CONDUCTED BY EPA, REGION III
AIR QUALI1Y MONITORING BRANCH
SURVEILU\NCE & ANALYSIS DIVISION
APPENDICES A THROUGH I
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B
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APPENDIX B
METEOROLOGICAL DATA
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IPO
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APPENDIX C
TEST PROCEDURES
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METHODS OF
AIR SAM
/nfersoc/e/y Comm/Vfee
American Conference of Governmental Industrial Hygienists
American Chemical Society
American Industrial Hygiene Association
Association of Official Analytical Chemists
Air Pollution Control Association
American Public Health Association
American Public Works Association
American Society of Civil Engineers
American Society of Mechanical Engineers
American Society for Testing and Materials
Published by
AMERICAN PUBLIC'HEALTH ASSOCIATION
1015 Eighteenth Street, N.W., Washington, D.C. • 1972
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INTERSOCIETY COMMITTEE
112
TENTATIVE METHOD OF ANALYSIS FOR FORMALDEHYDE
CONTENT OF THE ATMOSPHERE (MBTH—
COLORIMETRIC METHOD—APPLICATIONS
TO OTHER ALDEHYDES)
43502-02-70T
1. Principle of Method
1.1 The aldehydes in ambient air are
collected in a 0.05 per cent aqueous 3-
methyl-2-benzothiazolone hydrazone hy-
drochloride (MBTH) solution. The re-
sulting azine is then oxidized by a ferric
chloride-sulfamic acid solution to form
a blue cationic dye in acid media, which
can be measured at 628 nm (1,2,3).
1.2 The mechanism of the present
procedure as applied to formaldehyde in-
cludes the following steps: reaction of
the aldehyde with 3-methyl-2-benzothia-
zolone hydrazone, A, to form the azine,
B; oxidation of A to a reactive cation,
C; and formation of the blue cation. D
Me
I
S ^ \
I C = N-NH_
X.--^.
©
2. Range and Sensitivity
2.1 From 0.03 /xg/ml-0.7 /tg/ml of
formaldehyde can be measured in the
color developed solution 112 ml). A
concentration of 0.03 ppm of aldehyde
I as formaldehyde I can be determined in
a 25 1 air sample based on an aliquot of
10 ml from 35 ml of absorbing solution
and a difference of 0.05 absorbance unit
from the blank.
3. Interferences
3.1 The following classes of com-
pounds react wilh MHTFT to produce col-
ored products. These are aromatic
amines, imino heterocyclics. carhazoles.
azo dyes, stilhenes. Srhiff bases, the ali-
CH70
T
—•[ 7 xC = N -N=CH2
Me
N
C = N -
Me
I
,-N.
Me
^'-> r . / /-^^
! L,' i C = N = N = CH = N - N = C j''|
s-' ~*s- ^
199
c-a
-------
phatic aldehyde 2,4-d'mitrophenyl hydra-
zones, and compounds containing the
p-hydroxy styryl group. Most of these
compounds are not gaseous or water sol-
uble and. consequently, should not inter-
fere with the analysis of water soluble
aliphatic aldehydes in the atmosphere
"(3).
4. Precision and Accuracy
The method was checked for repro-
ducibility by having three different ana-
lysts in three different laboratories ana-
lyze standard formaldehyde samples.
The results listed in Table 1 agreed
within ±5 per cent.
5. Apparatus
5.1 Absorbers—I All glass samplers
with coarse fritted tube inlet. Figure 1
shows an acceptable absorber.)
5.2 Air metering device—Either a
limiting orifice of approximately 0.5 1pm
capacity or a wet test meter can be used.
If a limiting orifice is used, regular and
frequent calibration is required.
5.3 Air pump—A pump capable of
drawing at least 0.5 I of air/min for 24
hr through the sampling train is re-
quired.
5.4 Spectrophotometer—An instru-
ment capable of measuring accurately
the developed color at the narrow ab-
sorption band of 628 nm.
6. Reagents
6.1 Purity of chemicals—All reagents
must be analytical reagent grade.
6.2 3-Methyl-2-benzothiazolone hydra-
zone, hydrochloride absorbing solution
({>.(>:> per cent)—Dissolve 0.5 g of
MBTH in distilled water and dilute to 1
liter. This colorless solution is filtered
by gravity, if slightly turbid, and is sta-
ble for at least 1 week after which it be-
comes pale yellow. Stability may be in-
creased by storing in a dark bottle jn the
cold.
6.3 Oxidizing reagent -Dissolve 1.6
g of sulfainic acid and 1.0 g of ferric
Table 1. Comparison of Formaldehyde
Results from Three Laboratories
(Analysis of Standard Formaldehyde
Samples)
Absorbance
Micrograms/ml Labors- Labora- Labora-
Formaldehyde tory 1 tory 2 tory 3
0.05
0.10
0.30
0.50
0.70
0.078
0.151
0.430
0.720
0.990
0.077
0.156
0.457
0.700
1.04
0.082
0.146
0.445
0.728
1.02
chloride in distilled water and dilute to
100 ml.
6.4 formaldehyde standard solution
"A" (1 me/ml)—Dilute 2.7 ml of 37
per cent formalin solution to 1 liter with
distilled water. This solution must be
standardized as described in "Calibra-
tion'' section. This solution is stable for
at least a 3-month period.
6.5 Formaldehyde standard solution
"B" (10 pg. ml.)—Dilute I ml of stand-
ard solution "A" to 100 ml with 0.05
per cent MBTH solution. Make up fresh
daily.
6.6 Iodine 0.1 .V (approximate)—
Dissolve 25 g of potassium iodide in
about 25 ml of water, add 12.7 g of
iodine and dilute to 1 liter.
6.7 Iodine 0.01 .V—Dilute 100 ml of
the 0.1 N iodine solution to 1 liter.
Standardize against sodium thiosulfate.
6.8 Starch solution 1 per cent—Make
a paste of 1 g of soluble starch in 2 ml
of water and slowly add the paste to 100
ml of boiling water. Cool, add several
nils of chloroform as a preservative, and
store in a stoppered bottle. Discard
when a mold growth is noticeable.
6.9 Sodium carbonate buffer solution
—Dissolve 80 g of anhydrous sodium
carbonate in about 500 ml of water.
Slowly add 20 ml of glacial acetic acid
and dilute to 1 liter.
6.10 Sodium bisulfite 1 percent—Dis-
solve I <' of sodium bisulfite in 100 ml
200
-------
FORMALDEHYDE
APPROX. 140mm
GAS WASHING
BOTTLE 10 ml
and 20 ml.
12/b
12/5
3mm O.D.
22mm 0.0.
SIDE ARM CONNECTIONS
MUST BE SAME HEIGHT
ON RESPECTIVE BOTTLES
19mm O.D.
20ml - LENGTH
Figure 1—Absorber.
201
-------
of ualtr. It i> best lo prepare a fresh
solution weekly.
7. Procedure
7.1 'tir xd/nplinii — Draw measured
volumes <>f ihe \apor laden air at a rate
of O.o Ipiii for 21 lir through 35 ml of
MBT1I absorbing solution contained in
ihe absorber. A shorter sampling time
can be used providing enough formalde-
hyde is collected to be above the lower
limit of sensitivity of the method.
The average collection efficiency of
formaldehyde in air has been determined
to be 84 per cent when air was sampled
at a rate of 0.5 Ipm over a 24-hr period
in 35 ml of collecting reagent (3) in
an absorber equipped with an extra
coarse (EC) fritted tube inlet. Absorp-
tion efficiency may be improved by using
a coarse (C) frit although data are lack-
ing on (his likelihood.
7.2 Analysis.
7.2.1 Transfer the samples from the
sampling bottles to 50 nil graduates, di-
lute lo 35 ml with distilled water and
allow to stand for 1 hr.
7.2.2 Pipet a 10 ml aliquot of
the sampling solution into a glass stop-
pered test tube. A blank containing 10
ml of MBTH solution must also be run.
If the aldehyde content of the aliquot
exceeds the limits of the method, a
smaller aliquot diluted to 10 ml with
MBTH solution is used.
7.2.3 Add 2 ml of oxidizing solution
and mix thoroughly.
7.2.4 After standing for at least 12
min. read at 628 run on a suitable spec-
lr
-------
FORMALDEHYDE
8.9 Preparation of standard curve.
8.9.1. Pipet 0, 0.5, 1.0, 3.0, 5.0,
and 7.0 ml of standard formaldehyde
solution "B" into 100 ml volumetric
flasks. Dilute to volume with 0.05 per
cent MBTH solution. These solutions
contain 0, 0.05. 0.1. 0.3, 0.5, and 0.7
/tg of formaldehyde/nil.
8.9.2. After final dilution let stand
for 1-hour.
8.9.3. Transfer 10 ml of each solu-
tion to a glass stoppered test tube and
add 2 ml of oxidizing reagent and mix.
8.9.4. After 12 min read the absorb-
ance at 628 nm in a suitable spectro-
photometer using 1 cm cells.
8.9.5. Plot absorbance against mi-
crograms of formaldehyde/ml of solu-
tion.
9. Calculation
9.1 The concentration of total ali-
phatic aldehyde (as formaldehyde) in
the sampled atmosphere may be calcu-
lated by using the following equation:
PPM fVol ^ _ C X 35 X 24.4n
f mi vol.)-• VxMW x£
E=correction factor for sampling
efficiency (0.84 may be used if
absorber contains an EC frit)
V=liters of air sampled.
C=/tg/ml of formaldehyde in
sampling solution. (Since each
sample is diluted to 35 ml,
this figure must be multiplied
by 35 to give total micro-
grams in sampling solution.)
M.W.=molecular weight of formalde-
hyde (30.03).
24.45=ml of formaldehyde gas in one
millimole at 760 Torr and
25 C.
10. Effect of Storage
10.1 The time study of the reaction of
microgram quantities of formaldehyde
with 0.05 per cent MBTH shows that the
reaction is complete in approximately 45
min: therefor*1, a reaction lime of I hr
is selected for this procedure. Formalde-
hyde is fairly stable in 0.05 per cent
MBTH since only approximately .5 per
cent of the formaldehyde is lost after
standing in the VIMTII for 13 day?. The
samples are. therefore, stable enough for
later analsis
11. References
1. Sawickl. E.: T. R. Hoiivrr: T. »'. Slangy: a"'l
V(". F.lbcrt. Thr .|.\lrilivl-2.Bi-nniihia»iluiii- IK. Iran. m-
Te»t. Anal. Chem. 33 .-93. 1961.
2. Hauler. T. R.. anil R. I.. Cummin.*. Inrrro.ins tin-
Senailivity of 3-Mohrl-Z-Benzalhiaiolone Hydruone
Ten for Analytil of Aliphatic Aldehydes in Air.
Anal. Chirm. 37*79. 1964.
3. Hau«er. Thomai R. Determination at Aliphatic Al-
dehyde*: 3>Methv|.2'Benzothiazolone Hydratone Hy-
drochloridr I MBTH) Mrlhml. Srlrclnl Methodi for
the Measurement of Air Polliilanft. Public Hrnlili
Service Publication ,Vn. MO-AIMl. Pan- F 1. 19*3.
ADDENDUM
Applications to Other Aldehydes
Acetaldehyde and propionic aldehyde
both yield a blue dye after reaction with
3-methyl-2-benzothiazolone hydrazone
hydrochloride and a ferric chloride-sul-
famic acid solution. It has been found
that as the length of chain increases, the
sensitivity decreases. Therefore when
measuring total aldehydes as formalde-
hyde this method would -jive low results
if any aldehyde other than formaldehyde
is present.
From 0.05 /ig/ml-1.0 n§/m\ of both
acetaldehyde and propionic aldehyde
can be measured in the color developed
solution (12 mil. For the lower con-
centrations the method has poor repro-
ducibility. However, at higher concen-
trations (0.30 /xg/ml and above) repro-
ducibility was very good. These data
are summarized in Tables A and B.
Acetaldehyde (Eastman Kodak Com-
pany, Cat. No. 468) and propionic alde-
hyde (Eastman Kodak Company, Cat.
No. 653) were considered to be primary
standards when preparing solutions of
known concentration. Exactly 1.28 ml
of acetaldehvtle was diluted to 1 1 with
203
c-c.
-------
Table A. Arelaldvhvde
u^, ml
0.05
0.10
0.30
0.50
0.70
1. 00
Mg.'ml
0.05
0.10
0.30
0.50
0.70
I.(H)
Number of
Samples
29
29
29
2')
29
15
Number of
Samples
29
29
29
2'J
29
!.->
Average
Absorbanre
0.063
0.125
0.339
0.519
0.685
0.900
Table R. I'ropinnie
Average
Absorbance
0.046
0.082
0.243
0.399
0.538
0.732
Range
0.050-0.074
0.106-0.144
0.316-0.355
0.49.^0.538
0.660 0.710
0.890 0.910
Aldehyde
KaajiP
0.032-0.057
0.063-0.095
0.225-0.250
0.380-0.422
0.515-0.568
0.710 0.750
% Variance
From Avft.
±20
±15
± 7
± 4
± 3
± 1
'"< Variance
From Avg.
±27
±20
± 5
± 5
± 5
± 2
distilled water and then 1 nil of this
solution was diluted to 100 ml with
MBTH solution giving a final concentra-
tion of 10 pg/mi. Exactly 1.24 ml of
propionic aldehyde was diluted to 1 1
with distilled water and then 1 ml of
this solution was diluted to 100 ml with
MBTH solution giving a final concentra-
tion of 10 pg/ml. The strong standard
solutions have a 2 month shelf life. The
dilute standard solutions must be pre-
pared fresh daily.
A series of 34 ambient air samples
were collected in 35 nil of MBTH solu-
tion contained in each of two absorbers
in series. The sampling time was 24 hr
and the sampling rate was 1 liter 'minute.
Collection efficiencies varied from 69
per cent to 100 per cent with the average
for the 34 samples being 82 per cent
Subcommittee 4
R. C. SMITH. Chairman
R. J. BRYAN
M. FELDSTEIN
B. LEVADIE
F. A. MILLER
E. R. STEPHENS
N. G. WHITE
204
C-l
-------
PHENOLIC COMPOUNDS
and the ahsorbanre mensural directly
at 510 nin.
8. Standardization of Phenol Solu-
tion
8.1 Stock standard phenol solution—
prepare a 0.1 per cent solution of phenol
in distilled water. Into a 500 ml iodine
flask transfer 50 ml of stock standard
and add 100 ml of distilled water. Add
exactly 10 ml of bromide-bromate solu-
tion. Add carefully 0.5 ml of concen-
trated hydrochloric acid. Swirl the flask
gently, making certain that the stopper
is seated. If. at this point, the color of
bromine does not persist, continue to
add exactly 10 ml portions of bromide
bromate solution until the reddish-brown
bromine color does persist. If the stock
solution is made up to cunlain 1000
nig of phenol I, 4-10 ml portions of
bromide hrnmale solution will be re-
quired. With the stopper in position
let the reaction flask sit for 10 minutes.
Add quickly one p of potassium iodide.
Prepare a blank in exactly the same
manner, using 10 ml of bromide bro-
mate solution and distilled water.
Titrate both blank and sample with
0.025 ,V sodium thiosulfate. using starch
as indicator. Calculate the concentra-
tion of phenol solution as follows:
Milligrams of phenol per liter=
[(AX B)—C] X 7.835
A=ml of 0.025 .V thiosulfate used for
blank.
R=ml of bromide-bromate solution used
for sample, divided by 10.
C=ml of 0.025 .V thiosulfate used for
sample. The factor. 7.835. is based
on the use of an exactly 0.025 .V
thiosulfate solution in the titration.
!>.2 Primary standard phenol solu-
tion—Dilute the stock standard so that
1 ml is equal to 10 /xg of phenol.
8.3 Working standard—Dilute the
primary standard 1:10 with distilled
water. This solution contains one ft£.
of phenol in 1 ml.
9. Calculation
(J.l Working standards are used to
prepare a concentration vs absorbance
curve from which the concentration of
phenol in samples is determined. One
/ig of phenol I of air is equal to 0.26
ppm and one ppm is equal to 3.84 /ig/1
at 25 C and standard pressure.
10. Effects of Storage
10.1 The addition of 5 ml of copper
sulfate solution to the alkaline solution
of phenols will serve to stabilize the
sample.
10.2 Cautions.
10.2.1 Equipment which has been
lubricated with stopcock grease should
not be used.
10.2.2 Temperature variations will
affect the blank.
10.2.3 Filtration of the chloroform
extract before reading it in the spectro-
photometer will remove possible tur-
bidity due to presence of water disper-
sion.
10.2.4 The chloroform extract of
the dye will fade on standing.
10.2.5 It is advisable to work
quickly when serial readings are made.
11. References
1. Emenna, E. I. The Condensation of Arninnanti-
pyrine: A New Teat (or Phrnolir Compound!. J.
Organic Cheat.. 8:417. 1943.
2. F.ttinerr, M. D.; C. C. Ru.-hhoft; .mil R. J. I.iihk..
Srnftilive 4>Aminnantipyrine Nfethod for Phennlir
C.MRi|i.>iinil». Anal. Client. --1:1783 1788. I9SI.
.1. Jurtili*. M. II. Tlir Analytical Chrmiiilry of Inriilitrtal
INiiaont. Hazardt and Solvents. Intrr«rienr<» Pub*
lisliera. 2nd Edition, (pp TO",).
I Mnhler. K. F. and T.. N. jamb. Drl-rmin.itmn ••(
IMinnnlir.Typ** Compnuitdfl in Watrr and Industrial
\Va«lr Water-. \n.il. C.lii-ni. ;0:|.1M-nrt. 10".
".. Smih. K. G.. J. D. MwiKwen; and R. K. Barmx.
Sampling and -\niil\.'>9.
Suhconiiiiittee I
R. G. SMITH, Chairman
R. J. BRYA>
M. FELDSTEI^
I!. LEVADIE
V. \. MILI.EK
E. R. TKHUKN-
N. C. \Vnirt
223
-------
pare according to classical laboratory
method.
7. Procedure
7.1 Air Sampling—P articulates. Draw
a 24-hr air sample at a measured flow
rate through a Hash-fired fiberglass filter
using u high volume sampler.1
7.2 Air Sampling. Sapors and I'ar-
ticulates. Wet method—Draw a 30 min
sample lor larger if desired) of air
through a 0.1 N solution of sodium hy-
droxide in distilled water, at a standard
impinger flow rale of one ftY">inule. If
only vapor phenolics are required, use
a membrane filter in the sampling train
to remove particulates.
7.3 Analysis— (CAUTION—do not
u.ti' stopcock grease in any apparatus I.
7.4 Filter samples—Extract the filter
or any desired portion of it in a Soxhlet
extractor by reflux ing with benzene for
3 hours. Transfer the benzene extract
to a separatory funnel, filtering it
through a close (Whatman 42 or equiva-
lent) paper. Extract 3 times with 10
ml portions of 1.0 /V NaOH. Treat
according to Section 7.6 Determination
of Phenols.
7.5 Samples collected in 0.1 N NaOH.
7.5.1 Air samples. Proceed to
Section 7.6 Determination of Phenols.
7.5.2 Exhaust gases or process
effluents. Use the whole sample. Add
1 ml of 10 per cent copper sulfale solu-
tion. Acidify, using methyl orange as
indicator and 10 per cent phosphoric
acid solution. Transfer to an all glass
distillation apparatus and distill, collect-
ing 90 ml of the distillate. Cool the dis-
tillation flask and add 10 ml of distilled
water. Continue the distillation until
exactly 100 ml of distillate has^ liern col-
1 Proper method.-, for calibrating tin- high
volume sampler or other sampling devices
should-be provided by the manual supplied by
ih« manufacturer
lecleil. Acidify with 0.5 ml of 10 per
cent phosphoric acid solution, add 1.0
ml of 10 per rent copper sulfate solution
and transfer to a separatory funnel. Add
30 g of reagent grade sodium chloride
and extract with 3-10 ml portions, of
chloroform. Discard the aqueous phase.
Shake the chloroform extract with 2 -15
nd portions of O.I N NaOH. Discard
the chloroform phase. Meat the alkali
extracts until the traces of chloroform
have been removed, dilute the alkaline
extract to 100 ml volume with distilled
water and treat according to Section
7.6.2.
7.6 Determination of Phenols.
7.6.1 Adjust the alkaline extracts
to volume of 100 ml. either by aliquot-
ing or diluting to volume with distilled
water. Add 1 ml of 10 per cent copper
.sulfate solution. Acidify with 10 per
cent phosphoric acid solution using
methyl orange indicator. Distill from
an all glass distillation apparatus until
90 ml have been collected. Add 10 ml
of distilled water to the cooled distilla-
tion flask and continue the distillation
until a total volume of 100 ml of distil-
late have been collected.
7.6.2 Take a 50 ml aliquot of the
distillate. Prepare standards contain-
ing 0.5, 1.0. 5.0. 10.0 and 20.0 Mg of
phenol. Adjust the volumes of sample
and standards to 100 ml with distilled
water. Add 2 ml of ammonium chloride
solution. Using a pH meter adjust to
pH 10.0 ±: 0.2. with concentrated am-
monium hydroxide. Add 1 ml of 4-
aminoantipyrine solution and mix. Add
L ml of potassium ferricyanide solution.
transfer to a separatory funnel and wait
3 minutes. Extract with 3-5 ml por-
tions of chloroform and discard the
aqueous phase. Make up the chloro-
form extract to a known volume with
chloroform. Using a blank as reference.
record the absorbance at 460 nm. For
higher concentrations of phenol the
chloroform extraction mav he omillfd
222
-------
PHENOLIC COMPOUNDS
2. Range and Sensitivity
2.1 One cubic meter of air contain-
ing 1.3 ppb of phenol will produce suf-
ficient sample to give a coupling product
absorbance of approximately 0.2 units
in a 20 mm cuvet when measured at 460
nm wavelength in a speotrophotomeler.
3. Interferences
3.1 Any color, other than that due
to the reagents used, interferes with the
method. Turbidity, sulfur compounds
and certain metallic ions interfere (4).
However, the distillation procedure
described by Smith eliminates these in-
terferences.
4. Precision and Accuracy
4.1 Tn the range of 0.49-1.03 ppm
the standard deviation is 0.022 and at
the 95% confidence level 0.065. At
18—75 ppb the standard deviation is
3.3 and at the 95?v confidence level 10.7
ppb. Accuracy is plus or minus two per
cent (4).
5. Apparatus
5.1 Smchlet extractors.
5.2 Distillation apparatus—all glass.
5.3 Iodine bottles—500 ml size.
5.4 Impingers—Standard, midget or
equipped with fritted absorbers (extra
coarse porosity).
5.5 Fiber floss filter sheets, flash fired.
5.6 Spectrophotometer—any spectro-
photometer capable of measuring the
absorbance of the solution complex at
460-510 nm. as required.
5.7 High volume sampler or other air
sampling device for collection of particu-
late samples, equipped with a calibrated
gauge or flow meter to measure air vol-
ume flow accurately.
6. Reagents
6.1 Purity of chemicals. \ll reasents
should be ACS analytical grade.
6.2 t-iiiniiiiniiilii>\riiic .filiation—dis-
solve 2 g of 4-aminoantipyrine in dis-
tilled water and make up to 100 ml. This
solution should not be kept longer than
I week.
(>.3 I'nlussium jerricyanide solution—
dissolve 8 g of analytical reagent grade
potassium ferricyanide in distilled water
and make up to 100 ml. Discard when
the solution becomes darkened.
6.4 Ammonium chloride solution—
dissolve 50 g of analytical reagent grade
salt in distilled water and make up to
one liter.
6.5 Copper sulfate solution—prepare
a 10 per cent solution of the pentahy-
drate.
6.6 Sodium hydroxide sampling solu-
tion—prepare a 1 /V solution.
6.7 Bromide 'Rromate solution—dis-
solve 2.784 g of analytical reagent grade
potassium bromate in distilled water:
add 10 g of analytical reagent grade
potassium bromide and make up to 1
liter.
6.8 Ammonium. Hydroxide—Analyti-
cal reagent grade.
6.9 Hydrochloric Acid - Analytical re-
agent grade.
6.10 Phosphoric acid solution—pre-
pare a 10 per cent solution of orthophos-
phoric acid.
6.11 Potassium Iodide—Analytical re-
agent grade salt.
6.12 Sodium thiosuljate solution—
prepare a 0.1 A solution of the salt and
-tandardi/e according to classical labora-
tory procedures. Dilute to make an ex-
actly 0.025 V solution.
6.13 Starch solution—dissolve one g
of soluble starch in 100 ml of distilled
water. Prepare a fresh solution daily.
6.H Phenol—reagent grade.
6.15 llt'itzene—reagent grade.
6.16 C.hlorojorm—reagent grade.
6.17 Methyl orange indicator—pre-
221
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INTERSOCIETY COMMITTEE
116
TENTATIVE METHOD OF ANALYSIS FOR DETERMINATION
OF PHENOLIC COMPOUNDS IN THE ATMOSPHERE
(4-AMINOANTIPYR1NE METHOD)
I7320-OI-70T
1. Principle of the Method
1.1 Air is scrubbed with an alkaline
solution in u standard impinger. Par-
ticulate phenolic substances are collected
by passing air through a fiberglass Slier.
Phenolic compounds are separated from
other compounds by distillation from
an acidified system. Phenols are deter-
mined by coupling them with 4-amino-
antipyrine in an alkaline medium con-
taining an oxidant.
1.2 The method is based on a reac-
tion discovered by Emerson (1). This
procedure is essentially that of Smith
N
CH3 -N
c = o
I
CH3 -C
C-NH2
4 iimirio-iintipyrine
ft al (5). Discussions of theory and
eHiciency are given by Etlinger (2) and
Mohler "(4).
1.3 In the presence of a strong alka-
line oxidizing reagent this coupling re-
action will proceed as shown in 1.4
below. If the system is not sufficienlh
alkaline dimerization of 4-aminoanti-
pyrine to antipyrine red will take place,
as in 1.5 below. It is important, there-
fore, to have a high pH when the cou-
pling reaction is induced.
1.4 Coupling reaction of 4-aminoanli-
pyrine and phenol
C6HS
I
N
(OK CH3-N C-0
•-OH Tg^gT ! I
1B ' CH3 -C C-N =
•= O
phenol
1.5 Dirnerizalioii of 4-aminoaalipy-
rine
i
N
CH,-N C = O
! I i
CH, - C = (
o = c
NH2 H^N-C
N-CH,
C-CHn
F.C/3 ! [O]
C8H5
N
CH3 -C - C
HO -C
Antipyrine Red.
N
11
i >
- C-CH3
0
220
-------
criteria for a recommended standard.
OCCUPATIONAL EXPOSURE
TO
FIBROUS GLASS
U.S. DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE
Public Health Service
Center for Disease Control
»•
National Institute for Occupational Safety and Health
April 1977
ml* by the Superintendent of Documents. U.S. Government
Printing Office. Washington. D.C. 20402
-------
IX. APPENDIX I
AIR SAMPLING METHOD - MEMBRANE FILTER
General Reguirements
The following sampling and anlytical methods for fiber counting are
adapted from the NIOSH membrane filter method for evaluating airborne
asbestos fibers [90].
(a) Air samples representative of the breathing zones of workers
must be collected to characterize the exposure from each Job or specific
operation in each work area.
(b) Samples collected shall be representative of the exposure of
individual workers.
(c) Suggested records:
(1) The date and time of sample collection.
(2) Sampling duration.
(3) Total sample volume.
(4) Location of sampling.
(6) Other pertinent information.
Sampling
(a) Samples shall be collected so as to be representative of the
breathing zones of workers ^ without interfering with their freedom of
movement.
\
(b) Samples shall be collected to permit determination of TWA
exposures for every job involving exposure to fibrous glass in sufficient
119
-------
numbers to determine the variability of exposures in the work situation.
(c) Equipment
The sampling train consists of a membrane filter and a vacuum pump.
(1) Membrane filter: Samples of fibrous glass are
collected in the breathing zones of the workers using a personal sampler
with ••'cellulose ester membrane filter. The filter is a 0.8-jan pore size
mixed cellulose ester membrane mounted in a open-face sampling cassette
which can be attached to the worker near his or her breathing zone.
(2) Pump: A battery-operated pump, complete with clip for
attachment to the worker's belt, capable of operation at 2.5 liters/minute
or less.
(d) Calibration
The personal sampling pump should be recharged prior to calibration
and then calibrated against a bubble meter, wet test meter, spirometer, or
similar device at a flowrate of 1.0 to 2.5 liters/minute. The sampling
train used in the calibration (pump, hose, filter) shall be equivalent to
the one used in the field. The calibration should be performed to an
accuracy of + 5%.
(e) Sampling Procedure
(1) Sampling is performed using an open-face membrane
filter cassette.
(2) The sampler shall be operated at a flowrate between 1.5
and 2 liters/minute.
(3) The temperature and pressure of the atmosphere being
w
sampled are measured and recorded.
120
C-\4
-------
(4) One membrane filter is treated in the same manner as
the sample filters with the exception that no air is drawn through it.
This filter serves as a blank.
(5) Immediately after sampling, personal filter samples
should be sealed in individual plastic filter holders for shipment. The
filters shall not be loaded to the point where portions of the sample might
be dislodged from the collecting filter during handling.
(f) Optimum Sampling Times
A requirement for a minimum count of 100 fibers or 20 fields has been
determined to be the optimum choice to achieve low variability of the fiber
count (as approximated by a Poisson distribution) and reduced counting
times. In other words, the optimum fiber density on the filter should be 1
to 5 fibers/microscope counting field. To estimate optimum sampling times,
the approximate field area of the counting scope and the pump flowrate must
be known in advance.
The following equation is used to calculate the range of optimum
sampling times which can then be plotted on log-log paper:
Minutes - (FB/FL)(ECA/MFA)
(FR)(AC)
where: FB/FL - 1 to 5 fibers/field
EGA » Effective collecting area of filter in square
millimeters (855 square mm for 37-mm filter)
MFA - Microscope field area in mm (generally 0.003
to 0.006 square mm)
FR - Pump flowrate in cc/minute
121
C-Vf
-------
AC - Air concentration of fibers in fibers/cc
(NOTE: If air concentrations are expressed
in fibers/cu m they must be changed
to fibers/cc for this equation.)
122
C-M,
-------
X. APPENDIX II
ANALYTICAL METHOD - FIBER COUNT
Principle of the Method,
(a) Environmental dust samples are collected by drawing air
through a membrane filter by means of a battery-powered personal sampling
pump.
(b) The filter is transformed from an opaque solid membrane to a
transparent, optically homogeneous gel.
(c) The fibers are sized and counted by phase-contrast microscopy
at 400-450X magnification.
Range and Sensitivity
(a) This method has been successfully applied at concentrations of
10,000 to 20,000,000 fibers/cu m (0.01 to 20 fibers/cc) for fibers longer
than 5 ^m. Large deviations from the specified conditions of the method
may result in filters with either too few or too many fibers. Too few
fibers will yield air concentration estimates of low statistical precision.
(b) A sensitivity of 10,000 fibers/cu m (0.01 fiber/cc) has been
reported [JM Dement, written communication, 1975] based on a 4-hour sample
at 2 liters/minute air flow.
Interferences
All particulates, such as asbestos or mineral wool, with a length-to-
width ratio of 3 to 1 or greater, and length greater than 10 jan should, in
123
C-\i
-------
the absence of other information, be considered as glass fibers and counted
as such. Asbestos interference can be eliminated using phase contrast,
polarized light microscopy.
Advantages of the Method
(3) •• The fiber count method allows for repeated counts, and storage
for counting at a later time. The method consumes only part of the filter,
thereby allowing for at least one replicate sample analysis at a later
time.
(b) Fiber counts are assumed to be more toxicologically
significant than fiber weight for fibers less than 3.5 ym in diameter.
(c) Fiber size determinations may be performed.
Disadvantages of the Method
(a) The fiber count method is slow and tedious.
(b) Variation in counts may be significant between different
observers.
(c) The sensitivity of the method is dependent on the sampling
time and flowrate. The sensitivity and useful range of this method has not
been determined specifically for fibrous glass but is based on the method
recommended for asbestos.
Apparatus
(a) Optical Equipment
(1) Microscope body with binocular head, 10X Huygenian
124
C-ft
-------
eyepieces, and Koehler illumination.
(2) Porton reticle.
(3) Mechanical stage, and stage micrometer with 0.01-mm
subdivisions.
(4) Abbe or Zernike condenser fitted with phase ring with a.
numerical aperture equal to or greater than the numerical aperture of the
objective.
(5) A phase-ring centering telescope or Bertrand lens and a
green filter if recommended by the microscope manufacturer.
(6) Fiber mounting equipment
(A) Microscope slides, and cover slips, usually 0.17
mm thick.
(B) Scalpel, tweezers, lens tissues, and glass rod
or spatula for mounting procedures.
(b) Wheaton Balsam Bottle.
Reagents
(a) Dimethyl phthalate.
(b) Diethyl oxalate.
Analysis of Samples
(a) Calibration and Standardization
(1) Porton Reticle and the Counting Field
The fiber count procedure consists of comparing fiber length
with calibrated circles, and counting all fibers > 10 /an in length within a
125
-------
given counting field. A Porton reticle is used for this purpose. The
Porton reticle is a glass plate inscribed with a series of circles and
rectangles. The square on the left, divided into six rectangles, is
defined as the counting field.
(2) Placement in Eyepiece
Place the Porton reticle inside one Huygenian eyepiece,
resting it on the field-limiting diaphragm. Keep the reticle clean, since
dirt on the reticle will be in focus and will complicate the counting and
sizing process.
(3) Stage Micrometer
The Porton reticle cannot be used for counting until it has
•*•*
been properly calibrated with a stage micrometer. Most stage micrometer
scales are approximately 2 mm long, divided into units of 10 /tan.
(4) Microscope Adjustment
When adjusting the microscope, follow the manufacturer's
instructions while observing the following guidelines.
(A) The light source image must be in focus and
centered on the condenser iris or annular diaphragm.
(B) The object for examination must be in focus.
(C) The illuminator field iris must be in focus,
centered on the sample, and opened only to the point where the field of
view is illuminated.
(D) The phase rings (annular diaphragm and phase-
shifting elements) must be concerttric.
(5) Porton Reticle Calibration Procedure
126
COO
-------
Each eyepiece-objective-reticle combination on the microscope
must be calibrated. Should any of the three be changed (disassembly,
replacement, zoom adjustment, etc) the combination must be recalibrated.
Calibration may change if the interpupillary distance is changed. For
proper calibration, the following procedure should be followed closely.
Using a 10X objective, place the stage micrometer on the mechanical
stage and focus and center the image. Change to the 40-45X objective and
adjust the first scale division to coincide with the left boundary of the
Forton rectangle. Count the number of divisions between the left and right
boundaries of the long horizontal dimension of the largest rectangle,
estimating any portion of the final division. This measurement represents
200 L units and the measurement is then divided by 200 to find "L." The
large rectangle is 100 L units long on the short vertical dimension. The
calculated "L" is inserted into the formula D - L(2N)l/2 where "N" is the
circle number (indicated on the reticle) and "D" is the circle diameter.
Since the circle diameters vary logarithmically, every other circle doubles
in diameter. For example, number three is twice the diameter of number
one; number four is twice the counting field area consisting of the left
six smaller rectangles can be calculated from the relation 10,000 L. The
reticle calibration is now completed for this specific objective-eyepiece-
recticle combination.
(b) Preparation of Mounting Solution
An important part of-the sample evaluation is the mounting process
which involves a special mounting medium of prescribed viscosity. The
proper viscosity is important to expedite filter clearing and to minimize
particle migration. Once the sample has been mounted, an elapsed time of
127
-------
approximately 15 minutes is needed before the sample is ready for
evaluation.
Combine the dimethyl phthalate and diethyl oxalate in a 1 to 1 ratio
by volume and pour the solution into a Wheaton balsam bottle. Add 0.05
gram of new membrane filter/ml of solution to reach the necessary
viscosity. The-mixture must be stirred periodically until the filter
material is dissolved and a homogeneous mixture is formed. The normal
shelf life of the mounting solution is about 6 months. Approximately 300
samples can be prepared from 20 ml of mounting solution.
(c) Sample Mounting
Cleanliness is important. The working area must be kept clean to
prevent sample contamination and erroneous counts. The following steps
should be followed when mounting a sample.
(1) Clean the slides and cover slips with lens tissue. Lay
the slide down on a clean surface with the frosted end up. It is good
practice to rest one edge of the cover slip on the slide and the other edge
on the working surface. By doing this, you keep from becoming
contaminated.
(2) Wipe all the mounting tools clean with lens tissue and
place them on a clean surface (such as lens tissue). When mounting a
series of filters, wipe the scalpel clean before cutting a sector of each
sample [see (5) below].
(3) Apply a small drop of mounting solution onto the center
of the slide with a glass rod. It may be necessary to adjust the quantity
*. .,
t'
of solution used or the size of the wedge. The correct amount will result
in the solution extending only slightly beyond the filter boundary. If the
128
-------
quantity is greater than this, adverse particle migration may occur.
(4) With a spatula or a supplemental glass rod, spread the
mounting media into a triangular shape. The size of this triangle should
coincide with the dimension of the filter wedge.
(5) Separate the middle and bottom sections of the field
monitor case to expose the fragile filter. Cut a triangular wedge from the
center to the edge of the filter using a scalpel. The size of the wedge
should approximate one-eighth of the filter surface. The filter should be
handled gently so that no material will be lost.
Grasp the filter wedge with tweezers on the outer area of the filter
which was clamped between the monitor case sections. Do not touch the
«
filter with fingers. Place the wedge, fiber-bearing side up, upon the
mounting medium.
(7) Lift the cover slip with the tweezers and carefully
place it on the filter wedge. Once this contact has been made, do_ not
reposition the cover slip.
(8) Label the slide with the sample number and current date
before proceeding to the next filter.
(9) The sample should become transparent after about 15
minutes. If the filter appears cloudy, it may be necessary to press very
lightly on the cover slip. This is rarely necessary, however.
(10) Examine the slide within 3 days. The sample mounts
should be discarded after 3 -days if it has not been counted because
crystals which appear similar to glass fibers may begin to grow at the
mounting media/air interfaces; they seldom present any problems if the
slide is examined within 3 days. In any case, do not perform counting or
129
-------
sizing around the edges of the filter.
(d) Counting and Sizing—Finding and Inspecting Counting Fields
Place the slide on the mechanical stage and position the center of
the wedge under the objective lens and focus upon the sample. Nearly all
of the particulates (particles and fibers) will be found in the upper 10-15
im of the filter surface. When counting and sizing, continued use of the
fine focus control is required to insure that nothing is missed. Start
counting from one end of the wedge and progress along a straight line to
the other end (count in either direction from circumference to wedge tip).
Haphazard fields are selected without looking into the eyepieces by
slightly advancing the slide in one direction with the mechanical stage
control.
(e) Achieving Comparable Results
(1) Size only those fibers with a length-to-width ratio
equal to or greater than 3:1.
(2) Count only fibers greater than 10 ion in length. (Be as
accurate as possible in accepting or rejecting fibers near this length).
(3) Count up to 100 fields if necessary to yield a total
count of at least 100 fibers. Count at least 20 fields even if more than
100 fibers are counted.
(4) Select the field of view without looking through the
microscope's eyepieces to minimize unconsciously selecting "heavy" or
"light" areas.
(5) The fields are^ selected along the entire length of a
radial line running between the outside perimeter and the tip of the wedge.
130
-------
(6) When an agglomerate (mass of material) covers a
significant portion of the field of view (approximately 1/6 or greater),
reject the field and select another. (Do not include this field in the
number of fields counted.) Record the agglomerated field even though it is
not included in the count.
(7) Bundles of fibers are counted as one fiber unless both
ends of a fiber crossing another can be clearly resolved.
(8) For fibers that cross either one or two sides of the
counting field, the following procedure is used to obtain a representative
count. First, arbitrarily select: a) the left and bottom sides, and b) the
upper and lower left corners and vertical direction as "decision aids."
i
Then count any fiber greater than 10 micrometers in length, but only
if the fiber:
a. lies entirely within the counting area, or
b. crosses the left or bottom sides, or
c. crosses the upper or lower left corners, or
d. crosses both the top and bottom sides.
Reject and do not count all other fibers.
Calculations of Airborne Concentrations
Glass fiber airborne concentration may be calculated from the
following formula:
(F-B)(W)
C -
where:
C « Airborne fiber concentrations in fibers >10 jan/cu m.
-------
F - Average fiber count in fibers >10 jum/field.
B « Average fiber count of blank(s) or control filter(s) in
fibers >10 ^m/field. (It is subtracted to eliminate the
error or background contamination.)
W - 855 square mm for 37-mm diameter filters (the portion of
the membrane filter which is exposed when mounted in
the field monitor case, ie, the effective filter area).
A » The area of the counting field of a calibrated reticle
expressed in square mm/field.
V » Total air volume collected through filter expressed in
milliliters.
132
-------
fri
-------
APPENDIX D
OPERATION OF SAMPLING TRAIN-DATA SUMMARY FROM FIELD LOG BOOK
-------
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APPENDIX E
HASTINGS MASS FLOW METER DATA
-------
HAST3NGS-RAYDIST
A TELEDYNE COMPANY
Specification Sheet 505 C
HAMPTON. VIRGINIA 23361
HASTINGS MASS FLOWMETER
LF SERIES - NON LINEAR
FOR LOW FLOW RATE MEASUREMENTS OF AIR AND GASES
RANGES: 0-20 to 0-20,000 STD CC/MINUTE
MAJOR FEATURES
MEASURES EXTREMELY LOW FLOW RATES
READABILITY TO
OF RANGE.
^ACCURATE AND STABLE WITHIN 2% FROM 0.1
psia TO 250 psia
• NO CORRECTION NECESSARY OVER WIDE
RANGES OF TEMPERATURE AND PRESSURE
• RUGGED, VERSATILE, TROUBLE-FREE TRANS-
DUCER
LONG LIFE
The Hastings LF Mass Flowmeter features a thermal
technique wherein the flow transducer sensing ele-
ment is completely external to the flow stream and
has no moving parts to wear out. It is safe for toxic
.and hazardous gases. Gas flow contacts only monel
family alloys, solder and brass. Models with all
monel family alloys are available for measuring flow
rates of highly corrosive gases.
RUGGED- EASY TO INSTALL -
REL1ABLE
I
The LF meter circuitry is 100% solid state for
maximUm reliability and stability. Transducer can
withstand extreme vacuum, pressure and flow rates
withoutXdamage. No special tools or techniques£
_needed-j. _ . ---------- _ -- .
..\
HASTINGS FLOWMETER
TRANSDUCER
HIGH STABILITY AND ACCURACY
With the Hastings LF Mass Flowmeter pressure and
temperature need not be measured to determine
mass as with volume flowmeters. No ambient tem-
perature correction is required from 32"F to 110°F.
No gas pressure correction is required from 0.1 psia
to 250 psia or gas temperatures up to 200°F. Ac-
curacy is within 2% over this range.
Measurement repeatability is within 1%. Standard
factory calibration is for air. Curves for other usual
gases are available. Once installed and in use the
instrument needs no recalibration. Pressure drop
through the flow tube is nominal for most ranges.
MODELS FOR TUNGSTEN
HEXAFLUORIDE
Three of the models are especially constructed and
calibrated for directly reading the mass flow of
tungsten hexafluoride gas. They are also useful for
rhenium hexafluoride and similar corrosive gases.
Transducer construction of all monel alloys and
"teflon" seals. Slightly larger transducer (3"
diameter".)
Model: ALF-100W—0-100 seem
ALE. 3QQW—Q-3QQ seem. ..
-------
*
HASTMOS F-SOMCS TRANSDUCE*
CHARACTERISTICS
OPERATING PRINCIPLES
The Hastings LF Mass Flowmeter consists of an
electrically heated tube and an arrangement of
thermocouples to measure the differential cooling
caused by a gas passing through the tube. Thermo-
electric elements generate d-c voltage proportional
to the rate of mass flow of gas through the tube.
> fragile sensing elements project into the stream.
is design depends only on the mass flow and
specific heat of the particular gas and is, therefore,
practically insensitive to pressure changes in tem-
perature, thermal conductivity and viscosity.
APPLICATIONS
Hastings LF Mass Flowmeters have wide applications
in the measurement of leak rates and flow rates of
gases in the manufacture of tubes, lamps, neon
signs, semiconductors, fuel cells, valves and capil-
laries. They are also used for leak testing flanges
and valves in cryogenic gas lines, missile fueling
lines and for gas flow metering or for mixing gases
in atomic research, magnetohydrodynamics (MHO)
research, and in mass spectrometer type leak detec-
tors. Write details of your particular application and
requirements for recommendations by our Engineer-
ing Department.
POWER:
INDICATOR:
TRANSDUCER:
CABLES:
115 volt a-c (105 to 125 V a-c)
50-400 cycles, 15 watts
Dimensions: 7W X 5%" X
Weight: 6 Ibs.
Operating pressures: .1 psia
to 250 psia.
Gas flow temperatures: Up
to 200" F.
Ambient temperatures:
From 32° F to 110°F.
Sensitivity: 0.5% Full Scale.
Response Time: Approximately
5 seconds for most models:
Weight: 20 oz.
8-foot power and transducer
cables included with instrument.
SELECTION CHART
Range
Std. CC/Min
0-20
0-50
0-100
0-300
o.iooo
0-5000
0-10.000
0-20,000
Model
LF-20
LF-50
LF-100
LF-300
LF-1K
LF-5K
LF-10K
LF-20K
Transducers
(see Notes)
F-20
F-50
F-100
F-300
F-1K
F-5K
F-10K
F-20K
Pressure Dr
@ Full Sea
Inches Hz<
7O
12
1
3
1
1
1
1
Standard C.C. Per Minute
TYPICAL DIAL FACE SHOWN ACTUAL SIZE
NOTES:
Transducers are available in standard brass
"monel" construction. Monel type denotes all mat
rials in contact with the gas are monel family alloy
Transducers are rated to 250 psi.
All models include switch and binding posts f
connection to high impedance potentiometer ty;
recorder. Output signal is approximately 0-2.4 mil
volts dc. :
Also available as a complete flow recorder util
ing G. E. #520 recorder, direct reading scale ar
0-100 linear chart paper.
For linear type flowmeters and higher flow rat
to 200 scfm, see Hastings; Linear Mass. Flowmeter
Specification Sheet 508-A.
WTELEDYNE
MASTINGS-RAYDIST
HAMPTON, VIRGINIA 23661. U.S.A.
PRINTED IN U.SJV.
E-7. SPECIFICATION SHEET 0505C
PHONE (804) 72:
TWX: 710-88:
COPYRIGH1
-------
-------
APPENDIX F
ROTOMETER CALIBRATION DATA
-------
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-------
-------
APPENDIX G
LIST OF SAMPLES AND TEST RESULTS
-------
APPENDIX G
LIST OF SAMPLES AND TEST RESULTS
CODE DESCRIPTION
FG-D-A Fibrous Glass sites A & D - downwind
FG-D-D Monitors moved during sampling
P-D-A Phenol sites A ft D - downwind
P-D-D Monitors moved during sampling
F-O-A Formaldehyde sites A * 0 - downwind
F-D-D Monitor moved during sampling
FG-U-B Fibrous Glass site B - upwind
P-U-B Phenol site G - upwind
F-U-B Formaldehyde site B - upwind
FG-D-D Fibrous Glass site D - downwind
P-D-D Phenol site D - downwind
F-D-D Formaldehyde site D - downwind
F-U-G Fibrous Glass site B - upwind
P-U-B Phenol site B - upwind
F-U-G' Formaldehyde site G - upwind
FG-D-E Fibrous Glass site E - downwind
P-D-E Phenol site E - downwind
F-D-E Formaldehyde site E - downwind
F-D-E(prlme) Changed pump and new solution
FG-U-B Fibrous,Glass site B - upwind
P-U-B Phenol site B - upwind
F-U-B Formaldehyde site B - upwind
SAMPLE TIME
(5-2)
10:00-10:49 a.m.
10:00-12:00 p.m.
10:00-10:49 a.m.
10:50-12:00 p.m.
10:00-10:49 a.m.
10:50-12:00 p.m.
10:00-12:00 p.m.
10:00-12:00 p.im
10:00-12:00 p.m.
12:10- 2:00 p.m.
12:10- 2:00 p.m.
12:10- 2:00 p.m.
12:05- 2:05 p.m.
12:05- 2:05 p.m.
12:05- 2:05 p.m.
2:15- 4:00 p.m.
2:15- 4:00 p.m
2:15- 3:05 p.m
3:20- 4:00 p.m
:10- 4
2:10- 4:
p.m.
p.m.
2:10- 4:11 p.m.
FIBERS FOR FG
uftFOR PaTlAB
" J RESULT
0.8
7.6
9.2
LOST
0.5
6.8
0.6
4.2
0.6
8.4
3.6
4.2
6.8
25°C 76*>mn
TOTAL VOLUHIT"
ppb
SAMPLED HJ
.350
.092
.041
.325
.084
.076,
.312
.090
.032
.325
.071
.076
.296
,086-.
.014 C
.024J
.315
.074
.069
Cone.
9
181
110
6
223
9
55
308
57
98
2
151
29
1
173
2
45
251
14
80
G-l
-------
APPENDIX G
LIST OF SAMPLES AND TEST RESULTS
CODE DESCRIPTION
FG-D-E Fibrous Glass site EftF downwind
FG-D-F monitor moved during sampling
P-D-E Phenol site EftF downwind
P-D-F Monitor moved during sampling
F-D-E Formaldehyde moved during sampling
F-D-F Monitor moved during sampling
FG-U-B Fibrous Glass site B - upwind
P-U-B Phenol site B - upwind
F-U-B Formaldehyde site B - upwind
FG-D-G Fibrous Glass site G downwind
P-D-G Phenol site G downwind
F-D-G Formaldehyde site G downwind
FG-U-H Fibrous Glass site H upwind
P-U-H Phenol site H upwind
F-U-H Formaldehyde site H upwind
P-D-G Phenol site G downwind
changed pump
F-D-G Formaldehyde site G downwind
P-U-H Phenol site H upwind
F-U-H Formaldehyde site H upwind
(5-2)
SAMPLE TIME
FIBERS FOR FG
4:12
5:00
4:12
5:00
4:12
5:00
4:47
4:47
4:47
•5:00 p.m.
6iOO p.m.
•5:00 p.m.
•6:00 p.m.
•5:00 p.m.
•6:00 p.m.
6:01 p.m.
-6:01 p.m.
-6:00 p.m.
(5-4) 12:15-5:00 p.m.
12:15-2:30 a.m.
12:15-2:30 a.m.
12:26-5:00 a.m.
12:26-2:26 a.m.
12:26-2:26 a.m.
2:40-3:05 a.m.
3:05-5:00 a.m.
2:45-5:00 a.m.
2:31-5:00 a.m.
2:31-5:00 a.m.
ttt) FOR PtF LAB
J RESULTS
25°C 76° run
TOTAL VOLUME
LI
IP
PBb
Cone
0.6
3.4
0.9
4.2
9.6
2.7
0.5
2.7
ND
0.4
0.5
NO
.301
.079
.065
.197
.043
.035
.844
.155
.076
.693
.136
.054
.187
.057
.157
.114
8
52
21
120
63
36
4
50
0
7
3
0
2
43
5
98
17
29
1
41
0
6
1
0
G-2
-------
APPENDIX 6
LIST OF SAMPLES AND TEST RESULTS
CODE
FG-D-A
P-D-A
F-D-A
FG-U-B
P-U-B
F-U-B
FG-D-A
FG-D-C
F-D-A
F-D-C
F-D-A
F-D-C
FG-U-B-
P-U-B
F-U-B
FG-D-C
P-D-C
F-D-C
FG-U-B
P-U-B
F-U-B
DESCRIPTION
SAMPLE T1HE
(5-1)
Fibrous Glass-site A-downwInd 6:01-8:01 p.m.
Phenol - site A- downwind 6:01-8:01 p.m.
Formaldehyde - site A - downwind 6:01-8:01 p.m.
Fibrous Glass - site B - upwind 6:01-8:01 p.m.
Phenol - site B - upwind 6:01-8:01 p.m.
Formaldehyde - site B - upwind
Fibrous Glass - sites A&C - downwind
Monitors moved during sampling
Phenol - sites ASC downwind
Monitors moved during sampling
Formaldehyde- sites AftC downwind
monitors moved during sampling
Fibrous Glass - site B - upwind
Phenol • site B - upwind
Formaldehyde - site B - upwind
Fibrous Glass - site C - downwind 10:15-12 midnight
Phenol •• site C - downwind 10:15-12 midnight
Formaldehyde - site C - downwind 10:15-12 midnight
Fibrous Glass - site B - downwind 10:32-12:02
Phenol • site B - upwind 10:32-12:02
Formaldehyde - site B - upwind 10:32-12:02
6:01-8:01 p.m.
8:16-8:56 p.m.
8:56-10:01 p.m.
8:16-8:56 p.m.
8:56-10:01 p.m.
8:16-8:56 p.m.
8:56-10:01 p.m.
8:15-10:03 p.m.
8:15-10:03 p.m.
8:15-10:03 p.m.
FIBERS mo
ugFOR PftF LfiB
RESULTS
0.5
2.7
0.5
25° 76°mm
Tola
(5-2) a.m.
(5-2) a.m.
(5-2) a.m.
0.5
1.1
1.8
8.5
o.5
0.4
samp
-Si
~'i.n
ed tj3
.330
.124
.045
.357
.088
.061
.302
.104
.036
.281
.068
.055
.289
.104
.039
.221
.056
.042
Cone.
4
60
6
0
4
31
265
0
82
0
10
10
1
49
2
0
1
25
69
0
21
0
: 2
8
G-3
*HD - Non-detectable
-------
H
-------
APPENDIX H
HEALTH EFFECTS DATA
-------
TABLE 15. HUMAN RESPONSES FROM EXPOSURE TO PHENOL VAPORS30
Concentration
(ppm)
0.047
0.0 - 3.3
1.5 - 5.2
48.0
(plus 8 ppm
HCHO)
Duration of
exposure ^
minutes
8 hrs/day
8 hrs with two
30 min breaks
Response
Odor threshold
No ill effect. Rise in urinary
phenol
No ill effect; 60 to 88 percent of
phenol absorbed by lungs. Rise in
urinary excretion of phenol during
exposure with a return to pre-
exposure levels within 24 hours
5 to 10 min/hr, Marked irritation of the nose, throat
8 hr/day and eyes. Formaldehyde may be prima-
ry cause.
Reference
4
33
34
35
-------
TABLE 14. HUMAN RESPONSES FROM EXPOSURE TO FORMALDEHYDE VAPORS
Concentration
(ppm)
0.01
0.05
0.4 - 0.8
Duration of
expose
5 rain
-
Occupational
Response
Eye irritation threshold
Odor threshold
Acute exposures caused eye, nose,
Reference
13
3
1
0.13 - 0.45
0.25 - 1.39
0.9 - 1.6
exposure
s
Occupational
exposure
Occupational
exposure
Occupational
exposure
throat irritation, and lower
respiratory tract symptoms
Burning, stinging eyes, headaches, 21
intolerable irritation of eyes,
nose and throat; one illnes
Upper respiratory tract irritations, 20
burning of eyes and nose, sneezing-
coughing, headaches
Intense irritation, itching of eyes 22
dry and sore throat, increased
thirst disturbed sleep
1.0
4.0
4.0 - 5.0
10.0
16 - 30
50 - 100
-
5 min
10 to 30 min
few minutes
Occupational
exposure
(8 hr/day)
5-10 min
Detectable by nearly all people
Severe eye irritation
Intolerable to most people;
lachrymation, discomfort, throat
irritation
Profuse lachrymation
Skin reaction
May cause serious injury; serious
bronchial inflammation
23
24
23,25
23
26
17
-------
APPENDIX H
HEALTH EFFECTS DATA
1. Schoenberg, J. B., and C. A. Mitchell. Airway Disease Caused by Phenolic
(Phenol .- Formaldehyde) Resin Exposure. Arch Environ Health. 30:574-577.
1975.
2. Kerfoot, E., and T. Mooney. Formaldehyde and Paraformaldehyde Study
In- Funeral Homes. Am Ind Hyg Assoc. J. 36:533. 1§75.
3. Bourne, H., and S. Seferian. Formaldehyde fn Wrinkle-Proof Apparel
Processes - Tears for Milady. Ind Med Surg. 28:232. 1959.
4. Petrov, V. I. Causes of Phenol Vapor Poisining During Coke Slaking With
Phenol Water, in Levine BS (trans): USSR Literature on Air Pollution
and Related Occupational Diseases - A Survey. Springfield, VA., U.S.
Dept. Comm. (NTIS 63-11570) 8:219-21. 1963.
-------
-------
APPENDIX I
Participants In Survey
All participants are employees of the Environmental Protection
Agency, Surveillance and Analysis Division, Region III.
Robert Kramer - Task Manager
Theodore Erdman - Test Manager and Test Site Leader
David O'Brien - Test Site Leader
David Lorentz - Test Technician
Carmella Gualtieri - Test Technician
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