00
03/29/93
Warm Water
46.3
13
45.8
-0,5
0.08
04/08/93
Ice/Water
0.0
16
0.4
0.4
0.00
04/08/93
Warm Water
47.8
16
47.4
-0.4
0.08
TABLE C-3. CALIBRATION OF THERMOCOUPLE 3 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0
03/04/93
Boiling Water
100
16
99
-1.0
0.09
03/29/93
Ice/Water
0.0
13
0.2
0.2
0.03
03/29/93
Warm Water
46.3
13
46
-0.3
0.1
04/08/93
Ice/Water
0.0
16
0.3
0.3
0.04
04/08/93
Warm Water
47.8
16
47.7
-0.1
0.05
113
-------
TABLE C-4. CALIBRATION OF THERMOCOUPLE 4 (UNIT; °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
00
16
0.1
0,1
0.03
03/04/93
Boiling Water
100
16
99.2
-0.8
0.02
03/29/93
Ice/Water
0.0
13
0.1
0.1
0.04
03/29/93
Warm Water
46.3
13
45.7
-0.6
0.00
04/08/93
Ice/Water
0.0
16
0.2
0.2
0.00
04/08/93
Warm Water
47.8
16
47.6
-0.2
0.11
TABLE C-5. CALIBRATION OF THERMOCOUPLE 5 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.3
-0.7
0.03
03/29/93
lee/Water
0.0
13
0.1
0.1
0.05
03/29/93
Warm Water
46.3
13
45.9
-0.4
0.04
04/08/93
Ice/Water
0.0
16
0.1
0.1
0.05
04/08/93
Warm Water
47.8
16
47,6
-0.2
0.00
TABLE C-6. CALIBRATION OF THERMOCOUPLE 6 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.07
03/04/93
Boiling Water
100
16
99.1
-0.9
0.04
03/29/93
Ice/Water
0.0
13
0.1
0.1
0.05
03/29/93
Warm Water
46.3
13
45.8
-0.5
0.00
04/08/93
Ice/Water
0.0
16
N/A
N/A
N/A
04/08/93
Warm Water
47.8
16
N/A
N/A
N/A
114
-------
TABLE €-7. CALIBRATION OF THERMOCOUPLE 7 (UNIT: °C)
Date
Temperature
Media
Actual
Temp,
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.2
-0.8
0.05
03/29/93
Ice/Water
0.0
13
0.1
0.1
0.04
03/29/93
Warm Water
46.3
13
46
-0.3
0.05
04/08/93
Ice/Water
0.0
16
0.2
0.2
0.04
04/08/93
Warm Water
47.8
16
47.7
-0.1
0.06
TABLE C-8. CALIBRATION OF THERMOCOUPLE 8 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp,
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.1
-0.9
0.05
03/29/93
Ice/Water
0.0
13
0.2
0.2
0.00
03/29/93
Warm Water
46.3
13
46
-0.3
0.05
04/08/93
Ice/Water
0.0
16
N/A
N/A
N/A
04/08/93
Warm Water
47.8
16
N/A
N/A
N/A
TABLE C-9. CALIBRATION OF THERMOCOUPLE 9 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.4
-0.6
0.00
03/29/93
Ice/Water
0.0
13
0.1
0.1
0.00
03/29/93
Warm Water
46.3
13
45.9
-0.4
0.06
04/08/93
Ice/Water
0.0
16
0.2
0.2
0.02
04/08/93
Warm Water
47.8
16
47.7
-0.1
0.00
115
-------
TABLE C-10. CALIBRATION OF THERMOCOUPLE 10 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.2
1
O
bo
0.04
03/29/93
Ice/Water
0.0
13
0.2
0.2
0.00
03/29/93
Warm Water
46.3
13
46,2
-0.1
0.05
04/08/93
Ice/Water
0.0
16
0.2
0.2
0.04
04/08/93
Warm Water
47.8
16
47.7
0.06
0.06
TABLE C-ll. CALIBRATION OF THERMOCOUPLE 11 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
Ice/Water
0.0
16
0.1
0.1
0.00
03/04/93
Boiling Water
100
16
99.3
-0.7
0.03
03/29/93
lee/Water
0.0
13
0.1
0,1
0.00
03/29/93
Warm Water
46.3
13
46.3
0.0
0.04
04/08/93
Ice/Water
0.0
16
0.2
0.2
0.00
04/08/93
Warm Water
47.8
16
47.8
0.0
0.06
TABLE C-12. CALIBRATION OF THERMOCOUPLE 12 (UNIT: °C)
Date
Temperature
Media
Actual
Temp.
No. of
Readings
Mean
Temp.
Error
STD
03/04/93
lee/Water
0,0
16
0.2
0.2
0,00
03/04/93
Boiling Water
100
16
100.3
0.3
70.04
03/29/93
Ice/Water
0,0
13
0.2
0.2
0.05
03/29/93
Warm Water
46.3
13
45.9
-0.4
0.05
04/08/93
lee/Water
0.0
16
0.2
0.2
0.04
04/08/93
Warm Water
47.8
16
47.7
-0.1
0.02
116
-------
TABLE C-13. CALIBRATION OF HUMIDITY PROBE 1
Solution of
Salt
Temp,
CO
R.H,
(%)
Readings1
(Volt)
Temp.
(°C)
R.H.
(%)
Readings2
(Volt)
LiCl
22
11.3
0.62
21
11.6
0.60
LiCl
22
11.3
0.64
21
11.6
0.61
LiCl
23
10.9
0.63
21
11.6
0.62
NaCl
22
75.5
3.46
21
75.6
3.44
NaCl
22
75.5
3.44
21
75.6
3.44
NaCl
23
75.3
3.45
21
75.6
3.45
1 Calibrated on 03/23/93
2 Calibrated on 04/03/93
TABLE C-14.
CALIBRATION OF HUMIDITY PROBE 2
Solution of
Salt
Temp.
(°C)
R.H.
(%)
Readings1
(Volt)
Temp.
(°C)
R.H.
(%)
Readings2
(Volt)
LiCl
22
11.3
0.73
21
11.6
0.71
LiCl
22
11.3
0.74
21
11.6
0.71
LiCl
23
10.9
0.75
21
11.6
0.72
NaCl
22
75.5
3.52
21
75.6
3.51
NaCl
22
75.5
3.53
21
75.6
3.51
NaCl
23
75.5
3.51
21
75.6
3.52
1 Calibrated on 03/23/93
2 Calibrated on 04/03/93
117
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