-------
-6-
2. Time tunnel used (hrs)
3. Air temperature (°F) in flow system and barometric
pressure (inches Hg).
4. All checks for turbulance and flow distribution.
5. Velocity range (ft/min).
The pi tot tube information shall include:
1. I,D. number
2. Checks for physical dctfpages, errors noted and
modifi cations.
3. Dates and surveys pi tot tubes were used.
4. Date of calibrations, coefficient and dates of
re-calibration.
The calibration records will be kept on file at NEIC. Copies of
the appropriate calibration dates will be furnished for each source
test project.
-------
c
7"
•A
Figure 1. Measurement of Type-S pitot tubo length (dimension "a"') and impact-picr.e
separation distance (dimension "b").
TRANSVERSE
TUBE AXIS
IMPACT
PLANES
'Figure 2
e-S pitotitube, endi
pendlcular to transverse tube axis..
lA^ID'EPLAIJE
Ldhgitud^al
tube axis
B-SIOE PLANE
w CiiH. i
Figure 3. Type-§ tube, top view; impact-open
¦ing planes parallel to longitudinal tube axis.
From "A TYPE-S PITOT TUBE CALIBRATION STUDY" by
Robert F. Vollaro, October 15, 1975
-------
US Fnvironmental Protection Agency
Nat:onal Enforcement Investigations Center-Denver
Calibration Pitot Tube:ID Number AJ AS Cp C ¦ c/ /
Type-S Pitot Tube ID Number: -
p / £'c
6 - 1l<,
i^7 ' / A >-i
0 ¦ u
ft, t fro
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n
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r)-u z
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6.111
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ro
Ojn /
•J / /A7n
OOlo
Leg Average Cp
.u
probe sheath attached *
nozzle attached l.u '/jl
sampling'isokjnetical 1y
//
Performed By:
Calibration Date:
9 -23 - 77
if''' "
-------
US I'nviroiir.-nL?! Protection Agency
National Lnforces?nt Investigations Center-Denver
Calibration Pi tot Tube: ID flumbor / , 7~-» Cp / /
Type-S Pi tot Tube ID [lumber: ',? '/ ^
1 > v_"7 j> | C n-?^- C -
^ ^ j
A -•— / f.
^P
Standard
Pilot
Ap S--Tvpe Pi tot
CP
Cor.Tents
A leq
B leq
A
B
AO ¦
/' £2.
/• 7r b>
,777
.170
/ C
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// G>
. \
, 1%
r?x&
O 7"~
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,1%
,17?
/<
,7?X
.776
Leg Average Cp
During Pi tot Calibration:
probe sheath attached /c-•;
nozzle attached
sampling isokinetically .
j /' / ^ f
Performed By: ' "f /K~^' ' "c- Calibration Date: .v /.-/ J, ,
I /
-------
1 1 I t 1 ' 1
1 2 3 4 5 6
Decrease 'in Pitot Tube Coefficient, Percent
FigureB-2. Plot of Blockage - Percent vs. Decrease in Pitot Tube Coefficient - Percent
-------
C/3I 7- 8 £ ft JZ£ a.<>
AFi G!ZZ/!tL
SV^7
3. V7f
3. 5/y
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£
7
C4
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/, * .
(jl?^.
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. / '.^
.!'.
-------
Appendix C
Sampling Train Construction Details
-------
Aerotherm HVSS Description
The Acurex/Aerotherm High Volume Source Sampler (HVSS) consists
of a control unit, vacuum unit and a sampling unit. The units are con-
nected together with quick disconnect electrical and air lines, and
umbilical cords. Not all the equipment used was of Aerotherm manufac-
ture and this equipment is described below the item it replaced.
A) The HVSS control unit contains the following (figure 1):
1. All temperature and electrical switches and
controls.
2. Dry gas and orifice meters to accurately
determine the sample volume and sampling rate.
3. Magnehelic gauges to indicate the pressure
drop of the orifice meter and pi tot tube.
The magnehelic gauges were not used during
the Marana survey. Inclined manometers re-
placed the magnehelics.
4. Digital Temperature Indicator (DTI) which
gives an instant readout from several points;
stack, oven, impinger outlet, meter inlet,
meter outlet by use of a selector switch.
The DTI was only used to monitor the meter
inlet temperature. The duct temperature was
measured with a dial or glass thermometer.
B) The vacuum unit (pump) is capable of drawing a high vacuum
(65 CM Hg) and a high volume (280 1pm - free flow) of air. The
pump is a rotary fiber vane type which does not require lubrica-
tion, but oil bath filters are used for pump protection.
Attached directly to the pump are the flow control and bypass
valves for adjusting sampling rates.
C) The sampling unit is made up of three distinct sections; impinger
case (figure 2), oven and probe. All three units can be converted
to form one sampling unit or can be separated for unusual sampling
conditions. Below are the individual component descriptions:
*Information included in this description is from the report,
"Operating and Service Manual, Source Assessment Sampling System,"
D. Blake, Aerotherm Report UM-77-80.
-------
DRY GAS METER DIAL
ELAPSED TIME INDICATOR
MAGNlMfUC.
r\ AEROTHERM
' ACUREX Corporation
FAN ON/OFF SWITCH
PITOT INLETS
SAMPLE INLET
SAMPLE
EXHAUST
115V 15 AMP
POWER INPUTS-
POWER TO
PROBE AND
OVEN HEATERS
OVEN FAN
THERMO-
COUPLE
INPUTS —
MAGNEHELICS
SHOWING AP
FOR PITOT
TUBES
MAGNEHELIC SHOWING
£P FOR ORIFICE
PROBE HEATER
CONTROLS
OVEN HEATER
INDICATOR LIGHT
OVEN HEATER
ON/OFF SWITCH
OVEN HEATER
CONTROLS
•SELECTOR SWI TCH KEY
— MAIN POWER
ON/OFF SWITCH
MAIN POWER
INDICATOR LIGHT
-DIGITAL TEM-
PERATURE
INDICATOR
PROBE HEATER
INDICATOR
LIGHT
PROBE HEATER
ON/OFF SWITCH
Figure 1. Control unit.
-------
Figure 2 Impinger train.
-------
1. Impinger case - an uninsulated fiberglass case
capable of holding four plastic impingers (1
liter capacity) in an ice bath.
2. Oven - an insulated, double walled, stainless
steel (S.S.) box that can hold the cyclone and
- filter holder. The S.S. cyclone and filter-
holder connect with S.S. fittings and Teflon seals.
The filter support is a S.S. screen.
3. Probe - a S.S. lined, external sheathed probe.
The sheath, which contains the liner, pi tot
tube, and thermocouple connections, is 6.4 cm
(2.5 in) in diameter and connects directly to
the cyclone inlet.
The HVSS probe was replaced with a Scientific
Glass (S.G.) Inc. AP-5000 S.S. lined probe dur-
ing the Marana survey. The S.G. probe was used
because it has less duct blockage than the HVSS
probe. A flexible Teflon probe connected the
S.G. probe to the cyclone inlet.
-------
Rader HV Sampler Description*
"The Rader Hi-Volume Sampler provides a means of determining par-
ticulate matter in emissions. It has developed over several years, and
results obtained from a variety of sources have proven it to be a
versatile and reliable sampler.
"The Sampler is illustrated by Fig. 1. It consists of four assem-
blies. (1) The Filter Holder Assembly houses the filter support and
filter. (2) The Inlet Extension Section is clamped to one side of the
Filter Holder. The 1-7/8" inlet nozzle is recommended for velocities
below 2500 FPM, additional nozzle adapters are available for higher
velocities. (3) The Control Section is clamped to the opposide side
of the Filter Holder. It consists of the flow sensors, control valve
and suction blower attached with flexible hose. (4) The Control Com-
puter which performs all needed calculations to run the stack test.
"These operating instructions have been developed to enable the
operator to collect an accurate sample with a minimum of effort.
Briefly, a pi tot traverse is performed to determine the velocity at
the sampling points. In some instances, the velocity may be calcu-
lated with sufficient accuracy to select the nozzle size. The sampler
automatically regulates to achieve an isokinetic sampling rate, but the
pi tot traverse may be necessary to determine volume flow. Samples are
then collected on pre-weighted filters using blanks for monitoring any
changes to the filter tare weights.
"Since particulate will accumulate in the inlet probe during a
test run, the procedure provides for the collection and inclusion of
this particulate in the sampling results."
The HV sampler is all aluminum with rubber gaskets and seals. The
maximum sampling rate is about 90 cfm.
*Information included in this description is from the instruction
manual for the Rader Hi-Volume Sampler (Automatic) distributed by
Rader Companies, Inc.
-------
SUCTION BLOWER
CONTROL SECTION
CONTROL COMPUTER
FILTER HOUSING
INLET SECTION
RADER MODEL A-2000 AUTOMATIC STACK SAMPLER
FSG. 1
-------
The Rader HV sampler operates in the following manner:
1. A standard type pitot tube, adjacent to the sampling nozzle,
senses the stack gas velocity and this pitobe differential
pressure is transmitted to the control computer via air lines.
2. Simultaneously the unit sampling rate is measured by the
orifice meter and the orifice differential pressure is
transmitted via air lines to the computer.
3. Based on the velocity pressure, the computer adjusts the
solenoid valve until the orifice meter pressure corresponds
to the sampling rate necessary for isokinetic flow. The
computer uses the sampling rate at the orifice meter and
the sampling time period to indirectly determine the
sample volume.
The Rader HV sampler does not meet the following Method 5 requirements:
1. No moisture determination is performed.
2. No direct measurement of the sample volume is made.
3. Stack temperature readout is not available.
-------
Appendix D
NEIC Analytical Procedures and Data
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
to Mr. Paul dePercin, Field Coordinator DATE January 6, 1977
Marana Cotton Gin Study
from Chief
Chemistry Branch
subject Results of Particulates Analyses
Attached is a summary of the results of particulate analyses of filters and
acetone washes collected for the Marana Cotton Gin Study.
In addition, several samples are being analyzed for phosphorus pesticides
and those results will be sent to you shortly.
Theodore 0. Meiggs
Attachment
cc: Harp
Young
Stager
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
to Chief DATE January 6, 1977
Chemistry Branch
from w. E. Stager
(Reviewed by D. Vietti)
subject Results of Particulates Analyses for the Marana Gin Study
Analytical Procedures
Filters
The filters to be tared were desiccated at 20 +_ 5.6°C (68 + 10°F) and ambient
pressure for 24 hours and weiqhed to constant weiqht. The tare weights were
recorded to the nearest 0.1 mg. During each weighing, the filters were not
exposed to the laboratory for more than two minutes.
After sample collection the filters were returned from the field folded in
field data cards in sealed envelopes. The data cards and filters were re-
moved from the envelopes and placed into a desiccator after the circle charts
had been stapled to the cards. Indicating Drierite, which removes uncombined
water from the filters, was used as the desiccant. The filters were desiccated
at 20 + 5.6°C (68 + 10°F) and ambient pressure for 24 hours and weiqhed to a
constant weight, i.e., a difference of no more than < 0.5 mq, or 1% of the
gross weight minus the tare weight, whichever was greater, between two con-
secutive weighings.
The single pan analytical balance was calibrated against Class "S" weights
before weighing the filters. Additionally, desiccator and weiqhinq room
temperature and relative humidity readings were recorded. All handling of
the filters was performed with forceps.
Acetone Wash
The acetone probe washes were received in quart jars with Teflon lined lids.
The level of liquid in the containers was noted and no leakage had occurred.
It was noted, however, that the volume of acetone in the field blanks was
considerably less than the average sample volume. The volume of acetone in
each sample was measured volumetrically to within + 1 ml and recorded on
the bench sheets.
The samples were mixed to suspend the solids therein and transferred to
tared 250 ml beakers, as was the acetone used to rinse the jars. The beakers
were placed in an aluminum foil tunnel-designed to prevent particulate con-
tamination of the sample, yet allow efficient air flow for escape of acetone
vapors-in a hood. The hood door was kept closed and empty tared beakers were
used as blanks to verify that the samples did not become contaminated.
-------
- 2 -
After a minimum of 24 hours in the evaporating tunnel, the beakers were
transferred into a desiccator having Drierite as the desiccant. After 24 hours
the beakers were weighed to constant weiqht with at least 6 hours between
consecutive weighings.
Field and Laboratory Blanks
For both sizes of filters-6" and 8 x 10"-and for acetone washes-both field
and laboratory blanks were collected and weighed at the minimum rate of one
blank of each type for every ten sameles.
Statistical treatment of the field and lab blank data were used to determine
the detection limit utilizing the formula:
D.L. = x + 2^
-------
ANALYTICAL DATA REPORTING FORM v Page
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-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DEN1 ER FEDERAL CENTER
DENVER, COLORADO 80225
T0 Mr. Paul dePercin, Field Coordinator CATE January 23, 1978
Marana Cotton Gin Study
h»cm chief
Chemistry Branch
subject Resuits of Pesticide Analyses
Attached is Ms. Carlberg's report which summarizes the results of analyzing
four different samples from Station 2211 at the Marana Cotton Gin for phos-
phorus pesticides. Trace amounts of methyl and ethyl parathion were found
in the acetone washes ranging from 0.03 to 0.8 ug/kg (ppb). The filters
did not contain sufficient particulate material to detect these low concen-
trations which appear to be too low to be of concern.
Theodore 0. Meiggs
Attachment
cc: Young
Harp
Carl berg
-------
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53. BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80225
Chief 0ATE January 19, 1978
Chemistry Branch
K. A. Carlberg
SUBJECr Analysis of Samples from Marana Cotton Gin in Arizona for Pesticides
Background
Eight samples from the Marana Cotton Gin in Arizona were submitted for
pesticides analyses. These samples consisted of four filters and four
particulates/acetone washes. The acetone wash samples had been taken
to dryness and resuspended in acetone before they were submitted for
pesticide analysis. The pesticides of concern were ethyl parathion,
methyl parathion, malathion, and dimethoate.
Results
The four filters contained no detectable amounts of the pesticides of
interest. All four of the acetone washes contained methyl parathion,
ranging from 0.1 - 1.8 ug. Three of the acetone washes contained ethyl
parathion in amounts ranging from 0.1 - 0.5 ug. Malathion was not four.d
in any of the acetone washes. The analytical methods used to analyze
ethyl and methyl parathion and malathion prohibited analyzing the acetone
wash samples for dimethoate.
The results are given in the table following. In addition, the weight
of particulates found on each filter and in each acetone wash, as re-
ported in a memo by W. E. Stager dated January 6, 1977, is given. It
is not surprising that pesticide levels in the acetone wash samples
were greater than those on the filters due to the much higher particulate
levels in the acetone wash samples.
-------
- 2 -
Table of Results
FILTERS
ug on
Filter
Station
mg Particulates
Methyl
Ethyl
v Run §
Date
on Filter
Parathion
Parathion
Malathion
Dimethoate
2211
1
11/04/77
30
<0.05
<0.05
<0.1
<0.01
2211
2
11/05/77
37
<0.05
<0.05
<0.1
<0.01
2211
3
11/05/77
53
<0.05
<0.05
<0.1 '
<0.01
2211
4
11/05/77
78
<0.05
<0.05
<0.1
<0.1
PARTICULATE/ACETONE WASHES
ug
in Acetone Wash
Station
mg
Particulates
Methyl
Ethyl
H Date
Time
Sequence
in Wash
Parathion
Parathion
Malathion
2211
11/04/77
1500
01
3327
0.6
0.1
<1.0
2211
11/05/77
1030
02
1536
0.1
<0.1
<1.0
2211
11/05/77
1345
03
2429
1.8
0.5
<1.0
2211
11/05/77
1534
04
2530
1.5
0.5
<1.0
Methodology
A. FILTERS: Each filter was extracted with 150 ml of acetone for 1 hour
using a wrist action shaker. The extracts were then dried with sodium
sulfate and concentrated to 10 ml in a Kuderna-Danish evaporative concen-
trator. The concentrated extracts were analyzed using a gas chromatograph
equipped with an alkali-flame ionization detector. (GC-AFID)
B. PARTICULATE/ACETONE WASHES: Each acetone wash was filtered through
Whatman #1 filter paper and concentrated to 10 ml in a Kuderna-Danish
evaporative concentrator (KD). The concentrated extracts were then ana-
lyzed on a GC-AFID. The extracts were too dirty at this point to discern
the presence or absence of the pesticides of interest. The concentrated
extracts, therefore, were cleaned up using an Analytical Biochemistry
Laboratories Gel Permeation Chromatograph (GPC) equipped with a column of
SX-3 resin and eluted with 15% methylene chloride in cyclohexane. The
cleaned-up extracts were concentrated to 5 ml in a KD, since 5 ml was
injected onto the GPC. The extracts were then analyzed on a GC-AFID. At
this point it appeared possible that all of the pesticides of interest were
in each of the extracts. In order to confirm this, the extracts were ana-
lyzed on a gas chromatograph equipped with an electron capture detector.
Once again, because of the extreme sensitivity of the EC detector, the
extracts were too dirty to be analyzed. Therefore, the samples were sub-
jected to a Florisil column cleanup. The cleanup used was the one de-
scribed in the FDA, Pesticide Analytical Manual, Vol. 1, Section 211.14d,
-------
3 -
for cleanup of organochlorine and organoDhosphorous pesticides. Unfor-
tunately, dimethoate does not elute from this Florisil column and therefore
confirmation of the presence of dimethoate was not possible. The peak
which eluted at the same retention time as dimethoate in the GC-AFID
chromatograms appears in an area of the chromatoqram traditionally sub-
ject to many interference peaks. Therefore, in my judqment, the presence
of dimethoate in the acetone wash samples is doubtful.
The Florisil cleanup referred to above involves elutinq each sample through
4 inches of activated Florisil topped by one-half inch of sodium sulfate.
The column is eluted with 200 ml of 6% ethyl ether in petroleum ether,
followed by 200 ml of 15% ethyl ether in petroleum ether, 200 ml of 50%
ethyl ether in petroleum ether and finally 200 ml of ethyl ether. Methyl
and ethyl parathion elute in fraction 2 (15% EtO) while malathion elutes
in fraction 3 (50% EtO). This Florisil cleanup proved to be insufficient
to allow the samples to be analyzed by EC, however, using the AFID, it was
found that 2 peaks still appeared in fraction 2 in the area of elution of
methyl and ethyl parathion. However, fraction 3 was free of any peak
corresponding to malathion, thus eliminating malathion as a constituent
of the samples.
Fraction 2 of the extracts, which contained peaks suspected of beinq
methyl and ethyl parithion, were submitted to an alumina column cleanup.
The extracts were cleaned up on a 15 cm column of neutral alumina, deac-
tivated with 3% water which was eluted with three 50 ml portions of
benzene. Methyl parathion elutes from this colu.nn in fractions 2 and 3,
while ethyl parathion elutes completely in fraction 2. After this
cleanup, the extracts were clean enough to be analyzed on the EC-GC.
The peaks suspected of being methyl and ethyl parathion were confirmed as
such by proper retention times on the EC-GC and by their proper elution
pattern from the neutral alumina column.
Kathleen A. Carlberg
-------
Lint Cage
and
Appendix E
Dimensions, Flow Data
Calculations
-------
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Table E-1
LINT CAGE ISOKINETIC RATES*
PRODUCERS COTTON OIL COMPANY
MARANAj ARIZONA
Sampling
Station Rate
Number ft3/min
Nozzle
Area
ft2
Nozzle
Velocity
ft/mi n
Gas Flow
ft3/min
Lint Cage
Area
ft2
Screen
Velocity
ft/min
Isokinetic
%
Short-Staple Cotton Gin
2201 26.5
.0670
396
13,000
129.5
100
396
2202 27.1
.0189
1,430
10,300
no
93.6
1 ,532
2203 27.5
.0670
410
19,000
46.8
406
101
Long-Staple Cotton Gin
2301 27.2
.0670
406
4,000
32.7
122
333
2302 27.2
.0670
406
4,150
31.9
130
312
2303 27.1
.0670
404
2,880
31.7
90.9
444
2304 27.0
.0670
403
2,880
33.3
86.5
466
2305 27.0
.0670
406
5,060
39.7
128
317
* Average values for three runs} except for Station 2203 which is an average of six runs.
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m
<$f/t AGRICULTURAL
Z*ll RESEARCH