Document x5yrxwMwRjd78dOBV56veEp5m
R & D REPORT
""75 6192
DOW CHEMICAL U.S|
RESTRICTED: for use within The Dow Chemical Company only*
department
A0ORATORV REPORT CODE
____ LAEL385
DATE ISSUED
July 8, 1975 "CTaTN^T" PROBLEM NO.
RESEARCH AND DEVELOPMENT
TITLE
ASBESTOS REMOVAL, PART 2:
AZii J__ I__ L
FILTRATION OF TRENCH LIQUOR CELL EFFLUENT
46
auth6r isi
JOHN GROSS
AUTHOR (SI JICNAfUrtem
1 fpcim M MIDLAND CM
FEB 1 91987
PAG IN FI REPO
DESCRIPTIVE SUMMARY WITH CONCLUSIONS:
SUMMARY
lclude in this space rtfartncts to doto books, and to oarlior relof' "roporfi, patents ond publications.)
Production scale data obtained using a 550 ft2 pressure leaf filter on trench liquor (~ 80 gpl NaOH) cell effluent showed that the asbestos levels were reduced from 3 ppm (~ 90,000 M FPL) to 0.01 ppm (< 80 M FPL). Iron removal was not required for this stream. A perlite filter aid (Dicalite 476 or 436) is recoomended to minimize filter aid costs. At 0.75 gpm/ft2 flow rates, cycle times of 6 hours were obtained using Die 476 as the pre coat and body feed at a 6 to 1 ratio of body feed to the total suspended solids in the feed. This was for inlet turbidities of 20 to 25 FTU. At the same conditions as above except at a 0.5 gpm/ft2feed rate and a 3 to 1 body feed ratio, cycle times of 8 to 10 hours were obtained.
CONCLUSIONS
1. Asbestos removal was 99+$ using pressure leaf filtration and a variety of different filter aids.
2. Iron removal (not required for trench liquor) was from ~ 2.7 ppm (avg) in the feed to ~ 1.3 ppm (avg) Fe in the filtrate.
3. Dicalite 476 or 436 would be recommended for trench liquor filtration
due to the following:
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a. These perlites were the cheapest filter aids available at 3^4lb
(dlatomites at 10^/lb, cellulosics at 30^/ib),
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b. Outlet clarity and reasonable cycle times were obtained. A(rjQ
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c. Perlites require less complicated bulk handling equipment i}an
dlatomites.
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d. Dlatomites may be a health hazard (silicosis).
DISTRIBUTION:
DEPARTMENT FILES
RAD ADMINISTRATION CENTRAL REPORT INDEX - 5 COPIES
(566 Bldg. - Midland)
FORM C . 43 OO PRINTED R-1 -73
Distribution is continued on attached page.
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4. The cycle times obtained were affected by the solids concentration of the feed, the type of filter aid used, the body feed ratio, and the filtration rate.
a. Cycle times of 6 to 7 hours were obtained using DIC476 as the precoat and body feed at a 6 to 1 body feed ratio for operating at 0.75 gpm/ftz feed rates when the inlet turbidity was 20 to 25 FTU.
b. At the same conditions except at 0.5 gpm/ft2 feed rates, cycle times of 8 to 10 hours were obtained at a 3 to 1 body feed ratio.
5. Operating at 0.5 gpm/ft3 filtration rates with a 3 to 1 body feed ratio would give the lowest filter aid costs to obtain 8-hour cycles even though more filter area would be required than for operating at 0.75 gpm/ft2.
6. The results obtained on the plant scale (550 ft2) filter in general confirmed the testing done by the Midland Division using a pilot scale (20 ft2) filter.
INTRODUCTION
The work covered in this report is an expansion of earlier work done by the Midland Division of filtering cell effluent using a pilot scale (20 ft2) pressure leaf filter (report EMR-LR-120) and lab testing (report EMR-LR-116).2 This report is also a continuation of work done by the Louisiana Division on asbestos removal (report LAD-321)3 which was mainly concerned with the cathode washer water. The purpose of this work was to obtain data on filte trench liquor cell effluent (~ 80 gpl NaOH)and to confirm pilot scale testing on plant scale equipment (550 ft2 filter). The Louisiana Division trench liquor contains ~ 2 times as many total suspended solids as the evaporator feed cell effluent. The trench liquor is used by the Glycol Plant and is discharged to the river as part of the hydrolyzer bottoms stream. Asbestos removal is the major consideration, as iron removal is not required. This allowed a choice of less expensive filter aids than the cellulosic type recommended for iron removal by the Midland Division testing.
Other Louisiana Division asbestos removal work now in progress will be reported as Part 3: Filtration of Evaporator Feed Cell Effluent, Part 4: Flocullation and Settling of Cell Effluent Streams, and Part 5: Recommended Asbestos Removal System for the Louisiana Division. Report LAD-321 should be considered as Part 1: Asbestos Removal.
EXPERIMENTAL PROCEDURES AND EQUIPMENT
Filter - The filter system is shown by Figure 1. The filter used was an 1100 ft2 Sparkler filter originally designed for salt removal with 6" leaf spacing and an outlet manifold designed for 0.T to 0.15 gpm/ft2 flow rates. High pressure drops were obtained through the outlet manifold
9 I920OOii5
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when trying to operate at 0.75 gpm/ft2 flow rates. The filter had to be modified by removing every other filter leaf to give 550 ft2 of filter area to minimize pressure drop at 0.75 gpm/ft2. In addition, the measurement of the Ap through the filter was modified by running a tube into the outlet manifold so that the pressure drop across the leaves could be measured instead of the excessive drop through the outlet manifold.
2. Filter Cycle Controls - The filter system was set up for constant rate filtration to a constant Ap at the end of the cycle. The controls were automated as much as practical. The first step was the precoat cycle during which the filter filled up and was precoated until the pre coat cycle timed out. Then the "precoat complete" alarm was given. At this point, the operator moved the controls to the filter cycle and began filtering, during which the feed flow rate was automatically controlled. The feed flow rate and Ap across the filter were continuously recorded. At the preset Ap (50 psig), the filter was automatically tripped out of the filter cycle and drained. After the filter was drained, the "ready to sluice" alarm was given. The operator then moved the controls to the sluice cycle, and the filter was automatically sluiced and drained. At that point the "sluice complete" alarm was given. The filter was then ready for another run beginning at the precoat cycle again.
3. Precoat system - The precoat tank was a cone bottom tank equipped with an agitator. The desired quantity of filter aid was added to the tank and the contents of the tank were recirculated through the filter during the precoat cycle. The precoat was normally deposited at a rate of ~ 1 gpm/ft2 to give ~0.1 # precoat/ft2. The filter was filled and precoated with clear liquid to eliminate problems of blinding the filter cloth that occurred at the start of testing when using the feed to the filter.4
4. Body Feed System - Body feed is the filter aid added to the filter feed to keep the solids being filtered from rapidly blinding the pre coat. Body feed extends the cycle lengths obtained considerably over precoat only for use with trench liquor. The body feed tank used was a 3000 gallon cone bottom tank equipped with an agitator. The desired quantity of filter aid was added to the tank to give the desired slurry concentration (normally 1 to 5 wt. $). The addition rate of body feed was controlled to give the desired ratio of body feed to total suspended solids. This was obtained using a cascade control scheme for which the inlet turbidity was measured by an on stream, Hach surface scatter 4 turbidimeter. The signal from the turbidimeter was fed to a ratio set controller which drove the set point of the body feed flow controller. This allowed the desired ratio of body feed to total suspended solids to be set on the ratio set controller using the relationship between tur bidity and ppm TSS (total suspended solids) that had been determined. The body feed rate was measured by the orifice meter, and the tank levels were gauged at the beginning and end of each run to check the flow rate measurement.
ST0Q025I 7
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5. Sampling and Data Taking - Automatic composite samplers were installed on the inlet to the filter before the point where body feed was injected and on the outlet of the filter. Volumes up to five gallons were obtained during the cycles, and one gal samples were saved for analysis from each run. The turbidity of the inlet stream was continuously measured by the on stream turbidimeter, and samples were also taken periodically and run on the lab turbidimeter. The body feed rate, time, and Ap were also recorded periodically by ' the operators. The filter feed flow and Ap were continuously recorded. The tank level and time were recorded at the beginning and end of the filter cycle.
6. Sample Analyses - The composite samples were analyzed for ppm Fe, turbidity, ppm NaoCl, $ NaOH, and $ NaCl by the Caustic Plant lab personnel. Hie samples were analyzed for ppm asbestos, ppm ca, ppm Mg, ppm si, and ppm TSS (total suspended solids) by the R&D analytical lab. All of these analyses were performed by standard analytical procedures.
The ppm asbestos was determined by the A. A. method.4 The ppm asbestos can be corrleated to M FPL numbers based on a curve correlating the work of Hinze and Martin. Samples were saved for analysis of M FPL by the TEM procedure but this data has not been obtained as yet.
The turbidity was measured using a Hach Model #2100A lab turbidimeter. The samples were placed in an ultrasonic bath just prior to measurement to break up air bubbles from shaking the samples and to break up large flocks formed after the samples settled. This gave good agreement be tween measurements obtained on hot "fresh" samples and measurements obtained on cold samples that had been allowed to settle.
Ihe ppm TSS were determined gravimetrically by filtering 600 ml of the inlet feed samples or 3000 ml of the outlet samples through a glass fiber filter paper. The filtering was followed by washing with 1000 ml of hot distilled water. These large volumes were found to be needed to eliminate errors caused by being unable to thoroughly wash the salt out of the filter paper and solids. Due to the amount of time required to perform these tests, curves of turbidity vs. ppm TSS and Klett reading vs. ppm TSS were developed and`used. These curves are shown by graphs # 1 and 2. The turbidity vs. ppm TSS graph shows that the relationship becomes inaccurate due to a flattening out of the turbidity measurement above ~ 70 FTU. This may be due to nephalometer characteristic of going "blind". The fact that the relationship was a curve rather than a straight line function may also be due to the fact that the large flocks are being broken down into numerous smaller flocks when being diluted by fresh feed into the storage tank. This is typically true of the relation ship obtained for many types of flocks when diluted.5
7. Lab Pressure Leaf (Bomb) Filter - The lab filter used was a 3000 ml capacity Dlcalite bomb filter. The filter was used to quickly compare many different filter aids, and to determine the optimum body feed ratio for a filter aid. The lab filter operated as a constant pressure filter instead of a constant rate filter. This means that the flow rate obtained was an exponential function. By plotting the flow rate vs. time on log-log graph paper, a straight line is obtained which can be extrapolated to an eight-hour or sixteen-hour cycle time. This data can then be used to
ST00025 ! 0
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calculate the gpm/ft* flow rate that could be obtained for an eight-hour or sixteen-hour cycle of constant rate filtration at an average pressure equal to the constant pressure used in the testing. The calculations and leaf conversion factors are given in the appendix. The data taken were the total vdlume of filtrate, time in minutes, and filter cake collected thickness,filter leaf area, body feed used, and pressure. Samples were also saved of the filtrate and feed for analysis.
DISCUSSION OF RESULTS
The Louisiana Division trench liquor stream is essentially dirty cell effluent (~ 80 gpl NaOH) and should not be confused with other division's terminology for trench liquor (. 20 gpl NaOH) streams. The trench liquor stream is a significantly different stream from the cell effluent tested by the Midland Division using pilot scale equipment. Fe removal was not required for the trench liquor, which is sent to the user plants instead of the evaporators. The lowered Fe specification required for the filtrate allowed the use of cheaper types of filter aids than the cellulosic types recommended for iron removal in the Midland Division testing on cell effluent. Working with trench liquor on a plant scale also gave the opportunity to evaluate data from scaling up from the pilot filter to plant size equipment. The plant scale testing was carried out as constant rate filtration using a variety of different filter aids as precoats and body feeds over a wide range of body feed ratios. The data were obtained at flow rates of 0.75 gpm/ft* and 0.5 gpm/ft2. Lab filtra tion data were also obtained for comparison with the plant filtration data. From these tests the following results were determined.*
1. Filter Cycle Times - ~ 8-hour cycles were desired to obtain a reasonabl length of time for filtration and to minimize the down time for precoating, sluicing, and mixing of filter aids in the precoat or body feed tanks. The following variables were found to have a major effect on the cycle times obtained.*
a. Body Feed Ratio - The cycle times were found to depend upon the body feed ratio used for any filter aid type 'at a constant inlet feed turbidity and flow rate. This is shown by Tables #1-5. For Dicalite 476 cycle times of 6 to 7 hours were obtained at 0.75 gpm/ft2 at a 6 to 1 body feed ratio and inlet turbidity of 20 to 25 FTU. Above ~ 6 to 1 ratio little improve ment in cycle times was obtained as shown by graph #3. At flow rates of 0.5 gpm/ft* using Die 476, cycle times of eight to ten hours were obtained at 3 to 1 body feed ratios with 35 to 37 FTU inlet turbidities. There was little improvement in cycle times above a 3 to 1 ratio as shown by graph #4. In general, these results agreed with the data obtained by the Midland Division, but higher body feed ratios were required.6 This may be due to the higher solids concentration in the feed.
The lower body feed ratio needed at 0.5 gpm/ft* feed rates vs. 0.75 gpm/ft* rates would be expected from literature available on filtration. The literature states that to obtain the same throughput at higher flow rates
ST0002SI9
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requires more filter aid than at lower flow rates.7 The data obtained for Die 476 using the plant filter were confirmed by the lab testing as shown by graphs #5 and 6 and Tables #6A and 6B. The data agreed in the effect of body feed ratio, optimum body feed ratio, and the effect of inlet solids concentration. The plant data for Die 436 are shown by graph #7. Lab data for Die 436 are shown by Tables #7 A and 7B and graphs 8 and 9. The literature also agrees with data obtained in determining the optimum body feed ratios in that too high of a body feed ratio can actually reduce the cycle lengths obtained.8
b. Feed Turbidity (as a Measure of the Total Suspended Solids Concentration) The inlet turbidity as a measure of the total suspended solids concentration of the feed has a very significant effect on the cycle times when other variables are held constant. In general, the cycle times decreased as the turbidity increased as shewn by graphs #10, 11 and 12. These results confirm those reported by the Midland Division.9 The results also agree with the literature available.10
c. Comparison of Filter Aids - The majority of the plant scale testing was done using Dicalite 476 and 436. A comparison of cycle times obtained at approximately the same conditions showed that Dicalite 476 gave up to one hour longer cycle times than 436. This is shown by graph #13. Other plant scale testing was done using Dicalite 416, Die 437 and JM hyfloco super cel with JM BH 40 as a precoat. These results are shown by Table #5.---I However, the data given for cycle times by Table #5 may not be accurate CD due to progressive blinding of the filter cloths that occurred until the CD filter system was changed to allow the filter to be filled and precoated 5^ with clean (pre-filtered) trench liquor. A better comparison of a variety'^ of different filter aids was obtained in lab scale testing. The results of the lab testing are shown by Tables #8A and 8B. The lab scale testing ^ of the perlites confirmed the results obtained in plant scale testing as shown by graphs #14 and 15. The comparison of the cellulosics are shown by graphs #16 and 17, and of the diatomites are shown by graphs #18 and 19. These resulcs in general, confirm those obtained by the Midland Division, but there were some differences which may be due to the differences in the two streams tested.11 The choice of filter aids should not, however, be based on cycle times alone.
2. Outlet Clarity - The outlet clarity was measured by turbidity, ppm asbestos, ppm Fe, and ppm Si. The outlet clarity was affected by the type of filter aid used, body feed ratio used, and by the inlet total suspended solids. These effects are discussed by the following.
a. Asbestos Removal - The asbestos removal obtained was from ~ 3.4 ppm (average) to as low as 0.01 ppm, or from ~ 90,000 M FPL to < 80 M FPL based on the A.A. correlation to the TEM. This represents ~99^t removal of the asbestos. The inlet asbestos concentration ranged to as high as 15 ppm and the outlet concentration ranged from a high of ~ 0.04 ppm to < 0.01 ppm. These results are given by Tables #1-5. A comparison of the filter aids tested showed that Dicalite 416 or 436 consistently gave < 0.01 ppm
STOOD262 I
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outlet asbestos concentrations, and Dicalite 476 gave 0.01 ppm average outlet asbestos concentrations. The results also showed that the outlet abestos concentration was affected by the body feed ratio used. With precoat only or low body feed ratios (--1), the data showed higher asbestos concentrations than for body feed ratios of two or more.
b. Outlet Turbidity - The outlet turbidity was normally < 2 FTU, and was affected in the same manner that the asbestos concentration was. That is lower outlet turbidities were obtained with "tighter" filter aids or by using a higher body feed ratio. The effect of the body feed ratio is shown by graph #20. The effect of the body feed ratio was also determined by lab testing as shown by graph #21.
c. Outlet Silica Concentration - The data obtained showed that silica pickup was occurring using the perlite or diatomite filter aids. This, however was not a problem for trench liquor filtration because the trench liquor is not feed to the evaporators and there is no spec for silica. The results obtained are shown by Table #5.
d. Fe Removal - Since iron removal was not required the perlites or diatomites could be used which had been shown to' give iron pickup in testing by Midland. On the average, the inlet Fe was ~ 2.7 ppm and the outlet Fe was ~ 1.3 ppm which was ~ 50$ removal, but the outlet Fe would not be in spec for 50$ NaOH. Again, the iron removal was found to be affected by the body feed ratio with better results obtained above ~1 to 1 ratio. This was seen in the plant testing and lab testing as shown by graphs '#20 and 21 and Tables #1 and 6A.
3. Filter Aid Selection - The perlite filter aids would be recommended due to their lower cost than other types of filter aids (5^/lb for per lites, 10^/lb diatomites, 30^/lb for cellulosics). The cellulosic types recommended for filtration of evaporator feed cell effluent by Midland Division's testing were not needed for trench liquor because iron removal was not required. Hie perlites would be preferred over the diatomites due to easier bulk handling for the perlites. The diatomites are also a possible health hazard (silicosis). Of the different grades of perlites, Die 476 would be preferred to give the longest cycle times with acceptable clarity (0.01 ppm asbestos). If better outlet clarity was desired, Dicalite 436 would be recommended (< 0.01 ppm asbestos).
4. Filter Aid Costs - To obtain eight-hour cycles when operating at 0.75 gpm/ft* filtration rates, the projected costs of filter aids for trench liquor were ~ $140,000/year. This was based on using Dicalite 476 or 436 as a precoat and body feed at a 6 to 1 body feed ratio and a 0.1# precoat/ft2 precoat usage. It was also based on an average inlet turbidity of 26 FTU or 38 ppm total suspended solids, 2000 gpm of trench liquor, and for using two 1600 ft2 pressure leaf filters.
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A more economical point for operating at 0.75 gpm/ft2 would be to obtain ~ 5-hour cycles at a 3 to 1 body feed ratio. Hits would reduce the filter aid costs to ~ $90,000/year but would require better automation to reduce the manpower requirements for precoating the filters more often and larger surge tanks. The approximate filter aid costs vs. body feed ratio used at 0.75 gpm/ft2 flow rates is shown by graph #22.
For operating at 0.5 gpm/ft2 to obtain ~ 10-hour cycles, the filter aid costs would be ~ $80,000/year. This was based on using a 3 to 1 body feed ratio and on using three 1600 ft2 filters. The approximate filter aid costs vs. body feed ratio used at 0.5 gpm/ft2 are also shown by graph #22. From these data, it would seem that the lower filter aid costs of operating at 0.5 gpm/ft2 could offset the added capital cost for an additional filter if 8 to 10-hour cycles are desired ($140, 000/year vs. $80, 000/year).
RECOMMENDATIONS
Based on the data obtained, the system to filter trench liquor should be
designed for 0.5 gpm/ft2 filtration rates. A bulk handling system for
the perlite filter aids (Die 476 or 436) should also be considered to
reduce manpower requirements. Cycle times of 8 to 10 hours would be
expected using a 3 to 1 body feed ratio. Operating at 0.5 gpm/ft2 would
require three 1600 ft2 pressure leaf filters for the Louisiana Division
Caustic Plant.
GO
ECOLOGICAL CONSIDERATIONS
CD
The techniques advocated by this report would eliminate a source for
CD
asbestos to enter the river. This would be done mainly by eliminating
CD
asbestos from entering the river as part of the hydrolyzer bottoms stream I'D
ACKNOWLEDGEMENTS
ro rx>
Karl McKinstry and Dave Naessens of the Midland Division were very helpful in starting up the 550 ft2 plant scale filter at the Louisiana Division and transmitting their knowledge to the Louisiana Division personnel. Rick Wittmann of the Louisiana Division NaOH plant and other NaOH plant personnel set up the filter and operated it during the testing.
sb
9- -
REFERENCES lessens, H. D. and McKinstry, K. A., Report EMR-LR-120 (December, 1974). 2Potoff, A. D., Report EMR-LR-116 (December, 1974). 3Gross, J. W. and Lanaux, J., Report LAD-321 (December, 1974). 4Chagnard, H. A., Report LAD-AR-74.01 (November, 1974). 5Hach Turbidity Measurement, p. 10. 6Naessens, H. D. and McKinstry, K. A., Report EMR-LR-120 (December, 1974). 7Johns-Manville Celite Filter Aid Filtration, p. 12. aDlcallte Industrial Filtration Manual, p. 15. 9Naessens, H. D. and McKinstry, K. A., Report EMR-LR-120 (December, 1974). 1Dicalite Industrial Filtration Manual, p. 12. llPotoff, A. D., Report EMR-LR-116 (December, 1974).
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DATA SH EclT
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TABLE 66
DATA SHEET
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-43-
APPENDIX 1. A.A. to TEM Asbestos Correlation 2. Lab Filter Calculations and Conversion Factors
ZS90OOO1S
ln .n n n
MFPL ASBESTOS(DETERMINED BY THE TRANSMISSION ELECTRON MICROSCOPE)
S .44. CONVERSION CF P?b ASBESTOS VNORR BY C. rilKZE) TO MFPL ('HORN BY L, MARTIii) THE LIG'JID ANALYSED INCLUDES CELL EFFLUENT, BRINE; AID BIG-LAGGCN WASTE WATER. THE LINEAR REGRESSION CORRELATION CO-EFFICIENT IS ,6/
ICP 100 1000 PP3 ASBESTOS ON A V.T, BASIS (DETERMINED 3Y ATOMIC ABSORPTION) LEAST SQUARES REGRESSION
^-i000
-45-
BCHB FILTER ULAVES
Diameter Inches
Area So. Inches
0.750
O.Ui2
0.956
0.718
1.000
0.786
1.3 53
1.UU0
1.500
1.770
2. mo
3.600
0.50
0.196
Amount of Filteraid to use
Area Sq. Feet
Conversion Factor ml.
Gal*/Ft*
0.00307
0.0861
0.0050
0.0528
0.005U5 0.0100
0.0185 0.0261*
0.0123
0.0215
0.0250
0.0106
0.00136
0.1943
weight of liquor x % Filteraid
100
Dicalite Products
Superaid
UF Grade Specdflow Sp. Speedflow Soeedplus 372 Socedex U200
Relative Flowrate Rating_______
1
1 1
2 3 7 8 10 18
Competitive Offering
Filtercel FiUtercel Celite 50$ Standard Supercel Celite 512
Hyflo Supercel
Celite 501 Celite 503 Celite 5U5
Formulas
(1) F2 = FX x\ r1
F^ r Flow obtained during tests at
on bomb filter
Pi z Pressure used to obtain Fi
F2 = New flow to be obtained at new pressure
?2 z New pressure used to obtain new flow
f> (2) Rate: Gallons/Ft4'/'.it. r ml. Flow x Leaf Conversion Factor
Cycle length in Hours
(3) Total Flow in ml. - Gallons /pt^/Hr, x Cycle Length in ?Isurs Loaf Conversion Factor
(]j.) Cake Thickness - 21 min, Calce Thickness in inches x desired cycle n?.. _flow
21 minute ml. flow
ST0002659