Document QMk71x0DeMrobK4o24ypMz3pR
INDUSTRIAL CHEMICALS CO. RESEARCH &/DEVELOPMENT
--_ REPORT NO.- P-X733
--
JOB NO.- 43-000-760.22-1648005 43-000-760.22-1348305
PROCESS FOR MANUFACTURE OF INTERIM QUANTITIES OF MCS 1043
DATE- June 18, 1973
WRITTEN BY- D> R< Cova
Monsanto
ST. LOUIS, MISSOURI
AD-44? Rev ) n 2
COMPANY CONFIDENTIAL
MONS 057721
THE FILE COPY OF THIS REPORT
RECEIVED MANAGERIAL AND
, ...
|
MONSANTO INDUSTRIAL CHEMICALS COMPANY
Report No. P-1733
Job No. 43-000-760.22-1648005 43-000-760.22-1348305
PROCESS FOR MANUFACTURE OF INTERIM QUANTITIES OF MCS 1043
Date: June 18, 1973
Written by: D. R. Cova
Work done by: J. L. Bernhardt D. R. Cova K. W. Holbcrt J. E. Silver
MQNS 057722
Distribution of Report No. P-1733
1. Tech. Reports Library - Permanent Copy 2. Tech. Reports Library - Loan Copy 3. Tech. Reports Library - Loan Copy 4. Circulate to Director, Technology Planning and Evaluation,
R&D Managers, then to Tech. Reports Library - R229 5. D. R. Cova - T3C 6. J. F. Quinn- T3B 7. W. R. Richard - T3B 8. J. E. Maurer - Patent Dept. 9. J. R. Savage - Manufacturing Dept. 10. R. M. Kountz - CED 11. J. K. Grant - WGK
12. K. E. Boucher - WGK 13. R. H. Munch - TIB 14. Standards Department - W. G. Krummrich Plant
16. "
"
"
This document is the property of MONSANTO COMPANY. It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed te unauthorized persons or sent outside the Company without pro per authorization. The recipient is responsible for its safe keeping and return upon request.
HONS 057723
TABLE OF CONTENTS Page No.
INTRODUCTION ......................................................................................... 1 SYNOPSIS OF PROCESS ....................................................................... 1 CHEMISTRY OF PROCESS ....................................................................... I BILL OF MATERIALS...............................................................................2
Process Flow Diagram and Material Balance PROCESS IN DETAIL................................................................................... 2 DISCUSSION OF VARIABLES ............................................................. 4 MATERIAL SPECIFICATIONS AND
ANALYTICAL PROCEDURES ............................................................. 8 CONTROL ANALYSES ................................................................................ 8 TOXICITY AND HAZARDS..........................................................................8 ENVIRONMENTAL PROTECTION ......................................................... 15 APPENDIX
A. Material Specifications B. Analytical Procedures C. Stream Data
1. Specific Gravity versus Percent Chlorine for Chlorinator Control
2. Crystallizing Point versus 4,4'-Dichlorobiphenyl Content for Column Control
HONS aim*
INTRODUCTION
HCS 1043 is a chlorinated biphenyl containing 28-29t chlorine as
compared to Aroclor 1016 which contains 41.3% chlorine. MCS 1043
contains low concentrations of tetrachlorobiphenyls and essential
ly non-detectable levels of pentachlorobiphenyls. Its use is in
dielectric fluids.
'
It was made in drum quantities in the Monsanto Research Corpora tion pilot plant in Dayton, Ohio. The purpose of this report is to describe the procedure for manufacture of interim quantities
in the Aroclor department at the W. G. Krummrich Plant.
This process was written to cover specifically the case of a short plant run (probably only one fractionation batch) and was tailored to fit into the Aroclor 1016 equipment at the W. G. Krummrich Plant.
It is for this reason that product yields are low (60% of theo
retical) . With an extended run in proper facilities, product yields would be higher (about 88% of theoretical). The reason for this is that with an extended run it would be possible to recycle some of the non-product streams from the process.
SYNOPSIS OF THE PROCESS
Aroclor 1129 is manufacturered by chlorinating biphenyl. This material is then fractionated under vacuum through a 30 plate sieve
tray column. This is a batch fractionation in which two cuts are taken. The first cut is a biphenyl-rich forecut. The second cut
is the main fraction. This fraction after Porocel treatment is MCS 1043. The stillpot residue can be distilled in a straight
takeover still and then converted to Aroclor 12S4. The forecut can be recycled to chlorination'to make Aroclor 1016 or 1254.
CHEMISTRY OF PROCESS
+ X HC1
n
Where X - 1.76 for Aroclor 1129. Theoretically, n can range from 0 to 8. However, for Aroclor 1129 homologs with n greater than 6 have not been detected. The distribution of homologs resembles a normal.statistical distribution. For Aroclor 1129 the dichlorobiphenyl isomers (n 2) comprise the major homolog in the mixture
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MONS 057725
Fotetur
Ma/aS FpAc t10a/
Orr<*S ContentAit
&301 fA
CAT-At-YiT 0 rre-4nL
OfU- OKIJA TOKS ----------------- 3
L/MS
St/li. Caaxg
FfLfiC VMAWM fyere/i
Cm-oaM*
FesiPite
Pofoc-et* Pu.fi**
MCS /OiJ
t~ L6. _Zi_ FLow p/ACFAM FOR MCS 1015
Stream Component
B1phenyl Aroclor Line FeCl3 Chlorine H.C1
TABLE I MATERIAL BALANCE FOR MCS 1043
Biphenyl Catalyst Chlorine Offgas
Feed
Slurry Gas
Conden sate
HC1 Offgas
Aroclor
1129 Still Charge
Lime
Forecut
Main Fraction
to
Stlllpot Residue
Porocel Purge
Porocel
MCS 1043
113.9
6.1
0.06
97.0
4.2 4.1 0.1
0.1
1.6 0.03 161.3
29.3 103.9
28.0
4.0 99.9
0.6 0.6
0.06
0.06
49.9
TOTAL
Temperature, C Volume, Gal.
113.9 6.2 97.0
100 14.a
100 25 0.8 535
1.6 49.9
165.6
0.6 33.4 104.0 28.6
40 40 0.1 562
190 17.5
25 -
65 65 275 3.8 10.1 2.8
4.0 100.0
65 65 0.4 9.7
-2-
BILL OF MATERIALS
The following quantities of raw materials are required to produce 100 lbs. of MCS 1043:
Biphenyl Chlorine FeCl3 Catalyst Lime
120.0 lbs. 97.0 lbs.
0.06 lbs. 0.6 lbs.
Product yield on both biphenyl and chlorine is 60% of the theoreti cal. Most of the remaining 40% will be converted to Aroclor 1254.
PROCESS IN DETAIL
A. Chlorination
The chlorination is carried out in the 4-stage continuous chlorination system presently used at the H. G. Krummrich Plant for making Aroolor 1142. Except for a lower usage of chlorine the manufacture of Aroclor 1129 is very similar to that for
Aroclor 1142.
The chlorination is best started up by charging appropriate amounts of biphenyl and PeClj catalyst to each stage and then chlorinating each stage up to its normal operating level. The following table gives the chlorine concentration and specific
gravity for the product overflowing each stage:
Table II
Chlorination Levels in Bach Reactor Stace
Stage No. Wt. % Chlorine in Product
Specific Gravity c
1 8.8 2 16.9
3 23.4 4 29.0
1.041-1.061 1.100-1.120 1.152-1.172 1.210-1.220
After each stage has been chlorinated to itB proper level, the system can be placed into the continuous mode. 113.9 lbs. of biphenyl
and 6.7 lbs. of catalyst slurry (0.06 lbs. of FeClj in biphenyl) are fed to the first chlorination stage. A total of 97.0 lbs. of chlorine gas is fed to the reactors. Each stage is fed an equal portion of chlorine (or 24.2 lbs.). The chlorine gas feed rate to each stage is further adjusted so that the product over flowing each stage falls within the specific gravity range given in Table II.
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MOMS 057728
Reaction temperatures for each stage will be the same as for Aroclor 1142, 150C in the first stage, 160*C in the second, 180*C in the third, and 190'C in the last stage.
HC1 gas is given off as a product of chlorination. This gas carries with it some biphenyl and Aroclor. The gas from all the stages is collected in a common header and is then cooled to 40*C. This causes condensation of 1.6 lbs. of organic material from the gas stream. This offgas condensate is collected as a separate stream. The cooled HC1 offgas (49.9 lbs.) is piped to the chlorosulfonic acid department. At this point it contains 0.03 lbs. of Aroclors.
165.6 lbs. of Aroclor 1129 overflows the last chlorination stage and is collected for batch fractionation in the 30-tray column in the department.
Fractionation and Porocel Treatment
The fractionation is carried out in the 30-tray column presently used in the manufacture of Aroclor 1016. The system is operated under vacuum with a pressure of 40 torr at the head of the column. This should give a pressure in the stillpot of about 145 torr. Under these conditions stillpot temperatures will range from 230*C at the start of distillation to 280-290'C at the end of the cycle. Column head temperatures will rise from 165*C at the start to 215C at the end of the distillation. The distillation is carried out batchwise.
Aroclor 1129 is charged to the stillpot in the amount of 165.6 lbs. 0.6 lbs. of lime is added to the charge to react with dissolved HC1 in the charge and with any traces of HC1 formed during distillation. The system is placed under vacuum and heat is applied to the reboiler. The system is brought to total re flux and is allowed to line out. After lining out, distillate flow to the forecut receiver is started at a reflux ratio of 15/1. Flow to the forecut receiver is maintained until biphenyl concentration has fallen to 4.2%. At this point the forecut will be finished.
Biphenyl concentration can only be obtained by gas-liquid chrom atography (GLC). It will be necessary then to sample the distil late frequently as the end of the forecut approaches. Since some time will be required to generate analytical results it will be necessary to place the column on total reflux during this time. When the result has been obtained, it can be decided whether or not to continue with the forecut. in this way, 33.4 lbs. of forecut will be obtained.
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MONS 057729
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When the forecut is finished, the distillate flow is diverted to the Porocel column. Distillate temperature should be adjusted to 65*C before passing through the Porocel unit. The first 4.0 lbs. of distillate passing through the Porocel column will be the Porocel purge. It should be collected separately from the main fraction. When the purging has been completed, the flow of Aroclor from the Porocel unit is diverted to the MCS 1043 storage tank. The reflux ratio is reduced to 3/1. This reflux ratio is maintained until a total of 112 lbs. of distil late has been collected (this includes the forecut and Porocel purge). At this point, the reflux ratio is increased to 5/1 and is maintained there through the remainder of the distilla tion.
The distillation is finished when the overall concentration of 4,4'-dichlorobiphenyl (4,4') in the MCS 1043 in the storage tank approaches 2.0%. It is desirable to approach close to the 2.0% level (say 1.8%) in order to keep up the yield and to keep at a high level the concentration of 2,4'-dichlorobiphenyl in the MCS 1043. This latter component has valuable dielectric properties. It will distill over before the 4,4', but there will be some mingling of the two components. The endpoint of the distillation will be best found by chromatographic analysis of storage tank samples. This means that it will be necessary to place the column on total reflux while awaiting the results of analyses. Fig. 3 in the appendix gives a plot of 4,4' concen tration in distiTlate versus crystallizing point. We estimate that at the point at which the 4,4' concentration in the storage tank approaches 2.0%, the instantaneous concentration of 4,4' in the distillate coming off the column will be about 20%. This however is only an estimate. We recommend that when the instantaneous concentration of 4,4' rises over 7%, the column be placed on total reflux and the storage tank contents be analyzed.
In this way, 100.0 lbs. of MCS 1043 is collected in the storage tank. The fractionation is now shut down and the stillpot resi due is pumped to residue storage to await straight takeover distillation. Residue distillation should be the same procedure as the distillation of the stillpot residue from the Aroclor 1016 process.
DISCUSSION 9F VARIABLES
A. Chlorination
1. Reaction Temperatures
The reaction temperatures chosen were the same as those for Aroclor 1142. It is recommended that higher temper atures not be used, because otherwise losses to the offgas
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MONS 057730
-5-
condensate stream will be too large. Lower temperatures may give a product that is less stable.
2. Continuous versus Batch Chlorination
Laboratory process work used batch chlornated Aroclor. Comparisons of batch and continuously chlorinated Aroclors have led us to the conclusion that continuous chlorination will be adequate for this case. Nonetheless, the Aroclor 1129 produced should be checked against the tentative speci fications given in the appendix. It is likely that contin uous chlorination will give a product with higher biphenyl
concentration than would batch chlorination. However, we believe that it will fall well within the specifications.
3. Percent Chlorine in Product
The crude Aroclor should contain 29 weight % chlorine. A lesser degree of chlorination will leave too much unreacted biphenyl in the crude product. This could cause a large increase in forecut size at the expense of the main fraction. A higher degree of chlorination would cause a larger stillpot residue and a smaller forecut. Up to 31% chlorine, the size of the main fraction may not be affected very much.
Above that point we will lose yield.
4. Chlorine Distribution
The chlorine gas should be approximately equally distrib uted to all four reaction stages. Any gross variations from . an equal distribution could lead to changes in Aroclor homo log distribution such as increased biphenyl and residue component concentrations.
B. Fractionation and Porocel Treatment
1. Column Pressure and Temperatures
A head pressure of 40 torr was chosen. With this pressure and an estimated column pressure drop of 105 torr, the stillpot pressure will be 145 torr. With this pressure in the stillpot, temperatures will not exceed 300*C. Temper atures below 300"C are desirable to prevent possible thermal - decomposition. Therefore, a head pressure of above 40 torr should not be used. Lower pressures will only reduce column capacity and increase column vent losses.
2. Distillate Freezing Points
There should be no difficulty here. The highest distillate freezing point should not exceed 65*C except possibly for the
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MGNS 057731
-6-
first small portion of forecut. If this is relatively pure biphenyl the crystallizing point could be 70*C but no higher.
3. Reflux Ratios
The recommended reflux ratio program was demonstrated in the laboratory. There should be no need to deviate from this program, unless the biphenyl content of the crude is too high. In this case it would be necessary to run through the forecut at a higher reflux ratio to reduce the forecut size.
4. Column Control
There are four points in this fractionation where action has to be taken. These are: (1) the end of the forecut, (2) the end of the Porocel purge simultaneous with a lowering of the reflux ratio and the beginning of the product frac tion, (3) an increase in reflux ration, and (4) end of the distillation.
The end of the forecut is best found by chromatographic analysis. This is the only accurate way in which low levels of biphenyl can be detected.
The second point, the end of the Porocel purge, is best determined by the volume fad through the Porocel bed. In other words, when the distillate integrating flow meter has indicated that a volume equivalent to 4.0 lbs. has passed through the Porocel column, the flow from the Porocel column is then diverted to product storage and the reflux ratio is lowered.
The third point, at which the reflux ratio is increased, is again best detected by the integrating flow meter. When the meter indicates that a total volume of distillate equivalent to 112.0 lbs. has been taken off, the reflux ratio is in creased.
The last point, the end of the fractionation, is determined by the concentration of 4,4' in the product in the storage tank. When this level approaches 2% the fractionation is fihished and the distillate flow must be cut off. The level of 4,4' in the product can only be accurately determined by gas-liquid chromatography. As an estimate only, the crystallizing point of the distillate coming off the column can provide a guide to the approach of the end of the dis tillation. When the crystallizing point of the distillate rises to +10"C, the end of the distillation is near. This
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NONS 057732
-7-
crystallizing point test should only be applied after point 3 in the cycle has been passed, because there will be distillate with higher crystallizing points in the early part of the forecut and in the first portion of the main fraction.
5. Product Changeover
In going from Aroclor 1016 to MCS 1043 the greatest possibility of contamination is after fractionation, specifically in the Porocel bed and in piping and the storage tank. The storage tank and piping should be carefully cleaned. The last material through the Porocel bed will have been Aroclor 1016 from the end of the fractionation. This material from the end of the fractionation will contain high levels of highly chlorinated biphenyls (the High Boiling Homologs or HBH) . This material should be displaced from the Porocel bed. This can best be done by circulating Aroclor 1016 from the storage tanks through the Porocel bed until the high HBH material has been displaced. The Porocel bed will now con tain Aroclor 1016 which has a relatively low HBH content (0.4% is the specification, but product analyses generally show in the range of 0.1%). At this point, the Porocel bed should be drained of Aroclor 1016 as well as possible. However, Aroclor 1016 absorbed in the packing cannot be re moved. The Porocel purge with 4.0 lbs. of MCS 1043 distillate will displace some of this Aroclor 1016, but there is no doubt that some will remain to leach out into the MCS 1043 main fraction. Contamination (within reasonable limits) with Aroclor 1016 or Aroclor 1142 before fractionation should give no problem, because the fractionation procedure will keep this material in the reboiler.
Going from MCS 1043 to Aroclor 1016 will also require pre caution and cleanup. Any equipment (as, for example, inter mediate Aroclor 1129 storage) which has contained Aroclor 1129 should be carefully cleaned before any Aroclor 1142 is placed in it. The contents of the chlorinators at the end of the MCS 1043 run can simply be chlorinated up to their proper chlorine levels for Aroclor 1142 production. The first Aroclor 1016 distillate off the Porocel units should be examined for biphenyl content. It may be necessary to discard a first small portion of the first Aroclor 1016 run. The Standard Manufacturing Process for Aroclor 1016 describes the change over from MCS 1109 (monochlorobiphenyl> to Aroclor 1016 and this may provide some guidance for this changeover.
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MONS 0573
-8-
MATERIAL SPECIFICATIONS AND ANALYTICAL PROCEDURES
Material specifications are given in Appendix A. Included are tenta tive epecifications for the crude, Aroclor 1129. Theee specificationa on the crude should be met if the refining system is to produce satis factory MCS 1043.
Analytical procedures are given in Appendix B. Also, method numbers for standard methods are given in the specifications in Appendix A.
CONTROL ANALYSES
Control analyses are required in both process steps, chlorination and fractionation.
In chlorination, specific gravities must be run on effluent from each chlorination stage and especially from the last stage. The sampling procedures and frequency used now for making Aroclor 1142 should be adequate for this process. Samples of Aroclor 1129 should be analyzed by GLC to ensure that the material meets the tentative specifications. A 16 oz. sample taken once a day should be sufficient for this purpose.
In fractionation, control samples will be needed to determine the end of the biphenyl forecut and to determine the end of the fraction ation. As the end of the forecut nears, samples of the instantaneous distillate should be taken for every 1 or 2% of the charge distilled (approximately 200 to 400 gallon increments). A 16 oz. sample would be sufficient. A GLC analysis to determine biphenyl content will be required.
In determining end of the fractionation, it will be necessary to ana lyze both the material accumulated in the distllate receiver and the material accumulated in the product storage tank. GLC analysis will be required, and a 16 oz. sample should be sufficient. As the end of the fractionation nears, it is recommended that BampleB be taken for every 1 or 2t of the charge distilled (an increment again of 200 to 400 gallons of distillate). From analysis of these two samples it can be decided whether to take off more distillate or to shut down.
TOXICITY AND HAZARDS
The following section has been lifted bodily from the report "Sug gested Procedure for MCS 1043" by J. E. Silver (Report No. P-1584).
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MONS 057734
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. '
' ' SAFETY & TOXICITY DATA
Safety Equipment
The following is a list of safety equipment (personal and departmental)
required In department 246.
;
...
1. Fire extinguishers:
...
'
. . A. .Dry Chemical (3) - Southwest corner Bldg. CR - Main Floor.
.
- West wall at top of stairs of Second Floor.
, ; .B. Carbon Dioxide Snow - Southwest corner of Bldg. CR. ground level.
2. Chlorine Gas Masks (4) - southwest corner, second floor
`' .
'
'.
Control room, second floor
v ...
''
. .- East side, outside control room
- Wall, Southwest comer of sprinkler house,
i . ' sialn floor.
J. Scott Air Masks - West of Lean-To
4. Safety Showers (2) - Southeast corner of Bldg. CR, ground level.
' ... - Southeast corner of Bldg. CR, 2nd Floor.
5. Davis Vapotester
6. .Eye Baths
Safety Precautions
;.
' The following are safety precautions followed In the operation of
. department 246.
..
1. '-
.
Safety Equipment of Bnployee
`
Each- employee"has the following safety equipment: (1) Hard hat
(2) Safety glasses (3) Goggles (4) Rubber and canvas gloves
Special equipment may be Issued as
necessary for performing a particular job In a safe manner.
HONS 057135
-10-
SAFETY & TOXICITY DATA (Cont'd.)
Safety Precautions fcont'd.)
'
2. Sampling of Crude Aroclor
|.
The samples olJ Aroclor taken during the chlorination reaction are
I
j'
hot (170C.). Precaution must be taken to avoid skin contact of samples and inhalation of Hydrogen Chloride, Chlorine and Aroclor
1 vapors.
`
3. Fires
Fires may result from the Ignition of leaking gas. Xylene, Diphenyl,
rags, paper, wood, etc. Automatic fire extinguishers and sprinklers
. have been Installed to combat fires.
' 4. Explosions
_ ' Bxplosions' may be caused from accumulated pockets of natural gas
or a rapid burning of Diphenyl in a closed container such as a
Chlorinator. Chlorlnators are equipped with a 3" diameter
,,
pressure relief line with a rupture disc made to burst at <7 pal
. \ . In case Diphenyl within the Chlorinator Ignites.
5. Toxicity
*
. . ToxicTEy does not present a serious problem. However, a complete
dally change of clean clothes Is supplied to each person and time
' . is allotted at the end of each shift to take a bath. Instructions
' . are also issued to avoid actual skin contact with Biphenyl and
- Aroclor as much as possible and to wash hands and face before
eating.
. 6. Miscellaneous . There are many accidents that can occur that may be classified as
- health and safety hazards. These accidents may result from such
things as broken process lines, acid leaks, steam leaks, etc.
'
The worst Inherent hazards are as-follows:
.
'
. '
1. Free Chlorine from ruptured line or major leak.
..2.. HC1 Oas from ruptured line or major leak.
3. Dropping bottoms from stills.
..
4. Hot Aroclor & Diphenyl.
..
'
AROCLOR
Toxicity: This material Is a liquid under normal conditions and has a
medium toxicity range for liquid ingestion and high toxicity for vapor
Inhalation. The maximum allowable concentration (M.A.C.) is 1 mg/cublc
meter.
.
Fire Hazard: There is no fire hazard under normal conditions. Aroclor
mixes (xylene. Toluene, Butyl Acetate, etc.) may burn and explope at hlgn
temperatures when exposed to flames.
HONS 057736
-11-
SAFETY & TOXICITY DATft (Cont'd.)
Other Hazards: This material can cause dermatitis, systemic poisoning from the i'umes, and yellow atrophy of the liver. There are skin, mucous membranes and eye hazards encountered in handling this material.
Treatment and Antidotes: Call a physician and remove patient from fumes.
Storage and Handling: Protect the skin, lungs, and eyes by wearing approved protective clothing, respirator, and goggles. People who handle this material at elevated temperatures should have medical supervision, andthe air should be sampled to Insure compliance with M.A.C. There are no special storage restrictions under normal conditions except store in a
ventilated area.
Shipping: There are no special shipping restrictions.
.
FERRIC CHLORIDE (FeCl3)
Toxicity: This material is a solid under normal conditions and is non-
toxlc or has a rating as low.
.
Fire Hazard: There is no fire hazard under normal conditions, but it will emit toxic fumes at high temperatures.
Other Hazards: Some people are allergic to this material and may develop skin rash, and there is an eye hazard.
Treatment and Antidotes : Call a physician.
Storage and Handling: Protect the s.cin with approved protective clothing,
avoid the breathing of FeCl3 dust, wear approved respirator with adequate
cartridge, and protect the eyes with approved goggles. There are no
storage regulations.
.
Shipping: There are no shipping restrictions.
DIPHENYL (CfiHgCfiHQ
.
Toxicity: This material is a solid at normal conditions and is medium toxic. The M.J\.C. of vapor is 2 mg/cubic meter of air. If ingested, the lethal aose is 2.4 g/Kg of body weight. The fumes are not dangerously deadly, butrthey are poisonous over a prolonged time.
Fire Hazard: Diphenyl is very flammable and will burn when exposed to heat or name or oxidizing materials.
Other Hazards: Diphenyl is not too corrosive to skin, but it will affect
the eyes.
.
HONS 057737
-12-
SAFETY & TOXICITY DATft (Cont'd.)
DIPHENYL (C(3H5C6H5) (Cont'd. )
Treatment ami Antidotes:' Wash eyes with water and get the patient to fresh air. Try-to ,;ot patient to vomit, and call a physician.
Storage and Handling: This material can be stored In steel containers away lrom fire hazards and oxidizing agents. Wear suitable clothes and approved goggles when handling diphenyl.
Shipping: Ship In cars or other suitable containers with a red warning
'label of flammability.
-,
LIME Ca (OH) a
Toxicity;' Lime la not dangerously toxic, and It is regarded as more of
a nuisance. This material is a solid or slurry.
Fire Hazard; This material Is not flammable.
Other Hazards: Lime Is very hazardous to the eyes. It will burn the skin also/ and the dust will affect the mucous membranes.
Treatment and Antidotes: Flood eyes and skin with large quantities of water, if lime is ingested, get patient to vomit and call physician.
Storage and Handling: Lime can be stored In steel containers, and people
should wear protective clothing, respirators, and rubber or chemical safe
goggles when handling lime.
.
Shipping: There are no special restrictions for shipping, but the containers should have a white label, a caustic warning.
HONS OS??38
SAFETY & TOXICITY DATA (Cont'd.)
ATTAPUIC.US EARTH;
Toxicity: This.earth Is not toxic In general.
Fire Hazard; There Is no fire hazard.
.
Other Hazards: Attapulgus earth can create a dust hazard similar to other dusts tKat contain silica.
Treatment and Antidotes: Consult a physician.
Storage and Handling: Attapulgus earth presents no special storage problem and should be handled by'persons wearing an approved respirator.
Shipping: There are no special restrictions on shipping.
HYDROGEN CHLORIDE (HC1)
.
Toxicity: This, material is a gas under normal conditions and Is very
toxic. The M.A.C. Is 5-10 ppm and a concentration of 1500-2000 ppm would
be fatal to humans In a few minutes.
'
Fire Hazard: There is no fire hazard under normal conditions, but vret gas reacts with some metals to form hazardous hydrogen.
Other Hazards: This material Is hazardous to teeth, skin, eyes, and
mucous membranes.
.
Treatment and Antidotes: Wash profusely with water, if invested, eat chalk,
magnesium hydroxide, egg whites, and milk, and also administer oxygen.
Call a physician.
.
Storage and Handling: This material should be stored in a cool, well ventilated area away from oxidizing agents. This material can be stored In rubber lined, glass, or tantalum vessels. People handling this material should wear suitable clothing like rubber aprons, shoes, and gloves. Also rubber goggles or chemical safe grades and approved pack or canister gas masks.
Shipping: Shipping containers must have a white warning label and a
non-tlammable label. Ship In appropriate containers such as rail car
or carboy.
.
CHLORINE (Cla)
Toxicity: This material is a gas under normal conditions and is very toxic. The M.A.C. la .35 bo 2 ppm. A concentration of 1000 ppm would be rapidly fatal. Least concentration with detectable odor is 3-5 ppm
HONS 057739
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SAFETY & TOXICITY DATA (Cont'd.)
CHLORINE (Cla) (Cont'd.)
Fire Hazard: There Is no fire hazard under normal conditions, but there is an explosion hazard If chlorine is mixed with a strong reducing agent such as hydrogen or hydrocarbons at high temperature.
Other Hazards: This material causes eye, skin, and mucous membrane irritation
Treatment and Antidotes: The patient should be given oxygen immediately and treated for shock. Call a physician.
Storage and Handling: This material should be stored In a ventilated
and cool place away from fire hazards. When handling, wear a gas mask
or approved respirator, clothing and rubber or chemical safe goggles.
In strong chlorine concentrations, wear canister gas masks, Scott air
.pack, or oxygen breathing apparatus.
.
Shipping: The shipping containers must have a green gas label and a non-flammable label on. Ship In steel cars or cylinders.
HONS 057740
-15-
ENVIRONMENTAL PROTECTION
Thar* are six non-product streams leaving this process. These are: offgas HC1 which contains some Aroclor; the forecut fraction; the Porocel purge; the stillpot residue; the column vent loss; and the offgas condensate. These may be handled as follows:
The offgas HC1, 49.9 lbs. of gas containing an estimated 0.03 lbs. of Aroclor, can be handled in the same fashion as the offgas from the present Aroclor 1016 process. The gas is piped to the chlorosulfonic acid department where it is passed through a chlorosulfonic acid scrubber. The Aroclor content of the gas leaving the scrubber is down to the non-detectible level.
The forecut fraction, 33.4 lbs. of biphenyl and monochlorobiphenyl, and the Porocel purge, 4.0 lbs. of essentially monochlorobiphenyl, can be handled in two alternate fashions. They can either be piped back to biphenyl storage for subsequent chlorination to Aroclor 1142 or else they can be fed to the batch chlorinators for chlorination to produce Aroclor 1254.
The stillpot residue, 28.6 lbs. of the higher Aroclors, can be handled in the same way as the present stillpot residue from the Aroclor 1016 process. This material should be straight-takeover distilled to remove lime and FeCl3 catalyst. It can then be further chlorinated to produce Aroclor 1254.
The Standard Manufacturing Process for Aroclor 1016 shows a vent loss from the column of 0.09 lbs./day when city water is flowing to the vent condenser. Based on this and vapor pressure data, we estimate a column vent loss when running on MCS 1043 of 0.4 lbs./day with the vent condenser on. This will contain some biphenyl but will consist mostly of mono- and dichlorobiphenyls.
The offgas condensate (1.6 lbs.) is composed of unreacted biphenyl and Aroclors. It can be recycled to chlorination to make Aroclor 1254.
Approved by:
D. R. Cova
J. F. Quinn Manager
Engineering Specialties
HONS 057741
Appendix A Material Specifications
HONS Q577<|2
Monsanto
RAW MATERIAL SPECIFICATION
MATERIAL CROC 62601
PLANT WGK
.10/23/70
DIPHENYL (BIPHENYL)
246' SUPPLIER
Anniston Plant
P*Mv(llN a . js. telax-
, J. Leycrle
research
OIUfA--L'T,BT LCO.N-THROlcuLTh( CaMridf C_A_n_i_Ii R. Blowers
CHEMICAL FORMULA
0-0
mol wt. 154.20 specs or
2/6/69
CHAflSCtERISTiff
2 x 16 os. W. M, Bottles
UNRESTRICTED INFORMATION
<R) .Appearance and Color
Light Yellow Cryst. Solid
(R) Crystallizing Point (R) HtO GENERAL INFORMATION
68.7*C. , min. ppm mt;.
| ISSUED IV -iS.. Shaulter/G Sv.it-
10,252 10,298 13,155
Distillation Range: First Drop to Dry Point
2. 5*C. , max. .
Must Include 255*C. within range .
10,299
This specification is the property of Monsanto Company and is (or
internal use only.
'
HONS 057143
MOflSdlltO lit
FINISHED PRODUCT ! SPECIFICATION
T. w. iDalton A , E. Lelsv
IPTIOM
IChlorine (Snlft Oae)
B P, t'iiiti,fr
1-...."] ____ ___ 1-1-1
WOK
81060
Ubb'l COOK
11/69
| "'232 _IL_U|-- ' `1---------------------
Internal
fciugiiilr ` 1,1 1
' '
V.'. R. Richard
...
QUALITY eOMTKOb (CM(OimltU
R- M.. Blnwwrg IwimttL nilwiht
'
UMMiaii
or
10/66
Mixture
*M4I.Via 100 c.c. Gee Burette
|Wy4t S "-- 11 1 Hiqqer8on/Stites
UNRESTRICTED INFORMATION ' Cblorina (Clj)
Typical Analveee 8oft, By Volume
Oxygen (Oj)
3% "
"
Carbon Dloxidi (COt)
1.5ft "
"
Carbon Monoxide (CO)
0.1ft
"
Hydrogen (H|)
1.0ft " "
, Inert Gaeees (By difference) 8.4ft " "
Moletura (HjO) @ Std, Condition*
2.4 * 10' * lb*./ft.' (Average)
Direct pipeline-transfer* to uelng Dept*.
2 3 3 , 236 , 2 37 , 246
TJhie epecification 1* for Internal ue* at WCX Plant only.
I Atrutme inulytit.
' AnplyttJ by i
ftniy
HONS 057744
^Monsanto ^
,G. Krummrich Plant
RAW MATERIAL SPECIFICATION
*tnoN ?. Lelsv , Leyerle
33500 RbAMT
Ferric Chloride Anhydride U*lMO OIPTI,
WGK DATE VWWCCTIVW
SUfRlICM
233
: Jan. 31, 196<
McKesson tc Robbins
APPROVALS " aciiMCH
" ,r "
. V/. R. Richard
R. Blowers
T. Bell
CHtMUAL ypRMUCA
iolwt. 162.21 1/7/56
Fe Cl,
iampli for analysis
1 x 8 oz. W.M. Bottle
lueTKfiiaric
LIHtTI
INHESTRICTED INFORMATION
hpsarancs 1
kiuy aliate s rrous Salts
liability: 10:10 of Water
10:10 of Formula 30 Alcohol
Black powder or Granules 97.07a, min. 0.057o, max. frace, max.
Complete to slightly turbid, max. . Complete to slightly turbid, max.
[inuioa* ~
Hlggerson/'Stites
MlTHOe
J.F.Q. 16-A
22-570 120-570 S-570-1 112-B
isiysis, AtI slhsi Ivttd epyueef r
HONS 057795
Monsanto
R AW MATERIAL.
SPECIFICATION
MATERIAL COPE 38800
W.O.K. DATE EFFECTIVE
V7/70 APPROVALS
MATERIAL Lime, Hydrated Ul|N D(PTI> 287, 750. 246
Mississippi Lime Co.
A. G. Leisy
T. W. Dalton
W , R. Richard OUALITT control (Cm*/ CkMi/Mj
reverie___________________________________ ---- R ^ R1 QUA TTR
_________________________
CHEMICAL FORMULA
Ca (oh)2
MPtmion RCC*OF
AMPLE FOR AMALTAI*
a/i8/6.q_________________ 1 X 16 oa., W.M. Rattle____
na-nc
limit*
Appearance
Fine white or slightly gray
powder, free from lumps or gritty material.
Assay (Ca(OH)g)
92.00#j min.
Carbonates as (CaC03)
3.OOJ6, max.
Magnesium
0.50$, max.
Sulfates (as SO-j)
0.30JC, max.
'
hiihoo
-10,188
10,191
10,193 10,192 10,189
Supplier's certificate of analysis to be sent on day of shipment to:
Chief Chemist, Monsanto, Sauget, Illinois
HONS 057746
. Monsanto^
rawMaterial.
SPECIFICATION
itAinw1 y . Levari*
U4TIAk COM
48289
|MATCMtAL
.
REGULAR POROCEL
WGK
IMINO DIP Tl,
246
P*TI IPPICTIVK
APPROVALS
miiiamcm
Porocel Corp. (A Subsid. o 'S'...........................
W. n. Hlr.harrt UAWIT V CONTROL (CM#/ CMU
.
R. M. Blowers CNIMICAl WOeMULA
ACTIVATED BAUXITE
(mvio r
jtm--------------------------------------- 2 x 16 oz. H. M. Bottles -Higgeraon^fitltea
tSTRICTED INFORMATION
Appearance
' '
Hash Test: Less than 60 mesht
20 to 60 mesh inclusive! Greater than 20 mesh:
Water
Volatile Matter (at 1000*C. to constant
weight)
Free from lumps and foreign material
3%, max. 67%, min. 30%, max. 1%, max.
2%, max.
10,69210,100
**/ Antfftit. Ait eHew A*mir--4
mrif.
HONS 057747
TENTATIVE SPECIFICATIONS FOR AROCLOR 1129
Biphenyl Content
2,4'-Dichlorobipheny1 (includes 2,3-Dichlorobiphenyl) Content
4,4'-Dichlorobiphenyl Content
Specific Gravity at 65 C =
< 5.0*
>17.0* < 6.3*
1.215
HONS 057748
TENTATIVE SPECIFICATIONS FOR MCS 1043
Biphenyl Content
< 0.1%
2,4'-Dichlorobiphenyl (includes 2,3-Dichlorobiphenyl) Content
>20.0%
4,4'-Dichlorobiphenyl Content
< 2.0%
Higher Boiling Homologs
< 0.02%
Resistivity
>5000 x 109 ohm-cm
Power Factor
< 0.1%
Method No. See GLC Method
rt ii II M
H *1
T02302
See procedure in appendix
See procedure in appendix
HONS 057749
appendix b
Analytical Procedures
HONS 057750
\
Physical Chemistry Method No. 69-13 Job No. 1630022
GAS CHROMATOGRAPHIC DETERMINATION OF THE 4,4'-DICHLOROBIPHENYL CONTENT OF ISOMERIZED AROCLOR 1232___________________
I 1 PURPOSE OF ANALYSIS
'to measure the 4,4'-isomer content of isomerized Aroclor 1232. I CHROMATOGRAPHIC CONDITIONS
Instrument: Perkin-Elmer Model 800
Type Detector: Flame Ionization
Column: 0.02" X 50' Carbowax 20M S.C.O.T. (support coated open tubular) capillary
Column Temperature: 215C
Flow Rates
Detector Block Temperature: 250C
Helium: 15 ml/min.
Injection Port Temperature: 300C
Auxiliary Gas: 15 ml/min.
Sample Volume Injected: 0.001 ml Split 30-to-l
Hydrogen: 30 ml/min. Air: 400 ml/min.
i RETENTION TIMES (UNCORRECTED) OF COMPONENTS SEPARATED (CHROMATOGRAM I mKcmr---------------------------------------------- -------------------------------------------------------------
Biphenyl (3.4'); Orthochlorobiphenyl (4.9'); Metachlorobiphenyl (6.6') j Parachlorobiphenyl (7.0'); 2,6'-Dichlorobiphenyl (7.5'); 2,2'-
Dichlorobiphenyl (8.0'); 2,4'- and 2,5'-Dichlorobiphenyl (8.2'); 2,3'Dichlorobiphenyl (9.6'); 2,4'- and 2,3'-Dichlorobiphenyl (10.3'); Unknown A (12.3'); 2,5,2'-Trichlorobiphenyl (13.0'); 3,3'- and 3,4'-- Dichlorobiphenyl (13.6'); 3,4'-Dichlorobiphenyl (14.4'); 4,4 '-Dichloro biphenyl (15.6'); 2,3,2'-Trichlorobiphenyl (16.4'); 2,5,4'-Trichlorobiphenyl (17.7'); 3,4,2'-Trichlorobiphenyl (19.6'); Unknown B (20.5'); Unknown C (22.D; 3,4,4'-Trichlorobiphenyl (31.6').
CALCULATION TECHNIQUE
Normalization.
PRECISION
No determination of precision was made. The variability of a single CC analysis at the 954 confidence limits is usually +1 to 24 relative.
db
Monsanto Company ` Organic Chemicals Division t Applied Sciences Section I St. Louis, Missouri
| 2/20/69 - G. M. Gasrer, E.M. Emery
MCN<: ,, 0577sl '
PROCEDURE roil MEASURING DISSIPATION FACTOR OR ft POWER FACTOR, DIELECTRIC CONSTANT AND RESISTIVITY OF ASKAR ELS
ft
INTRODUCTION This procedure covers the measurement of dissipation factor, dielectric
constant or permittivity and resistivity of electrical insulating fluids. The dissipation factor and the power factor of a fluid differ by less than one per cent of the numerical value when the dissipation factor is less than 0. 14. Since good insulating fluids have dissipation factors much below this, their dissipa tion factors and power factors can be considered equal for ordinary purposes. In some cases, power factor is given in percent. Care must be used in com paring values to be sure that all are given as fractions or in percent. Calcu lations given in this procedure give the fractional value of the dissipation factor. To convert these values to percent, multiply by 100.
Precautions: In the early development of this procedure Aroclor 1242 was found to be light sensitive. Light from sources such as fluorescent lamps, mercury vapor lamps, and incandescent lightbulbs caused a marked increase in dissipation factor and a decrease in resistivity. For this reason all dis sipation factor and resistivity measurements should be made in subdued light.
When measuring fluids having low dissipation factor values such as those found in Askarel fluids, it is extremely important that the utmost care be taken to prevent contamination of the sample. Minute quantities of contamination introduced into the sample either from the test cell, glassware, or in other ways will cause extreme differences in dissipation factor values. As little as 0. 1 part per billion of some impurities can be detected. Therefore, the test
a a aa a a a e
HONS 057753
-2cclls must be handled only with the cell holders or tongs. No part of the test cell or glassware which might contact the sample should be touched with hands or any support. Strict adherence to the cleaning and sample prepar ation sections of the procedure is a must. Dissipation factor measurements have been made using test cells that were cleaned and stored for 16 hours in the drying oven with satisfactory results: however, longer storage periods give increased dissipation factor values.
The cells are ordinarily cleaned without disassembling. However, if coatings or impunities remain after the standard cleaning procedure the cells can be taken apart and cleaned with soap and water on a soft cloth or bristle brush. This should not be done unless several passes through the standard cleaning; procedure fail to get the cell clean enough.
To take the cell apart for cleaning, first unscrew the 874 connector shell and pin from the top. Then unscrew the outer electrode from the body of the cell. Finally, unscrew the knurled nut from the center electrode and push it gently out of the body. No attempt to further disassemble the cell should be made. To reassemble, reverse the above procedure.
After cleaning the cell parts with soap and water, it should be reassembled, rinsed with distilled water and reagent grade acetone, then put through the standard cleaning-procedure until it gives the correct value when used to measure a known good sample.
Caution should be exercised when making resistance measurements on the Type 1644A Megohm Bridge. Never touch the cell or leads from the test Cell to the bridge when in the charge zero or measure position. 500 volts
MONS 057754
-3-
is applied to the cell in either position. Always return the switch to the
discharge position alter completing the resistance measurement before
attempting to remove the leads from the bridge to the test cell. The red
light on the upper right corner of the panel is on when the switch is in either
position. However, it is important to look at the switch itself; the pilot light
could be burned out.
APPARATUS
1. Electro Scientific Industries Capacitance Measuring System
Model '.II.
2. General Radio Type 1644A Megohm Bridge.
3. 110-24 Volt Step Down Transformer, Selenuim Rectifier type
RT201, Chicago Standard Transformer Corp. , Chicago, 111.,
with plug in adaptor unit for 60 cycle measurements.
4. Special Plug in Connector for measurements above 60 cycles 5. Two General Radio Type 874-Q9 or 777-Q3 adaptors.
6. General Radio Decade Resistor Type 1133-L. or box made using
one General Radio Type 510D and one 510E decade resistor in
series in a suitable metal box.
7. General Radio Type 274 NQS Patch Cord.
8. Coaxial Cable lead (General Radio Type 874 Patch Cord Cat.
' No. R22A).
9. Patch cord with banana plug terminals such as H. H. Smith Type 1863-36-102, Allied Radio Stock No. 47D1904.
10. Balsbaugh Test Cells (Stainless Steel) Type 350G modified
according to Monsanto specifications.
HONS 057755
-411. Constant Temperature Rath, a 12" x IE" Pyrex jar, insulated.
a. Constant Temperature of 100C. is maintained with a Fisher Proportional Controller using a thermistor probe as a temperature sensing device.
b. A 125 watt Cenco knife blade heater is used for intermittent heating controlled by the Fisher Proportional Controller.
c. A 450 watt Cenco knife blade heater is used as a continuous heater controlled by a variac to supply enough heat so that the intermittent heater is about half the time.
d. A Bodino stirring motor with attached stainless steel pro peller is used to maintain good agitation of bath liquid. The propeller is surrounded by a draft tube. It should draw the bath fluid up through the draft tube*
e. Glycerine is used for the bath medium with the liquid level maintained to within 3/4 inch from the top edge of the bath cover.
i. Standardized Centigrade thermometer for temperature read out (Princo Q-7, range 75-110C.)
g. Bath cover constructed from Extren 500 manufactured by J. T. Ryerson Son, Inc. , 2558 West 16th St. , Chicago, 111. 60608.
12. Drying Oven (Fisher Isoternp Junior Model 202) 13. Xylene Vapor Bath containing calcium oxide lumps (Test Cell
Cleaning).
MOMS 057756
-514. Boiling 29% NH^OH Bath (Test Cell Cleaning). A 1.5 liter beake r 15. Distilled H2O steam bath (Test Cell Cleaning). 16. Acetone Vapor Bath (Test Cell Cleaning). 17. Xylene Vapor Bath (Glassware Cleaning). 18. Distilled H^O Steamer (Glassware Cleaning). 19. Sample Vessel (Glass). 20. Teflon Lid for Sample Vessel. 21. Supporting Clamp (Sample Vessel). 22. Special Wrench for removing cente." pin connection from test ceil. 23. 50 ml. Pyrex Pipette (Taper Tip cut off to allow faster sample
delivery). 24. Fisher Thermix Hot Plate Cat. No. 11-493 (Acetone Vapor Bath). 25. Teflon Covered Stirring Bar (For Acetone Vapor Bath). 26. Laboratory Tongs (Fisher Cat. No. 15-202).
Drawings of the items of apparatus which cannot be obtained from laboratory supply companies arc attached. Numbers on drawings correspond to numbers on apparatus list. ELECTRICAL CONNECTIONS ). Electro Scientific Industries Capacitance Measuring System,
Model 701. a. With the power switch off, plug the power cord of the Model
' 701 into a standard 110 volt outlet. This will supply power for the bridge null detector and internal power supply.
HONS 05775?
-6b. Remove the plug-in shield covering the generator output and
bridge in put terminals and the links which connect them. To make measurements at 60 Hz, connect the 12 volt terminals of the 110-24 volt transformer to the terminals marked GEN 1 and 2 on the bridge through a switch. A GE Type 47 pilot lamp connected in series with a 100 ohm resistance across the 24 volt leads serves to indicate when the bridge power is on. The switch and pilot lamp with its resistor are mounted in a small metal shield box with banana plug connectors in its back so that the 60 Hz 24 volt source may be plugged into or disconnected from the generator terminals of the bridge quickly and easily. The 110 volt terminals of the transformer are connected to a 110 volt outlet with a suitable cord and plug. c. To make measurements at other frequencies than 60 Hz, connect the generator output terminals marked BEN OUT ' to the bridge GEN 1 and 2 terminals with the links provided or more conveniently with a connector made of a 1/4" x 1-1/4" x 1-3/4" Lucite block with 4 properly spaced banana plugs mounted in it and wired to connect the proper terminals. d. To make dissipation factor measurements at higher values * than provided by the Dissipation Factor Dial of the bridge, make the following connections: Remove the link connecting the EXT D ADJ terminals. Plug one end of a General Radio
H0N3 057758
-7-
Type 274 NQS double plug patch cord into these terminals and
the other into the terminals of the decade resistor.
e. The Balsbaugh cells are connected to the unknown terminals of
the bridge as follows: Plug the center connector of a General
Radio 874-Q9 or 777-Q3 Adaptor into the Unknown No. 1 terminal
so that its shield terminal connects to the GRD terminal. Use
the General Radio Type 874 Patch Cord to connect between the
adaptor and the Type 874 connector on top of the Balsbaugh cell.
Plug one end of the banana plug patch cord into the Unknown No. 2
terminal of the bridge and the other end into the banana plug jack
at the top of the cell.
General Radio Type 1644A Megohm Bridge
a. With the bridge power switch off, plug the power cord into a
110 volt outlet.
b. Connect the Balsbaugh cell to the bridge as follows. Plug the
center connector of a General Radio 874-Q9 or 777-Q3 Adaptor
into the bridge terminal marked + Unknown. Connect the shield
terminal of the adaptor to the bridge terminal marked Guard.
Connect the Guard and Gnd terminals of the bridge with one of
therlinks supplied with the bridge. Then use the Type 874 patch
cord to connect the 874 adaptor on the bridge and the Type 874
connector at the top of the cell. Use the banana plug patch cord
to connect the Unknown - terminal of the bridge and the banana
plug jack at the top of the cell.
057759 HONS
-8-
MATKRIALS
1. Glycerin for constant temperature bath. 2. Xylene, Reagent Grade .
3. 29% Ammonium Hydroxide, Reagent Grade .
4. Distilled H.,0.
5. Acetone, Reagent Grade.
6. Benzene (Non-Reagent Grade).
7. Acetone (Non-Reagent Grade)
. 8. Calcium Oxide Lump Form (Fisher Cat. No. C -116).
9. Boiling Chips (Used in cleaning baths).
PROCEDURE
A. Clean Test Cell
- 1. Using tongs place tost cell into cell holder.
2. Clean in xylene vapor bath for 15 mins.
3. Clean in boiling 29% NH^OH for 10 mins.
4. Clean in distilled I^O steam bath for 30 mins.
5. Clean in acetone vapor bath for 15 mins. oo
5. Dry in 100 C-110 C oven for 30 mins.
Note: Cells must be handled only with cell holders or
tongs. The cleaning baths require cleaning once per week.
-B. Cleaning Glassware
'
1. Clean Pipette.
a. Use tongs to hold pipette.
b. Benzene wash.
c. Acetone wash.
05770 HONS
I -9-
d. Distilled Hj,0 wash-
e. Reagent grade acetone wash.
f. Draw clean air through pipette.
g. Dry by flaming with bunsen burner.
h. Draw clean air through pipette.
Note: No part of the pipette which might contact sample
should be touched with hands or any support.
2. Clean Sample Vessel
' a. Pour sample into solvent can-
fa. Benxene wash.
c. Acetone wash.
d. Rinse off glycerin with water.
e. Acetone wash.
f. Clean in xylene vapor bath for 15 mins.
g. Fill 3/4 full with 29% NH^OH boil for 10 mins.
h. Steam for 30 mins. i. Dry at 100-110C for 30 mins.
j. Draw clean air through vessel before using.
C. Sample Preparation J, Remove sample vessel from drying oven. Use tongs.
2. Draw clean air through sample vessel.
3. Pipette sample into sample vessel by means of a suction bulb.
4. Remove test cell from drying oven and insert coaxial cable,
connector shell and pin.
mons 057761
-10-
5, Place test cell in sample (check to make sure that the saj-nple
level is just above the bottom of the holes on the unguarded electrode).
6. Fasten sample vessel supporting clamp in such a position to
allow 1/8 inch of the vessel to extend above the top edge of the clamp. This insures proper immersion depth in the bath.
7* Connect leads to the cell and put on Teflon lid. 8. Place sample vessel in the 100C constant temperature bath
and reco.d entrance time.
Note: The required amount of sample is just enough to insure sample
flowing through the holes on the unguarded electrode (outside). This
amount is approx. 50 ml. D. General Operating Procedure for Electro Scientific Industries
Model 861A AC Generator Detector
1. 60 cycle Measurements
a. Plug in the step-down transformer adaptor into Gen.
position 1 It 2 on capcitance bridge.
.
b. Turn the AC line switch on, allow 15 min. warm up.
c. Rotate the output Power control fully counterclockwise. d. Set Ffequency Control for 60 cycles.
,, e. Set Range Control at the IX position. f. Set the Selectivity control to the Sharp position.
g. Turn the Log-Linear Switch to the Log position.
MOWS 057762
11-
h. Turn outer Sensitivity control know to such a position that a
deflection on the meter can be seen. (Not more than 50% of scale)
i. Rotate the Fine Tunine control to the position giving the
maximum meter deflection. Detector is now properly tuned
for 60 cycle measurements.
2. For Frequencies Above 60 Cycles
a. Plug in special adaptor in generator out terminals 1 It 2.
b. Turn the AC line switch on,
c. Set the output Impedance switch to 100-ohm position.
d. Rotate the output Power control full clockwise.
e. Set Freouency Control for desired frequency.
f. Set Ranee Switch to match frequency.
. g. Set Selectivity control to Sharp position.
h. Turn the Log-Linear Switch to the Log position,
i Turn outer Sensitivity Control knob to such a position that
a deflection on the meter can be* seen. (Not more than 50% of scale)
j. Rotate Fine Tuning control to the position giving the
maximum meter deflection. Detector is now properly tuned.
E. Make Dissipation Factor Measurements Using ESI Type 701 Capacitance Measuring System
1. Turn on bridge null detector (allow 15 mins, warm up).
2. Set Frequency control to desired frequency using proper plug
in unit, tune detector for maximum sensitivity (See General
Operating Procedure for Model 861A AC Generator Detector,
. Section E).
HONS 057763
-123. Set Capacitance range switch in the Picofarads C range. 4. Set Dissipation factor range switch to the 10 ^ position.
5. Connect leads from the test cell to the bridge.
6. Apply bridge power.
7. Adjust bridge sensitivity (inner knob) until needle reads 40 on
the meter scale.
l
8. Balance the bridge by adjusting the capacitance and then the
dissipation factor knobs alternately until the best null is achieved at 10^ sensitivity range.
9. A IK and 10K step external decade resistance box is used to extend the bridge dissipation factor scale readings. Each 1000 ohm step on the decade box is equal to 100 divisions on the disspiation factor scale. It then becomes necessary to divide the total reading of the decade box by 10. This value is added to the Dissipation Factor scale reading.
10. Record the capacitance and dissipation factor readings 30 mins, after placing sample in the constant temperature bath.
HONS 057764
-l^-
Formula for calculating dissipation factor:
(S + R) x A x F ' Dissipation Factor
Where S
- Dissipation factor scale reading
R = External Decade box reading in ohms divided by 10
A = Dissipation factor range F Frequency in KHz (kilocycles)
Example for 60 cycle measurements: S = 41. A = IO'3, F = 6 x ID-2, R = not needed to balance bridge From the formula S x A x F = Dissipation Factor (41 x ID-3) 6 x lO*2 = 41 x 6 x 10*5 = .00246
Example when the External Decade Box is needed to extend the Dissipation Factor Scale readings
S = 41, A = 10'3, F = 6 x 10-2. R 250 From the formula (S + R)x A x F = Dissipation Factor
(41 + 250)x 10`3x6 x 10"2 = 291 x 6 x 10'5 = .01746
Example For 100 cycle measurements -1
5 * 41, A = 10 , F 1 x 10 , R = not needed From the formula S x A x F = Dissipation Factor
41 x 10'3 x 1 x 10'1 = 41 x 10'4 = 0.0041
HONS 057765
-14ExJtmple for 1000 cycle measurements
S - 41, A = 10 \ F = 1, R = not needed to balance bridge From the formula S x A x F = Dissipation Factor 41 x 10'3 x 1 = .041
Dielectric constant calculations can be made by using the following formula.
Formula for calculating Dielectric Constants .
= Dielectric Constant
- Measured capcitance of sample = Air Capacitance of the test cell in air
at room temperature F. Make Resistivity Measurements Using Type 1644A Megohm Bridge
1. Turn on bridge to discharge position, allow 10. min. warm up. 2. Connect leads from test cell to Megohm Bridge. 3. Zero resistance bridge while charging zero at 500 volts for
30 seconds. 4. Measure for 30 seconds. 5. Read 1 minute after applying bridge voltage. 6. Return switch to discharge position. 7. Record resistance reading.
HONS 057766
-168. Resistivity to be measured immediately after 30 minute
dissipation factor measurement. Note: Never touch cell or leads when bridge is in charge or measure position. After completing resistance measurement return switch to discharge position before removing leads.
Formula for Calculating Resistivity:
R x M x k Resistivity
Where R = Resistance reading at 500 volts
k = test cell constant (The cell constant is
.
obtained by measuring the air capacitance of
the cell at room temperature and multiplying this
value by 11.3)
M - Resistance multiplier
*10Us 5??6 J
Appendix C Stream Data
HONS 057768
FfC. 3$talliUfa Point of fiCSiaiJ P/ST ILL A r/F VFFSF S 4, 1 ' CMT&rfT
HONS 057769
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