Document rxDdEOEGwQyX95bmnvEBw3JgJ

0 PT ' i )' June 4, 1941 r. R* 1. Jenkins, Anniston RS?x TOUR LETTER, HAY 30, 1941 cc: Hr* Gerber, Anniston si'>. ** >:v,XX ; . .... Troops,^ . ($%? dWtefrnl: tionof aoisture in the Pyronala and Aroclors, whereas the latter gives detailed instructions as to the preparation and standardiza tion of the Sari fisUher Reagent* - . , - Jlgx - -- Wo 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 * .titrated to the end point before-the sanple 10 addpd* This should m X*,..- lie contamination of the sanple With adsorbed Weisture* '" r . ... V ' -v:.-' ; V . ' jX1.,.-X :....... ** ^ .- gglffiS V," -i-\v. , -X : ' W-v -^' J\ V'-v -. --^V-v^v j, .-. -, y\ff._w\.v-_.-_^ -,,.r^zXX?- / - ,-y ->.; .... : `3. ' H* J. Wiegand * ' -r ^ -r* **** ,, . ... --f> **-*-" r-..V 1. ~'w` ^ ~ ' ^ * " ' :. . ; .. ^ . .. ^ % ^'hVj^s-T- *y"'\ X i. . , X4f* 'X" i-i S ^ -i. ' ~ If l ** X ' ij?, 'K ?* 'i ) tt*"/1 ' t,***^H, * * %^ 4 f X^ * * V' " ,, 4y \l y* ,5 it * % * ^~ h . - \ % 1-X^ j , y, _ v. . - . ,,, .; - . V tt X'X: ;/. :> VC'aV' V'V XiJXX-X XgXyi:^ - DSW 330527 STLCOPCB4077171 ' * ' * ... * * * 9 * - -ft -* * a * i* - * * Material: ;; . V. . _ .. Test; Aroolors and Fyranols i * . * *i -.-- Sa0 * -.*..*** '~ HolstUT6 In Aroolors and Pyranols is determined with Earl Fischer reagent (Method Ho* 10v 100r40, (G.HL, 7})* Because of the varying solubility of the products tested, different proportions of a nixed solvent are required* The analysis itself, however, is the same for all Aroelora and Pyranols* The analysis is aade as follows; Pyranol 1478 Pyraaol 1498 Pyranol 1495 All Aroolors o 50 al* 80 al* 80 al* WM 50 al* 50 al. 50 SI, 50 al. 8) Titrate the solvent to the characteristic brown end point with Fischer reagent* 5) Beflll the buret to the zero mark* - ,, s , ^ - v -, V.. " ' ^ '.V' . s" ' p.' W'-X'Svtt}' . .S " 'ft'"-'- ' % / 4) Veigh a 100*0 g* sample by difference Into the solvent* Mix well, i 5) Titrate the solution to the sane endpoint as before. . -Calcul ation; jE Ha0 * al* Fischer reagent x R20 factor x 100 ""r,,,"' " 1" Baaple Veight - - ' ' The Method is accurate to O.OOOS - - vr"............................-- k..... J' Report the results to the nearest 0.0005J&* ' ', tii. ; n. \ ;J ' ' - r- % * : \ JSateriSl# General Sethodf Tfethod Ete^l0,10CM0 ; : - -i. - i. ' r * * . - v* " * * * ^.'r^r * * * * 4:.. . * ^ *** ** . -:v- -' Test; - / ^ ^ater> Tracesv^v^, " : ' ' - Traces of water nay be determined by moans of a titration with Sari Fischer Reagent* The reagent is prepared as follows: Place 667 al. of dry methanol and 69 ml. of dry 2* pyridine in a dry 1000 al* Florence flask* Add 84.7 g. of iodine and shake to dissolve* Stopper and cool to 0* to 2*C in a slurry of ice and water* When . cooled to proper temperature* add 64 g. of SO* at such rate as to requlre ebout 90 . ninutes for complete addition. Keep cohd during the procedtira, and diake frequently* The SOg is best dispensed from a graduated cylinder, froa which the lip has been .* -j ' *'?r1"k'v reao^* Vind. is provided with a one hold rubber etopper through i^iich a bectr glaks > tube is passed* This bent tube should be connected to another tube leading into . ; ' the Florence flask the outlet of which la below the surface of the liquid* Prepare the reagent in one liter quantities only* This reagent should be put into use be tween three and seven days after preparation* Two bottles should always be onhand* Ihen not in use. Store the reagent in a 52 ounce glass stoppered bottle* sw 330528 STLCOPCB4077172 Standardize the reagent as follows: Prepare a solution of dry sethanol containing a known amount of water -- about 6.0000 g. per liter* Titrate 10.0 ml. of this solution with the reagent* The endpoint ia a color change from yellow to brown. Call this titration B. Also titrate 10.0 nl. of the methanol used in the prepara tion of the water standard. Call this titration A. Titration A will account for 101$ of the water present In the raethanol used for the standard. This correction Is negligible. CalcMf the water factor as follws: It will be found that one liter of rsethanol contains about 1.000 g. of water. This amount plus the amount of water added la the total amount of water In the standard. After the original calculation* the total water in the standard is known, and the following calculation for daily determinations of the factor can be employed: lz) Ml. factor Total g. water pefr 10.0 ml. . ' '*>. "at"*". Nitration v /' Poraula (l) is Used only in determining total water in the standard. Poraula (2) Is used for all routine standardisations* -The total g of water per 10.0 ml. of standard will be posted on the bottle containing the standard solution. r1 The standardization is carried out in a clean, perfectly dry 250 ml, Erlenmeyer flask. The factor will be a-prox. 0.00330 g. Ha0 per Kl. Standardize the solution every day, Immediately before first urn in the morning. * The reagent is dispensed from an automatic burette set-up provided with a liter reservoir and a drying bottle provided with alternate layers of glass wool and Pe06. , | The drying agent must; he renewed whenever examination shows that it is necessary, v> The air used in moving the reagent is drawn frou the drying bottle through, a pressure bulb and forced into the reservoir. All air vents are connected to the drying bottle. 1 i DSW 330529 /0 STLCOPCB4077173 * t ^..v- : .. . - DIR8CTI0HS FOR TEST NO. 14-39-41 SUBJECT: %tter Content-of liquid Aroclors . Method: titration wlthKarl Fischer Reagent OutllPi /- v '' TheArodpr la dissolved inanixture of benzene and ethanol Alch has teen p|^g;|i9>ltttii^|fc^^in tlj^tffho ohtsft%he wat Solutiong andApparatus ,,. ,, " .V / 'ft TTfjtra^ t Karl Fischer Reagent: Weigh, into a flask 264 graft* of pyridine* Barrett S-A, or Eastman 214-H* and add 61 grans of liquid sulfur dioxide* Add the sulfur v dioxide directly from the inverted cylinder by attaching to the outlet valve a glass tube extending into the pyridine* Store in a glass stoppered bottle# ~ Transfer 65*6 grans of the pyrldlne-SOg fixture and 134 oe of absolute methanol to a 1 liter Florence fLaak, vCool thoroughly in an ice vsater bath# Add 16*9 ` /' grass of i|diaa^f.stopper* cool again before shaking*- Alternately cool and ' ( swirl until the iodine is in solution* Hakes 200 cc of reagent* Store in glass ' stoppered bottle* let stand 24 hours before using. When fresh* one oc of reagent is equivalent to about 0*0033 gas* of water* Aroclor Solvent: Mix 2 parts dry benzol with 1 part absolute nethanol* The dry benzol is prepared by shaking the comarcial grade with anhydrous calciua ... chloride* decanting into a flask and distilling* rejectingthe first 10j to cone over* Keep in glass stoppered bottles with minimus exposure to air* v Micro Buret: 10 cc x 0*06 ce* Koch automatic with glass stoppered reservoir* l Eck Vnd Krebs $2460, ,Eauip reservoir with a moisture guard tube* -3 --.. - Procedure ' - > '" 'S'S IK rfS* Heat a clean 600 oc narrow mouth orloruasyor in an oven or on hot plate until thoroughly dry* Cool in desiccator* Sweep out for 10 minutes with air which has been thoroughly dried by passing through tubes containing 8 raesh drierite* Disengage the flask from the aspirating train and in.idlately .close with a paper cap held by a rubber band* `. '^iWitttput delay* 'i^jsnsfer 90 cc of tbc^hejBBakne-^ to the flask ff^thrCu^a. a saail%ple punctured into j^ie'-paper cap, ' Titrate at^aoc %ith Ksri^/.., /hj. Fi'bdher .ycogeni to - n^istinet' red-biown ond point' tdildh' does 'not' fade after' -s< fy* 3 swirling several'times* the Fischer reagent is dispensed troa the aieroburet the tip of which projects into the flask through the puncture' in the paper cap* At t ' the end point any water content of the solvent has been reacted. Superimpose a fresh paper cap* - ' , Obtain weight of the solvent and well-covered flask on e Torsion balance or equivalent, Quickly introduce about 100 grains of the slightly war.-sed Aroclor to be tested* Cover at once and weigh again to obtsin the weight of Aroclor to nearest gram. Shake until the Aroclor is dissolved* DSW 330530 STLCOPCB4077174