-------
COMPANY:
SOURCE:
CLAYTON ENVIRONMENTAL CONSULTANTS, INC.
CRITICAL ORIFICE SAMPLING DATA
DATE: 3-/S-78
GAS METER NO.
FIELD PERSON:
BAROMETRIC PRESSURE:
ORIFICE NO.
/
/
*
cal
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
A"~-igp
Test
Number
'-roA
*\
'^
*w ^ .
Time
r-0.^
K*p
'tfUjAjs
JO
\c\ *<&_>
Orifice
Inlet
Temp.
T0 (F°)
"70
/A<^\'/L!//
Kit
r/
Or i f ice
Inlet
Vacuum^O
Pol (^)
' ' f Q
\^'^\^
VI ,'
^,7. /6i/
Or if iceX
Outlet
Vacuum
POO ("HS)
('/> \y* f 1^ ,J/.^
?t
/.^2_ JO,U>
-------
COMPANY:
SOURCE:
p J.i it i i vj it r. w v 4. iv n n 1-1 li is j /\ i. \, 4.1 ™ .' i 11 u 1 " >" ' ••> j i «i i. ,
_CJ\1'!1LCA.I: OJLL™! .?_AM_PLJ.NC. j?ATA
DATE: "?," /4 " 79
GAS METER NO.
FIELD PERSON:
BAROMETRIC. PRESSURE: ,'^9.. ~1 Q
ORIFICE NO. /G£
QFstd =
A TStd ,v /Teal
I Tcal
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Test
Number
•'I, -';,^
"fOA" "3
1b A ^ .
Time
'iSMt
«
Orifice
Inlet
Temp.
1C>
•74
Orifice
Inlet
Vacuum
POI (Iln2o>
12.5"
10/3
ID. i
Orifice
Outlet
Vacuum
POO ("HS>
^-c/^» ' V
0 0 4-
•S't
Gas
Meter
Volume
VM (CF)
89, 547
9)t«
Gas
Meter
Temp.
°F
73
7f
Gas
Meter
Pressure
"Hg
0
0
O
0
Sample
Volume
(Liters)
Qstd
I.W" Jl.l
1
\.oS JI.5
-------
DATA
Company:
Source Designation:
Date:
Q
Job No . :
Field Person: {\^/(/
Clock
Time
Time
(min)
7:40
2-6
/ f a &
/V/c
4-c
20
9o
eli-
L-o
2°
te 4o
ic So
US
// o &
10
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its'
// 0
.'9*
its'
it 30
I 20
3?
/ 7*
; 40
.90
i 60
/ I 3 v i
0
17*'
a ** ;
'//y
/3 r,
Clayton Environmental Consultants, Inc
-------
DATA
Company:
Source Designation:
Date: j
/ cf ///te i- v
t/Jt Co.
Clock
I Time
Job
Field Person
Time
(min)
*£
'•'
« *•
/c
/O < 0
20
30
47
/£>.
40
JO
£,11.
7*
f 0 .0
/&. 0
i 10 2.
/?/ z.
9. o
^s
46.0
i 2.0
/ 30
,7*
*'
j-t.*
* 4-
7, o
V
i 4
'7c>
7.0
/CO
0
. so
rn • h' /o1"/
Clayton Environmental Consultants, Inc
-------
DATA
Company:
Source Designation:
Date:
L
No. '
Field Pers.on
Clock
Time
Time
(min)
fiATZ
/in**
OOP
4
'*•
0 V
/t*
40
90
70
.90
70
/*'
"
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ft.*
g.o
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13 'o
// / o
1 40
/ / I 0
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60
46
<*$
iff"
*-*>
ii^-f .
Clayton Environmental Consultants, Inc
-------
• DATA
Company:
Source Designation:
Date:
\ '
Job No.:
Field Pers.on
I—~
Clock
j T ine
Time
(min)
-ZT/J-Tr
0
,96
Jfl
2.0
-9*
/**
•3U7
3*
40
/
Co
47. o
70
. 9"
4*.*
'*-
/ 7 ^ 2-
/ 7/
70
/ts
3,0
/ 0 O
/t-
// o
.
-------
DATA
Company:
Source Designation:
Date: .;
Job No
I
-2- Field Person: //>iv///? j
Clock
Time
Time
(min)
A fir* i
C-P« 1
// /
0
0,7-
31 f?
lo
5"
,1/Vf
4
C
11'-
vc
*
Clayton Environmental Consultants, Inc
-------
DATA
\
Company:
Source Designation:
Date: i - / i
\^\(\
/ //•
Job No..:- "
Field Pers.on:
. *>
Clock
Tine
Time
(min)
&7X
JTV4J?
•j
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tit
l.At
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/J
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'It'
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i-
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H
n
6
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I?
1 1: 1'
14
Hi'
I,
4^
Clayton Environmental Consultants, Inc
-------
DATA
Company: ^ELf/j ~ 7/15A 2
Source Designation:
Date: j> IlL/l f
A^.
-^ Job No.: (, jtjtj-
Field Person:
Clock
Time
Time
(min)
Ll\-\
flfc/VC-
0
e,
JO
H
o
HO
10
A;
/ .?£
ofte
f*>
/
/-e
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tec)
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/OC
*/.$
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JJL
Ho
i/ac
1 60
/A/
n
JlfC
^ 5
/.Of
II 10
n_o_
1L&.
II5.C
ISO
II 5-
Clayton Environmental Consultants, Inc
-------
DATA
Company:
Source Designation:
Jate: '3
Job No.:
\ '[ - 7_
Field Person
Clock
lice
Time
(min)
} Of:
' 'J
/#}
to
I '-(6
-to
i <'/
40
U
12L
4L
LI
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Clayton Environmental Consultants, Inc.
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-------
APPENDIX B
SECTION II SAMPLING SUMMARY DATA
-------
I' 1 :i ii I:
Koichliold Clicunicii 1, Inc.
SAMPLING SUMMARY SllfiliT
Luc ii t i o n
S a r.i p11; il Sou r c c
Total organic acids
Out lot
Run
TOA-1
TOA-2
TOA-3
TOA-4
Date
3-16-78
3-15-78
3-16-78
3-16-78
NP
12
12
12
12
PTTI
1.95
1.88
1.74
2.26
Pb
29.67
29.64
29.70
29.70
vm
114.940
136.243
125.837
132.868
T
im
91
94
94
94
Vmstd
110
129
120
126
vv
211
247
230
230
Vwp,as
9.93
11.6
10.8
10.8
7.M
8.3
8.2
8.3
7.9
i
Md
0.917
0.918
0.917
0.921
Run
TOA-1
TOA-2
TOA-3
TOA-4
MWd
28.92
28.92
28.95
28.99
MW
28.01
28.02
28.04
28.12
Pst
0. 004
0.006
0. 007
0. 007
Ps
29.67
29.65
29.71
29.71
°P
0.99
0.99
0.99
0.99
*
v4>PsX(Ts+460)c
12.6
12.6
12.1
12.1
Vs
2220
2210
2740
2120
*
Ts
122
122
115
115
Tt
180
180
180
180
• Dn
0.251
0. 251
0.251
0.251
%I
97.0
114
84.1
' 114
18 (t •
5120. e,» Cp x
ijon
100 X V,
OJI
"tld
H.-ICO-S
Iffo
ToUl Co. of Stir.pl Ing Pol lit
Avrr«gi;irHlc8 Presturt
Drop, In. llO .
P. Oiroinelrlc Prcisur*, In. <}.
n Absolute
V. Volume of Oi-y C«i it Kctar
u T-^dl lions. OCF
T(J Average He lor Temper slur*,
V, Volunxs of Ory Cat it STP,
a«M OSCFJ
V^ Totsl'lUO Collected In Iir-jln-
w jcrt ind Silica Ccl. »l
V..
W0»
SH
Hd
X C02
2 Oj
X CO
t }<2
>U,
Vo1in« of Water Vspor CoUcetad
«t MP, SCF°
I Uoliture by Vo'lumj
Hole fraction of Dry (Ul
Voluna t Dry
Volura t Dry
Voli/ne X Dry
Volwnc 1 Dry
Molecular Vtlght of Stsck Cit0
Dry Dill*
Holecuhr Usl(jht of Jlack
(Uj. Vet Bull
Stillc Prcuvra of Stick
Gilt In. n>j
Stick Cti Prcituf«, In. Hj
Pilot Tube Crtfflcltnl.
Stick Cat Velocity *l SlicV
Condi llont, fp.ni.
Stack Tempenturg
Kst TIM Of Ttsl, Wlfl,
Konli
ta,
I P«rt:tit
* Dry lUndjrd cubic feet tt fcS F« 29.92 In. II;.
* St»r,flirJ conditions itfc&'r, 29.52 In. !lj,
*From traverse data sheet.
_
* /"If JTrf
n* *
If dolor-mined !>y swraalng tho »c,ij:re roat ef
pnclutt of th] voloclty lietd (u's) sr.d t^t
-------
Plant Reichhold Chemical, Inc.
Sampled Source
SAMPLING SUMMARY SHEET
Loca tion
Outlet
Total aldehydes and formaldehyde
Run
ALD-1
ALD-2
ALD-3
ALD-4
Date
3-15-78
3-15-78
3-16-78
3-16-78
NP
12
12
12
12
Pm
1.95
1.90
1.70
2.44
Pb
29.67
29.64
29.70
29.70
Vm
113.922
132.808
122.762
131.547
T
im
89
89
88
90
Vjnstd
109
127
118
126
vw
199
240
229
232
v
wgas
9.37
11.3
10.8
10.9
%M
7.9
8.2
8.4
8.0
Md
0.921
0.918
0.916
0.920
Run
ALD-1
ALD^2
ALD-3
ALD-4
MWd
28.92
28.92
28.95
28.99
MW
28.06
28.02
28.03
28.11
Pst
0. 004
0. 006
0. 007
0. 007
Ps
29.67
29.65
29.71
29.71
CP
0.99
0.99
0.99
0.99
V^PSX(TS+460)C
12.6
12.6
12.1
12.1
Vs
2210
2210
2330
2120
*,*
122
122
115
115
Tt
180
180
180
180
Dn
0.251
0.251
0.251
0.251
. 7.1
96.3
113 •
97.4
115
ffll
d.
(Ta *
100 x
S H»
,6,» Cp i / if x lTf
II » {T,
H
P
'.
\
\
\
\«
\
Totil Ko. of Simpllng FoHU
Averigi; Orifice Preitur*
Drop, tn. HjO
Siroratrtc Prcisur*, In. <].
Absolute
Volunc of Dry Cat «t Meter
T^dltloni. DCF
Avertfjc Kctor Temperature,
Volume of Dry Cil it STP,
oscrs
Totil'll.O Collected 1n Iipjln-
jcri ind SHIea Cel, il
* Dry slind£,'F.
. i
s.
X H
"d
SCO,
802'
t CO
'""'
»
8°F, 29.92 tn,
29.92 tn. Kg,
• j * .
Vc
X
He
Ve
Vc
V<
Vc
He
Kc
Hi
_ 4 _
IUM of Uiter Vtpor Collected
it Slf>, SCF°
X Kolilure by Volume
Hole Friction of Dry C*i
Voluna X Dry
Volume X Dry
Volume X Dry
Voluno I Dry
Molecular Weight of Stick &U,
Dry Dull
Koleculir Height of Stack
GJS, Uet Outs
.t
1
a
S I
Stitle Prtlture of Stick
Cn, tn. 117
Stick Cil Prctlv't, tn. Ha
Ab-.olute
Pilot Tub? Coefficient.
Stick Cst Velocity at
Condition}, f(v«.
Avrrige Stic* TcmpjritUrt
Ntt Tlra of Ttst, Kin.
Koult OttouUfi ta»
Purtsnt
* From traverse data sheet.
'- def—'- d by «jlnf "- -uuer ef "-
td-^i ha v y lie t) t tin
-------
TABLE B-l. DAILY COMPOSITE TEST LOG
March 15, 1978
Clock Time
Sample
'. 0923
0925
0930
0959
1030
1119
1129
1229
1230
1530
1532
1534
1635
1645
1649
1703
1724
1737
1830
1832
Regen.
eration
DES #3
DES #2
DES #1
DES #3
DES #2
DES #1
Integrated
Bag Sample
Inlet
B
E
B
\|
p
E
B '
\
.
E
Outlet
B
1
E
B
\
E
TOAA
Sampling
Train
B
\
f
E
B
\
E
Aldehyde0
Sampling
Train
B
\
E
B
\1
E
Water
Samples
!
:
•
c
c
c
c
I
1
i
A - Total organic acids
B - Begin test
C - Aliquot collected
D - Total aldehyde and formaldehyde
DES - Begin desorption cycle on given unit
E - End cycle.
- see Appendix A,
-------
TABLE B-2. DAILY COMPOSITE TEST LOG
March 16, 1978
Clock
Sample
0850
0853
0954
0958
1018
1031
1055
1150
1358
1400
1500
1502
1602
1608
1628
1653
1658
1800
1902
Time
Regen-
eration
DES #1
DES #3
DES #2
DES #2
DES #1
DES #3
. Integrated
Bag Sample
Inlet
\
I
3
:
B
V
E
Outlet
\
I
B
:
I
\
E
$
TOAA
Sampling
Train
\
I
B
:
1
\
E
3
Aldehyde15
Sampling
Train
\
I
B
S
]
\
E
3
Water
Samples
C
C
C
C
C
C
A - Total organic acids
B - Begin test
C - Aliquot collected
D - Total aldehyde and formaldehyde
DES- Begin desorption cycle on given unit
E - End cycle.
- see Appendix A,
-------
TABLE B-3. SUMMARY OF STACK CONDITIONS
Samp le
Locat ion
Inlet
Outlet
Sample
No.
1
2
3
4
1978
Sample
Date
3-15
3-15
3-16
3-16
Average
1
2
3
4
3-15
3-15
3-16
3-16
Average
Temperature
Stack
OF
115
115
115
116
115
125
125
124
119
123
°C
46.2
46.2
46.3
46.4
46.3
51.7
51.7
51.1
48.3
50.7
Drum
OF
195
171
159
162
172
165
141
130
129
141
°C
90.6
77.2
70.6
72.2
77.7
73.9
60.6
54.4
53.9
60.7
Stack Flow Rate2
DSCFM
17,600
17,500
17,100
17,200
17,400
17,600
17,500
17,100
17,200
17,400
ACFM
21,300
21,200
20,500
20,500
20,900
21,300
21,200
20,500
20,500
20,900
DNm3
m
499
496
485
487
492
499
496
485
487
492
ANm3
m
603
601
580
580
591
603
601
580
580
591
Temperatures were taken from the integrated bag sampling data sheets.
2Flowrates were calculated from same day traverse sheets run on the outlet only.
Inlet flowrates were assumed to be the same as outlet flowrates.
-------
TABLE B.4. SUMMARY OF ORSAT DATA
Sampling
Location
Inlet
Outlet
1978
Sampling
Datfi
3-15
3-15
3-16
3-16
3-15
3-16
3-16
Sample
No.
1
2
3
4
2
3
4
Exhaust Gas Composition
(Percent Dry Basis)
Carbon
Dioxide
1.7
2.1
2.3
2.3
1.9
2.2
2.4
Oxygen
15.5
15.2
14.9
13.7
15.4
15.0
15.1
Carbon
Monoxide
1.1
1.2
1.0
0.8
l.o
0.9
1.2
Nitrogen
and Inerts
81.7
81.5
81.8
83.2
81.7
81.9
81.3
-------
APPENDIX C
DETAILED SUMMARY OF
SAMPLING AND ANALYTICAL
PROCEDURES'
DETERMINATION OF BENZENE FROM STATIONARY SOURCES
LAAPCD METHODS FOR ORGANIC ACIDS, ALDEHYDES. FORMALDEHYDES
TENTATIVE METHODS FOR ISOKINETIC DETERMINATION
OF POLLUTANT LEVELS IN THE EFFLUENT OF
FORMALDEHYDE MANUFACTURING FACILITIES
FORMALDEHYDE IN AMBIENT AIR
INDUSTRIAL HYGIENE, AND STACK GAS SAMPLES
-------
DETERMINATION OF BENZENE FROM STATIONARY SOURCES
-------
27SLP
METHOD DETERMINATION OF BEHZEKF
FROM STAtlONARY SOURCES
INTRODUCTION
Performance of this mathod should not be attempted
by persons unfamiliar with the operation of a gas
chromatograph, nor by those who are unfamiliar with
source sampling, as there are many details that are
beyond the scope of this presentation. Care must
be exercised to prevent exposure of sampling personnel
to benzene, a carcinogen.
1. Principle and Applicability
1.1 Principle. An integrated bag sample of stack gas containing
benzene and other organics is subjected to gas chromatographic (GC)
analysis, using a flame ionization detector (FID).
1.2 Applicability. The method is applicable to the measurement
of benzene in stack gases only from specified processes. It is not
•
applicable where the benzene is contained in participate matter.
2. Range and Sensitivity
The procedure described herein is applicable to the measurement
Of benzene in the 0.1 to 70 ppm range. The upper limit may be
extended by extending the calibration range or by dilution of the
sample.
3. Interferences
The chromatograph columns and the corresponding operating
parameters herein described have been represented as being useful for
producing an adequate resolution of benzene. However, resolution
interferences may be encountered on some sources. Also, the chro-
matograph operator may know of a column that will produce a superior
-------
resolution of benzene without reducing the response to benzene
as specified in Section 4.3.1.
In any event, the chromatograph operator shall select a
column which is best suited to his particular analysis problem,
subject to the approval of the Administrator. Such approval shall
be considered automatic provided that confirming data produced
through a detnonstrably adequate supplemental analytical technique,
such as analysis with a different column or g.c./mass spectrosccpy,
is available for review by the Administrator.
4. Apparatus
4.1 Sampling (see Figure 1).
4.1.1 Probe. Stainless steel, Fyrex glass, or Teflon ti:b'":ig
•
according to stack temperature, each equipped with a glass wool pU;cj
to remove particulate matter.
4.1.2 Sample Line. Teflon, 6.4 mm outside diameter, of .sufficient
length to connect probe to bag. A new unused piece is employ-ad for
each series of bag samples that constitutes an emission test.
4.1.3 Male (2) and female (2) stainless steal quick connects,
with ball checks (one pair without) located as shown in Figure 1.
4.1.4 Tedlar or aluminized Mylar bags, 100 liter capacity. To
contain sarr.ple.
4.1.5 Rigid leakproof containers for 4.1.4, with covering to
protect contents from sunlight.
Mention of trac'3 ncr^ea on specific products does not constitute
endorsement by the Environmental Protection Agency.
-------
FILTER (GLASS WOOL)
STACK WALL
PRO 3=
TEFLON
SAMPLE LIN:
QUICK
COfJfJECTS
FEMALE
PUM?
MYLAR
RIGID LEAK-PROOF
CONTAINER
Figure 1. Integrated-bag sampling train. (Mention of trade names on specific products
does not constitute endorsement by the Environmental Protection Agency.)
-------
4.1.6 Needle Valve. To adjust sample flow rate.
4.1.7 Pump—Leak-free. Minimum capacity 2 liters per minute.
4.1.8 Charcoal Tube. To prevent admission of benzene and other
organics to the atmosphere in the vicinity of samplers.
4.1.9 Flow Mster. For observing sample flow rate; capable of
measuring a flow range from 0.10 to 1.00 liters per minute.
4.1.10 Connecting Tubing. Teflon, 6.4 mm outside diameter, to
assemble sample train (Figure 1).
4.2 Sample Recovery.
4.2.1 Tubing. Teflon, 6.4 rr,nu outside diameter, to connect bag to
gas chromatograph sample loop. A new unused piece is employed for each
series of bag samples that constitutes an emission test, and is to be
discarded upon conclusion of analysis of those bags.
4.3 Analysis.
4.3.1 Gas Chromatograph. With FID, potentiorrietric strip chart
recorder and 1.0 to 2.0 ml heated sampling loop in automatic sample
valve. The chromatographic system shall be capable of producing c
response to 0.1 ppm benzene that is at least as great as the average
noise level. (Response is measured from the average value of the
baseline to the maximum of the waveform, while standard operating
conditions are in use.)
4.3.2 Chromatographic Column.
4.3.2.1 Benzene in the Presence of Aliphatics. Stainless Steal,
2.44 n x 3.2 ram, containing 10 percent TECP on 80/100 Chromosorb P AW.
-------
4.3.2.2 Benzene With Separation of the Isomers of Xylene. Stainless
steel, 1.83 m x 3.2 nun, containing 5 percent SP-1200/1.75 percent Bentone
34 on 100/120 Supelcoport.
4.3.3 Flow Meters (2). Rotaneter type, 0 to 100 ml/min capacity.
4.3.4 Gas Regulators. For required gas cylinders.
4.3.5 Thermometer. Accurate to one degree centigrade, to measure
temperature of heated sample loop at time of sample injection.
4.3.6 Barometer. Accurate to 5 n:m Hg, to measure atmospheric
pressure around gas chromatograph during sample analysis.
4.3.7 Purcp--Leak-free. Minimum capacity 100 ml/min.
4.3.8 Recorder. Strip chart typa, optionally equipped with disc
integrator or electronic integrator.
4.3.9 Planirr.eter. Optional, in place of disc or electronic
integrator, for 4.3.8 to measure chromatograpn peak areas.
4.4 Calibration. 4.4.2 through 4.4.6 are for section 7.1 which
is optional.
4.4.1 Tubing. Teflon, 6.4 irm outside diameter, separate pieces
marked for each calibration concentration.
4.4.2 Tedlar or Alurninizsd Mylar Bags. 50-liter capacity, with
valve; separate bag marked for each calibration concentration.
4.4.3 Syringe. 1.0 pi, gas tight, individually calibrated, to
dispense liquid benzene.
4.4.4 Syringe. 10 yl> gas tight, individually calibrated, to
dispense liquid benzene.
4.4.5 Dry Gas Meter, V.'ith Temperature and Pressure Gauges.
Accurate to +2 percent, to meter nitrogen in preparation of standard
gas mixtures.
-------
4.4.6 Midget Impinger/Hot Plate Assembly. To vaporize benzene.
5. Reagents
It is necessary that all reagents be of chromatographic grade.
5.1 Analysis.
5.1.1 Heliuin Gas or Nitrogen Gas. Zero grade, for chrcmatographic
carrier gas.
5.1.2 Hydrogen Gas. Zero grade.
5.1.3 Oxygen Gas or Air as Required by the Detector. Zero grade.
5.2 Calibration. Use one of the following options: either 5.2.1
and 5.2.2, or 5.2.3.
5.2.1 Benzene, 99 Mol percent pure benzene certified by the
manufacturer to contain 'a minuvjin of 99 Mol percent benzene; for use in
the preparation of standard gas mixtures as described in Section 7.1.
5.2.2 Nitrogen Gas. Zero grade, for preparation of standard gas
mixtures as described in Section 7.1.
5.2.3 Cylinder Standards (3). Gas mixture standards (50, 10, and
5 ppm ber.zene in nitrogen cylinders) for which the gas coir.positicn has
been certified v/ith an accuracy of +3 percent or better by the
manufacturer. The manufacturer must have reccnrcendsd a rnaximun shelf
life for each cylinder so that the concentration does not change
greater than +5 percent from the certified value. The date of gas
cylinder preparation, certified benzene concentration and recommended
jnaxiniurn shelf life must have been affixed to the cylinder before ship-
ment from the gas manufacturer to the buyer. These gas mixture
standards may be directly used to prepare a chromatograph calibration
curve as described in Section 7.3.
-------
5.2.3.1 Cylinder Standards Certification. The concentration
of benzene in nitrogen in each cylinder rcust have been certified by
the manufacturer by a direct analysis of each cylinder using an
analytical procedure that the manufacturer had calibrated on the day
of cylinder analysis. The calibration of the analytical procedure
shall, as a minimum, have utilized a three-point calibration curve.
It is recommended that the manufacturer rcaintain two calibration standards
and use these standards in the following way: (1) a high concentration
standard (between 50 and 100 ppm) for preparation of a calibration curve
by an appropriate dilution technique; (2) a low concentration standard
(between 5 and 10 ppm) for verification of the dilution technique used.
5.2.3.2 Establishment and Verification cf Calibration Standards.
The concentration of each calibration standard must have been established
by the manufacturer using reliable procedures. Additionally, each
calibration standard must have been verified by the manufacturer by one
of the following procedures, and the agreement between the initially
determined concentration value and the verification concentration value
must be within +5 percent: (1) verification value determined by com-
parison v:ith a 923 r.-ixture prepared in accordance with the procedure
described in section 7.1 and using 99 Hoi percent benzene, or (2) veri-
fication value obtained by having the calibration standard analyzed by
the national Bureau of Standards. All calibration standards must be
renewed on a time interval consistent with the shelf life of the cylinder
standards sold.
-------
6. Procedure
6.1 Sampling. Assemble the sample train as in Figure 1. Perform
e bag leak check according to section 7.4. Determine that all connections
between the bag and the probe are tight. Place the end of the proba at
the centroid of the stack and start the pump with the needle valve
adjusted to yield a flow of 0.5 Ipm. After a period of time sufficient
to purge the line several times has elapsed, connect the vacuum line to
the bag and evacuate the bag until the rotameter indicates no flow.
Then reposition the sample and vacuum lines and begin the actual sampling,
keeping the rate constant. Direct the gas exiting the rotameter away
from sampling personnel. At the end of the sair.ple period, shut off the
pump, disconnect the sample line from the bag, and disconnect the
vacuum line from the bag container. Protect the bsg container from
sunlight.
6.2 Scrn.ple Storage. Sample bags must be kept out of direct sunlight.
Analysis must be performed within 2[, hours of sample collection.
6.3 Ssrnple Recovery. With ?. new piece of Teflon tubing identified
for that bag, connect a bag inlet valve to the gas chronetograph sa~.ple
valve. Switch the valve to withdraw gas fron the bag through the sample
loop. Plumb the equipment so the sample gas passes from the sample valve
to the Isak-fres pump, and then to a charcoal tube, followed by a
0-100 ml/rr.in rotameter with flow control valve.
6.4 Analysis. Set the column temperature to 80°C for column A or
75°C for column B, the detector temperature to ?.25°C, and the sample loop
temperature to 70°C. I/hen optimum hydrogen and oxygen flow rates have
-------
been determined, verify and maintain these flow rates during all
chromatograph operations. Using zero helium or nitrogen as the
carrier gas, establish a flov; rate in the range consistent with the
manufacturer's requirements for satisfactory detector operation. A
flow rate of approximately 20 ml/niin should produce adequate separations.
Observe the base line periodically and determine that the noise level
has stabilized and that base line drift has ceased. Purge the sample
loop for thirty seconds at the rate of 100 nl/min, then activate the
sample valve. Record the injection time (the position of the pen on
the chart at the time of sample injection), the sample number, the
sample loop temperature, the column temperature, carrier gas flow rate,
chart speed and the attenuator setting. Record the laboratory pressure.
From the chart,Tots the peak having the retention time corresponding to
benzene, as determined in section 7.2. Measure the benzene peak area, A ,
in
by use of a disc integrator or a planirretrr. Record A and the
retention time. Repeat the injection at least two times or until two
consecutive values for the total area of the benzene peak do not vary
more than 5 percent. The average value for these two total areas will
be used to compute the bag concentration.
6.5 Measure the ambient temperature and barometric pressure near
the bag. From a water saturation vapor pressure table, determine and
record the water vapor content of the bag. (Assume the relative humidity
to be 100 percent unless a lesser value is known.)
7. Calibration and Standards
7.1 Preparation of Benzene Standard Gas Mixtures. (Optional--
del ete if cylinder standards are used.) Assemble the apparatus shown
-------
SYRINGE
JJ7— SEPTUM'
X
BOILING
WATER
BATH
~—
L- MIDGET
IM FINGER
HOT PLATE
CAPACITY
50 LITERS
FIGURE 2. PREPARATION Or GnNZEflE STANDARDS
(optional)
-------
in Figure 2. Evacuate a 50-liter Tedlar or alufr.inized Mylar bag that
has passed a leak check (describee! in Section 7.4) and neter in about
50 liters of nitrogen. Measure the barometric pressure, the relative
pressure at the dry gas meter, and the temperature at the dry gas r.eter.
While the bag is filling use the 10 yl syringe to inject 10 ul of 99 + '
percent benzene through the septum on to? of the impingar. This gives
a concentration of approximately 50 ppni of benzene. In a like manner,
use the other syringe to prepare dilutions having approximately 10 and
5 ppm benzene concentrations. To calculate the specific concentrations,
refer to section 8.1. These gas mixture standards may be used for
four days from the date of preparation, after which tine preparation of
new gas mixtures is required. (Caution: Contamination ray be a
problem when a bag is reused if the new gas mixture standard is a lower
concentration than the previous ess mixture standard.)
7.2 Deter/r.ination of Benzene Retention Tine. This section can be
perforniad siinultansously with section 7.3. Establish chromrrtograph
conditions identical with those in section 6.3, above. Determine proper
attenuator position. Flush the sampling loop with zero helium or
nitrogen and activate the sample valve. Record tha injection tirre, the
sample loop to.-sperature, ths column temperature, the carrier gas flow
rate, the chart speed and the attenuator sotting. Record peaks and
detector responses that occur in the absence of benzene. Maintain con-
ditions, with the equipment plumb ing arranged idcntially to section 6.3,
and flush the sample loop for 30 seconds at ths rate of 100 nl/nin with
one of the banzene calibration mixtures end activate the sample valve.
-------
F.ocord the injection time. Select the peak that corresponds to
banzene. Measure the distance on the chart from the injection time to
the time at which the peak maximum occurs. This quantity, divided by
the chart speed., is defined as the benzene paak retention time. Since
It is quite likely that there will be other organics present in th.-;
sample, it is very important that positive identification of the benzene
peak be made.
7.3 Preparation of Chromatograph Calibration Curve. Make a gas
chromatographic measurement of each standard gas mixture (described in
section 5.2.3 or 7.1) using conditions identical with those listed in
sections 6.3 and 6.4. Flush the sampling loop for 30 seconds at the
rate of ICO ml/min v/ith one of the standard gas mixtures and activate the
sample valve. Record C , the concentration of bsnzene injected, the
attenuator setting, chart speed, peak area, sample loop temperature:,
column temperature, carrier gas flow rate, and retention time. Record
the laboratory pressure. Calculate A , the peak area multiplied by the
attenuator setting. Repeat until tv:o consecutive injection areas arc
within 5 percent, then plot the average of those two values vs C . V.'iien
the other standard gas mixtures have been similarly analyzed and plotted,
draw a smooth curve through the points. Perform calibration daily, or
before and after each set of bag samples, whichever is more frequent.
7.4 Bag Leak Checks. While performance of this section is required
subsequent to bag use, it is also advised that it b= performed prior to
bag use. After each use, make sure a bag did not develop leaks as
follows: to leak check, ccnnoct a water manometer and pressurize the
-------
bag to 5-10 cm H20 (2-4 in. H20). Allow to stand for 10 minutes. Any
displacement in the water manometer indicates a leak. Also, check the
rigid container for leaks in this manner. (Mote: an alternative leak
check method is to pressurize the bag to 5-10 en H-O or 2-4 in. FLO and
allow to stand overnight. A deflated bag indicates a leak.) For each
sample bag in its rigid container, place a rotain^ter in line between
the bag and the pump inlet. Evacuate the bag. Failure of the rotameter
to register zero flow when the bag appears to be empty indicates a leak.
8. Calculations
8.1 Optional Benzene Standards Concentrations. Calculate each
benzene standard concentration prepared in accordance with section 7.1
as follows:
X(/8787 mg) ^ V:C] v5 ' imle 2'1'055 ::1 "6
p „ jiKj 78.11 JJCJ yC] . IVQ]
C v IP6 ul 293 _JTI_
Y 1 T" 760~
293 Pm
Eau,t1on
76°
where:
C . = The benzene standard concentration.
X = The number of ul of benzene injected.
Y = The dry cjas meter reading in liters.
P = The absolute pressure of the dry yas meter, irsn Hg.
m /
T = The absolute temperature of the dry gas meter, °A.
m . '
.8787 = The density of benzene at 293PA.
-------
78. 11 = The molecular weight of benzene.
24.055 = Ideal gas at 293°A, 750 n-m Kg.
10 = Conversion factor, ppm.
8.2 Benzene Sa.Tiple Concentrations. From t'r.2 calibration curve
described in section 7.3, above, select the value of C that corresponds
to A . Calculate C as follows:
Cs = P.Tr (l-Bwb) Equation 2
wnere:
B . = The v/ater vapor content of the bag sarrple, as analyzed.
C = The concentration of benzene in the sample in ppm.
C = The concentration of benzene indicated by the g?.s chrc:-;?.tocraph,
\*
in ppm.
P = The reference pressure, the laboratory pressure recorded d'jrinj
calibration, n?n Hg.
T. = The seinple loop temparat'jr'i1 on the absolute scale at the ti;ne
of analysis, °A.
P, = The laboratory pressure at tir,i5 of analysis, rmi Hg.
T = Ths reference temperature, the sample loop temperature recorded
during calibration, °A.
-------
List of Instruments Used
Gas chromatograph: AID Model 511
Chromatographic columns:
for total hydrocarbons: 2' x 1/16" unrestricted column
(flame ionization detector)
for benzene: 6' x 1/8" 5% SP-1200 + 1.75%
Bentone - 34 on 100/120 Supelcoport
(flame ionization detector)
-------
AIR POLLUTION
SOURCE TESTING MANUAL
by
HOWARD DEYORXIN
ROBERT L. CHASS
ALBERT P. FUDURICH
CARL V. KANTER
Edited by
RAYMOND G. HOLMES
Organic Acids 5,4.2
Aldehydes 5.4.3
Formaldehyde 5.4.4
Air Pollution Control District - Los Angeles County. California
S. SMITH GRISWOLD - Air Pollution Control Officer
price 55.00
-------
5.4.2 ORGANIC ACIDS
5.4.2.1 METHOD SUMMARY
The only collection 'method used by the
APCD for organic acids is continuous sampling
with an impinger absorption train. The proce-
dure entails the collection of the sample by
bubbling the gases through dilute caustic fol-
lowed by acidification and ether extraction of
the free organic acids. A liquid-liquid ex-
tractor is used to provide multiple contact of
ether and aqueous media. The organic acids in
ether are subsequently titrated with a standard
base and reported as acetic acid. The lower
limit of the method is about 0.2 ppm in a 60
cubic foot sample.
Aliquot portions of the impinger solution
can also be analyzed for total oxides of sul-
fur (see Sect.5.4.7).
-------
5.4.2.2 PREPARATION FOR SAMPLING
The collection train is assembled as shown
in Figure 5.1. The first two impingers each
contain exactly 100 ml of 5% sodium hydroxide
solution, while the third is operated dry to
catch any carry-over spray and to protect the
gas meter. An ice bath is used to cool the im-
pingers. Glass, quartz-composition, or stain-
less steel sampling probes of any convenient
size may be used. All equipment is tested for
proper operation and freedom from leaks.
5.4.2.3 SAMPLING
Any convenient sampling rate, not to exceed
1 cfm, may be used. Proportional sampling, as
described in Section 5.2.1, may be necessary
when there are wide fluctuations in both gas
flow rate and composition.
The data recorded during sampling should
include:
a) Time (clock) of test and data re-
cordings
6) Gas meter reading (initial), cubic
feet
c) Gas meter vacuum, inches of mercury
below atmospheric
d) Gas meter temperature, degrees Fah-
renheit
e) Temperature of gas at. exit of third
impinger, degrees Fahrenheit .
Readings may be taker, at five- or ten-minute
intervals during a one-hour test, and the data
are recorded as indicated on the upper tabular
portion of Figure 4.9. Sampling for particulate
matter usually accompanies this procedure; if
this is not the case, reference point velocity
head and temperature readings should be made,
as described in Section 3.3.2.
At the completion of sampling, the pump is
shut off and the train allowed to come to at-
mospheric pressure before disconnecting the
vacmin line. The final gas me-ter reading is
recorded. The impingers and associated tubing
are suitably sealed for transfer to the labor-
atory for processing. Condensate, if any, in
the probe and inlet tubing is allowed to flow
into the first impinger.
5.4.2.4 SAMPLE PROCESSING
The total volume of liquid contained in
the impingers is carefully measured. The dif-
ference from the initial volume is recorded as
the condensate volume.
The impingers and associated tubing are
carefully rinsed with small portions of dis-
tilled water, the liquid and washings being
kept in a beaker or flask. If aliquots are to
be taken for analysis, the combined liquid and
washings are made up to an exact volume. Ali-
quots can be tatan if the organic acids exceed
50 ppm by volume.
5.4.2.5 ANALYTICAL PROCEDURE
The reagents needed for the analysis are
concentrated sulfuric acid, reagent-grade ethyl
ether, and 0.1 \ sodium hydroxide solution.
The 0.1 N sodium hydroxide solution should be
prepared and stored in a manner to avoid con-
tamination by atmospheric carbon dioxide. The
solution is standardized by titration using
potassium biphthalate (primary-standard grade)
and phenolphthalein indicator.
The liquid-liquid extractor (IteraNo. 92232,
Corning Glass Works, Corning, New York, or
equivalent) and water heating bath are shown
disassembled in Figure 5.5. The procedure for
each sample is as follows:
An 80-100 ml aliquot of the solution is
transferred to a 500-ml three—neck glass flask
equipped with a reflux condenser, separator)'
funnel, and gas inlet tube. The latter should
project below the level of the liquid in the
flask. Four drops of methyl red indicator are
added and the sample is acidified by addition
-------
FIGL'KE 5.5. Equipment used for extraction
of organic acids. Equipment shorn is (1) steam
bath; (2) rounrf botton flask; (3) extractor;
(4) inner collector tuie; (5) condenser.
of concentrated sulfuric acid from the sepa-
ratory funnel. Daring acidification, the sample
is agitated by intermittent bubbling of nitrogen
into the flask. After acidification, nitrogen
is bubbled through the sample until sulfur
dioxide ceases to evolve from the condenser
(deter-dned by holding wet litmus test paper
strips at the top of the condenser). The sample
is now heated just to the boiling point to
ensure complete removal of $0-2. The sample is
allowed to cool and the condenser is rinsed
with water into the flask. The sample is trans-
ferred to a volumetric flask and diluted to a
suitable exact volume. Fifty ml aliquots are
transferred to 150-rnl beakers and adjusted to
pH 2 (pH paper) with 3®% sodium hydroxide so-
lution. A blank containing the same amount of
original sodium hydroxide as the aliquots is
adjusted to pH 2 with concentrated sulfuric
acid and is analyzed with the aliquot samples.
Transfer the sample and blank mixtures to
separate 500-ml liquid-liquid extractors. A
long-stenrved funnel is useful for making the
transfers. The final aqueous levels should be
3 or 4 inches below the side arms. Carefully
insert the inner collector tubes, and attach
the condensers and 500-ml round bottom flasks.
Slovly add ether through the condensers, allow-
ing it to rise in the extractors. Continue
adding ether until about 200 ml has overflowed
into the flasks. Heat the flasks to steady
boiling on water baths or with Glass-Col heat-
ing mantles, and allow the extractions to pro-
ceed for 8 hours.
After the flasks have cooled, tilt the ex-
tractors to allow as much as possible of the
ether to decant over into the flasks without
removing any aqueous material. Transfer the
ether extracts to separatory funnels and remove
any traces of aqueous material that may be
present. Add about 40 ml of water and 3 drops
of phenolphthalein indicator to each of the
ether solutions in the separatory funnels.
Titrate the mixtures in the funnels with stand-
ard 0.1 N sodium hydroxide to the phenolphtha-
lein end point. As the end point is approached,
stopper the separatory funnels and shake with
each small titration increment until a pink
color persists.
5.4.2.6 CALCULATIONS
The sequence of calculations, using the
data obtained during sampling, processing, and
analysis, is as follows:
a) Volume of stack gas sampled
6) Organic acid concentration
c) Emission rate of organic acids
d) Water vapor content of stack gas
The APCD forms shown in Figures 4.9 and 4.13
are convenient for many of the calculations to
lie described.
5.6.2.6.1 Sample Volume
The volume of stack gas sampled is calcu-
lated in the same manner as described for ammo-
nia (Sect.5.4.1.6.1). It may be noted that a
slight error occurs in the sample volume cal-
culation when stack gases containing moderate
amounts of carbon dioxide are sampled with ab-
sorption trains containing sodium hydroxide
-------
solution. The alkali will react with the car-
bon dioxide, forming water, sodium carbonate,
and possibly some bicarbonate. The pM of the
resulting solution is still high enough, how-
ever, for efficient absorption of oxides of
sulfur, organic acids, or fluorides. As a re-
sult of this reaction, the measured condensate
volume will be high due to production of water,
and the metered gas volume will be low due to
loss of a small volume of carbon dioxide from
the gas sample. These two small errors will
tend to cancel each other for calculation of
total sample volume.
5.4.'2.6.2. Concentration
The weight of organic acids (expressed as
acetic acid) collected by the sampling train
is given by <. • ,» -.
\V^ = 0.0601fn(vg - vb)* , (5.7)
where,
WQ. = weight of organic acids, grams
f = aliquot factor: the ratio of total
solution volume to aliquot volume
n = exact normality of 0.1 N sodium hy-
droxide
vs = volume of 0.1 N sodium hydroxide used
for the sample titration, milliliters
vjj = volume of 0.1 N sodium hydroxide used
for the blank titration, milliliters
The concentration of organic acids in the gas
sample is given by the two relations,
Vk
and
where,
,15.53^.
= 13,900 -yj ,
(5.9)
= concentration of organic acids (as
acetic acid), grains per standard
foor
CQ\ =concentration of organic acids, parts
per million by volume
^7 = volume of stack gas sampled, from
Equation 4.9, standard cubic feet
Although weight-volume concentrations (Eq. 5.8)
require that some particular acid such as ace-
tic he used as a basis, volune-volume concen-
trations (Eq. 5.9) will be the sane for any
monocarboxylic acid.
5.4.2.6.3 Emission Rate
The emission rate of organic acids at the
sampling station location is given by either
of the two relations,
0. 00857 CQ^Q
or
= 9.52 x
(5.10)
(5.11)
where,
= emission rate of organic acids,
pounds per hour
= concentration, from Equation 5.8,
grains per standard cubic foot
COA = concentration, from Equation 5.9,
parts per million by volume
Q = stack gas flow rate, from Equation
3.12, standard cubic feet per minute
5.4.2.6.4 Moisture Content
The water vapor content of the stack gases
is calculated by the procedure described in
Section 4.4.1.8.3. The calculation is made only
for comparison with the results from the par-
ticulate train processing. The difference is
due to errors in condensate volume and water
vapor volume calculations, caused by chemical
reactions during absorption and the lowered
vapor pressure (relative to pure water) of the
absorbent solution. Both effects mentioned will
produce small positive errors in calculation
of water vapor content.
5.4.3 ALDEHYDES
5.4.3.1 METHOD SUMMARY
In practically all tests, samples for
aldehyde analysis are collected in evacuated
flasks, using grab sampling techniques (Sect.
5.3.2). In rare instances, impinger absorption
trains have been used, but this collection
method is more applicable to the low aldehyde
* The constant for determination of maleic acid is 0.0580.
-------
concentrations experienced in atmospheric
monitoring.
In either case, aldehydes in the sample
react with a solution of sodium bisulfite to
form addition compounds. The excess bisulfite
ion is destroyed with iodine solution. By ad-
justing the pH of the solution, the addition
compounds are decomposed, freeing bisulfite
ion equivalent to the aldehydes present in the
sample. The liberated bisulfite ion is then
titrated with standard iodine. Methyl ketones,
if present in the sample, will be included in
the results. The lower limit of the method,
using 2-liter gas samples, is about 1 ppm.
Since the collection methods are iden-
tical, aliquot portions of the solutions can
be analyzed for formaldehyde alone (Sect.
5.4.4).
5.4.3.2 PREPARATION FOR SAMPLING
Two-liter round bottom flasks, as shown in
Figure 5.2, are used for grab sampling. Ten ml
of 15c sodium bisulfite solution (Igper 100 ml
solution) are added to each flask. The flask
is then evacuated to the vapor pressure of the
solution, the screw clamp closed, and the solid
glass plug inserted into the open end of the
tubing until ready for sampling.
For continuous sampling by impingers, the
collection train is prepared as described for
ammonia or organic acids, adding exactly 100
ml of \% sodium bisulfite solution to each of
the first two ircpingers.
5.4.3.3 SAMPLING
The inlet tube of the 2-liter flask is
connected to one leg of a glass tee or three-
way stopcock attached to the sampling line.
An aspirator bulb, connected to the other leg
of the tee, is used for flushing the sample
probe and tubing with stack gas just prior to
sampling, as illustrated in Figure 5.6. The
FIGURE 5.6. Crab sampling of a gas strean.
screw clamp is opened to admit gas to the
evacuated flask. When the flow of gas has
ceased, the screw clamp is closed and the
glass plug reinserted into the short rubber
tube to the flask. The flow of gas may con-
tinue for many minutes when the gases are
almost 100 per cent steam, thus requiring the
flask to be cooled during this process. Such
a situation may be encountered, for example,
when testing rendering cookers. The proced-
ure in Section 5.5.3 should then be followed
for calculations. In order to obtain an av-
erage value, four grab samples are usually
taken during an hour test.
When absorption impinger trains are used,
the sampling procedure is the same as described
for organic acids. The sampling rate should
not exceed 0.3 cfm.
5.4.3.4 SAMPLE PROCESSING
The sealed collection flasks are shaken
for 15 minutes on a mechanical shaker, with
frequent rotation to provide a thorough scrub-
bing action. The temperature and absolute gas
pressure in each flask are recorded after the
gases have reached ambient temperature. The
contents of each sample flask are then rinsed
-------
into conical flasks. A blank is prepared,
using the same amount of 1% sodium bisulfite
solution used for each sampling flask.
The impinger train collection is processed
in a manner analogous to that described for
organic acids in Section 5.4.2.4. Unless the
aldehyde concentration is very low (below 0.1
ppm), aliquots may be taken for analysis.
5.4.3.5 ANALYTICAL PROCEDURE
The analytical procedure is identical for
samples collected either by grab or absorption
train sampling.
The reagents needed for the analysis are
0.05 N sodium thiosulfate solution, 0.005 N
iodine solution, approximately 0.1 N iodine
solution (made by disolving 12.7 g of iodine
in a solution of 25 g of potassium iodide in
50 ml of water, and diluting to one liter
with water), and a special buffer solution.
The sodium thiosulfate solution is standard-
ized with potassium dichromate (primary
-standard grade) according to standard iodo-
metric procedure. The 0.005 N iodine solu-
tion, prepared by dilution from the 0.1 N so-
lution, is standardized by titration with
the sodium thiosulfate solution u si ng
starch indicator. The buffer solution is pre-
pared by dissolving 80 g of anhydrous sodium
carbonate in 500 ml of water, slowly adding 20
ml of glacial acetic acid, followed by dilution
toil. The pll of the solution is adjusted to
9.6 ± 0.1 with sodium carbonate or acetic acid,
as required, using a pM meter.
Two nil of 1% starch indicator solution are
added to each sample, and 0.1 N iodine is added
dropwise until a dark blue color is produced.
Care should be taken to ensure that all of the
sulfur dioxide resulting from the decomposi-
tion of bisulfite is removed since it may
cause the end point to fade. Ihis can be con-
veniently accomplished by blowing a small jet
of air into the flask while swirling the con-
tents vigorously for several minutes. Each
solution is decolorized by dropwise addition
of 0.05 N sodium thiosulfate. The 0.005 X
iodine solution is added, to a faint blue end
point. The solutions are cooled thoroughly in
an ice bath, and 50 ml of chilled buffer are
added to each flask. The flasks are kept in
the ice bath for 10 to 15 minutes after the
buffer addition. The liberated bisulfite is
titrated with 0,005 N iodine solution to the
same faint blue end point present before addi-
tion of the buffer. The sample must remain
chilled in order to avoid a fading end point.
5.4.3.6 CALCULATIONS: IMPINGER TRAIN
SAMPLES
The seqxience of calculations for aldehyde
samples collected by impinger trains is as
follows :
o) Volune of stack gas sampled
6) Aldehyde concentration
c) Emission rate of aldehydes
5. 4.3. 8.1 Sample Volume
The calculations for the volume of stack
gas sampled are made, in the same manner as
described previously, in Section 5.4.1.6, for
ammonia .
5. ft. 3. 6. 2 Concentration
The weight of aldehydes, expressed as for-
maldehyde, collected by the impinger train is
given by the expression
where,
^'
f
0.015fn(vs - vb)
(5.12)
= wiont of aldehydes collected, grams
= aliquot factor; ratio of total sol-
ution volume to aliquot volume
= exact normality of the 0.005 N
iodine solution
-------
vg = volume of 0.005 N iodine solution
used for sample titration following
the addition of the buffer solution,
milliliters
vjj = volume of 0.005 N iodine solution
used for blank titratioa,milliliters
The concentration of aldehydes in the gas
sample is given by the two relations,
w
and
15.43
27,800
'AID
(5.13)
(5.14)
where,
CAIJ-) = concentration of aldehydes (as for-
maldehyde), grains per standard
cubic foot
c.\jj) = concentration of aldehydes, parts
per million by volume
Vf = total sampled volume, from Equation
4.9, standard cubic feet
Unlike weight- volume concentration, volume-
volune concentrations will be the saire for any
aldehyde or methyl ketone having one carbonyl
group per molecule.
5. 4. 3. 6. 3 Emission Kate
The emission rate, or mass flow rate, of
aldehydes at the sampling station location is
given by either of the two relations,
CAU)* '
(5.15)
or
where,
MALD " 4-75 x 10
emission rate of aldehydes, pounds
per hour
concentration, from Equation 5.13,
grains per standard cubic foot
c.j_ = concentration, from Equation 5.14,
parts per million by volume
Q = stack gas flow rate, from Equation
3.12, standard cubic feet per minute
5.4.3.7 CALCULATIONS-. GRAB SAMPLES
The sequence of calculations for aldehyde
samples collected with evacuated flasks is as
follows:
a) Volume of stack gas sampled, dry
basis
b) Aldehyde concentration, dry basis
c) Aldehyde concentration, stack condi-
tions
d) Emission rate of aldehydes
5.4.3.7.1 Sanple Volune
The dry volume of stack gas sampled is
calculated as follows:
"•IB
Vf
-------
excess moisture in the stack gases, precipi-
tated upon cooling in the flask, is usually
negligible in comparison with the absorbent
solution. Thus, moisture calculations from
measurements of the condensate, as done for
impinger trains, are not made. An exception
does, however, occur when sampling steam (see
Sect. 5.5.3).
5.4.J.7.2 Concentration
The aldehyde concentrations are calculated
and reported in two ways: (1) on a dry basis;
and (1) on a wet basis, or under actual stack
water vapor conditions.
The calculation of aldehyde concentration
on a dry basis uses the relation,
(c
11.85 x 103 n(vs - vb)
ALT) d
where,
= concentration of aldehydes, dry
basis, parts per million by vol-
ume
= exact normality of the 0.005 N
iodine solution
= volume of 0.005 N iodine solution
used for the sample titration
following the addition of the
buffer solution, milliliters
= volume of 0.005 N iodine solution
used for the blank titration,
milliliters
= dry volur-e of gas sample, from
Equation 5.17, standard liters
In order to convert concentrations from
the dry basis to stack water vapor conditions
(sometimes called the wet basis), the following
relation is used:
CALD = (cAL!)'d
[ !V,i
(100 - W.V.)
100
where,
CALD = concentration of aldehydes, at
stack conditions, parts per nil-
lion by volume
(CALTJ)(J = concentration of aldehydes, dry
basis from Equation 5.18, parts
per million hy volume
\V.V. = water vapor content of stack gas,
per cent by volume
It may be noted that this is identical to the
concentration defined by Equation 5.14.
The water vapor content of the stack gas
is usually determined from the data obtained
when sampling and processing the collection
train or trains for particulate matter. In
other instances, it may be determined with a
condensate sampling train, or by dry-wet bulb
themoretry, as described in Section 5.5.
The concentrations may be converted from
volume-voluTe to weight-volume units using the
conversion
QMD = 0.000554 cAIJj , (5,20)
whe re,
C>VLO = concentration of aldehydes, ex-
pressed as formaldehyde, grains per
standard cubic foot
5.4.3.7.3 Emission Kate
The emission rate, or mass flow rate, of
aldehydes at the sampling station location is
given by either of the two relations,
or
VALD
HvU3=<1.75x
cALrp . fs.:
where ,
(5.22)
(5.19)
emission rate of aldehydes, as for-
maldehyde, pounds per hour
concentration, from Equation 5.20,
grains per standard cubic foot
-------
CALD = concentration, from Equation 5.19,
parts per million by volume
Q = stack gas flow rate, from Equation
3.12, standard cubic feet per minute
5.4.4 FORMALDEHYDE
5.4.4.1 METHOD SUMMARY
The methods of sample collection and pro-
cessing prior to analysis are identical to
those described for aldehydes. The samples are
collected in a dilute solution of sodium bisul-
fite . Any aldehydes present form the bisulfite
addition compounds. An aliquot of the resultant
solution is then treated with chromotropic
acid in .strong sulfuric acid. Formaldehyde
forms a unique colored compound, the exact na-
ture of which is unknown but which appears to
be of a quinoidal type. The intensity of the
colored compound is then determined in a color-
imeter and the corresponding concentration of
formaldehyde read from a calibration curve.
The lo-A-er limit of the method, using 2-liter
gas samples, is about 1 pprn.
Two-liter round bottom flasks, prepared in
the same manner as described for aldehydes,
are used for sampling. Sampling and processing
of the flasks and collected samples also are
the same as described for aldehydes, except
that the solutions from each flask are meas-
ured to an exact volume, which should be as
small as possible.
5.4.4.2 PREPARATION OF REAGENTS
The special reagents needed for the analy-
sis are 0.05 N sodium thiosulfate solution,
approximately 0.1 N iodine solution. 0.005 N
iodine solution, buffer solution, standard
formaldehyde solution, 76% sulfuric acid solu-
tion, and chromotropic acid reagent.
The sodium thiosulfate, iodine, and buffer
solutions are prepared and standardized as
described for aldehydes; the other solutions
are prepared and standardized as follows:
Standard formaldehyde solution: Dilute 3 ml of
formalin (approximately 37/b) to 1 1 in a volu-
metric flask. To standardize, pipet 1 ml of
the solution into a 250-ml Erlenmeyer flask,
and 1 ml of water into another flask as a
blank. Add 30 ml of 1% sodium bisulfite and 2
ml of 1% starch to each flask. Add 0.1 N iodine
dropwise to each flask until a.dark blue color
results. Decolorize each flask with 0.05 N
sodium thiosulfate and then return to a faint
blue with 0.005 N iodine. Chill each flask in
an ice bath and add 50 ml of chilled buffer.
After addition of the buffer, allow to stand
in the ice bath for 10 to 15 minutes, th^n
titrate the liberated bisulfite in each flask
to the same faint blue end point with 0.005 N
iodine. Subtract the volume of 0.005 N iodine
used for the blank determination from the vol-
ume used for the sample determination. The
strength of the standard in micrograns per
milliliter is 1.5 x 10^ vn, where v is the
volume, in milliliters, of 0.005 N iodine used
for titration following the addition of buffer,
less blank; and n is the exact normality of
the 0.005 N iodine.
Dilute 1 ml of this standard formaldehyde
solution to 1 1. The diluted solution contains
approximately 1.2^2 of formaldehyde per ml.
76% sulfuric acid: Slowly add 725 ml of
concentrated sulfuric acid to 350 ml of water.
It is advisable to place the container in which
the dilution is to be made in a water bath to
absorb some of the heat generated.
Chromotropic acid reagent: Weigh 0.875 g
of 4,5-dihydroxy-2,7-naphthalenedisulfonic
acid, disodium salt (Eastman No. P230 or equiv-
alent) into a 100-ml beaker and add 4.25 ml of
water. Rapidly add 45.75 ml of 76% sulfuric
acid and stir to dissolve. Prepare fresh for
-------
each rlay's analyses because this reagent de-
composes on standing. The final mixture con-
tains approximately 71% sulfuric acic! by weight.
Prepare a calibration curve for each new
bottle of chromotropic acid as follows: Trans-
fer 50 ml of 76% sulfuric acid, by means of a
graduate, to each of a series of six 150-ml
beakers. Warm the solutions in a water bath to
60 ± 2 C. Add 2 ml of chromotropic acid reagent
to each beaker. Pipet 1 ml of the 1.2 A»Hes the color devel-
opnr.-nt somewhat. Hapiclly transfer to the col-
orimeter cell for reading. Measure the light
absorption of the solutions in the photoelec-
tric colorimeter (a Klett-Surnnerson industrial
colorimeter, No. 54, or equivalent) with a 500-
to 560-mu green filter and a 20 mm light path.
Use tho blank solution for zeroing the color-
imeter. Prepare a calibration curve by plot-
ting Llie colorimeter readings against micro-
grams of formaldehyde contained in each solu-
tion.
5.4.4.3 ANALYTICAL PROCEDURES
Pour 50 ml of 76% sulfuric acid into each
of two 150-ml beakers. Warm the solutions in a
water bath to 60 ± 2 C. Add 2 ml of chromo-
tropic acid reagent to each. Transfer a 5-ml
aliquot of the sample by pipet to one beaker
and 5 ml of water to the other for a blank
determination. Stir the solutions frequently
and maintain at the specified temperature for
20 minutes. At the end of 20 minutes, remove
the beakers from the water bath and immerse
them in ice water. Rapidly transfer to the
colorimeter cells for reading. Measure the
light absorption of the solutions in the photo-
electric colorimeter with a 500- to 560-mu
green filter and a 20-mm light path. Use the
blank for zeroing the colorimeter. Read the
weight of formaldehyde in micrograms from the
previously prepared calibration curve.
5.4.4.4 CALCULATIONS
The sequence of calculations for formal-
dehyde samples collected with evacuated flasks
is as follows:
a) Volume of stack gas sampled, dry
basis
b) Formaldehyde concentration, dry
basis
c) Formaldehyde concentration, stack
conditions
d) Emission rate of formaldehyde
The dry volume of stack gas sampled is
calculated using Equation 5.17.
The formaldehyde concentration is calcula-
ted on a dry basis by the relationship,
(CFA)H = 0.790'
(5.23)
"g
-------
where,
(c ) . = formaldehyde concentr.ition, dry
basis, parts per million by volume
'VA = weisnt of formaldehyde found in
5-nl aliquot of collection solu-
tion, micrograms
f = aliquot factor: ratio of total
collection solution volume to 5-ml
aliquot
Vj = dry volume of gas sample, from
Equation 5.17, standard liters
The conversion of formaldehyde concentra-
tion to stack moisture conditions is made using
Equation 5.19 and 5.20, previously given for
aldehydes. The conversion factors are identi-
cal, since total aldehydes are expressed as
formaldehyde.
The emission rate of formaldehyde, as for
aldehydes, is calculated by either Equation
5.21 or 5.22.
-------
TENTATIVE METHOD FOR ISOKINETIC DETERMINATION
OF POLLUTANT LEVELS IN THE EFFLUENT OF
FORMALDEHYDE MANUFACTURING FACILITIES
-------
Second Draft
7/26/73
TENTATIVE METHOD FOR
ISOKINETIC DETERMINATION OF POLLUTANT LEVELS
IN THE EFFLUENT OF FORMALDEHYDE MANUFACTURING FACILITIES
1. Principle:
1.1 General: An air sample is drawn isokinetically through an
impinger train containing water as the scrubbing medium. Formaldehyde
and methanol are scrubbed from the gas. An integrated bag sample is
taken anisokinetically to measure dimethyl ether content.
1.2 Formaldehyde: The analysis consists of reacting an aliquot
of the impinger solution with chromotropic - sulfuric acid reagent to
form a purple chromogen. This resulting solution is analyzed colorime-
trically using a spectrophotometer at 580 nm; the absorbance of the
colored solution is proportional to the quantity of formaldehyde in the
solution.
1.3 Methanol: An aliquot of the scrubber solution is analyzed using
a gas chromatograph and flame ionization detector.
1.4 Dimethyl ether: The contents of the integrated bag sample are
analyzed for dimethyl ether using a gas chromatograph and flame ionization
detector.
2. Applicability:
2.1 This method is applicable for the determination of formaldehyde,
methanol and dimethyl ether in-the effluent of formaldehyde manufacturing
facilities.
-------
3. Range:
3.1 Formaldehyde: 0.25 vg/ml - 2.0 vg/ml; based on impinger solution
of 600 ml and 60 ft gas collected: 6-240 ppm; upper limit is easily ex-
tended by diluting aliquot taken.
4. Sensitivity: unknown
5. Precision:
5.1 Formaldehyde: +_ 5%
6. . Collection Efficiency:
6.1 Formaldehyde 95% +
6.2 Methanol 95+ %
7.. Interferences
7.1 Formaldehyde: This method is specific for formaldehyde although
other hydrocarbons in concentrations in excess of formaldehyde to the
order of 10:1 will give interferences in absorbance readings:
Saturated Aldehydes <.oU (*)
Unsaturated Aldehydes 1 - 2%(+)
Ethanol, High Alcohols, Olefins (r)
Phenols (8:1 excess) 10-20%(-)
Ethylene, Propylene (10:1 excess) 5-10 (-)
Aromatics (15:1 excess) 15% (-)
Methanol (10,000:1 excess) None
Nitrogen Oxides* (-)
7.2 Methanol: sane as above
7.3 Dimethyl ether: unknown
* Use of Aqueous bisulfite solution as the scrubbing medium will reduce
interference of nitrogen oxides.
-------
8. Apparatus:
$.1 Sampling
8.1.1 Stainless steel nozzle
8.1.2 Pyrex probe - heated
B.I.3 Pitot tube; s - type
8.1.4 £lass impingers: 1 Creenburg-Smith, 3 modified Green-
burg-Smith, 1 silica gel
8.1.5 Metering - Vacuum System as required to maintain an iso-
"fcirretic sampling rate
S.I.6 Metering - Vacuum System as required to obtain integrated
bag sample
8.2 Sample recovery
8.2.1 Probe brush
8.2.2 Wash bottle
8.2.3 Graduated cylinder
8.2.4 Glass sample storage jars.
8.3 Analysis
8.3.1 Spectrometer capable of measuring absorbance of the color
developed solution at 580 nm.
8.3.2 Hamilton syringe for injection of liquid sample (methanol)
to gas chromatograph.
8.3.3 Gas chromatograph
8.3.4 Flame ionization detector
8.3.5 Recorder
-------
9. Reagents:
9.1 Sampling
9.1.1 Distilled water
9.1.2 Silica gel
9.1.3 Crushed ice
9.2 Sample recovery
9.2.1 Distilled water
9.3 Analysis: Formaldehyde
9.3.1 Chromotropic acid reagent: Dissolve 0.10 g of 4, 5
dihydro^y-2,.7 - naphtha!ene-disulfonic acid disodium salt (Eastman
Kodak Co. Cat. No. P230)* in water and dilute to 10 ml. Filter, if
"necessary; store in brown bottle. Make fresh weekly.
9.3.2 Sulfuric acid: Concentrated reagent grade
9.3.3 Formaldehyde standard solution "A": (1 mg/ml).- Dissolve
4.4703 g sodium formaldehyde bisulfite (Eastman PG 450) in distilled
water and dilute to 1 liter. Alternatively, 37 percent formalin solution
may be used. Dilute 2.7 ml of 37 percent formalin solution to 1 liter
with distilled water. Solution "A" must be standardized as described in
section 11.1. Stable for one month.
9.3.4 Formaldehyde standard solution "B": (1 ug/ml). Dilute 1 ml
of standard solution "A" to 1 liter with distilled water. Make fresh daily.
9.3.5 Iodine (0.1 N, approximate): Dissolve 25 g of potassium
iodide in about 25 ml of water. Add 12.7 g of iodine and dilute to 1 liter.
* Mention of brand name does not constitute Environmental Protection Agency
endorsement.
-------
9.3.6 Iodine (0.01 N): Dilute 100 ml of the 0.1 N iodine solu-
tion to 1 liter. Standardize against sodium thiosulfate. Stable solution.
9.3.7 Starch solution, 1 percent: Hake a paste of 1 g of soluble
starch and 2 ml of water. Slowly add the paste to 100 ml of boiling water.
Cook, add several ml of chloroform as a preservative, and store in a stop-
pered bottle. Make fresh weekly.
9.3.8 Sodium carbonate buffer solution: Dissolve 80 g of anhy-
drous sodium carbonate in about 500 ml of water. Slowly add 20 ml of gla-
cial acetic acid and dilute to 1 liter.
9..S.9 Sodium bisulfite, 1 percent: Dissolve 1 q of sodium
bisulfite in 100 ml of water. Prepare fresh weekly.
9.4 Analysis: Methanol
9.4.1 Chromatographic column: 1055 triethyl acetyl citrate
(Charles Pfizer Co. "Citroflex A-2")* on Chromosorb T Teflon solid support
(or equivalent); dimensions 1/8 in. x 20 ft.
9.5 Analysis: Dimethyl ether
9.5.1 Chromatographic column: same as 9.4.1
10. Procedure:
10.1 Sampling (Formaldehyde - Methanol)
10.1.1 The sample train is assembled as shown in Figure 1. The
first two impingers are modified Greenburg-Smith impinger and are each fil-
led with 200 ml distilled water. The third impinger (Greenburg-Smith Type)
* Mention of brand name does not consitute Environmental Protection Agency
endorsement.
-------
is also filled with 200 ml. distilled water. The fourth impinger (modi-
fied Greenburg-Smith) is left dry. The fifth impinger contains approxi-
mately 200 gm silica gel.
10.1.2 A minimum sample of 60 ft is collected isokineticaVly
as per EPA Method 5 at a rate of 0.5 to 1.0 cfm.
10.2 Sample Recovery (Formaldehyde - Methanol)
10.2.1 The solution from each impinger is measured and.then
placed Into a single container.
10.2.2 The probe and impingers are sparingly washed with v/ater
(It is important to dilute the sample as little as possible.) and the
wash from each impinger and the probe is added to the sample collection
jar.
10.2.3 The weight gain in the silica gel is recorded.
10.2.4 Keep sample jars tightly capped.
10.3 Analytical: Formaldehyde
10.3.1 Measure and record the volume of each of the sample solu-
tions.
10.3.2 .Agitate sample then pipette a 4 ml aliquot from each of
the sampling solutions into glass stoppered test tubes. A blank contain-
ing 4 ml of distilled water must also be run. [If the formaldehyde content
of the aliquot exceeds the limit of the method a smaller aliquot diluted
to 4 ml with distilled water is used.]
-------
10.3.3 Add 0.1 ml of 1 percent chromotropic acid reagent to
the solution and mix.
10.3.4 Using a burette, add to the solution slov/ly and cau-
tiously 6 ml of concentrated sulfuric acid. The solution becomes ex-
tremely hot during the addition of the sulfuric acid. If the acid is
not added slowly, some loss of sample could occur due to spattering.
10.3.5 Allow to cool to room temperature (Important)!! Read
at 580 nm in a suitable spectrophotometer using a 1 cm cell.
10.3.6 Determine the formaldehyde content of the sampling solu-
tion from a curve previously prepared from standard formaldehyde solutions.
10.4 Analysis: Methanol
10.4.1 Analyze each sample on a gas chromatograph by injection of
a liquid sample.
10.4.2 Recommended conditions:
Oven Temperature: 115°C
Carrier Gas: Helium
Carrier Gas Head Pressure: 21'lbs.
10.5 Sampling (Dimethyl Ether)
10.5.1. As per Method 3 for integrated gas sample; Federal Register
Volume 36, Mo. 247, Part II, Page 24886
10.5.2 Condenser and probe filter not applicable for this method
10.6 Analysis: Dimethyl Ether
10.6.1 Direct injection of gas sample into Chromatograph.
10.6.2 Recommended conditions:
-------
Oven Temperature: 115°C
Carrier Gas: Helium
Carrier Gas Head Pressure: 25 Ibs.
11. Calibration
11.1 Standardization of formaldehyde solution
11.1.1 Pipette 1 ml of formaldehyde standard solution "AV
into an iodine flask. Into another, flask pipette 1 ml of distilled water.
This solution serves as the blank.
11.1.2 Add 10 ml of. 1 percent sodium bisulfite and 1 ml of 1
percent starch solution.
11.1.3 Titrate with 0.1 N iodine to a dark blue color.
11.1.4 Destroy the excess iodine with 0.05 N sodium thiosulfate
(titrate to clear).
11.1.5 Add 0.01 N iodine until a faint blue end point is reached.
11.1.6 The excess inorganic bisulfite is now completely oxidized
to sulfate, and the solution is ready for the assay of the formaldehyde
bisulfite addition product.
11,1.7 Chill the flask in an ice bath and add 25"ml of chilled
sodium carbonate buffer. Titrate the liberated sulfite with 0.01 N iodine,
using a microburette, to a faint blue end po.int. The amount of iodine added
in this step must be accurately measured and recorded.
11.1.8 One ml of 0.0100 N iddine is equivalent to 0.15 mg of
formaldehyde.. Therefore, since 1 ml of formaldehyde standard solution was
titrated, the'ml of 0.01 N iodine used in the final titration multiplied
-------
by 0.15 mg gives the formaldehyde concentration of the standard solution
in mg/ml. Record formaldehyde concentration of standard solution "A".
11.2 Preparation of standard curve, formaldehyde
11.2.1 Pipette 6, 1.0, -2.0 and 4.0 ml of standard solution
"B" into glass stoppered test tubes. Dilute to 4 ml with distilled water.
11.2.2 Pipette 1.5 and 2.0 ml of standard solution "A"-into
volumetric flasks and dilute to 1 liter. Take 4 ml aliquots of these stan-
dard solutions.
11.2.3 Develop the color as described in the analytical procedure
(10.3). Approximate concentrations of standard solutions will be 0, 1.0,
2.0, 4.0, 6.0, and 8.0 iig/4ml aliquot. Exact concentrations will depend
on exact concentration of standard formaldehyde solution "A" determined by
standardization as per (11.1).
11.2.4 Plot absorbance against micrograms/4 ml aliquot in the
color developed solution.
12. Calculations:
12.1 Formaldehyde
12.1.1 Correct the volume of air sampled to the volume at stan-
dard conditions.
V = V x >p"Pm * x ( 530 .
s '• ^29792' VT + 460 '
12.1.2 Calculate concentration of formaldehyde in the sample.
-------
ppm (volume) - (c? * (S) x (24.15)
HH«i vvuiumej (4) (A) (V,.) (HW)
V = Volume .Sampled, (Liters)
V = Volume S.T.P., (Liters)
O
S.T.P. = 70°F, 29.92 "Hg
P = Barametric Pressure, "Hg
P - Meter Pressure, "Hg
.T = Meter Temp., °F
C = pg of formaldehyde/4 ml aliquot (from calibration curve)
S - Total ml of sampling solution
A = Dilution factor, (ml original sample/total ml diluted to)
MW = Molecular weight of formaldehyde, 30.03
24.15 = Ml of formaldehyde gas in one millimole @ S.T.P,
12.2 Methanol
12.2.1 PPM (volume) derived from chromatograph recorder charts
and calibration charts
12.3 Dimethyl Ether
12.3.1 PPM (volume) derived from chromatograph recorder charts
and calibration charts.
13. Major References:
13.1 Cares, Janet Walker: "Determination of Formaldehyde by the
Chromotropic Acid Method in the Presence of Oxides of Nitrogen"; Amsr. Ind
Hyg..Jour.; July, 1968.
13.2 "Determination of Formaldehyde: Chromotropic Acid Method11., PUS
Standard Methods.
-------
13.3 "Tentative Method of Analyses for Formaldehyde Content of
the Atmosphere (Colon"metric Method)"; Health Life Science Journal',
Vol. 7 £1; January, 1970.
13.4 Walker, 0. F.: 'Formaldehyde; Reinhold Publishing Co.; 3rd
Edition; 1964.
13.5 Federal Register, Volume 36, Number 247> Part H, December
23, 1971.
13.6 "Method for the Determination of Toxic Substances in Air:
Methanol (Adopted 1949"); International Union of'Pure and Applied
Chemistry, London, 1959.
-------
1. Stainless steel nozzle
2. Glass-lined stainless
steel probe
Heated box
Ice bath
Modified impinger
G-S impinger
Modified impinger
Modified impinger
Silica gel impinger
Thermometer
Check valve
Umbilical cord
Pressure gauge
Coarse adjust valve
Purap
Fine adjust valve
Orifice
Inclined manometer
Pi tot tube
20 L
FIGURE 1
-------
FORMALDEHYDE IN AMBIENT AIR,
INDUSTRIAL HYGIENE, AND STACK- GAS SAMPLES
-------
FORMALDEHYDE IN
AMBIENT AIR, INDUSTRIAL HYGIENE, AND
STACK GAS SAMPLES
(CHROMOTROPIC ACID METHOD)
January 18, 1974
APPARATUS;
i
1.. Graduated cylinders, 25ml, SOral, 100ml
2. Volumetric flasks, 100, 1000ml
3. Hot water bath
4. Pipettes, volumetric (1, 2, 3, 5ml) and graduated
(10ml in l/10ml increments).
5. Micropipettes (Pasteur .pipettes)
6. Visible spectrophotometer, 1-cm glass cells
REAGENTS;
1. Sodium formaldehyde bisulfite, stock standard solution:
add 0.4466g sodium formaldehyde bisulfite (sodium bi-
sulfite, formaldehyde addition product) to a 1-1 volu-
metric flask. Dissolve and dilute to volume with dis-
tilled water. Mix by inverting 25 tines. This solu-
tion is equivalent to lOOjag formaldehyde per ml.
2. 0.5% chromotropic acid solution: Dissolve 0.5g chroir.o-
tropic acid (4 ,5-dihydroxy-2,7-naphthalene disuifonic
acid) in distilled water and dilute to 100ml in a gradu-
ated cylinder. Mix well and filter immediately before
using. This reagent is stable for one week if kept re-
frigerated.
3. Sulfuric acid, concentrated, reagent grade.
4. 5% potassium permanganate solution: Dissolve 5g potassi-
um permanganate in distilled water and dilute to 100ml.
Mix by inverting the cylinder 10 times. The reagent is
stable if stored in the dark.
5. 57. phosphoric acid: Dilute 10ml of 507, phosphoric acid
to 100ml and mix by inverting the cylinder 10 times. The .
reagent is stable.
6. 17. sodium bisulfite: Dissolve 1. Og sodium bisulfite in
distilled water and dilute to 100ml in a graduatedcylinder.
Mix by inverting 10 times. Prepare weekly to avoid con-
tamination by absorption of formaldehyde from air.
-------
7. Bromine water, saturated: Add approximately 1.5ml
bromine to 100ml of distilled water and mix thoroughly.
There should be a small amount of undissolved bromine
remaining under the solution. Use and store the solu-
tion only in the hood. Store only in a glass-stoppered
bottle, and prepare fresh weekly. Caution; Bromine is
very hazardous. Observe all precautionsnormally assoc-
iated with its handling. Dispose of the reagent only by
decanting the saturated* solution into the sink under the
hood. Add 100ml of water, mix, and decant again. Re-
peating until no undissolved bromine remains. Fill the
.bottle completely with water to expel bromine vapor be-
fore removing from the hood. The preparation of the rea-
gent may be carried out in the reagent bottle itself, in
order to minimize transfers of bromine.
INTRODUCTION:
Stack gas and ambient air samples are collected in im-
pingers containing 100ml of 1% NaHSO^- Following col-
ection, distilled water rinses are added during transfer
to sample bottles. Industrial Hygiene samples are col-
lected in 10 or 15 ml of 1% NaHSO^ solution, and may or
may not have rinses added.
The reaction is:
NaHS0
HCHO
o ,
L-->HOCH2S05 Na (water soluble)
The bisulfite addition product is stable in neutral solu
tion, but decomposes to formaldehyde in acid solution:
H2S04
ONl - ) HCHO+S02+H20
The formaldehyde forms a violet complex with chromotropic
acid in hot cone. t^SO^. The absorbance is read at 580nm
on a spect rophotometer , using a distilled water reference.
INTERFERENCES:
1. Phenol interferes significantly since
H
HCHO
H2S04
H
CH2OH
CH2OH
HEAT
V
POLYMERS
-------
High levels of Phenol are indicated by the appearance of
a rose color upon the addition of concentrated l^SO^.
To prevent reaction of the phenol with formaldehyde, the
phenol is brominated, blocking the ortho- and para- positions;
iH
BlV
phenol
As a result of the bromination, no ortho- or para- positions
are available for reaction with formaldehyde.~
Nitrate ion interferes by reacting with the chromotropic
acid to produce a strong yellow color. For this reason all
glassware (except pipettes) should be thoroughly rinsed by
the analyst immediately before use to remove any traces of
HNOo remaining from the cleaning procedure.
Bromide ion, if present in high levels, may interfere upon
addition of cone. HoSO/•
The bromine thus generated reacts with the chromotropic acid
to form a colored product which has been shown to interfere.
High levels of bromide ion are avoided by the addition of
permanganate which destroys the bisulfite before bromination
of the phenol.
STANDARDIZATION OF METHOD:
(To be done
analyzed).
each day samples are
Prepare standard solutions corresponding to 1.0, 3.0, 5.0,
and 7.0 micrograms formaldehyde/ml. Pipette 2.Oral of each
into separate 25-ml graduated cylinders. Add 2.0ml of dis-
tilled H20 to a fifth 25-ml cylinder as a O.O^g standard.
Treat each sample as follows;
a) Add 5.0ml of cone. H2S04 and mix by swirling.Immediately
add 0.4ml (&• 8 drops) of the 0.57, chromotropic acid solu-
tion, and -mix again immediately.
b) Boil in the water bath for 15 minutes to allow full coloi
(purple) development.
cool.
Remove from the bath and allow to
-------
c) Add distilled water to the 10-ml nark. Mix by inverting
several times (may generate slight pressure), and allow
to stand until cool again. Transfer to a 1-cm cell and
read the absorbance vs distilled water at 580nm.
Plot the absorbance vs total micrograras KCHO for each stand-
ard. If the recommended standards were used, the standards
correspond to 0.0, 2.0, 6.0, 10.0, and 14.0 total micrograms
formaldehyde, and the absorbance of the 14.0^g standard should
be in the neighborhood of 0.7. A least-squares-fitted line
should have a slope in the neighborhood of 0.05 absorbance
units/microgranj formaldehyde.
ANALYSIS OF SAMPLES:
A. Routine Analysis (including test for phenol interference):
1. Stack and ambient air samples; Mix all fractions
of the sample (unless fractions are to be analyzed
individually) and record the total sample volume
(a 500-ml graduated cylinder is useful for this).
2. Industrial Hygiene samples; Record the total vol-
ume of the sample (dr y 10-ml cylinders are often
useful for volume-taking).
3. Pipette 2.0ml of the sample into a 25-ml graduated
cylinder. Add 5.0ml concentrated H2S04 with swirl-
ing, and observe the color for a few seconds. If
any pink or red color appears, discard the cylinder
contents, and proceed as in "Analysis of Samples in
the Presence of Phenol."
4. If no pink or red color is observed after a few
seconds, add 0.4ml (zzS drops) of the 0.57» chromo-
tropic acid solution, and mix immediately by swirling.
5. Boil in the water bath for 15 minutes. Remove, allow
to cool; then add water up to the 10-ml mark. Mix by
inverting a few times, and allow to stand until cooled
again. Read the absorbance at 580nm in a 1-cm cell vs
distilled water.
ANALYSIS OF SAMPLES IN THE PRESENCE "OF PHENOLS;
If a pink or red color was observed above, or the sample is
known to contain phenol, the sample must be pretreated as follows;
1. Pipette an aliquot (e.g. 10ml for a stack or ambient
air sample, or 2-3ml for an I.H. sample into an ap-
propriately-sized (25- or 50-ral) graduated cylinder.
Add 1 drop of 5% t^PO/^ for each ml of sample and mix
by swirling. Add 5% KMnO^ drop-by-drop with mixing
until a persistent pink or violet color is obtained.
Add bromine water (hood!) until observable bromine
fumes persist over the solution after shaking in the
stoppered cylinder. Allow to stand 5 minutes, then
bubble a rapid stream of air through the sample until
-------
the bromine has been driven off (about 5 minutes). Pasteur
pipettes work nicely for this. Add 17, NaHS03 with mixing
until the solution is clear. Dilute to a known volume in
the cylinder, and mix by inverting 10 times. Pipette 2.0
ml into a 25-ml cylinder and proceed as in "Routine Analy-
sis."
CALCULATIONS:
From the standard curve, calculate the total micrograms of
formaldehyde present in the original sample. Report total
micrograms formaldehyde/100ml for ambient air and stack gas
blanks. Report total micrograms formaldehyde/lOinl for In-
dustrial Hygiene blanks. Remember to take into account any
dilutions which were made in the course of analysis or pre-
treatment of the samples.
Examples: (In the following examples, ao= intercept
and a^= slope of the least-squares-fitted
' . _ Sample absorbance - ao \
A *"" • • - • i . i • • i .-.<•. ii r .1. . i ^— 1
31 /
A) Routine Analysis
1. No dilutions required:
/Original volume \
Total ug HCHO (original sample) = f\\ 2ml /
2. Dilution of original sample used:
I original vol.I /vol. diluted to \
Total ug HCHO (orig. sample) = A \2mlj'\ Aliq. vol. /
B) Analysis in Presence of Phenol
1. Pretreatment was only dilution:
/orig. vol.\ / vol. pretreated to I
Total ug HCHO (orig. sample) = A\2ml/ \Aliquot for pretreatment/
2. Dilution of original sample and pretreatment
(or dilution of pretreated sample).; ^
orig. vol.Vfvol. diluted to\/pretreated t
Total ^ig HCHO(orig. sample)
(orig. vol.\(vol• di
2ral f\ aliq.
vol. i\ aliq. for
pretreabner
NOTE S:
a) CAUTION: BROMINE!!
b) A slight yellow color may appear in pretreated samples upon
addition of cone. H2SO^, due to generation of bromine from
residual Br.~ This is compensated for in the method by use
-------
of an excess of chromotropic acid, which reacts with
free Br2. This is the reason for the use of 0,4ml
of reagent rather than the 0.2ml called for in the
source method for this procedure (see reference).
c) A yellow color appearing upon addition of chromotropic
acid to unpretreated samples is probably caused by
nitrate interference. Should this occur, discard the
processed sample and start again after carefully rinsing
a clean cylinder with distilled water,
d) Dilutions may be made with distilled water upon original
samples or pretreated stack gas and ambient air samples
only, in order to insure that the sample absorbance falls
within the range of the standard curve. The developed
colors may not be diluted to any volume except the 10-ml
mark on the 25-ml cylinder, as per the procedure.
REFERENCES;
1. Levaggi, D.A. and Feldstein, M. , J_. Air Pollution Control
Association, , 312 ( ).
2. Boos, R.N., Anal. Chem., 20, 964 (1948).
-------
APPENDIX D
ANALYTICAL DATA
SECTION I BENZENE DATA SUMMARY
SECTION II CONTINUOUS MONITOR DATA SUMMARY
SECTION III LABORATORY DATA SHEETS
SECTION IV GAS CHROMATOGRAMS
-------
APPENDIX D
SECTION I BENZENE DATA SUMMARY
-------
i'an
'„
Peat
,
1
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t'na
Benzene
Standard
Analysis
CYL #
SP-10511
SP-10517
SP-10530
ORIGINAL
REQUESTED ANALYSIS
GRAVIMETRIC
lOppm Benzene
Bal. Air Zero
lOOppm Benzene
Bal. Air Zero
SOOppm Benzene
Bal. Air Zero
10.1
Bal.
100.4
Bal.
501.0
Bal.
REANALYSIS
GAS
CHROMATOGRAPH
9.7
Bal.
103.0
Bal.
392.0
Bal.
zoo
-------
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-------
APPENDIX D
SECTION II CONTINUOUS MONITOR DATA SUMMARY
-------
CONTINUOUS MONITOR DATA SUMMARY
The continuous monitor data were collected using a Century Model
OVA 108 portable flame ionization detector. The instrument was calibrated
with benzene in air. Subsequent research indicates that the instrument
calibration is sensitive to oxygen content of the carrier gas stream.
(The instrument uses the sample being analyzed as the source of oxygen
for combustion.) The exhaust gas stream, however, had a reduced percentage
of oxygen and, therefore, the calibration was invalid for quantitative
analysis of the exhaust gas stream. The data are summarized and presented
to show the cyclic nature of the emissions, assuming that the oxygen
content of the exhaust stream remains relatively constant. Because of
excessive noise and zero drift of the recorder during field operation,
the data collected have been summarized on the following three figures;
recorder strip charts are not included.
(All continuous monitoring data collected and reported by
EPA).
-------
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-------
APPENDIX D
SECTION III LABORATORY DATA SHEETS
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LABORATORY ANALYSIS REPORT
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Sampling Date '
Investigators ]/ t
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Log-in Date
Sample Source: f • Stack I I Community L_l Ind. Hyg. DT" Process i.jj. Water
Identity, Volume and Concentration of Collection Media: (].''/rr: .-...-. ^ • :; T
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Major Components NOT Listed Below:
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-------
LABORATORY ANALYSIS REPORT
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-------
LABORATORY ANALYSIS REPORT
Lab. Nos.
Sheet No..
{^ ) Continued From Previous Sheet
Project g/% JU& 2,
Job No. j
Investigators \J' I/J
Sample Source:
.._! Emergency (Needed:
/
Sampling Date '
Log-in Date
^ Stack I I Community L_l Ind. Hyg.
Process
Wat
Identity, Volume and Concentration of Collection Media: QAsrr ?.•;&. t,=-.-.-?7
_ I
Hajor Components NOT Listed Below; :
Other Comments :
Analyses Requested:
Estimated Concen. :
Analyst: .
Date Completed:
let?
Lab.
No.
Field Description
Stack or 1 Test No.
Site No. ' & Date
I
I ,
! BLANK: !
i
Fraction
Identification
//Zr'/*?/. .' ,?.'. ,"*.!. f*£-^ :'XS~ ' 5"/^5"/Si //."!?/ il'L' J~"-.S>~:-S?'--'
97 i . * ito-z-
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i
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4/ LO-/O >
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Total
Original
Volume
of Sample
11,0 (JL)
JLL,t
US ' -
1 1>0
Ut
ZLO
1UO
MO
UO
UB
•
Analyses , Completed
Detn'n^^L-V;^, .-•>
Units: '...:• L.f.:. ...
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Blank
Correct.
^rtv/t ^>/i7*M - ——
Additional analyses on next sheet for samples listed above
Additional samples on next sheet for analyses listed above
Approved and forwarded
Date:
(FT
-------
LABORATORY ANALYSIS REPORT
Lab. Nos. 1.239/3-';
Sheet No..
l_ ] Continued From Previous Sheet
Project
Job No.
. I I Emergency (Needed:
c ,
Sampling Date
Log-in Date
. / . ' t,
Investigators ;• . tv £/<*-•. v.'TJi.' . .- T A . * _
Sample Source: f"Xl Stack fh Community L_J Ind. Hyg. CZ2 Process [_J W
^^ \C .**-, t .c ."^
Identity, Volume and Concentration of Collection Media: /*% f\' '. ^:>C-r < /fel/.
Major Components NOT Listed Below:
Other Comments:
Analyses Requested:
Estimated Concen.:
Analys t:
Date Completed:
?/ £/;);.}„•)„•//<, ./^•/i^'/-/-/1,-/^ •^•'/f.J^/'.-
V '' ^' '
Lab.
No.
\L3<\ \~5
ItSll'l
Field Description
Stack or
Site No.
BLANK:
Test No.
& Date
17, A-:'W..
Fraction
Identification
•'/ -Jr
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Total
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Volume
of Sample
1
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Analyses Completed
Detn'n.: Hem \' ' "T.V?>
•
Units: TOTAL M - -. 'j^Corrt
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L _ .1 Additional analyses on next sheet for samples- listed ab"ove . ~ i
Additional samples on next sheet for analyses listed above
Approved and forwarded:
Dal
-------
LABORATORY ANALYSIS REPORT
Lab. N?
Sheet No..
Continued From Previous Shee
Project r^ ~1*-b •?
Job No.
_, [ L_l Emergency (Needed:
Sampling Date .3-Ih . /<- - 7ft
Log-in Date 3 - y f - ?;<
Investigators
Sample Source: f" \ Stack L I Community L_J Ind. Hyg. f ' Process LJj Wat
Identity, Volume and Concentration of Collection Media: /'/-. .(•• /M/'v.
MajorComponents NOT Listed Below;'
Other Comments:
Analyses Requested: /72>fr/ fi&k,jji ^^•jcf,i-,:/ii't-'.- 575
^C t,w
V<."-} 5"7fl
Analyses Compl-eted..'-
D e t o ' n ; W^HO • I : ^.'.'-^t
Units : lOTAi. M '• >-.•>-
/ l . •« — .-
^•iO.L O. /
/^ ,55,, | 7,
7. f 7f • 'i:.
5.673 /.:\
T ^5 / /, '
j
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••
(L:
'Blank
Corrects
Additional analyses on next sheet for samples listed above
Additional samples on next sheet for analyses, listed above
Approved and forwarded:
Date:
\
-------
£.P.ft.
Z - K&IC.HOLO
L/B to.
J*3?I3 0
MM 5
/*3?/5
/*#«,
I&H?
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l<o
IZ3
-------
LABORATORY ANALYSIS REPORT
Lab. Nos.
Sheet No..
Continued From Previous Sheet
-f'A
~1 Emergency (Needed:
Job No.
Investigators '.' j,'.- fJ*:>..'->\. . r '• >'
Sampling Date
Log-in Date
0/ /
.;/ / • '/..•/ 7S
/ . . -,'j
Sample Source: '. \^ Stack I I Community I ' I Ind. Hyg. f — 2 Process L. __ ! Watft
!«••*-. .0 .•**-
•* *
Identity, Volume and Concentration of Collection Media: ,' / /[-••' ^-f ,
Major Components NOT Listed Below:
Other Comments:
Analyses Requested:
Estimated Concen.:
Analys t:
Date Completed:
f-!;-i •}•//• lf< ' ••' 'l'i-'i .•/<"]' *"• -V'' •/•'//-•
-'
Lab.
No.
Field Description
Stack or 1 Test No.
Site No. ' & Date
BLANK: ' ' /' '• •' •''•''•'
! .'7 «
. ' ',••-,
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' tfl -'
-------
LABORATORY ANALYSIS REPORT
Lab. Nos.
Sheet No..
^ } Continued From Previous Sheet , [_~
Project t(& dltk'2 fattkW Ckn*&V
Job No.
Investigators
.._! Emergency (Needed:
Sampling Date 3-/•••). /£. - 7,j
Log-in Date 5~;-'£•-?%
Sample Source: \ "l Stack IZZ1 Community L_l Ind. Hyg. f—2 Process i.^ Wate
Identity, Volume and Concentration of Collection Media: / /£ •(:/ rr V^:'?.
Major Components NOT Listed Below:
Other Comments:
Analyses Requested:
Estimated Concen.:
Analyst:
Date Completed:
Lab.
No.
Field Description
Stack or
Site No.
1 BLANK:
•*5 l'fSZ& tr.'fr?'/'
U.
lit
11311?
Test No.
& Date
5S
Fraction
Identi f icat ion
^••L. A"
7. f 7f
5.&7J
^ /-f 5
•
Blank
Correc 1
\
Additional analyses on next sheet for samples listed above
Additional samples on next sheet for analyses listed above
Approved and forwarded:
Date;
-------
APPENDIX D
SECTION IV GAS CHROMATOGRAMS
-------
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-------
APPENDIX E
CALIBRATION DATA
-------
3 —
C'T
a \
•/
cr
nb
RftC
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rcge
re
rage
3
.r t
rage
P
rt
rcgc
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Orifice
Mar.or.cter
Setting, An
(in. H20)
0.5
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1.0
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2.0
7 • / •'; "]
3.0
v-'-^V
4.0
~ry. v/
5.0
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Gas Volume
Wet Test4
Meter v
rz ^ 7^ oo
-2.676.o6
(5) ^,00
2to
3, 7 /O t& o
(10) /^,6V>'
Gas Volume
Dry Gas
._ Meter
0 72.C>$4
O £•/.'£ £"£
/o , 204
& 'tZ.177
0 72.&S4
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/ 0 . - / V 1
Temperature
W e t
Test
Meter
is
75
75
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75
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Inlet
tdl
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9 £ \ %£
-------
ictric pressure Pb ("i'.g) 2. c/. 3
Calibrator . <£,xy/. Gas Meter Number
>
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sge
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age
,
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6.5
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3.0
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4.0
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Gas Volume
17 et TeEt^
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(f$)
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(5) >-..€.«.
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(10) /o. *">
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(ft^)
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4. <*<*£
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Time
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(min)
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AVERAGE
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6>. 79
-------
0 =
C"
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Pitot Tube Type JT Pitot Tube No.
Standard Pitot Tube No._
Date
C1 i e n t:
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-------
CPteot"
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* '•'.
.4
*•*
I
f; •
1
-
:
0.
ijji
n
j.»-
—
i
iO
5
;;
i!
• 1
"i:
i
i '.
•
ii :
ll. 1
1
' J_i _
" T
- - -
-• — -
j^:
1.
-------
Client:
Date: ':
7
CRITICAL Ollli _CE CALIBRATION
/./.'> ; •' A:l Barometric Pressure:
Calibrator:
"Hg
Orifice
Number
IDS
|o:i
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Stop
Start
Average
Test Meter
Gas Volume
(£t3)
Vw
2"7$L5So
£780. see
1.55
Tr^^oo
yi^i.-sso
1. -.'::.
Time
(min)
9
4o.':^o
'!%.>>?>
-iC,1. .U
* . *" • . " • '
Test Meter
Temp
(°F)
Tw
ti; . £
IA
^
(^;.b
^/:-.-.'
. ,'
Test Meter
Vacuum
. ("H20)
PW
G<0£
0.0 5"
O..5'j
o.o^
'.-• (.v^r
^.c:'C.'
Orifice
Temp
(°F) .
To
M
(A
6.6
in
1C-
fcs
Oril
Vac
iLOOiSl
ifeVciii
Cf'Vi«»*
£)/7b
0.7rT
0.75
o.-ifi'
^)/lb
C/.'7-T
lice
uum
l:O^T»q
Ar/*-'J
jtnfi"
^.^
.«.*
c^/,.5
3&J7
0(fv?
/•..' '
.•• .•••. •/
Orifice
Flowrate
(1pm)
Qcal
l.Ot,
1.02
28.32
- P)(T
460)
9 (Pb - P0)(TW + 460)
Clayton Environmental Consultants, Inc.
-------
Client:
Date:
CRITICAL ORi .CE CALIBRATION
Barometric Pressure; 2-7<(
Calibrator:
"He
Orifice
Number
•df[(j7x
t\jC>
~L\yj
0(o
^
2. ; 51
0:0
^
Test Meter
Temp
6^
^6"
(', :-:
6T
62^
(o \:'
^6ft
C,8C
U
Test Meter
Vacuum
("H20>
a/o
4/0
o.,, .
o./o
o,/o
C,0,'
0<(0.
08*
6S1
Orifice
Vacuum
C"H20)
(•>,,!-
/i.S"
ft^
/3»r-
/3.r
0.-J-1
/>,5~
/3.r
.G/;'?
Orifice
Flowrate
(1pm)
Qcal
././/
' /./*.'
/.// •
_£A//)
28.32 Vw(Pb • PW)(T0 + 460)
e (pb - PO)(TW + ^6°)
•tc
nv
su
\t!
nc
-------
APPENDIX F
PROJECT PARTICIPANTS
-------
PROJECT PARTICIPANTS
Clayton Environmental Consultants, Inc.
N. Steve Walsh
Victor W. Hanson
Gerald E. Hawkins
Timothy V. Mattson
Daniel J. Casiraro
Thomas J. Geyer
J. Douglas Opthoff
Kent Shoemaker
Genevieve Depa
Dusanka Lazarevic
Donna L. Schick
Director, Air. Resource Engineering
Senior Environmental Control Specialist
Source Sampling Specialist
Source Sampling Specialist
Source Sampling Specialist
Environmental Chemist
Environmental Chemist
Environmental Chemist
Laboratory Technologist
Environmental Data Specialist
Environmental Data Specialist
Environmental Protection Agency
R. Terry Harrison
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