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96
-------
MEMBRANE RECORD SHEET
Budget Bureau No. 85-R0084
Expires 1-31-75
NATIONAL AIR POLLUTION CONTROL ADMINISTRATION
NATIONAL AIR SURVEILLANCE NETWORK
>AMPLER SERIAL NO.
ilTE
FILTER NO.
( CITY or TOWN )
(SAMPLER LOCATION )
WIND
DIRECTION
Q] CALM
Q] LIGHT
Q GUSTY
DATE
DOOOO TO 2400
HOURS
Q OTHER EXPLAIN
^
VISIBILITY
Q] CLEAR
Q HAZY
METER READING
START
END
SKY
Q CLEAR
Q3 SCATTERED
Q OVERCAST
HUMIDITY
Q DRY
[~] MODERATE
Q HUMID
CH RAIN
TEMP. ฐF
EH <2ฐ
Q 20-40
[^\ 41-60
Q 61-80
D >8ฐ
REMARKS & UNUSUAL CONDITIONS OR ACTIVITIES NEAR THE SITE
97
-------
Daily
MEMBRANE MAINTENANCE SCHEDULE
Check pump for sluggish operation. Flush with kerosene
to clean pump vanes if necessary, and recalibrate flowrate.
Weekly
IT Check the tubing connections for snug fit, kinks, or
obstructions.
98
-------
PROCEDURES FOR THE CASCADE/MEMBRANE
PARTICULATE FRACTION SAMPLER
99
-------
ANDERSON TYPE CASCADE IMPACTOR*
- Contents -
Quantity Item
1 Field Operating Instructions for the Anderson Cascade Impactor
I Sampling Schedule
1 Membrane Record Sheets
1 Forceps
~ NOTE -
The cascade head is an attachment to a standard membrane sampler,
and attaches in place of the face plate. Therefore, the operational
procedures including calibration are the same as the membrane sampler.
See the previous section for these instructions. The following
procedure is concerned with the cascade head only.
100
-------
FIELD OPERATING INSTRUCTIONS FOR
THE ANDERSEN CASCADE IMPACTOR
The modified andcrsen cascade impactor is a sampler designed
to operate for 24 hour periods at a sampling rate from A to
6 cubic feet per minute. This sampler can fractionate and
collect suspended particulates in air in sufficient quantities
for gravimetric measurement with a microbalance . The parti-
culates are collected on pre-weighed aluminum collection
surfaces and on a membrane filter placed past the last stage.
After collection these surfaces are to be returned to the
laboratory for microweighing .
The sampler is composed of five stages (numbered 1 through
5) and a membrane filter holder located past the fifth stage.
The entire head of the. sampler including the sar-plir. z stages
and the filter holder is designed to be removed and serviced
indoors. The stage marked number 1 has the largest jets or
hole?, v herons tho s t a o o .cr]- pr] nmbpr 5 has the s "->."' 1 e ซ t .
The following is a step by step procedure for changing
the collection surfaces on the sari pier.
BEFOPE COLLECTING A SAMPLE
1. Carefully disassemble the s t a e e s by releasing t h e sprir. ?
loaded c 1 a in p s . Always keep your hand firr.-.ly or. c'r.t? top
of the s_ta?c-s until . r. 11 .. ttio cJr.ons hnvr> j:_c-er re- leaped
to prevent t ! c parplcr fror. f 1 vi ng nr ar t_ .
/% 1 - ป U <~ ฃ ** ~* ~ ~. ~* T- 1 - -. ป. 1 . -
o . i t * c * c * ^ i c r r> PJซ*CL. Li.e
surface s;:ir. y side cicvn (nurbered sice \ip) i~rec" i?. t e ly
past stage 1 , i.e., on top of the plate r a r !. o d s t -. c e 2.
Repent for all the other surfaces,, i.e. a I u n i n u collection
surface 2 should be placed on top of the stainless
steel cover' on stage 3, aluminum collection surfr.ce 3
should be placed on top of the stainless steel ccver marked
4 and so on. Refer to dravinp. 1.
3. Reassemble thr cascade impactor 'so that st'ace 1 is the top
s t n n e and P l ci c e 5 becomes t ! e bottom s t a .t
-------
o
the top of the nenbrane filter holder to the bottom
so that an air tight seal is formed.
5. Take the assembled cascade impactor and hack-up filter
outside to the sampler and screw it back on the pipe.
Place the. rain cover on top of. the assembled sampler
so that it fits snugly in place.
6. Turn on the sampler making a note of the starting time.
. Allow the sampler to run approximately 5 r. inutes, then
depress the test button under the magnehelic and record
the reading on the Meribrane I", c cord Sheet. After the
reading has been taken, depress the zero button on the
map, nc he lie so thrt the needle returns to zero. Record
a]] readings on the folder or data card provided.
AFTER COLLECTING THE SAMPLE
1. After the sample has been collected, usually . 24 hour
period, press the test button again on the rr a g n e h c 1 i c
and record the fina] reading. Then depress the zero
button again to bring LJ:e gauge uack LU icru. Turn
the sampler off after noting the final time. Record all
readings on tht; folder or data card provided.
2. Unscrew the as sent ltd cascade impact or and backup filter
3.
4.
holder fror, the pipe and br:r.g indoors. Car f; f \: 1 2 ;
disassemble th e cascade impactor as in the early steps.
Using "the forceps provided, carefully fold the aluminum
collection cover over onto itself so that only the. sampled
sides are touch, ing. (see Figure 2). b 0 NO V 1 0 i' C H W 1 1 h
the
T>ir
T>lnce
folded collection surface in the
appropriate envelop i.e, aluminum surface marked 1 should
be placed in the glassine envelope marl: ed 1. Repeat
for all the other collection surfaces and backup filter.
\
Place all 6 collected sanplos into the folder provided,
insert into tae envelop, ar.J nail to the ?iAI CA laboratory
102
-------
FIGURE I
LARGE HOLES
TO
103
-------
A.
,.... . .
ซ.',',; ,.'.-..'.-. V.'"''^
^^_ , i ปซ ,-'
Remove collected sample from
each stage vn'th tweezers.
U s i n a tv/o t\-/e e 7. C1 r s, fold
collectsd sair.ole in half
colleclecl side touching
DO IIDT TOUCH WITH fir.'GERS.
Place folded sample into
orui_ij;/;_!_ e n velope.
Return envelope to folder
end plr.cr- entire folder
into railing envelope.
O-
104
-------
PROCEDURE FOR THE ASSEMBLY AND OPERATION OF THE
24 HOUR GAS SAMPLER
(BUBBLER)
105
-------
The NASN gas sampling system consists of a collecting unit
and a vacuum pump (Figure 1). The collecting unit is a metal
box which houses five individual bubbler trains operating in
parallel under the inlet and outler manifolds, making it possible
to sample concurrently over a 24-hour period for a maximum of
five different gaseous pollutants.
The sampler is
maintained at a constant temperature with a thermostatically
controlled heater, which is plugged into a 24-hour a day circuit
not to the timer. (Fig. 1).
Each sampling train consists of a bubbler, trap, membrane
filter unit and hypodermic needle (Fig. 9). Wi ch a vacuum of 20
inches or more of mercury, the needle acts as a limiting orifice
and gives a constant air flow. The trap collects any solution
which might be carried over from the bubbler. The
membrane filter removes any reagent droplets which might be in
the air stream as it leaves the trap, thus protecting the needle
from corrosion and blocking. Each train is color-coded to assist
in making correct connections.
A bubbler (Fig. 9), consists of polypropylene test tube with
a two-hole stopper into which is inserted iซ a straight
impinger tube. The trap is a polypropylene tube with a
two-hole stopper into which is inserted a glass tube. It is
half-filled with glass wool, or foam which is wrapped loosely
around the glass tube. Fittings consist of sections of teflon,
glass, polypropylene and tygon tubing when glass is butted together.
A diaphram pump capable of continuous operation is used to
produce the required vacuum of 20 or more inches of mercury. A
vacuum guage, range 0 to 30 inches of mercury, mounted on the
vacuum side of the pump, measures the vacuum in the sampler
exhaust manifold.
The sampler must be installed indoors, or in a protective
shelter with a probe connected to the glass manifold (Fig. 1).
106
-------
UNPACKING THE SAMPLER
1. The sampler is shipped in a heavy cardboard container. The
package contains the gas collecting unit, puir.p with vacuum
gauge and the following accessory items:
1. One electrical power extension cord.
2. One membrane filter unit color-coded with a black ring
on one side,'and label for dates it was used.
3ป Cue length of black tubing (to hook up pump to sampler).
^. One pinch clamp for use with pump tubing.
5ป One packet of sample reco7:d sheets
6. Extra polypropylene caps for shipping b^ck samples.
7ซ "Ducany" bubblers of polypropylene tubes serve to
complete the bubbling trains. The dummy bubblers should
remain in the acnipler, except when they are exchanged
for reagent-filled bubblers for a sampling run.
8.' Funnel for probe end.
9. Polypropylene tubing 4 feet long for probe.
ซ
2. Unpack with care, examine and account for all items mentioned
abovt.
/
3ซ If damage has occurred during transit or if any items are
missing, please notify the office at once.
4. The polypropylene tubing through which the air is drawn into
the sampler is included in this shipment. This is an expensive
item so only a minimal length has been included. It must be
long enough to connect to the ruanifold.
107
-------
SETTING UP THE SAMPLER
Assemble the sampler as follows:
t 9
1. Attach the membrane filter unit to the glass nipple of the
inlet manifold. A portion of the insulation has been cut
away from inside of the box to provide support for this
filter. Be sure the filter is attached with the taped side
away from the manifold. Care should be used in making this
connection so as not to break the glass manifold. (Fig. 2)
2. Attach the funnel to one end of the polypropylene tubing
included and extend out of doors through a windcv or other
opening. Attach the probe to the outside filter on the
taped side. Attach probe and filter to the glass manifold.
If attached properly, the connection should not be under
strain and not require removal except to change outside
filter quarterly. (Fig. 1) The tubing is quite rigid but
can be straightened by flexing against the curve. It is
necessary to support and secure the probe in position so that
it will not come loose during sampling. Allow the funnel to
hang down so that rain will not be drawn into the sampler.
See Fig. 1.
3. Attach the black.tygon tubing to the metal exhaust manifold
nipple (marked pump) on box (Fig. 3)- Place the pinch clamp
on the tubing, but do not tighten. Attach the other end of
the tubing to the intake nipple of the pump. Be sure all
connections are tight and none of the tubing is constricted.
4. Plug the male connector of the sampler cord into a convenient
24 hour 110V AC electrical outlet, and the female connector
into the recessed male connector on the side of the sampler
box. Plug the electric power cord of the pump into the
female connector on the timer (See Fig. 1). Use the timer to
control sampling operation (see timer instructions).
108
-------
COLLECTION OF SAMPLES
Installation of Bubblers and Needles
Reagent-filled bubblers, calibrated needles and a return
mailing label are shipped to the collection stations in
time for sampling on each scheduled date.
CAUTION: The bubbler train must be connected correctly,
or the collecting solution may be sucked over
into the trap. The stoppers and glass tubings
of the bubblers and traps have been color-coded
to assist in locating bubblers in the right
positions and making correct connections.
1. If the following rule (which applies to aJJL. tubing &
stopper connections) is ALWAYS observed, bubbler trains
will always be correctly connected. The accordian or
pleated tubing attaches only to the colored side of
sample tube, (see Fig. 4). Match sampling train colors
with the tube colors.
2. Remove the inlet and outlet tubing from the lid of the
dummy bubbler tube by gently but firmly pulling them
from the lid (see Fig. 5).
3ซ Exchange the new bubbler for the dummy bubbler.
4. Transfer the caps from the sampling bubbler lid to the
dummy bubbler lid. PULL OFF THE CAP ON THE UNPAP7TED
SIDE OF THE LID FIRST, otherwise (see Fig. 6) some of
the collecting solution may bubble out and be lost.
Keep the red caps with the red dummy tube, green with
green, e tc.
5. Gently but firmly insert the accordian inlet tube onto
the hole of the bubbler lid. Be sure to
press firmly until an airtight fit is assured. (Fig. 4)
-------
6. Gently but firmly insert the appointed end of the sample
tube into the clear tubing that goes to the trap in back.
7ซ Remove the new needle, and remove rubber cap from the
needle. (Save the cap). NOTEj Each needle is calibrated
for that particular colored tube which it accompanies in
the mailing block.
8- Insert the new needle into the center of the red rubber
stopper attached to the membrane filter unit. This
operation requires some skill. If the needle goes in
crooked, the point may be obstructed. If this happens,
it must be withdrawn and put in straight. A steady firm
thrust is best. Do not bend the needle. Figure 7 shows
the filter assembly while the needle is inserted.
(See Fig. 7).
9ซ Connect the shank end of the needle to the metal connector
attached to the exhaust manifold. Manipulate the needle
and/or rotate the trap a little to obtain a tight connect-
ion (See Fig. 8)
10. Repeat steps 2 through 8 i'f mo,-e -Hi** one bo,We<- * u%^ matching
the color on the bubblers and in the sampler. The properly
connected bubbler trains should appear as in Figure 2.
11. Recheck the arrangement, alignment, and tightness of all
connections.
Are sample tubes connected
to the pleated tubing?
Are the needles bent or obstructed?
Are all needles tight at the exhaust manifold connection?
Are the inlet filter and teflon tubing tightly connected?
Are the vacuum pump connections tight?
110
-------
B. Collection of the Sample
1. Completely close the pinch clamp between the sampler and
the pump. (Fig. 3)
2. Turn the timer switch to the "on" position. This should
start the vacuum pump, ALWAYS USE THE TIMER SWITCH TO
CONTROL SAMPLING. (See Timer instructions)
3ป Record the vacuum gauge reading to the nearest whole
number on the sampling record sheet, in the space marked
"Start-Clamped". The gauge should read 20 inches or
above. If it does not, make sure the pinch clamp is
closed and the tubing is securely connected to the
pump nipple. (See record sheet)
4. Open the pinch clamp, observe and record the vacuum gauge
reading on the record sheet in the space marked "Start-
Open". The gauge should read a little less than the
reading with the clamp closed. If it reads below 20
inches, check for loose connections in the system.
5ป Record the date (one day only, the day sample was
actually taken), and the time (if other than 0000-2400
explain under "Remarks").
6. Gently lift the whole train halfway out of sampler (DO
NOT TILT) (See Fig. 2). Examine bubblers to make
certain that they are "bubbling". If not, check for
loose connections in the train.
? Turn off timer and set for sampling period.
See timer instructions.
8. At the end of the sampling period, record the vacuum
gauge reading on the record sheet in the space marked
"End-Open".
in
-------
9- Close the pinch clamp as tightly as possible. Observe the
vacuum gauge and record the reading on the record sheet in
the space marked "End-Clamped".
10. Turn the timer switch to Lhe "off" position. Open pinch
clamp.
11. Gently pull off the connecting tubing from the stopper
of the bubbler. (Do one bubbler train at a time so as
not to intermix bubblers, needles or caps). REMOVE FRONT
PLEA TED TUB PIG FIRS T (See Fig. 5).
12. Remove the sampling bubbler. Replace the dummy bubbler
in the sampler.
13. Replace the caps on the sampled bubbler. BE SURE TO
PLACE THE CAP OVER THE OPENING NEAR THE PAINTED SIDE
OF THE BUBBLER LID FIRST. Press on firmly and place in
shipping block (See Fig. 6).
14. Disconnect the shank end of the hypodermic needle from
the metal connector attached to the exhaust hanifold.
(Fig. 8)
15' Withdraw the needle from the small red rubber stopper,
replace the protective cap and place with the correspond-
ing bubbler. THE NEEDLES MUST BE RETURNED.
16. Repeat steps 12 through 16 for the other bubblers.
112
-------
C. Preparation for Mailing
1. Fill out the record sheet in duplicate.
2. Note any unusual activities or conditions near the site,
such as fires Involving burning coal or oil. largecoal
burninK power plants, smoking stacks, rain, snow, fog,
Inversions, etc.
3. Note the conditions of the membrane filters. If they are
discolored or cracked, request new ones. If any other-
parts are broken or appear to be in doubtful condition,
request replacements. (See fig. 9 for ordering parts)
4. Fold the original copy of the record sheet and wrap around
one of the sampling bubblers. Retain the duplicate copy.
5- Pack the bubblers in the mailing container.
6. Affix the return mailing label. Mail promptly, or deliver whichever
procedure is adapted.
113
-------
FIGURE 1
-------
FIGURE 2
115
-------
116
-------
117
-------
118
-------
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119
-------
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121
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MOD Si C GAS SAMPLER
-------
GAS SAMPLE RECORD SHEET
Budget Bureau No. 85-R0084
Exp.res 1-31-75
NATIONAL AIR SURVEILLANCE NETWORK
SAMPLER SERIAL NO.
SITE
BLOCK NO.
CITY or TOWN )
(SAMPLER LOCATION )
WIND
DIRECTION
[~~| CALM
[J LIGHT
f | GUSTY
DATE
DOOOO TO 2400
HOURS
Q OTHER EXPLAIN
VISIBILITY
Q CLEAR
Q HAZY
METER READING
START
END
OPEN
CLAMP
SKY
Q CLEAR
Q SCATTERED
| | OVERCAST
HUMIDITY
D DRY
[~] MODERATE
(_J HUMID
[ ~| RAIN
TEMP. ฐF
tZ3 <2ฐ
Q 20-40
[j] 41-60
[71 61-80
CU >8ฐ
REMARKS & UNUSUAL CONDITIONS OR ACTIVITIES NEAR THE SITE
123
-------
Calibration Procedure - Flow needle on SOp bubbler
A Becton-Dickson 27-guage, 3/8" long hypodermic needle is used
as the critical flow orifice in the S02 bubbler train. The expected
flow range is 180-240 cc/nn'n. The needle flow is measured and recorded
at the beginning and end of each run. An average is then calculated
from both flov/s and recorded on the orange data card. All recording on
Data Card should be initialed by operator.
Procedure
1. Turn on pump.
2. Put needle on needle holder.
3. Push needle through serum stopper. Make sure the end of the
needle is unobstructed in the glass tube.
4. Allow air to flow until the rotameter ball indicates
a steady reading.
5. Note this reading and refer to the calibration curve
to obtain the corresponding flowrate in cc/min. See
Notes A & B.
6. Record the flowrate on the orange data card..
7. Remove the needle from the serum stopper and holder.
8. Return the needle to service or store in packet,
rating the flowrate on the packet.
9. Turn off pump.
Notes:
A. The flowrate range for the initial flow of a new or used
needle must bo between 180-240 cc/min. Discard tHe~ needle
if it is outside this range.
B. The final flow measurement must not be different than the initial
flow measurement by more than ฑ10 cc/min. Discard the needle
if it is outside this range.
-------
Daily Operating Procedure
for CO Analyzers
Note: During Steps 1 - 8, it is important that no adjustments be made
to the instrument. Record the necessary readings only.
1. Fill in the top part of the "Daily Check Sheet" and record the
following information in the indicated columns:
a. Date - record current date.
b. Sample flow reading. Record the reading of the sample flowmeter
reading the center of the ball.
c. Water trap. Record a checkmark if water is observed. If
water is observed, drain the trap and have the air dryer
checked.
d. Pressure guage. Record the reading of the cell pressure
guage.
e. Catalytic oxidizer. Record a check mark if the meter is not
in the red. If the meter does not read in the red, use the
zero gas cylinder in place of the oxidizer.
f. Air dryer. Record the temperature of the sample gas leaving
the air dryer, as recorded by the thermometer in the sample line.
If the temperature is not between 35 - 39 ฐF the dryer is not
operating properly. All data must be invalidated if outside
this range, back to the last acceptable temperature check.
g. Silica gel. Record a checkmark when 3/4 used, then replace.
h. Instrument filter. Check to make sure the filter holder is tight.
i
126
-------
2. Place the toggle valve under the dryer to the closed position.
Readjust rotameter to the same setting as recorded in Step Ib.
3. Connect a line from the manifold on the dilution system to the
pump inlet of the CO analyzer. NOTE: See instructions the
Catalytic oxidizer if it is not working properly.
4. If the span gas does not require dilution, adjust the flow
through the catalytic oxidizer to 4.0 liters/inin. and allow the
gas to vent. Do not exceed 4.5 1/m through the oxidizer.
5. Leave valves C and D in the sample positions.
6. Allow an excess of span gas to flow for at least 5 nrin. to
establish a span trace on the chart. Record the span reading in the
Unadj. Span column; and record the span knob setting.
7. Allow zero gas to flow for at least 5 min. to establish a trace
on the chart. Record the zero reading in the Unadj. Zero
column, and record the zero knob setting.
Adjustments
8. Check to make sure the rotameter is set at 3.0, and the flow through
the catalytic oxidizer is sufficient as in step 4. The toggle
valve on the air dryer should still be closed.
9. If the zero reading is not 5.0% of chart, adjust the Zero knob until
the reading is 5.0%. Allow 5 min. to establish the new zero trace
if an adjustment has been made.
10. Vent the zero gas from the catalytic oxidizer and turn on the span
gas, adjust the rotameter to 3.0 and adjust the span gas flow
through the dilution system so it exceeds the sample flow of the
instrument as done previously.
127
-------
11. Observe the scale reading and use the calibration conversion table
to convert to PPM.
12. The unadjusted span indication at this point must agree with the
span gas calibration within +5.0% chart. If it does, correct the
difference with the span adjustment. If it does not, a 6 point
recalibration must be performed. See the section pertaining to this
procedure. Also INVALIDATE all of the data back to the previous
acceptable span check.
13. Disconnect the span gas and reconnect zero gas, if necessary
adjust the zero control as in step 10.
14. Reconnect the sample probe line to the instrument, turn off the span
gas cylinder valve at the tank. Turn the catalytic oxidizer to
vent and adjust the flow through the oxidizer to about 0.5 1/m.
15. Make sure the instrument is still in the sample position.
a. Adjust the valve on the rotameter to a reading greater than 3,
such as 7.
b. Open the toggle valve at the base of the dryer.
c. Adjust the regulating valve at the base of the dryer until the
rotameter reads 3.
d. Adjust the cell to 25 psi.
16. Record the following on the "CO Instrument Check Sheet" in the
proper column.
a. Adjusted zero knob setting
b. Adjusted span knob setting
c. Span gas cylinder pressure
c. Zero gas cylinder pressure.
17. Inspect the strip chart recorder ink supply.
'128
-------
18. Inspect the strip chart paper supply.
19. Check and adjust the chart time synchronization.
20. Inspect the preceding 24 hours of recorder trace. Note the follovnng:
a. Trace is a straight line for several hours
b. Trace has square corners or is stepping.
c. Trace is noisy or erratic.
d. Trace has any other abnormal pattern.
e. Trace is not a straight line during zero or span tests.
f. Drift exceeds 1.0% of chart in 24 hours.
21. Recheck flowmeters, ink supply, time sync, chart supply, and water
trap.
129
-------
WEEKLY CHECKS
Inspect the pre-filter located on the inlet of the pump.
NOTE: This filter should not have to be changed more often
than once a month, but under extremely dirty conditions you
may find it necessary to change it more often.
Check the instrument and air dryer for leaks, in the following
manner.
a. Make sure the valves on the air dryer are in the sample position.
b. Close the toggle valve at the base of the air dryer.
c. Adjust the rotameter on the analyzer to read 3.0 center of ball.
d. Connect a line from the inlet of the analyzer pump to one of
the mass flow meters on the zero- dilution system the flow
should read between 2.5 and 3.0 liter/nn'n. if it exceeds 3.0 liters/min
there is a leak in the system from the pump through the analyzer.
e. If any leaks are found make necessary repairs and repeat zero
and span checks because the possibility exists that some ambient
air is diluting your system during zero and span giving erroneous
readings.
f. Make entries at the bottom of the daily sheet in the spa-ce
weekly checks of any inspections, adjustments, repairs, etc.
performed on the instruments.
.130
-------
Procedure for Six Point Calibration of MSA CO Monitor
Equipment Required:
a. Dilution apparatus
b. CO SPAN GAS CYLINDER (Certified)
c. Calibration curves for mass flowmeters
d. Necessary tubing and guages for hooking up to instrument.
NOTE: The calibration procedure should not be preformed before the
instrument has been operating at least 24 hours, the oxidizer should
be up to normal operating temperature, and after all the operational
tests have been completed and instrument operating acceptable.
Procedure:
Step I - Zero the instrument to 5.0% of chart, allow at least 5 min.
trace.
a. Selector valve in sample position
b. Span Gas Toggle valve closed
c. Zero air flow set at 4.0 liters/min.
d. Connect a line from the dilution apparatus
manifold to the inlet side of the pump.
Note: The toggle valve on the air dryer must be
closed and the dryers checked for leaks as indicated
in the weekly operator's procedure.
e. After zero baseline is established, turn the
selector valve to vent. Lower the flow through
the oxidizer to 0.5 liters/min.
Step II - Span the instrument to the concentration marked on the cylinder.
Allow at least a 5 minute trace.
a. Open span gas cylinder valve and the toggle valve on
the dilution apparatus to inject span gas to the instrument.
b. Adjust the cylinder pressure regulator and regulator valve
until a flow of about 4.0 liters/min is obtained.
c. Adjust span to correct % chart.
EXAMPLE: Span cylinder contains 40.0 PPM. You calculate the
correct % chart by the the following:
Span gas concentration X 2 + 5.0% baseline.
40.0 PPM X 2 + 5 = Correct Span Setting
d. Recheck the zero,adjust if necessary as done in Step I.
-------
Step III - Multi-point calibration
a. Span the instrument as in Step II
b. Turn the zero air selector valve on the
dilution apparatus to sample and prepare to
make 4 additional calibration points by
dilution of the span gas.
NOTE: When making dilutions make sure the
total flow of span gas and zero air is about
4.0 liters/min.
c. Example: Calculation of multi-point calibration
SPAN GAS L/MIN X CONCENTRATION OF SPAN GAS = PPM
ZERO AIR L/MIN + SPAN GAS L/MIN
3.0 LITERS/MIN X 40.0 PPM = 120 _ ,n
1.0 LITERS/MIN + 3.0 LITERS/MIN 3.0 -JU-
30.0 PPM X 2 + 5.0% ZERO = 65.0% Chart
d. Plot the 6 calibration points including the zero on
the calibration curve, also complete the calibration
log sheet.
132
-------
133
/-/->_ -^..'l
l_-ป v-' .
IJ LiLWTl'o/J
-------
EXTERNAL AUDIT PROCEDURE'S
FOR CO SPAN GAS
In order to check the long term calibration accuracy of the CO
span gas used at the A and C sites, an external audit procedure will
be followed. This procedure uses ccparate "C" cylinders of 35-45 PPM
CO in air that have been calibrated by Tom Clark of the Quality Control
Branch at NERC. Once a month one of these "audit" cylinders is sent
to L. A. to coincide with the routine monthly 5 point calibrations
using the "working" standard cylinders. Immediately after calibration
with the "working" standard, a complete recalibration with the "audit"
standard is performed. If the calibration curves differ by more than
+_ 5.0%, the "working" standard should be recalibrated against the "audit"
standard. The "audit" standard should then be returned to NERC for a
recheck of the standard calibration. Do not INVALIDATE the previous
month's data unless the "audit" and "working" standard disagree by
more than + 10.0%.
134
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CO Instrument Daily CHECK SHEET
City
Site Location
Site Number
Instrument S/N:
Date Last Calibration
Sample Rotameter Setting
Pressure Guage Reading _
Zero % Recorder Chart
Span % Recorder Chart
Span Knob Setting
Operator
a.
b.
/ c.
/ d.
/ 0.
/ f.
/ g.
/ h.
/ i.
Date
Sample Rotameter
Water Trap
Pressure Guage
Catalytic Oxidizer
Ai r Dryer
Silica Gel
Instrument Filter
Manifold & Probe
Unadjusted Zero % Recorder
Unadjusted Zero Knob Settina
Unadjusted Span % Recorder
Unadjusted Span Knob Setting
Adjusted Zero Knob Setting
Adjusted Span Knob Setting
Span Gas Tank Pressure
*Zero Gas Tank Pressure
Comments or Problems:
135
-------
O
3:
UJ
90
^ 80
70
60
50
40
30
20
10
NAME
LOCATION1.. .
(
SAMPLE ROTAMETER SETTING _
ZERO BASELINE.'(% RECORDER
SPAN (% RECORDER CHART) _
CALIBRATE. ADJUST. SETTING...
DATE ; |__ j :_J
S/N . . ; . ' ... i _ .
CHART)!.
CALIBRATOR
FSU #7
10
20
30
PPM CO
40
136
50
-------
READING STRIP CHARTS TO ESTIMATE r
HOURLY AVERAGE CONCENTRATIONS '
f
Instructions for converting strip chart traces to hourly
averages.
The ink trace on the strip chart represents the instantaneous
pollutant concentration at any given time. For this project,
all concentrations will be reported as hourly averages. The
conversion from instantaneous values to hourly averages must
be made manually, according to these instructions.
1. Obtain the strip chart pertaining to the pollutant.
Also obtain the calibration curve for* the instrument
which produced the strip chart.
2. If the previous day's data is to be converted, the strip
chart will still be on the chart recorder. In this case,
carry out a zero and span operation before converting
the drita in order to establish an updated zero baseline,
3. Obtain and fill in the top part of a blank hourly average
form.
4. Locate the two most recent calibrations on the strip
ซ
chart (usually today's and yesterday's) and determine the
percent of chart corresponding to 0 ppm for each. See
Figure 1.
5. Use a straight edge to draw a straight line from the first
zero (after adjustment) to the second zero (before
adjustment). This line will provide a'correction factor
to account for baseline drift of the instrument during
the time between the two calibrations. See Figure 1.
6. For each hour, consider th'e trace between the two hour
lines marking each hour's readings. For example, the trace
for the 8:00 o'clock to 9:00 o'clock hour will lie between
the line marked 0800 and the line narked^0900. Note that
military time is used so that the hours run from 2400 (same
as 0000) to 2300.
137
-------
7. Using a straight edge or a reticle, construct a line
on top of the trace and parallel to the chart division f
lines, such that the area bounded by the trace and the
two hour lines is equal on both sides of the line. See
Figure 2. A suitable reticle can be constructed as
>i,.
shown in Figure 3.
8. When the areas are judged to be equal, read the position
* of the line as percent of chart. Record this on the
data f orm.
9. Determine the baseline value in percent of chart for each ,
hour. Do this by reading the position of the straight line
drawn between the calibration points.. Use the value at
the center of the hour. See Figure 2.
10. Repeat this for each hour, recording the readings and baselin
values on the data form.
11. When all readings have been recorded, subtract the baseline
valuer from the readings and record the differences on the
data form .
12. Now, for each hour, convert the percent-of-chart values to
ppm valuc^ by using the calibration conversion table
*
prepared by the calibration team.
138
-------
CARI>
Z PIECES
nit:
FULL SIZE
Figure 3. Construction of reticle. Cut a notch in a
cardboard card as shown, put two pieces of transparent
tape over notch and draw a vertical straight line on
the tape with a ball point pen.
139
-------
*J~-, P.rj/t:/''/, j, ..
, .'/ / /: t . J.'* i .^i i- <, ,T , G
40:. i i '50 : 'GO ':'701
r.,*;,",~c '^P-T-']' .;".
'('"^fTl!;! Mi! :!
FIGURE 1
CONSTRUCTION OF^STRATCHT LINK FOR IJ.V.KLINM; CORRHCTION
140
-------
r
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HOUR
9-10
10-11
11-12
12-13
13-14
11E -\D-
ING
30.0
ซ
33.5
22.5
28.5
22.5
BASE-
LI NE
5.0
4.5
4.0
4.0
3.5
UIFFP:R-
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25.0
29.0
18.5
>%
24.5
19.6
+5 FOR
PPM CONV
30.0
34.0
23.5
29.5
24.0
PPM
J_LL_i
3
',1
O
FIGURE 2
ESTIMATING BASE LINT. AND AVERAGE VALUES FOR EACH HOUR
141 ^
-------
HOURLY AVERAGES
CITY
/o5
SITE NUMBER
'"". LOCATION
POLLUTANT
Co
DATE
OPERATOR
- HOUR
0-1
1-2
2-3
3-4
4-5
5-6
6-7
7-8
3-9
9-10
10-11
11-12
12-13
13-14
14-15
15-16
16-17
17-18
18-19
19-20
20-21
22
22-23
23-24
READING
/O. 0
9- 5
?.o
7.0
6.0
/o-o
/5.a
/?. o
ttf.o
ll.o
iS.o
W.o
If.o
/3.0
/5-o
2-^/^0
77.0
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IS.o
/>f.o
ttj-o
/5-o
/^.o
ZERO
BASELINE
5.o
I
I
V
.. . ... _ _ I/O
DIFFERENCE
*
5.o
^.5
3. o
7.o
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5. o
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ADD
+ 5
ppm
7.5
^.0
A 5
/. 0
.5
?.S
So
7-0
4". 5 '
ฃ.0
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V-5
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75
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5.0
^ 5
*+,s
So
I 3.^
-------
General Description
For analysis of total sulfur, this instrument uses the flame photometric
detector, which detects the 394 nm-centered band emitted by sulfur-containing
compounds in a hydrogen rich air flame. High specificity is achieved by the
geometric arrangement of the burner that optically shields the photomultipljer
tube from the primary flarne and by use of a narrow bandpass interference filter.
Most of the operational problems in the past with FPD analyzers has been
attributed to air sample flow fluctuations. With the addition of a dilution
air orifice inlet filter, better known as the C.F. Smith modification, this
problem has been corrected.
Numerous ratios of hydrogen to air sample can be used i"n FPD analyzers.
The only reason to increase the hydrogen to air sample ratio is to decrease the
sensitivity of the FPD detector to flow variations.
For the California study, we will use a hydrogen flow of 140 cc/min arid
an air sample flow of 175 cc/min. The recorders will be connected to the
0-1 volt connecting posts on the rear panel (red +, black -) and operated on the
0 to 1 volt range. It is necessary to use a recorder that has zero offset
capabilities (Esterline Angus Speed Servo II).
Although; the analyzer has both a metered sample inlet and a-direct sample
inlet we will use only the direct sample air inlet and monitor the air sample
flow periodically with a 0-300 cc range mass flow meter.
It is important that you use a short (2-foot) length of tubing that has
never before been exposed to SOp to connect the analyzer to the drying tower
(zero scrubber). If 3'ou accidentally expose this tubing to S0o> you will have
to replace it with a new unused section.
144
-------
Operating Information
I Front Panel Description
(1) Hydrogen Flow Control Knob; This control is located at the base
of the H2 rotameter. It is used to set the flow rate of the H2 gas.to the
photometric detector. CAUTION: This is not a shut-off valve. When
turning the hydrogen off, close the flow control until the ball in the
rotameter just comes to zero. If the flow control knob is turned beyond
this point, the valve may be damaged.
(2) Sample Air Flow Control Knob: This control knob, located below the
air flow rotameter, adjusts the sample air flow to the flame photometric
detector.
(3) Power Switch: The power switch is located in the lower left area
of the panel and when in the "on" position, it provides power to the
instrument from the AC power source.
(4) Ignition Button: This button, located below the H_ flow control
knob, is a momentary contact push button, operated off the 6.3 volt
circuit to energize the glow plug. It is used to ignite the hydrogen
and air mixture in the burner chamber of the detector.
(5) Zero Control: This control, located just below and to the left of
the panel meter, is used to adjust the zero reading when calibrating the
instrument. A mechanical locking feature is part of this control and it is
operated by rotating the base of the knob clockwise to lock and counter-
clockwise to release.
(6) Span Control: This control, located to the right of the zero control
i and below the panel meter, is used to adjust the scan when calibrating the
instrument. It has the same mechanical locking feature as the zero control,
145
-------
II Rear Panel Description
(1) Power Source Lead: The power-source lead is provided for connection
to a 115 VAC, 60 HZ source. It is located in the lower left corner.
(2) Electrical Outlets: Two electrical outlets (115v) which are on/off
controlled by the analyzer power switch are provided for the external
vacuum pump and recorder. The pump may be connected to a separate source
if desired.
t3) Connection Posts: The one volt (red) and ground (black) connection
posts are on the left side of the panel for use with a strip chart
recorder. This is the nonlinear output connection that we will use.
Don't use the 1 volt linearized connecting prsts.
(4) Dilution Air: Dilution air is furnished to the analyzer through
an orifice inlet near the center of the panel. The 4 liters/min. flow of
dilution air is provided by the ^18 hypodermic needle which is lodged
in the rubber septum which caps the dilution inlet pipe and is connected
to a 37 mm mi Hi pore filter holder.
(5) Vacuum Outlet: Located directly below the dilution inlet is the
vacuum outlet from the analyzer to which the external vacuum inlet hose
is attached.
(6) Sample Air Inlet: Located to the right of the electrical outlet
plugs is the direct sample air inlet. Don't use the metered air sample
inlet.
146
-------
I
Calibration and Set-Up, k
I Set-up
(1) Connect the analyzer to a 115 VAC, 60 HZ power source, Plug the
external vacuum pump into the electrical outlet on the back of the analyzer
which is controlled by the power switch (a separate 115 VAC, 60 HZ power
source may be used). Use 1/4" tubing to connect the pump air intake side
to the vacuum outlet.on the rear panel.
(2) Connect a strip chart recorder that has a zero offset capability to
the 0-1 volt nonlinear connecting posts on the rear panel (see II (3)
Operating Information). Use the recorder 0-1 volt range.
(3) Connect the regulated hydrogen source to the hydrogen inlet on the
rear panel in the upper right hand corner.
(4) Fill a drying tower with soda/lime and connect it to the instrument
with a two-foot length of new tubing that has never before been exposed
to S02 to the direct inlet (see n (6)) Operating Information).
IL Calibration
0) Turn on power. Allow the analyzer to warm up for 15 minutes.
(2) Ignite the burner as per instructions at the NERC.
(3) Roughly adjust the Hฃ flow to 140 cc/min and the air sample flow
to 175 cc/min and allow the analyzer to warm up for at least 4 hours.
(4) Adjust the hydrogen generator output pressure to 20 psi.
(5) Set the recorder range selector to 0-1 volts, short out the input
and adjust the zero offset to 5% chart.
(6) Disconnect the drying tower from the two-foot length of tubing.
(7) Connect an accurately calibrated 0-300 cc/min,mass flow meter to the
two-foot length of tubing that is connected to the direct inlet of the
analyzer.
147
-------
(8) Adjust the H2 flow to 140 cc/min and the air sample flow to 175 cc/min.
These adjustments must be accurate and precise. Use the supplied H2 curve
to determine the H2 rotameter setting for this flow rate.
(9) Disconnect the mass flow meter and reconnect the drying tower.
(.10) Allow the analyzer to sample zero air for one hour, then carefully
reset zero to 5% chart using the zero adjust knob.
(11) Disconnect the two-foot length of tubing and the drying tower from
the direct inlet air sample of the analyzer.
(12) Connect the direct inlet air sample to a . calibrator manifold using
a length of Teflon tubing that is the same length as the tubing that
will be used to connect the analyzer to the air sample mani.old. Generate
a sample concentration of .080 ppm S0?. After the analyzer stabilizes
on this concentration, adjust the span control to make the recorder pen
read 58.0% chart. NOTE: DO NOT CALIBRATE THROUGH THE AIR SAMPLE LINE.
(13) Generate the following concentrations of SOg and record the analyzer
response to them: .080, .054, .0429, .0365, .0256, .0187. Compare these
values to the supplied calibration curve. If it doesn't match, recheck
the H2 and air sample flows. This curve should repeat within 0.5% chart
at the span point of .080 ppm.
(14) When running a calibration check after the initial set-up and
calibration, generate a .080 ppm SOp concentration and observe and record
the analyzer response before any adjustments are made.
Daily Instrument Operation
To assure accuracy and uniformity of the data, the following operational
procedures must be carried out by the instrument operator each day. It is very
important that they be performed exactly as directed and in the directed sequence.
Record all readings requested on the daily check sheet.
'148
-------
(1) Short out the recorder input and adjust the recorder pen to 5% chart.
(If you use Ester!ine Angus recorders this can be done with the red range
selector switch in the upper right hand corner.)
(2} Record the unadjusted hydrogen generator output pressure on the daily
check sheet.
C3) Record the unadjusted hydrogen flow on the daily check sheet. Convert
the rotameter readings to cc/min using the rotameter calibration chart.
(4) Remove the sample line from the direct input port. Connect one end
of the two-foot zero air line to the direct input port and connect the
other end to the output port of the mass flow meter. After the mass flow
meter reading stabilizes, record the unadjusted air sample flow, in cc/min,
from the mass flow meter calibration curve, on the daily check sheet.
NOTE: WE WILL NOT USE THE METERED INLET.
(5) Adjust the air sample flow to 175 cc/min again using the mass flow
meter calibration curve for this value.
C6) Disconnect the mass flow meter from the two-foot zero air line and
connect it to the drying tower (zero scrubber).
(7) Adjust the hydrogen generator output pressure to 20 psi.
(8) Adjust the hydrogen flow to 140 cc/min (46 on the h^ rotameter at 20 psi).
(9) Allow the-analyzer to sample zero air for 30 minutes. Record on
the daily check sheet the unadjusted zero value in per cent chart.
(10) Disconnect the zero line and drying tower from the direct input port
and reconnect the sample line.
(11) Check water level in the hydrogen generator and refill when it is
half empty. Be sure there is enough water to last over weekends and
holidays.
-------
(12) Replace the miTHpore filter on the dilution air orifice
(hypodermic needle) every two weeks.
Rotameter Calibration
Center of Ball Readi'i.i, *
at 20 psi
49
48
47
46
45
44
43
42
157.0
151.9
146.7
140.0
135.9
132.3
127.2
122.5
ccm
if
ii
11
ii
n
ii
u
150
-------
5 *
N N^
x >
<
-------
DAILY INSTRUMENT OPERATION BENDIX T.S.
To assure accuracy and uniformity of the data, the following
operational procedures must be carried out by the instrument operator
each day. It is very important that they be performed exactly as
directed and in the'directed sequence. Record all readings requested
on the daily check sheet.
(1) Short out the recorder input and adjust the recorder pen to 5%
chart. (If you use Esterline Angus recorders, this can be done
with the red range selector switch in the upper right hand corner.)
p ae$iปfie
(2) Record the unadjusted hydrogen generator^ output on the daily check
sheet.
(3) Record the unadjusted hydrogen mass flow meter reading on the
daily check sheet.
(4) Switch the sample flow switch to the "meter" position. After one
minute record the unadjusted sample flow on the daily check sheet.
Readjust the rotameter to 55. Return the switch to the "meter by-pass"
position.
(5) Disconnect the sample input line from the analyzer. Connect a
drying tower that is filled with soda lime to the sample inlet port
of the analyzer.
(6) Adjust the hydrogen generator output pressure to 40 psi.
(7) Adjust the hydrogen flow to 200 cc/min. on the mass flow meter.
(8) Allow the analyzer to sample zero air for 30 minutes. Record
on the daily check sheet the unadjusted zero value in percent chart.
(9) Disconnect the drying tower from the analyzer and reconnect the
sample line.
(10) Recheck the hydrogen flow and sample flow to make sure they are
200 cc/min. and 55. Readjust them if necessary.
i
J153 :
-------
SET-UP BENDIX TOTAL SULFUR ANALYZER
(1) Connect the analyzer to a 115 VAC, 60 Hz power source.
(2) Connect a stri'p chart recorder that has a zero offset
capability to the 0-10 MV connecting posts on the front
or rear panel. The multirange analyzer S/N 27949-2 will
be operated on the 0-5 MV recorder r,$.ng,e with the
selector switch in the .2 ppm position. The 0-1 ppm
fixed range analyzer S/N 27949-1 will be operated with
the recorder range of 0-1 MV. This will make both analyzers
have a 0-.095 ppm scale on the recorders. The fixed
range analyzer may have a somewhat noisier trace but this
will be tolerated to achieve equal operating scales.
(3) Connect a 0-300 cc/min. mass flow meter in the H? line.
(4) Connect the regulated hydrogen source from the mass flow
meter to the inlet on the rear panel.
(5) Connect the MSA filter assembly to the dilution air
inlet on the rear panel.
(6) Adjust the recorder zero to 5% chart.
(7) Precede to step 3.3-b. Turn-on procedure.
(8) Adjust the hydrogen output pressure to 40 psi. at a flow of
200 cc/min.
j 154
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SECTION 3 OPERATION
3.1 GENERAL
This section contains the operational instructions for the Total Sulfur
Analyzer. These instructions include the identification and function of
the controls and indicators, the turn-on procedure and initial calibration,
operating procedures, routine calibration, and the turn-off procedure.
3.2 EQUIPMENT CONTROLS AND INDICATORS
The controls and indicators of the Total Sulfur Analyzer are illustrated
In Figures 7-2 and 7-15 and listed in Tables 3-1 and 3-2. Table 3-1 presents
the indicators in reference number sequence defining name, and function.
Table 3-2 presents the controls in reference number sequence, defining
name, position, and function. Prior to energizing the equipment, it is
recommended that the operator become familiar with the function of each
indicator and control.
3.3 TURN-ON PROCEDURE AND INITIAL CALIBRATION
Complete the following steps in the sequence indicated to turn on the
equipment and complete the initial calibration:
b. Ensure that the output regulator on the hydrogen generator is set
for an output of 40 psi.
c. Set the POWER switch to the ON position and verify that the POWER
indicator illuminates, the cooling fan is operating, and the
FLAME OUT indicator illuminates.
d. Set the PUMP switch to the ON position and verify that the
evacuation pump is operating. Evacuation pump operation may
be determined by placing the SAMPLE FLOW selector switch in
the METER position and observing and indication on the SAMPLE
flowmeter.
e. Momentarily depress the IGNITE switch and note the indication on
the mass flowmeter in the H2 line. Ensure that the indication
is as specified on the base of the rotameter. If it is not, adjust
the HYDROGEN valve on the front panel to obtain the correct reading
(200 cc/min.).
155
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TABLE 3-1 TOTAL SULFUR ANALYZER INDICATORS
FIGURE 7-2
CALL OUT NAME FUNCTION
1 POWER indicator (DS1) Indicates presence of primay power
2 PUMP indicator (DS2) Indicates presence of pump power
3 FLAME OUT indicator (DS3) Indicates'Vlame is extinguished in the
detector cell
4 PPM SULFUR meter (Ml) Indicates concentration of total sulfur(TS
5 HYDROGEN rotameter Indicates hydrogen flow
6 SAMPLE flowmeter ' Indicates sample flow rate to the
detector cell
156
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TABLE 3-2 TOTAL SULFUR ANALYZER CONTROLS
FIGURE 7-2
CALL OUT
NAME
POSITION
8
9
10
11
12
13
14
ure 7-15
ure 7-15
ure 7-15
SPAN adjustment As required
Control (R15)
ZERO adjustment As required
Control (R16)
POWER switch (SI) ON
PUMP switch (S2) ON
IGNITE switch (S3) Momentarily
Down
SAMPLE FLOW
METER
Selector switch (S4)
METER
BYPASS
ADJUST needle
Valve
HYDROGEN
Needle Valve
NONSULFUR
SUPPRESSION
adjustment control
(R17)
EXPONENT ADJ
Control (R18)
EXPONENT ADJ.
Control (R20)
As required
As required
As marked
As marked
Factory
adjustment
Used as a find adjustment to calibrate
system to a known sulfur concentratior
Electronically zeros the instrument
with burner flame out.
Applies primary power to instrument.
Applies power to evacuation pump.
Used to initially ignite hydrogen in
detector cell after flame out.
Connects SAMPLE flowmeter into flow
path.
Bypasses SAMPLE flowmeter.
Used to adjust the flow rate of the
dilution air.
Used to adjust the hydrogen pressure
at the input to the capillary to
assure the correct flow.
Offsets the background luminescence
of the flame with no sulfur into the
instrument.
Adjusts the voltage applied to the
photomultiplier tube in the detector
cell (coarse span adjustment).
Establishes the exponential curve
for the exponential amplifier.
157
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158
-------
NOTE
THE HYDROGEN mass flowmeter reading
should be 200 cc/min. at 40 psi.
WARNING
Hydrogen is highly explosive and extreme
caution must be exercised when connecting
the bubblemeter. Vent the output of the
bubble flowmeter (hydrogen) to a safe
venting area.
f. Set the SAMPLE FLOW selector switch to the METER position. Note
that the indication on the SAMPLE flowmeter is an specified on the
supplied data sheet. If it is not, vary the ADJUST needle valve
to obtain the correct reading.
NOTE
This SAMPLE flowmeter indication 55 corresponds
to a flowrate of approximately 170 cc/min.
g. Set the SAMPLE FLOW selector switch to the METER BYPASS position,
NOTE
Allow a minimum of thirty minutes warm up
time to allow the temperatures to stabilize
prior to proceeding to the next step.
159
-------
3.3.1 ZERO ADJUSTMENT
Adjust the Total Sulfur Analyzer for electronic zero by
performing the steps outlined below, with the flame
a. Inject zero gas into the instrument via the SAMPLE bulkhead connectt
b. Adjust the ZERO adjustment control for a zero indication on
the recorder at 5% chart. ^ ., ,
c. Depress the IGNITE switch until the FLAME OUT indicator
is extinguished.
d. Adjust the NONSULFUR SUPPRESSION adjustment control for a
zero indication on the recorder.
e. Operate the instrument on zero gas for 30 minutes to ensure that
there is no zero drift.
3.3.2 SPAN ADJUSTMENT
Calibrate the Total Sulfur Analyzer by performing the steps outlined
below. All switches remain in the same position as 3.3.1 step e except as
noted.
a. Connect the SAMPLE input to the calibration system and adjust
it to obtain a .080 ppm concentration of S0~.
NOTE
Ensure that the flowrate of the span gas source is
greater than 300 cc/minute to prevent further dilution
of the span gas. Also, ensure that the span gas is
routed via an open manifold to prevent pressurization
of the input to the instrument.
b. Allow the instrument to stabilize for five minutes and adjust
SPAN adjustment control to obtain 85% chart on the recorder.
160
-------
c. Operate the instrument on span gas for 30 minutes to ensure
that there is no calibration drift.
d. Check linearity by generating the following concentrations of
S02 and record the analyzer response to them: .054, .0429,
.0365, .0256, and .0187.
3.4 OPERATING PROCEDURES
Prior to operating the Total Sulfur Analyzer, the turn-on procedure
and initial calibration must be performed as outlined in Section 3.3.
Perform the following steps to measure the total sulfur concentration
in an air sample:
a. The SAMPLE FLOW selector switch should remain in the .METER BYPASS
1'"" fฐr normal operation.
b. The sulfur concentration is indicated in ppm on the strip chart
recorder.
3.5 ROUTINE CALIBRATION
The Total Sulfur Analyzer routine calibration should be performed
every month. Depending upon the application, it may be desirable to
check the calibration at shorter intervals. Normally, the user will
determine the calibration interval based upon the monitoring assignment.
The routine calibration i-s performed by completing the zero adjustment
and span adjustment as described in subsections 3.3.1 and 3.32, respectively,
3.6 TURN-OFF PROCEDURE
Normally, the Total Sulfur Analyzer will remain on for extended periods
of time. In the event it becomes necessary to turn off the unit, proceed
in the following manner:
a. Set the POWER switch to the OFF position.
b. Set the PUMP switch to the OFF position.
NOTE
If the Total Sulfur Analyzer is to be left off for an
extended period of time, close the valve on the hydrogen
cylinder.
161
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PACKET A-MET
MRI MECHANICAL WEATHER STATION
CATALYST STUDY
- CONTENTS -
Quantity Item
1 Operating Instructions for Mechanical Weather
Station
1 MRI Instruction Manual for Mechanical Weather
Station
1 Weather Data Reporting Procedure
140 SAROAD Hourly Data Forms
NOTE: For the Sulfate Study it is possible that it will be necessary
to look at wind direction with respect to beginning and end
of sampling periods. If the sample on one side is to be
considered a background sample, then the wind record must be
examined to see that the disection did not shift to bring the
thruway pollution to it for any appreciable time. Hourly
direction alone could mask this occurrence.
163
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OPERATING INSTRUCTIONS FOR
MECHANICAL WEATHER STATION
The MRI mechanical weather s+^tion will be installed at
one of your sites and oriented by EPA personnel. The station
operator will be responsible for maintaining the weather
equipment and for reporting the data.
The weather stations used in the Smelter Project will
record wind speed and wind direction. Temperature information
will not be used, and need not be transcribed to SAROAD data
forms. The weather recorder is mechanically operated, but
the chart drive is driven by batteries at 20 mm per hour.
The station operator should read sections 3.2, 3.4,
3.4, 3.5, and 5.1, and Figures B and C in the Instruction
Manual to become familiar with the instrument. EPA personnel
will provide further instructions on the operation of the
instrument.
Maintenance-Daily Checks
1. Orientation. Check the orientation marks on the
weather station to be sure it has not moved.
2. Time sync. Rotate the direction vane all the way
around once. This will put a straight line across the
chart. Write the correct local time near this line.
Then, check if the line corresponds with the time marks
printed on the chart. If the error is 10 minutes
or more, move the chart forward or backward to synchronize
the chart to the correct 1 oca! time.
3. Identification. Each day record the date, site, location,
and your name on the chart.
4. Check to make sure the writing scrolls are uncaged,
(lowered), and recording properly. The chart drive
should "tick" when operating.
Other Maintenance
5. Batteries. The 2 chart drive batteries are to be replaced
every 2 weeks. You will be provided a supply of standard
"D" Size cells. Access to battery holder is on the bottom
of instrument. Record date of battery replacement on
the instrument so you will know when replacement is
again due.
\ t'.
-------
6. Data. .Cut the chart weekly and submit the data.
See "Weather Data Reporting Procedure."
7. Chart paper. Chart paper must be replaced when necessary.
Check the chart supply every day to determine when
replacement is necessary. Be sure to raise (cage)
the recording scrolls by pulling out the caging lever
whenever you service the chart recorder. And lower
(uncage) when finished.
8. Call EPA headquarters if any operational problems are
encountered. Possible problems are chart drive gain-
ing or losing time, wind vane or anemometer bearings
developing friction (binding), orientation change due
to vibration or buffeting from high winds.
165
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Weather Data Reporting Procedure
The success of the entire Catalyst Study is dependent
on the validity of the data it produces. In this study,
it is necessary that the data be legally valid. Thus it is
imperative that the instrument operator be particularly
meticulous and accurate in reporting the data to EPA, and in
identifying any data of questionable validity. The following
instructions must be followed exactly and completely:
1. Only the Wind Direction and Wind Speed meed by
reported.
2. All data from continuous weather instruments is to
be submitted in the form of hourly averages determined
by visually integrating the instantaneous strip
chart data.
3. All data is to be submitted on SAROAD Hourly Liata Forms.
4. Data is to be submitted each week, preferably on
Friday.
5. Since the weather recorder is located outdoors,
it will be necessary to remove the chart from the
recorder and bring the chart indoors to transcribe
the readings. You may allow the chart to remain
in the weather recorder for a full week, then cut
it and transcribe the entire weeks' data at once.
Alternatively, we would recommend that the chart be
cut each day. After the day's data has been tran-
scribed, the daily sections can be taped together
in the original sequence and submitted weekly with
the other data. This way, the operator can keep
his data forms up to date each day and avoid a
week's backlog of data to transcribe.
Prompt submission of the data from each site is
necessary so that all the data can be validated and
reported on schedule.
Always cut the chart at the 2400 hour mark on the chart.
6. Wind Speed. Wind speed is recorded by the weather
station as "wind run" which is the integrated value
of wind speed. Therefore, wind speed data is transcribed
differently from continuous pollutant readings.
166
-------
6.1 Each line on the "WIND RUN" section of the chart
represents 1 mile. For a one-hour period, each
line represents one mile per hour, and a complete
traverse of the chart in one hour represents 10
miles per hour. Thus, the number of chart division
lines passed in one hour is the wind speed in
miles per hour.
6.2 For each hour, count the number of chart divisions
crossed in that hour. Try to estimate to 1/2
chart division (1/2 mile per hour).
6.3 Hrite the number of chart divisions (wind speed)
on the chart for each hour, trying not to obscure
any of the record.
6.4 Fill in the top part of a SAROAD Hourly Data
Form as shown in Example 1, WIND SPEED.
6.5 Transfer the wind speed values for each hour from
the chart to the SAROAD form using the same format
as for pollutant data. Note that the decimal is
in front of the last digit. For example, a wind
speed of 2 miles per hour is recorded as 20, and
4.5 miles per hour is 45. Double check your
readings to make sure no mistake was made in
transferring the numbers or filling in the Form.
NOTE: Never put data from 2 different months on
the same SAROAD Form; use 2 SAROAD Forms, one for
each separate month.
7. Wind Direction.
7.1 Determine the prevailing disection for each hour.
When the direction is steady or shifts quickly from
one direction to another, the prevailing direction is
the one which occurred longest during the hour.
When there is continuous change the midpoint can be
used as prevailing. When there is a changeable
period and a steady period in 'the same hour more emphasis
should be given to the study portion of the hourly record.
7.2 Usually values can be read to half a chart division.
On the MRI chart a division is 30 so values should be
accurate to 15ฐ. However, with wind the variation
is often so continuous that one person's estimate of
the prevailing direction may easily be more than a whole
division different from another person's estimate.
360ฐ is used for north, 000 is used for calm, do not
use 000 for north.
167
-------
First line (N) 360 degrees
second line 30 "
third line 60
fourth line (E) 90
fifth line 120
sixth line ' 150
seventh line (S) 180
eighth line 210 "
ninth line 240 "
tenth line (W) 270
eleventh 300 "
twelvth 330
last line ' (N) 360
CALM 000
7.3 For any hour during which the wind speed was less than
2_ MPH, the wind is considered to be CALM. CALM wind
direction should be reported as 000 on the SAROAD Form.
7.4 Fill in the top part of a SAROAD Hourly Data Form as
shown in Example 2, WIND DIRECTION.
7.5 Transfer the wind direction values, in degrees, for
each hour from the chart to the SAROAD form using the
same format as for pollutant data. The decimal is
after the last digit so 120 degrees is recorded as 120.
Double check the form, when you finish, to make sure
no mistake was made in transferring the numbers or in
filling in the form.
NOTE: Never put data from 2 different months on the
same SAROAD Form; use 2 SAROAD forms, one for each
separate month.
8. To insure legal validity of the data, it is necessary that the
local instrument operator certify that the data submitted is
correct to the best of his knowledge. This requires that he:
(a) Permit no unauthorized persons to contact or have
access to the monitoring instrument.
(b) Personally carry out all required operational and
maintenance procedures.
(c) Personally carry out all data reporting procedures.
(d) Maintain custody of all data and data forms and
permits no unauthorized person to handle or have
access to this material.
768
-------
(e) Sign full name to the bottom of each SAROAD Data Form
thereby certifying validity and uninterrupted custody of
the data and data forms.
(f) Personally mail the data forms and materials to EPA-RTP
by registered mail.
9. If the instrument operator is absent, the alternate operator
must also carry out the above steps. If both operators worked
on the project, both must sign the forms.
10. Each week, sign the bottom of each of the following forms and
mail to EPA-RTP BY REGISTERED MAIL, DELIVER TO ADDRESSEE ONLY:
Completed SAROAD Hourly Data Forms (normally 2)
Strip Chart for the period covered on the other
forms
11. Use the pre-addressed mailing envelopes and send by registered
mail to:
Charles Rodes
Environmental Protection Agency
NERC, L-116, EMB, QAEML
Research Triangle Park, N.C. 27711
169 .
*l
-------
i '
iJoto: Do termini rig Average Wind Direction
Determining an average wind direction for an hour is somewhat
different than delorrnin'ing an average pollutant concentration. This
is because lie wind direction is really a vector instead of a simple
arithmetic value. For example, a half hour east wind (90ฐ) plus a
half hour west \'irv (270ฐ) average to zorp_wind for the hour, not
south (1GOJ) as a p~ir;;;.le averaging procecure would indicate. (See
Figure 1). Also, <.\ III' wind (45ฐ) and a NW wind (315ฐ) would produce
a North (2GO!i) average direction, not South (180ฐ) as the simple
averaging procedure would indicate. (See Figure 2).
Consequently, the procedure for determining hourly average wind
direction must be changed slightly, as follows:
1. If the wind direction changes less than 90ฐ during the
hour, continue to use the simple procedure of estimating
the average direction from the chart. Remember., however,
that a wind w'n'ch changes from fill to NE (or vice versa)
will appear tc change from the extreme left of the chart
(or vice ver^a), but the average direction will be northerly.
2. If the wind appears to shift by more than 90ฐ during the
hour, simply choose the direction which occurred for the
longest tine during the hour, and ignore the other directions-
Do not try to get an average direction. (If you are sure
that you understand how to average vectors, you may try
to determine the vector average. Otherwise, just select the
predominant direction without trying to get an average.)
170
-------
1/2 hour WEST wind
W
1/2 hour EAST wind
.E
Average wind
is zero
Figure 1
N
1/2 hour NW wind , AVERAGE wind is North
W
1/2 hour NE wind
Figure 2
.' 17]
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,173
-------
SAROAD HOURLY DATA FORM INSTRUCTIONS
Coding Carbon Monoxide (CO) Concentrations
f
1. The SAROAD Hourly Data Form is an approved form for the recording of data
observed on averaged at intervals of less than 24 hours. In this case
the form-is to be used for recording hourly averages of Carbon Monoxide
observations.
2. Entries on the upper left of the form (See example form) provide identificaton.
These are:
(1) Agency - group recording the observations.
(2) City - city in which instrument is operated.
(3) Site - specific location of the sampler.
(4) Project - EPA, 1974 Catalyst Study.
(5) Parameter observed - Carbon Monoxide
(6) Time Interval - Hourly
(7) Method - Nondispersive Infrared
(8) Units of Observation - parts-per-million
3. In the upper right hand corner of the SAROAD Hourly Data Form appears three
lines of blocks for coding identifying information. These correspond to
the card columns of the numbers beneath each box when punched on an 80
column Hollerith card. EPA will assign codes for the first line of blocks
to the reporting agency when Site Identification Forms are initially sub-
mitted. They consist of a two-digit code for state (SS), a four-digit
code for the area of the state in which the sampler is located (CCCC), and
a three-digit number specifically identifying the site (XXX). For the
remaining two lines of blocks the codes for this study are:
(1) Agency - A
(2) Project -
(3) Time - 1
(4) Year - 1974
(5) Month - As appropriate, 01:to 12
a. July - 07
b. August - 08
-------
c. September - 09
d. October - 10
e. November - 11
(6) Parameter Code - 42101
(7) Method - 11
(8) Units - 07
(9) DP - 1
On the body of the form, the two-block first column, "Day", is the
calendar day of the month (e.g., 01, 02). "ST HR" (start hour) calls
for either 00 or 12 to denote the starting hour for which data on that
line are recorded. Two lines are used for each day's observations. The
first line gives "00" (midnight) for "ST HR" and lists the a.m. observations
Record the hourly averages in the "Rdg" columns: "Rdg 1" would be for either
the 0 to 1 hour reading or the 12 to 13 hour reading; "Rdg 2" would be for
either the 1 to 2 hour reading or the 13 to 14 hour reading; etc. In
entering the hourly averages, the decimal point is located between the first
and second column.
For Example:
40.5 ppm would be entered as 4 I 01 51
6. Forms should be submitted weekly with the strip chart for the period of
data recorded on the form. These should be mailed to:
Environmental Protection Agency
Division of Atmospheric Surveillance
Air Surveillance & Field Studies Branch
ATTN: Catalyst Study
Research Triangle Park, N.C. 27711
175
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51
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DATA REPORTING PROCEDURE
1. Data is to be submitted each week, on Friday.
2. We strongly urge that the operator determine the hourly averages for
the previous day's data EACH DAY, and keep his data forms up-to-date
each day. He should never allow a backlog of several day's data to
accumulate. Prompt submission of the data from each site is necessary
so that all the data can be validated and reported on schedule.
3. Unroll the last day's strip chart from the recorder and lay it out on
the table in front of the recorder. This can be done without cutting
the chart paper off the roll. For convenience, it is suggested that
the operator work on the data only up to yesterday's zero baseline
check. This avoids the need to use today's baseline which may still
be on the face of the recorder. Since the zero baseline checks are
used in the conversion of the readings to hourly averages, it will
be necessary to work on the data in the block of hours between two
zero baseline checks. These blocks of hours normally fall on two
different dates, so care must be used to make sure that the readings
are correctly entered on the Hourly Average Sheets, each of which covers
only one date. Thus, if the baseline checks v/ere at 10:00 a.m. each day,
the 24-hour block of data would extend from 11:00 a.m. one day to 10:00
a.m. the next day, and would be recorded as hour 11 to hour 23 on one
Hourly Average Sheet and hour 0 to hour 10 on the next Hourly Average
Sheet.
4. Refer to the instructions "Reading Strip Charts to Estimate Hourly
Average Concentration" and proceed to convert the chart readings to
hourly averages as directed in those instructions. Record the hourly
averages on the Hourly Average Sheet, taking care to insure that the
date on the sheet agrees with the date and time the readings were obtained.
5. If more than 1/2-hour of data readings are missing or invalid on the strip
chart for any hour, do not enter an hourly average for that hour. Instead,
indicate on the Hourly Average Sheet why there is no reading. For each and
every hour there must be an hourly concentration average or a reason why not.
Be as specific as possible, for example: "zero baseline check," "pump mal-
function" or "recorder pen clogged."
6. Transfer the hourly averages form the Hourly Average Sheet to the SAROAD
Hourly Data Form. Refer to the SAROAD Hourly Data Form instructions.
Double check the SAROAD Form, ad it is easy to make a mistake on it.
7. Each Friday, mail in the Following:
Completed Hourly Average Forms (normally 7)
Completed SaROAO Hourly Data Form (normally 1)
Completed Catalyst Instrument Check Sheet (normally 1)
Strip Charts for the period covered on the other forms
179
-------
Use the pre-addressed mailing envelopes or send to:
Catalyst Study
Environmental Protection Agency
Division of Atmospheric Surveillance
Research Triangle Park, N.C. 27711
180
-------
LACS VALIDATION PROCEDURE*
1. Compare printout data with strip chart. Check at least 5 hours of
each day's data and all values over .1 ppm. Acceptable tolerance
is +_ .01 ppm.
2. For all readings which do not agree within the tolerance, check hours
both before and after to determine the extent of the invalid period.
3. Determine the correct values and fill in a SAROAD hourly data form
with the corrected values. Be absolutely sure that the city and
site number are correct on the correction sheet. Sign your name
to thcTcbTrection sheet, and work the top "CORRECTIONS." A separate
SAROAD form must be used for each city and for each month.
4. If printout readings exist for which there is no valid strip chart
readings, the data must be deleated. To do this, put 9999 in each
hour block on the SAROAD form for which the data is to be deleated.
Again, work the top of the form "CORRECTIONS" and sign your name.
A separate SAROAD fotm must be used for each city and for each month.
5. On printout copy, enter all corrections by crossing out incorrect
reading and entering corrected reading. Mark all deleations by
crossing out the deleated value with a heavy black mark. For all
missing or deleated data, enter the explanation or reason. Look
up the daily average sheets for this purpose.
6. Hhen printout page is completely validated, sign name to page and
mark it " / VALIDATED."
*This procedure is to be followed by the data clerk at NERC in validation
of the computer printouts as compared to the SAROAU forms.
181
-------
"orm Completed
ENVIRONMENTAL PROTECTION AGENCY
National Aercwetric Data Bank
Research Triangle Park, N. C. 27711
SAP.OAO Sits identification Form
Charles E. Rodes Dgte 6/25/74
.New
Revised
TO CL CC.Vr'LnLD BY THE r.E?CRT!NG AGENCY
|Aj California Catalyst Study - 02
< 14-361
^/-Stl
0 0
State
Los Angeles
Project
City Name (23 characters)
Los Angeles
County Warns (15 characters)
City Population (rirht justified)
0 2 fs jT~ 6 f 0 0 0
52 53 54 5b 53 b/ bd b!*
Longitude
Dcg. Mm. Sec.
I I '.V !l ]l | 8.J 2 7 ! 2 ] 3 j
CO 1. 1 (.? b3 (,
Action
OMB No. 15S-R0012
Approval expires 6/30/76
I1 13
80
(over)
182
-------
SAROAD Site Identification Form (continued)
O
rO BE COMPLETED BY THE REPORTING AGENCY
DO NOT WRITE HERE
(F).
11300 Waterford St.
Sampling Site Address (41 characters)
Check the ONE
major category that
best describes the
location of the
sampling site.
1.0 CENTER CITY
Address, continued
Next, check the subcategory
that best describes the domi-
nating influence on the sampler
within approximately a 1-mile
radius of the sampling site.
2. DO SUBURBAN
3, EH RURAL
4. EH REMOTE
Specify
units
1. Industrial
2. Residential
3. Commercial
4. Mobile
1. Industrial
2. Residential
3. Commercial
4. Mobile
1. Near urban
2. Agricultural
3. Commercial
4. Industrial
5. None of the above
6 ft.
Specify
units _
Elevation of sampler above ground
370 ft.
Elevation of sampler above mean sea level
Citcle pertinent time zone: EASTERN CENTRAL
MOUNTAIN PACIRC YUKON ALASKA BERING
HAWAII
183
State
Area
Site
MT1
V 2 3 4 56 78 9 10
Agency
n
Project
55 56
County Code
57 58 59 6O
AOCR Number
61 62 63
AQCR Population
64 65 66 67 68 69 70 71
Elevation/Gr
72 73 74
Elevation/MSL
Time
Zone
Action
75 76 77 78
79
80
O
O
-------
ENVIRONMENTAL PROTECTION AGENCY
National Aerometric Data Bank
Research Triangle Park, N. C. 27711
SAROAO Site Identification Form
Fnrm Pnmpl*tpH Ry Charles E. RodeS ^ 6/25/74 M, X R0>,,cH
TO BE COMPLETED BY THE REPORTING AGENCY
^ California Catalyst Study - 02
State Project
Los Angeles
<"ป-*5> City Name (23 characters)
Los Angeles
37-511 County i\arne (1li characters)
City Population (right justified)
[o 2 8 1 ] 6 0 0 0
52 53 !,4 55 bo 67 58 59
Longitude Latitude
Dec). Mm. Sec. Deg. Mm. Sec.
0 0 | IV 1 1 8 .[ 2 7 J2 2 N 3 4J 0 3 3 9
GO 61 62 63 64 bi C6 O7 trt 69 ICl 71 /? 73 74 75 76
JTM Zone Eastim Coord., motors Northinn Ccord., meters
_ -j- .....^ ^^
60 61 6? 6U 04 6S (.6 67 ea 63 10 71 7? 73 M 75 76
/RV EPA - QAEML - EMB
n8'78' Supporting Agency (61 characters)
Supporting Agency, continued
^ Site B - 25 ft. SW of 405 freeway, 0.50 miles NW of
"f:"' , . Optional: Comments liiat will help identify
Wil shire 'Blvd.
trie sampling site (132 characters)
n)
(14-791
F>
DO NOT WHITE HERE
State Area Site
A
1 2 3 4 -b 6 7 8 9 10
Agency Project
It 12 13
Region Action
77 80
State Area Site
B
1 2 3 4 b b 7 b 9 li>
Vjsncy Project SMSA Aciic
II f 13 14 15 16 I/ 00
State Area Site
C
1 234 56 7 8 9 1O
Agency Project Action
11 t? 13 80
State Area Site
D
173456 789 10
Agency Project Action
11 1213 80
State Area Site
E
Abbrevuned Site Address (2o characters) Agency ? Project & ' Action" 'ฐ
3MB No. 158-R0012
Approval expires 6/30/76
(over)
184 '
11 I1 13 80
-------
ENVIRONMENTAL PROTECTION AGENCY
National Aorometric Data Bank
Research Triangle Park. N. C. 27711
SAROAD Site Identification Form
ormC
nm |M|iHR Charles E.
I V
Rodes ^ 6/25/74 K, X n
HatA .. ' ''^ NPW A Rpvi^prl
TO BE COMPLETED BY THE REPORTING AGENCY
M California
14-381
37-511
0 0
State
Los Angeles
City Name
Los Angeles
Catalyst Study - 02
Project
(23 characters)
County i-Jams (lu characters)
City Population (right justified)
0 281600
52 53 h4 5b 55 57 68
Longitude
Deo. Mm.
. W 1 1 8-1 2! 7
0
59
Latituda
Sec. Deg. Win. Sec.
2 joj LN 3 4 [o 3 .4 0
60 61 02 63 04 65 66 0 / C8 69 70 71 7? 73 74 75 76
FiVi Zone Easting Coord., motors Northmq Ccord.. tr.oters
60 61
}\
1 1
fa? 63 64 65 66 67
EPA - QAEML EMB
08 69 70 71 72 73 74 75 70
ne'7Sl SuppGUm:) Agency (61 cliaiactois)
Supporting f-
.gency, contmucci
-j Site C - 25 ft. NE of 405 freeway, 0 50 pi IPS NW
(14"79i II-T Qj^lonri,(i Comments that will help i'Jentiry
of Wilsliire Blvd.
tfiG sampling site (' 32 characters)
114-791
H4-38) Abbreviated Site Address (25 characters)
MB No. 158-R0012
| DO NOT WRITE HERE
State Area Site
A 1
1 2 34-56 78010
Agency Project
11 12 13
Region Action
77 80
State Area Site
i i 1 1 1 1 r 1
1
Anency Project SMSA Aciio
D
11 1 ' 13 14151617 SO
State Area Sit?
1 , . . . 1 i r f 1
c i
1 23456 78910
Aqency Project Action
11 U 13 80
State Area Site
D |
1 73456 7 8 9 10
Agency Project Action
L
11 12 13 80
State Area Site
E J
1 7 3 4 r. b 7 11 'i 10
Agency Project Action
n
pproval expires 6/30/76
13
80
(over)
-------
ENVIRONMENTAL PROTECTION AGENCY
National Aercxnotric Data Bank
Research Tnanyle Park, N. C. 27711
SAROAD Site Identification Form
r'orm Completed By.
Charles E. Rodes
Date.
6/25/74
.New
Revised
TO BE COMPLETED BY THE REPORTING AGblMCY
r
DO NOT WRITE HERE
IA\ California
State
Los Angeles
Catalyst Study - 02
Project
'14-3G> . City Name (23 characters)
Los Angeles
>37-5" County Name (15 characters)
City Population (rir.'nt justified)
028 16[00
52 53 54 J,5 56 r, 1 68
Longitude
Deg. Mm.
jD
59
Latitude
Sec. Deg. Min. Sec.
State Area Si if;
1
> 2 3 4 -5 6 7 8 9 10
Agency Project
It 12 13
Region Action
77 eo
0
N
0
0
60 61 Cl 63 1,4 t .'. oo 67 63 t/.i
UTM Zone Easting Coord., rooters
70 71 II 73 74 75 73
Coord., rooters
Tin
GO 61
61 63 64 Cb G6 67 08 69
70 71 72 73 74 75 76
EPA - QAEML - EMB
Area
Si to
(18-78)
Supporting Aooncy (61 cinrncters)
[5
Supporting Arcncy. continued
1 2 34 56 7 0 0 10
Agency Project S'v'SA Act
C
11 1^13 14151617 80
(C)_..S1te D - 110 ft. NE of 405 fre?\yay. 0.50 mi
State Area
Ontionai- CcT.me.its tiut wiil iioip identify
of Wil shire Blvd.
the ssiiipttng site (132 ciiaracters)
I 734 56 789 10
Agency Project Action
12 13
80
State
Area
Site
114-79)
D
t 3 4 5 6 7 8 9 1C
Agency Project Action
12 13
80
State
Area
Site
114-331
Abbreviated Site Address (25 characters)
1 734S6/89U
Agency Project Action
OMB No. 158-R0012
Approval expires 6/30/76
13
(over)
186
-------
SAROAD Site Identification Form (continued)
TO BE COMPLETED BY THE REPORTING AGENCY
DO NOT WRITE HERE
(F).
799 South Sepulveda Blvd.
[14-541
Sampling Site Address (41 characters)
Check the ONE
major category that
best describes the
location of the
sampling site.
1.D CENTER CITY
Address, continued
Next, check the subcategory
that best describes the domi-
nating influence on the sampler
within approximately a 1-mile
radius of the sampling site.
2. L& SUBURBAN
3fl I RURAL
4.O REMOTE
Specify
units
1. Industrial
2. Residential
3. Commercial
4. Mobile
1. Industrial
2. Residential
3. Commercial
4. Mobile
1. Near urban
2. Agricultural
3. Commercial
4. Industrial
5. None of the above
6 ft.
Specify
units _
Elevation of sampler above ground
370 ft.
Elevation of sampler above mean sea level
Circle pertinent time zone: EASTERN CENTRAL
MOUNTAIN PACIFIC YUKON ALASKA BERING
HAWAII 187
State
Area
Site
nil
123456/89 10
Agency
Project
55 56
County Code
J? 53 59 60
AQCR Number
61 62 63
AQCR Population
64 65 66 67 68 69 70 71
Elevation/Gr
72 73 74
Elevation/MSL
Time
Zone
Action
75 76 77 /8
79 80
-------
LABORATORY ANALYSES
The filter and reagent analyses for the background phase of
LACS is under contract to Rockwell International. Rockwell's
corporate office is located in Thousand Oaks, California. The
Rockwell project .officer is Dr. Ed Parry and EPA's project officer
is Franz Burniann. Only Hi-Vol filters and cascade plates and
24 hour bubbler reagents are being analyzed for the background
phase, with membrane filters being analyzed for TSP, $04, NOo,
and Pb.
The filters are taken to Rockwells Westlake laboratory once a
week for analyses. The laboratory director to whom filters are
taken is Mr. George Colovos. The laboratory address is:
Rockwell International Science Center
Westlake Facility, Suite J
756 Lakefield Rd.
Westlake Village, Calif. 91361
A schematic map for getting to Rockwell's laboratory from the sampling
sites is included.
188
-------
O
03 4->
C rt3
i- S-
O> O
189
-------
LACS Daily Operation Routine
1. Connect Site A CO unit to zero air. (See Note A)
2. Exchange bubbler tube in rack not bubbling.
3. Remove and calibrate orifice needle, then replace. Adjust
timer if necessary. t} .
4. Record flowrates and date on orange data card. Mark log book.
5. Change Hi-Vol and membrane filters as required (See Schedule)
on Platform A; Adjust timer if necessary.
6. Change Hi-Vol and membrane filters as required (See Schedule)
on Platform B. Adjust timer if necessary.
7. Return to Site A CO, note unadjusted zero, check span, and rezero
if necessary. (See Note B) Put CO back on-line and mark operation
sheet and log book.
8. Fill in data required on filter folders, envelopes, data cards,
and platform log books.
9. Chock and time-synch climet recorders (See Note B)
10. Drive to Site D.
11. Change Hi-Vol and membrane filters as required (See Schedule)
on Platform D. Adjust timer if necessary.
12. Check MRI recorder and time-synch chart. (See Note B)
13. Drive to Site C.
14. Connect Site C CO unit to zero air (See Note A).
15. Exchange bubbler tube in rack not bubbling. Remove needle and tape
to orange data card for calibration at Site A. Replace with previously
calibrated needle. Adjust timer if necessary.
16. Change Hi-Vol, Cascade, and membrane filters as required (See Schedule)
on Platform C. Adjust timer if necessary.
17. Return to CO, note unadjusted zero, check span, and rezero if necessary.
(See Note B) Put CO back on-line and mark operation sheet and log book.
18. Return to Site A and calibrate bubbler needle from Site C.
19. Fill in data required on filter folders, data cards, envelopes, and
platform log books.
Notes: A. Since CD's are vibration sensitive, allow instruments to
obtain zero trace while changing platform filters.
B. When marking strip charts always record date, time, site,
and operator, as well as notations such as zero check, span
checkf etc.
C. All filters and bubblers are taken to Rockwell on Fridays for
analysis and exchange for prepared materials.
D. All samplers are calibrated once a month. See Schedule.
E. All strip chart data is reduced and mailed to RTP, NERC weekly.
190
-------
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APPENDIX B8.4
COLLECTION AND ANALYSIS OF AIRBORNE SUSPENDED
PARTICULATE MATTER RESPIRABLE TO HUMANS
FOR SULFATES AND POLYCYCLIC "ORGANICS
to
ENVIRONMENTAL PROTECTION AGENCY
October 8, 1974
by
W. M. Henry and Ralph I. Mitchell
(Contract No. 68-02-0752)
BATTELLE
Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
194
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SIXTEENTH MONTHLY TECHNICAL PROGRESS REPORT
on
COLLECTION AND ANALYSIS OF AIRBORNE SUSPENDED
PARTICUIATE MATTER RESPIRABLE TO HUMANS
FOR SULFATES AND POLYCYCLIC ORGANICS
to
ENVIRONMENTAL PROTECTION AGENCY
from
BATTELLE
Columbus Laboratories
by
W. M. Henry and Ralph I. Mitchell
October 8, 1974
PURPOSE AND SCOPE
The primary objective of this study is to obtain elemental
and compound compositions of those species which may have deleterious
effects upon human health. To accomplish this objective, the following
tasks shall be performed.
(1) Design and construct a sampler which will obtain
collected suspended particulate matter in a respir-
able size range in quantitites of at least 1 g in a
form amenable for detailed chemical analysis.
(2) Demonstrate the collection efficiency of the sampler
using known atmospheres generating particulate matter
to show at least 90 percent efficiency for particles
in the respirable size range, with no more than 5
percent particles above this range appearing in the
sample.
195
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(3) Collect two to three sets of samples (at least
duplicates) in urban areas. (Revision based on
December 18, 1973, meeting).
(4) Analyze the samples quantitatively for total elemental
composition, qualitatively formations and anions, and
qualitatively for compounds with a particular interest
in sulfate species.
(5) Explore pathways to quantitative analysis for compounds,
particularly those compared in part of oxygenated sulfur
species.
SUMMARY OF PROGRESS TO DATE
Sample Classification
A proposed sampler design was submitted to the EPA Project
Officer for review and comments. Prior to a final decision on sampler
design and construction to meet current definitions by EPA and knowledgeable
respiratory physicists on the definition of respirable size range particu-
lates, small-scale prototype sampler was assembled. The prototype, using
2 Aerotec-2 cyclones and a full-scale electrostatis precipitator, was
assembled for the purpose of experimental trial in collection and recovery
of samples from the precipitation plates and to provide a working sample
for chemical analysis.
In addition, a small-scale (approximately 5 cfm) impactor stage
was constructed. This stage has the same slit width as envisaged for the
full-scale sampler. The slot length can be adjusted to give the sampling
capacity and cutoff size desired to meet the respirable size definition.
A Bergland-Liu monodisperse aerosol generator was used to calibrate the
impactor stage at the 3.5-micron cutoff stage.
Two meetings were held during December, 1973, at Research
Triangle Park to review and approve the final sampler design and
196
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sampling characteristics. After considerable consultation the 3.5-micron
cutoff size for respirable aerosols, as used by industrial hygienists, was
decided suitable. Subsequently a second meeting was held among three
consultants, EPA health personnel, the EPA Project Officer, and BCL per-
sonnel to determine the specific collection characteristics of the sampler.
It was decided at this meeting that the respirable aerosol
fraction should be divided into two size groups with a sharp cutoff at
1.5 microns. It also was decided that the aerosol should be scalped at
the inlet at approximately 20 microns.
To accommodate these changes it was necessary to redesign the
sampler. The revision of sampler design to provide two cuts, its subse-
quent construction, and field collection entails more effort than originally
planned. The collection efficiency(ies) need to be checked at three size
'"^"fractions instead of two, and up to four size cuts will be obtained for
analysis from each selected urban area. To compensate for the added effort,
it was agreed to limit the collection sites to two or. three tentatively
Los Angeles, New York City, and possibly Salt Lake City.
The redesigned high-volume sampler will use inertial impaction
to obtain the two desired size classifications of the respirable aerosol
fraction which might be representative of both primary and secondary
aerosols. Both the primary cutoff of 3.5 microns and the secondary size
of 1.7 microns will utilize multiple long slots for the plate type oriface.
The slots will be 1/4 in. x 1 in. and 1/16 in. x 1 in., respectively. It
was found in the Battelle calibration the impaction parameter was equal to
0.39 for both slots using the desired cutoff size of droplets of unit
density. The impaction efficiency curve obtained in calibrating the
1/4-in. slot (shown and discussed in the Tenth Monthly Technical Progress
Report dated April 10, 1974) yields a curve very similar to the Los Alamos
curve for respirable aerosols.
The sample collected with the prototype sampler was found to be
very difficult to remove completely from the fixed, closely spaced (~ 1/4-in.
separation) electrostatic precipitator plates. Additionally the removal
process included analytically significant portions of the electrostatic plates
substrate. To minimize these problems it was attempted to find a material
197
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which would provide a hard, nonreactive and analytically insignificant
substrate. Certain of the noble metals, Pt, Pd, and Rh, were ruled out
because of current interest in their possible occurrence in the atmosphere
f.rom catalytic systems to be incorporated in 1975 auto exhaust systems.
Gold and silver, unless alloyed, were judged too soft; and several harder
surface metals, such as tantalum, tungsten, etc., are not available in
sufficient purity to meet the analytical requirements. High-purity 99.99
percent aluminum was selected as the most suitable compromise since aluminum
itself is not of high interest in this program and its impurity content--
mostly Fe, Si, Mg--at a total of 100 ppm should be insignificant in respect
to the collected aerosol mass. The electrostatic precipitator was designed
so the plates could be removed for subsequent recovery of the sample in the
laboratory, with two sets provided for each sampler.
Results of analyses of the sample fractions collected with the
prototype sampler were reported in the Ninth Monthly Technical Progress
Report dated March 15, 1974. These data will be useful in guiding methodo-
logy selection for samples collected using the final design sampler.
Preliminary calibration of the impaction stages were completed,
and the redesign of the sampler was finalized in April, 1974, and detail
drawings were completed in May, A source of high-purity aluminum for
fabricating the electrostatic precipitator plates was located, but delivery
could not be obtained until the first week in June.
The large-volume sampler was assembled and final calibrations were
performed. The sampler was designed for a total pressure drop of about 3-1/2
inches of water which would produce a total flow of about 850 cfm with a 1-hp
pressure blower. It was found that the total Ap was 6-3/8 inches and over
half of this was produced by the exit plenum. This section was modified
with flow straighteners which eliminated this defect.
The sampler was challenged with a fluorescent aerosol with a mass-
median diameter of 6.5 micrometers. It was found that about 90 percent of
the aerosol deposited on the first stage and that the penetration through
the electrostatic precipitator stage was less than 0.01 percent. Calibra-
tions of the second stage and electrostatic precipitor were performed
similarly.
198
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The samplers were found to perform adequately in the initial
laboratory tests on air sampling. Subsequently in further testing it was
found that high-voltage leaks were occurring in the electrostatic section.
This was attributed to moisture pickup of the construction material used
to hold the electrostatic plates in place. This material was replaced with
Teflon. Following this change the sampler was operated in tests up to 3-day
periods with no loss in ,high voltage. The collected particulates were readily
removed from the Teflon-coated impactor stages. It was found much more
difficult to recover the less than 1.7-micron fraction from the same 100 sq ft
of aluminum plate surface area with a short test period. However, with the
far greater particulate loading which will be encountered in the L.A. area
and other field site uses, adequate recovery can be accomplished.
Current Efforts
Field Site Application
The initial field site application of the sampler(s) was carried
out during the period September 6 through September 13, 1974, at the Los
Angeles Catalyst Study site. Two samplers were taken as cargo on the same
commercial air flight as carried the Battelle sampling and engineering team.
Those were set up the same day as departure at sites A (upwind) and C (down-
wind). They were operated at approximately road level.
After a preliminary 2-day run to observe loadings obtained at
these sites, a 4-day sampling effort was performed. During that period
the particulates were removed from the first and second impactor stages
each day. The particulates on the electrostatic plates were allowed to
accumulate for the entire 4-day period and subsequently removed at the
Battelle-Columbus Laboratories.
The approximate masses obtained during this period are given
in Table 1.
199
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TABLE 1. PARTICUIATE COLLECTION AT L. A. SITE
Site Location
Site A
Site C
(downwind)
Size Fraction
3.5-20 jim (1st stage)
1.7-3.5 (im (2nd stage)
< 1.7 urn (electrostatic plates)
Total
3.5-20 jim (1st stage)
1.7-3.5 p,m (2nd stage)
< 1.7 u-m (electrostatic plates)
Total
Time Period
~ 4 days (100 hr)
~ 4 days (100 hr)
~ 4 days (100 hr)
~ 4 days (100 hr)
~ 4 days (100 hr)
~ 4 days (100 hr)
Mass
1.440 g
0.845 g
3.370 g
6.655 g
1.245 g
0.945 g
4.495 g
6.685 g
Cascade impactor runs were made of both upwind and downwind sites.
These were made on two consecutive days (not concurrently) and covered
approximately a 24-hour period for each run. Particle distribution data
from the cascade impactor runs are shown in Figures 1 and 2.
Vapor phase (chromosorb bed) samplings also were made at each
site for about a 24-hour period each--again not concurrently. Analyses of
these may be more significant and enlightening than previously thought due
to the distinct odors emanating from the collected particulates.
Analyses of Collected Samples
The approximately 4-day, 100-hour samples, have been analyzed
in part. The data available to date are given in Table 2.
Some caution should be observed in drawing strong conclusions
from a single sampling taken under somewhat adverse conditions of cleanli-
ness. However, based on the lead values, there is definitely a traffic
effect shown between the upwind and downwind samples. Also, there are
definite size-fraction/composition variations shown in the total sulfur,
the benzene-soluble extract, and the iron values. Further detailed analyses
200
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O Special automobile exhau
impactor
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Equivalent Particle Diameter, microns
8 10
FIGURE 1. PARTICLE SIZE DISTRIBUTION OF DOWNWIND POLLUTANTS AT
SAN DIEGO FREEWAY SITE
201
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Equivalent Particle Diameter, microns
FIGURE 2. PARTICLE SIZE DISTRIBUTION OF UPWIND POLLUTANTS
AT SAN DIEGO FREEWAY SITE
202
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being considered include GC-MS on the organic extracts, additional metal
content determinations and analyses of the vapor phase samples taken con-
currently with the particulate samples. These further analyses require
relatively large efforts and may be deferred until better samplings can
be performed.
TABLE 2. ANALYSES OF COLLECTED PARTICUIATES FROM L.A. BACKGROUND CATALYST
STUDY SITE - RESULTS IN PERCENT
Sample Designation
Site A
Upwind
Site C
Downwind
Pb
1st stage 0.86
2nd stage 1.13
Electro- 0.93
static
1st stage 2.43
2nd stage 3.16
Electro- 3.74
static
Determination
Benzene-Soluble , .
Total S Fe OrRanics S^3'
2.0 3.6 8.0
5.6 2.9 9.0
8.7 1.0 16.6
2.0 3.8 4.3
4.7 3.1 8.8
5.5 1.9 16.0
(a) After benzene extract data not completed.
CURRENT PROBLEMS
Proposal requests have been sent EPA for extensions and ampli-
fications of the contract effort. If these are found acceptable, current
problems involving additional sample collection, analyses, reporting, etc.,
will be resolved.
funding.
FUTURE WORK
Future work will be dependent on the possible receipt of additional
203
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9. PERFORMING ORGANIZATION NAME AND ADDRESS
Health Effects Research Laboratory
Office of Research & Development
U.S. Environmental Protection Agency
Research Triangle Park, N.C. 27711
ANNUAL CATALYST RESEARCH PROGRAM REPORT
AoDendices, Volume VIII
6. PERFORMING ORGANIZATION CODE
7. AUTHORIS)
0. PERFORMING ORGANIZATION REPORT NO.
Criteria and Special Studies Office
12. SPONSORING AGENCY NAME AND ADDRESS
Same as above
September 1975
10. PMOGMAM ELEMENT NO.
1AA002
11. CONTRACT/GRANT NO.
13. TYPE OF REPORT AND PERIOD COVERED
Annual Program Status 1/74-9/7)4
14. SPONSORING AGENCY CODE
EPA-ORD
Ib. SUPPLEMENTARY NOTES
This is the Summary Report of a set (9 volumes plus Summary).
See EPA-6QQ/3-75-010a through 01 Oh & 01 Oj. Report to Congress.
16. ABSTRACT
This report constitutes the first Annual Report of the ORL) Catalyst Research
Program required by the Administrator as noted in his testimorv before the
Senate Public Works Committee on November 6, 1973. It includes all research
aspects of this broad multi-disciplinary program including: emissions charac-
terization, measurement method development, monitoring, fuels analysis,
toxicology, biology, epidemiology, human studies, and unregulated emissions
control options. Principal focus is upon catalyst-generated sulfuric acid
and noble metal particulate emissions.
I 7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
Catalytic converters
Sulfuric'acid
Desulfurization
Catalysts
Sul fates
Sulfur
Health
I). IDENTIFIERS/OPEN ENDED TERMS <-. COSATll
Automotive emissions
Unregulated automotive
emissions
Health effects (public)'
I "I. DISTRIBUTION STATEMENT
Available to public
19 SECURITY CLASS ( I Ills Rrporl}
21. NO. OF PAGES
210
Unclassified
72. PRICE
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