Document qanMa0NZNKvgJ94y30rm5D0VM
4* vi
Dr* R. L. Jenkins, Anniston
t :
* REFl YOOR LETTER* MAI 80* 1941 ..
Mr. Gerber, Anniston
X am sending* yon, herewith, copies of ear method for r Moisture in Pyranols end Aroclors, and our General1 Method for Traces of Moisture* The first gives specific directions for the determination of moisture in the Pyronals and Aroclors, whereas the latter gives detailed Instructions as to the preparation and standardisation of the Sari Fischer Reagent*
i
We do not take any specific precautions in the sampling, nor for removing adsorbed moisture from the titration
flasks* The flasks are dried in the usual type of drying
oven and the solvent is titratfed to the endpoint before
the sample is s44ed* >.This should preclude contamination
of the sample with adsorbed moisture. * * ........
1
As to the cloud point method, the only information I have
(r1' is that which you gave in your report of conference held
at Pittsfield, on August 14, 1929* fh this you state that
Clark used the ASTH method fop the^dO^djpolnt* You also
gave a table ^showing the. relationship between the ppm of
water and the'" cloud, point*' X .a showing a copy of that .
table belowt
\
laS. Cloud Point
5 ppm* 18 ppm* 29 ppm. 50 ppm* 68 ppm* 100 ppm*
7C 5*0 4 8C 480*0
In % subsequent letter to you (Oct** 10, 1989), Mr* Clark gave a correlation Of the ppm* water and the dielectric strength* X am likewise showing a copy of that* ...
Water Content (ppm* by weight)
Dielectric Strength (85C)
10 ) \ 5
40 }. 60 \
48 84 86
19
DSW 330629
STLCOPCB4077273
S' *
*2
The thing I particularly wanted to discuss with you while you were in 8t. Louis was the setting up of specifications for 0# E* Pyranols# particularly Ho. 1476, which is now !, being made at Anniston* As you know# Mr* Clark was also ! In St* Louis about, that time and I contacted him with re* f gard to all of the* Pyranols indicating to him some changes whlbh I thought should be made* Be noted these and was taking the* back to Pittsfield for decking with his men ':: ! up there*' I am sending "you, herewith* a copy of the sped* flcations which X think Monsanto should set up for Arodor 1254 (Q*E* 1476)* Qiould you have any comments they would be appreciated* If not# please advise me as I would like to send these along to Mr* Watt so that we can have a for* mal Plant B specification set up on this material along with the .other Pyranols and Aroclors*
RR M, J* Wlegand
P*g.
r \
Will you please check the figure for total chlorine
content* Our old specifications indicated it to be
58.5 to 55.5# while in a memo to Dr* Kyrides, dated
5/12/38# you stats bhat the specifications on chlorine
content of O.E* 1478 is 54*5 to 55*5.
.
DSW 330630
STLCOPCB4077274
8
Material! Aroclora and pyranola
Tastl________________laS---------------*
u . -tar# in' Aroclors and *ypanola la determined with lari ?lschr (Mathod io. 10,100^40, (0Jt. 7}). -Because of the varying
-IiMMittv of the products tested, different proportions pf e mixed aSlventare required. The analysis itself, however, la the same tor all lfoclpra and Fyranols.
.
The analysis is made aa follow^
1) Add the solvents as Hated below to a 500 ml. Srlenmeyer flask*
material
Afford. Benaane
fBfryfli.JUthftagI
Pyranol 1478 ' 1^7fa
0 ml.
Pyranol 1488
50 ml .
!
pyranol 1495 I All Aroclors
80 ml. 80 ml.
50 ml.jTO 50 ml. 50 ml. 50 ml.
) Titrate the solvent to the characteristic brown endpoint with
Pi acher reagent*
'
a) Refill the buret to the sero mark.
4) weigh a 100.0 gf sample by difference into the solvent. Mix wel
Titrate the solution to the same endpoint as before.
Calculation! % H,0 Plj-gisdher reagent x g.O factor_X 1QQ ; ? Sample Weight ^
The method is accurate to % 0.0005^ - $
Report the results to the nearest 0.00059C* ffr^
Materials General Method Method Ho. 10.100*40
: ------- ---r*-. ' **> ^ --g*t*r* Traces
___ .....
Tracer of; water may be determined by Hasans of m titration with
Karl Fischer Reagent*
~
f-upeafht "18 prepared as foliowsi" ft&l 667 ml." of dry methanol and 269 ml. of dry Sr pyridine In a dry 1000 ml. Florence flask. Add 84.7 g. of iodine and shake to dissolve. Stopper and cool to 0 -2C in a slurry of ice and water. When
. 3J& y //rV i
_
/Jt* 3-\
./, i ^ i'r"~
..
-
_
DSW 330631
STLCOPCB4077275
4
cooled to proper temperature* edd 64 fig* of BO* at such rate as
to require about 90 minutes for complete addition* Meep cold
during the procedure* and shalee^f^eanently*
SO* is best
dispensed from a graduated cylinder* from which the lip has been
rumored* and is provided with a%a hole rubber stopper through
which a bent glass tube is passed* This bent tube should be
connected to another tube leading- into the Florence flask the
outlet 'of which is below the Surface of the liquid* Prepare 7
the reagent in one liter quantities only* This reagent should
be 3>ttt. into use between three and seven days after preparation*
Two bottles should always be on hand* When hot in use* store
the reagent in a 2 ounce glass stoppered bottle* .
Standardise the reagent as follows* Prepare a solution of
dry methanol containing a known amount of water - about 6.0000 g*
per liter* Titrate 10.*0 ml* of this solution with the reagent*
The endpoint is a color change from yellow to brown* Call this
titration B. Also titrate 10*0 ml* of the methanol used in the
preparation of the water standard* Call this titration A*
Titration A will account for 101JC of the water present in the
methanol used for the standard* This correction Is negligible*
Calc* dt the water factor a* follows* " ' ...
'
, (l) >1* factor * g. of water per 1Q.Q ml*
v -v ..
b-a ; .
Calc*dl the amount of water originally present in the liter ' of methanol*
r Titration A x Factor x 100
It will be found that one liter of methanol contains about 1.000 g* of-water* This amount plus the amount of water added is the total amount of water in the standard* After the original cal- ; culation* the total water in the standard is known* 'and the fol-' lowing calculation for daily determinations.of-the factor can
be employed! - - .
- : :
C l V (2) Ml* factor - ToIQ.tP.JlU
Formula (l) Is Used only in determining total water in the
standard* Formula
is used for all routine standardlsatlont*
The total g* of water per 10.0 ml* of standard will be posted
on thr bottle containing the^standard solution* ........................
V:.
the standardisation is carried out in a dean, perfectly dry
250 ml* Brlenmeyer flask* The factor will be approx* 0*00320
HaQ per Ml. Standardise the solution every day* immediately
before first use In the morning#- ...... ' - *
` - .....
. .
a
' h\
The reagent, is dispensed from am automatic burette sat-up
.
provided with a liter reservoir and a drying bottle provided
dtK alternate layers Sf glasi wool and ?*0~* The drying agent
must be renewed whenever examination shows that it is necessary.
The air used in moving the reagent is drawn from the drying bottle
through a pressure bulb and forced into the reservoir. All air
emits are connected to the drying bottle*
%7
DSW 330632
STLCOPCB4077276
*
\
<* 8PECIFICATIOH FOR PROKJCT
Product Jto. 46 _ Sales Code.Jta*__ IQ4Q-^g-7g-Qg Data _6-4-41
Jan* - - - Arodor* Distilled- Mo*-J.S54 Ifl* 1* Compound Ho. 1476V
rhealoal Formula
' MlxturW-., _ . _ : , . ol Wt* loa -a ------ :. 5-1-56 .... . . :... . - .
f.
V
ye.tUoa.JLot.
Color v Yellow tinted viscous
10,084-40
liquid 150 APH lax.
Condition
Clear
`.
10,084-40
Specific Gravity 65/15.5 1.495 to 1.505
10,114*40
Acid Ho. (Mg MaQH per f*)
0.01*ax.
10,087-40
Inorganic Chlorides^ 0*0000135 Max*
.
10.118-40
Viscosity 98*9*0 (10F) 44-47 Seconds, Saybolt 10,036-40
.
'v -i- *'
MniverSal
. ..
Dielectric Constant 100*0-1000 cycles 4*5 * 4*5 ` ,, 10.119-40
Resistivity - 1006C * 500 Volts 100 x 109ohms/C*8 10,180-40
........ "" !
" " Min* '
Dielectric 8trength
SO EV* Min*
10,188-40
Refractive Index 25*C 1.6570 to 1.6590
10,125-40
Distillation 105
560 - 570C
10,117-40
50* 570 - S80C
580 - 59Q*C
four point
. > 0 - XSTG
10.115-40
1*0
0.0055* Max*
10,680-48
Loss on Meeting 100*C-6 hrs* 0*45 Max*
10.116-40
Corrosion Test (Effect of 6 Mrs* at 810*C in contact tilth
" .;* * . alumima) j ' * " ' > lo,/u* - ho
Lose In weight of brlght aluminan lone v
Inorganic Chlorides ..
v 0*000015% Max.
Acid Mo*
* "f 0*01 Max*
Color
400 AfB
Condition
Clear
8amplt for Analysis 8 x 1/2 gal* friction top tinned cans for lot samples* 4 x l/2 gal* friction top tinned cans for advance Q.E.
f"}^m . _
'
_
Ibtef^lipecific tfraWty changes minus 0.00095 per *C '(50 to 105C)
Special Specification* ` Tested only oh request*
ElectrlcAl Stability lo decrease in Resistivity
. (Aging feat}'
After 96 hrs* at 100*C 10,121-40
" Born Point .
Above boiling point
10,125-40
Total Chlori4*f ' 54.5 to 55.55
. 10,088-40
,<jr ?/
'"*
x &0 fS
DSW 330633
STLCOPCB4077277