Document Y9jo1OKJv7EzJ2nqxaXVQEyLE

SEaE S3EE V TO Or BXHPsm. AW ABPCLQBB SSfrE* ,::--v>* v-,1 .-7-; E/E ;S.^..ho:/foter/fnt.^in-..gTyP.-eoei,^.n'.Et ., .v ;* /. Mid Humber (aeldity) SliflllEip : ' ffl&smijMm ' V -: . Efltajai. r "Wr e Speoifio amity .' ;;fI- Freezing Point of Diphenyl ^en^ag Point; of A^oXorr^;-' iW&M. u u X5 E-, M JOOntl Insoluble Vaporization Lose v EE M so Crude Diphenyl & Still Bottomsa ' I- L "-' - . ' -\'V-'. .-"'r , - j . -. - ': -a- ~ : Magnesium carbonate' . . :. .- . -; .'., - - - : - : " - - v-.-(- E, ' .- a:- .;- E'A- AEEE ,*. a -.-E. EE S' ... e V: E/E. >' - '; ^ ^EEEEE*.' - r' . .-'-: rr'-r .' ;- - r. - r.~--' vee'v- Eva; '.- ,':V-'?: ' . : fhir^^tor oomottonn -T .. .;>;;- .-,;. - ..-../f ." ";'-E E| E EE;:' E:|EEEE-i:E.. . -.. . - e ee = /EE, v ee E ' ' -. eVi. /> - - - - - E ' a e ; *J *' EEE/./- 'EE:E it E DSW 331903 / r STLCOPCB4078479 :r^x SOFTENING POINT OF SOLID AROCLORS ^ " TgOTWTO,'HoW'',,t1------- - , W- ? ' V--. .. .: ' . This method is a modification of the AST#M* stan- > dard method of teat for*softening point of bituminous material#, serial designation* D 36-26# The method differs from the otan- ' dard method la that the rings are larger than spoolfled* a two ring support Is also used In order that too tests may he made simultaneously# \t i i The apparatus oonslsts of the following* (a) Tso i . brass rings,3/4" Inside diameter and 1/Z* deep* thlokness of -V wall 3/32"* (hi Two stool halls, 3/8" diameter weighing 3*45 > to 3.55 grams each* (0) A 800 co Griffin low form beaker* (d) a ring support Xhr the two rings having a brass plate exaotly one inch below the plate supporting the ring* (e) A 300 C A*S*T*M* low distillation tl rmometer graduated to lo* . y PREPARATION OF THE SAMPLE .ii- V; V:^.- The Sample shall be melted and stirred thoroughly, avoiding overheating or incorporating air bubbles in the mass . . and then poured into the ring so as to ;teave a alight excess on v cooling* since the Aroolors shrink cohsiderably on cooling, the V ring should be well filled, nearly to overflowing* A little of , the excess should be drawn over the top of the ring at several points so as to prevent the oooled Aroolor from dropping out of the ring* In the Same way, tho second'ring is filled with a standard Aroelor of known softening point* The standard Aroolor should have a. softening within at least 10 to 15 of { the Aroolor being tested# 7 The rings while being filled Should rest on a clean can lid or on a brass plate which has been amalgamated to prevent the Aroolor from adhering to it# The Aroolor In the rings Should ^ be fully cooled and hardened before preceding with the test* prooedukb Add eool e*p. glycerin (not above room temperature) to the beaker until the surface of the glycerin is 2* above the plate holding the rings when the ring support is suspended In the beaker# Place the rings eontainlng the Aroolor to be tested and DSW 331904 STLCOPCB4078480 .r: the standard Aroolor on the ring support* Place i WI w the center of the upper aurfaee of the drooler each ring# suspend r.' . tbs thewfcmeter $f the bulb u lw with .... Jig the bottom of the ring* and .*wv .'..v.r+..r*.^.*.r..v.s.s*- -pla-.c...e......b- -e...e.. ker &ek'ro^ Plata and heat at ouch a rata that the temperature la raised yo taoh minute* _ ,/ The temperature recorded by the thermometer at the instant theAroolor touches the hottom plate is reported as the softening point* The heating is continued until hath droolers have dropped to the bottom plate* Ho corrections are made for emergent stem# .-: -'`fe-*y- ' 1* f r; m a 1* The standard Aroolor is run along with the sample under test in order to compensate for variations in rate of heat* ing* dilution of glycerin* and thermometer variations* 2* The softening point of the standard sample is deter* mined by making several determinations using fresh glycerin and tarefully checking the rise in*temperature of the glycerin so that '/- Jy ; t Is m hear ;,|s ypeasibie to rc per minute* : 3* t^ie giyuerin mav be used repeatedly for the tests after removal of the droolor*A > l* Benzol Is used for cleaning the rings end balls* 5* water-can be used instead of glycerin for soften* Ing points up to 90 0* ;//!' Vv m s 6# for softening points above I0<rc# sell boiled ' erature remains practically constant* It Is well to have a supply of high*boillng glyoerin on hand to be used only for softening points above 100 0* 7* Air bubbles on the rings and balls during the test should be avoided as far as possible* 8* The rate of rise of temperature of the glyoerin shall be uniform for each minute after tho first 3 minutes of heating end not averaged over the period of the test* "' : s DSW 331905 STLCOPCB4078481 .vi-CW^y. : JL a-- DETERHIHATION & ass' ' ;v:7- r 5SS*a.r t*4 xVi ..'^v "VMflMMm;" ,,-w a second waWr xtreoUon r-v ^:*?*. .y 3 .; :>' ' .7 . . ,v DSW 331906 * '- A STLCOPCB4078482 SfTTJ { " ' "jSlT ( '^K. ' 3 mmjijmimMMpmm. chlorine in Aroclorsmay he determined by fueioii of the sample with sodium peroxide in a Brruuggeeass-parr f`usion cup, extracting the fusion with ewaatteer, aaoojidifying t.h...e......... ............... with nitric noid, eadprecipitating the chlorine by addition of thiocyanate* using ferric anmonium sulfate as indicator# ire# | The fbrfiaae fusion eup used ie the Burgees*parr sulfur Booh, the hoofe is suspe0nllud9eudi ^ ........ xe Jinm _ tranelte plate* all_ows the ffceion eup to extent the. plate for about Ignition is effected by strongly heating t_h_e bottom of ,..., _lon e% with the full flame of a Maker burner* The bottom of the oup should some to redness in not more than two minutes* ... -.*;>*- ' . . - : - --v / The fusion mixture ie made up of about 15 grams [on# m..e..a..s..u..r.ei full) sodium peroxide powder, 0*5 gram of powde: sugar, and 1*0 gram or powdered potassium nitrate. The reagen* ^ be f_r_e_e__of c...h..lo...r.i.n...e....or a. b,,.l.a..n..k. must. beo run end the neeesei. orreetlons made* The fusion mixture must be wen mixed an of lumps# solid droolers: of .crushed sample (prefer# ably 15 to 0 mesh) is added ' of the fusion mixture Contained in the fusion eup# Mixinng is maccomplished by stirring with a narrow metal spatula, 1/6 to l/4n wide* The remainder of the fusion mixture is then added to the fusion oup end the outer made tight by. drawing down the screw cap#, . . /- : < *4--, - Aroclorst 6*a5 to 0*55 gram of sample is ighed by dif e into a clean fusion cup* Rotate the ;; fusion cup to * bute the liquid over the bottom# Add the fusion mixture which has been previously well mixed# Attach the outer tightly by drawing down the screw cap# 0s*^01 STLCOPCB4078483 J 'X ; . ... .Mg. plaoe the fusion eup# which contains the prepared sample end fusion mixture! In the transits ignition plate ana apply the fall flam* of the JMker humor to the bottom of the fusion cup for 1 minutes* qabtioh DC not stand too near the fusion during iH33.ltlOn* , .. .. V.... r ' ' ' ^ &/V?4v-s / # name.and afteraireooiing for^r* minute or mors, place the cup in a panoontainiag about 3/4." depth of water* let tool until boiling of water ceases, then remove MSn.TlSrMnr|oo, :oT"wltl1 ^ tV5'1>V............... Then place the fusion eup on its side in the beaker end cover with a watch gists* Add water slowly so that the fusion is decomposed without violent boiling# Remove the cup and rinse well* Heat the contents of the beaker to boiling and boil for about 5 minutes* Remove from heat and lot cool for a few moments, then raicnisdeisofpflocsodvhetr-gInlasesxcaenssd atoddthpeureea5c0t$ent^~f'a^^lO^^ ea^tif&it $1^ co of acid are required). Cool the aoldlfled solution in sunning water to room temperature, add exactly 50 cc of standard silver nitrate solution from a pipette and stir to effect coagulation of the silver chloride precipitate* Filter with suction through In asbestos pad on a l-i/2* perforated porcelain plate and wash beaker and niter f t|mes with smallportions of cold water* Alio the ^"IliWterte btCfe intCoom&peiet6^0Lby ebeetwbeeeankewraasnhdinrgisn*seTtrhaensfflearskthetwiee# adding the rinsing to the beaker* Add 5 ee of ferrie titrate with standard KGN5 |ust obtained#v:-.-v \~ ~ to the solution end unti a diotlnet pink tint is gl^ gubtraet the volume of KCNS requiredfrem the volume of kOHS retired to titrate 50 ec Of standard AgjfOg solution* This will give the volume of KCNS equivalent to the chlorine in the Sample* Multiply the volume So obtained by the chlorine value of each Cc of KCNS and divide by the weight of sample taken* For example! if 50 oc of silver nitrate solution is equivalent to 61.4 oe of KCNS solution and the value ef 1 eo of KONS solution is *003770 gram clj then if it is found that 0*5 gram of sample Shows a KCNS titration of 10*4 so* the percent of chlorine 1st DSW 331908 STLCOPCB4078484 r (<$M AM . 64.09 6 01 <& amount muet be determined and deduoted from tho^ ^ffcjorin* fbwMU :-i-a^afci:-:. Jgi|;,.}.-.Mmi ,~- fit? IT ^C-/ llftfill^ ...:.v_. ^..y._..........,.. f standard Ap}( solution! About 0*13 HI dissolve It gram* of silver nitrate la eaoh liter of water* protoot the s.. oluti*on- - - - - * - ,. uiirfit|y^ 00o; oo f thi* Motion will preoiplta^ by theory 6*83 gram of ohlorine* &;-v i -: slmliil Kom solution*: - About 0*1 Htdiseolve 10 grams of Kousjin X^liief of water* 1 00 * about QQjp graa chlorine* y tit -;Sv Ferrio Iron indicator* use V*athrai$l solution of " ferric anmoalw olwt * -: :;/ .,.-.; V'-.--*:--.'- ; ; ' v\ , : - pure Kltrio Aoid, 50$* nix 5 of nitric acid, Sp*gr* 1*40, with 30 00 of water end beH until the acid ie colorless# thus insuring absence of lower oxides of nitrogen* '-#.. tit'V.'-w"? .--,ir , rtlM 0? PU*e'1*7 HaOl into eepaya ^ - diisstitliXlleed water to e_aoli and^ 101 00 O_f p_urs_5_^ n_itrlo ao_id# HkekasMolution is occommppxlete* add 50'from * pipette* stir noil and Tilt** throw an asbestos mat on 0 perforated porelain ^v: plate, using miction* wash filter and transfer the filtrate l bask to tbs beeper in the same banner as ebon working witha Mplo# fltrato^ tbo filtratOO with standard KOKS solution, :s*mmr^**l** forrlo iron indicator* ^ *_..w ^ ,,. *v\ & She Vslae of 50 #0 Of AgHO* elution in terns of irons ^^^^sointioiiis foundby subtreeting the o ofjroi solution used in titrating the 0*1 gram of Haoltfroa twiei the number of ee of . KCK3 eolutioa used In titrating the 0*15 gram of naol* This yelue is obeoked by titrating 30 eo of AgNOt solution addsd to 400 00 of water and 10 ee of p: ure 50^ HNO* with KCK3 solution* ibis titration should agree Tteorr,y closely (J 0.1 00) with the value found from the titrations of Naol* The titration must be made slowly to avoid drainage error* DSW 331909 STLCOPCB4078485 r-s : -- . -- 4 #44i4:4t4;.,' Since pure Heel contains 60*6636 pi by theory, the tie of the K0H interne of ohiorlne may 'be found hy dividing 1 weight of ehlorine in the Naol taken by the 00 of KCHS equivalent to the silver nitrate required, ,,4 4' , ^4^ - . - 4Wm,~ Examplet Swo titrations of s& of Had choir kohs M^|i5fdfea_?oftions of Naol Show KCBS titret lone of end |7|4 oo ^ee of AgHO* ie then (57#28 ;. ...4;4 >4- By titration of S 00 Of AgHO* against KOKS solution* it A# lbuoA that 61,56 00 are retired* Si agree within *04. 00 of the value obtained from the Haol titrations* She ehlorine value of the KONS ie then) #6066 x *1 divided by 61*4 * 15*12 or *005770 grams el per 00 of KCHS. She ehlorine value nay also be calculated from the titration of 0*15 gram of Heel# 0,6066 x *15 divided by ol*4 ` "" * gram 01 per e of KGHS# im 4. 1 - She fusion materiel have explosive propertie * if wrongly handled) consequently care suet be taken to use safe proportions* to secure a good mixture free of large lumps, and to properly seat the oover of the fusion cup# she fusion mixture must be kept away from water or moist air, either of whieh may ignite the charge# She fusion mixture should not be ground to redoes lumps# : 44:v 4 444444,:: - 44--- 4.4. -4 44?............m.. t * On account of the high ehlorine content of many of 4. the drooler* and t&i: Smell amount of sample taken. greet - -44,4 accuracy is required in weighing, transfer, and mixing of the sample# She pipette and burette far measuring the standard Solutions must be very elean to avoid drainage errors# 4 *. solid Aroolors should preferably be about 15 to 5 mesh when weighed# if the sample is finely powdered there is difficulty in transfer of the material to the fusion dup due to jumping of the small particles when touched witha brush* DSW 331910 STLCOPCB4078486 7 5 * Reasonable variations in the amount of excess HNO* present when titrating cause no difference in the titration*, m Boiling of the acidified solution before addition of silver nitrate causes slight loss of chlorine if the boiling is prolonged (15 to JO minutes)# Boiling at this point should 7 - Fusions which chow black Carbon deposits on the Cover and side of the fusion own may or nay not give the fall Chlorine content* If a carbon deposit is found* a second fusion Should be made using a smaller sample or reducing the amount of sugar in the " -v:.;--7.^7 8 * Mixing the fusion charge by shaking after the screw cap has been drawn down may lead to incomplete fusions. The mixing of the sample with the fusion mixture ehouid be done in eueh a way that the sample is fully covered with the mixture, j * The temperature at ifeleh the standard solutions are Standardised should be noted, in Case room temperatures vary from this temperature, appropriate volume corrections should be made* ` 10 ~ The fusion mixture materials should be essentially free of ohlorine* The chlorine content may be determined by making a blank fusion, that is* without addition of sample, and titrating in the usual way* Five oo of AgNO, may be added instead of JO cc* The kcks titration is then compared with titrations of 5 cc portions of AgN0t solution in like volumes of solution and nitric acid* _; .; 7` .. . ^ XX - Xh Case the solid scabies are difficult to :. transfer without loss by, brushing from the weighing pan of the balance, the sample should be weighed by difference from a agnail weighing bottle* _ - ' ? v%? 1 ~%m-r ' <" . V:^, ;/ . ; :v;-^ i' COPY/pw 9-1-30 DS\|\/331911 STLCOPCB4078487 t V ./ . ;; ' v - ,'.v DETERMINATION OF ACID NUMBER AflID ftPMKBR OF DISTILLED AROOLORS Dissolve 50 to 50 grams of sample la 50 00 0f c,p* V benzol contained in a 50 09 beaker* Add $0 00 of 9536 ethyl aloMohokl, s Vti*rjr tVhHovrcovuHgQhiUltyf awnud titrate with 0*01 H KaOH solution using 10 drops of 1$ phenolphthaleia solution us indicator* The and point is a faint plnkccoollor 1which is permanent for at least 2 minute* after rigorous stirring* r f Determine the blank titration for the reagents hp talcing the Same amounts of each (50 oc benzol and 5 00 alco hol) and titrating with the same 0,01 N NaOH using the same procedure and end point as In the determination* ; ` Subtract the blank titration from the titration of tee Sample and calculate the acidity in milligrams of NaOH required per gram. Of sample* For *01 N sodium hydroxide solution the calculation 1st UgK NaQH/gm* sample titration in eo x 0*4 T gras* or sample "" . \. L0 grams of sample give a titration of 2*7 00 of *01 N NaOH and the blank titration is 1*5 sc* then the acid number 1st (2*7 ** 1*5) x 0*4 divided by 4O * 0*014 Mga* NaOH per gram of Aroolor* ' kk---.li . ' k-kv.;-::v AOID NUMBER OF PRODS AROOLORS Dissolve 20 to 50 grams of Aroolor (depending on the amount of acid present) In $0 oc of cp* benzol contained In a 250 oc beaker* Add 50 ee of 95# othyl aloohol and titrate with 0*5 N 'NaOH solution using 10 drops of 1$ phenolphthalein solution as indidhior* calculate the Soldity in milligrams bTTJaOH~^quired'per gram of cample* ^on account of the strong NaOH solution used ^ar titration* the blank titrate of the Yeagents may be `" ............ ...... llga NaOH per gram sample * -titra--tjji-oji nsaiinnp^oee....x....2.0 -i Examplet If the titration of 40 grams of sample Is 1*2 00, the acid number is found as follows: 1*2 x 20 divided by 4 m O.OfrMgm NaOH per gram of Aroolor* ho DSW 331912 STLCOPCB4078488 3 mmm.mrnumJ^SkJL . vv . -yvA"- v_ .;' .. . ' ,. . - * prepare one liter of solution* Transfer 20 ss of 0*5 K HaOHmeasured by a pipotto or burette to a liter Volwmetrie flask* Fill to the martc with water end mix well* Unless the standard 0*5 IT HaOH is considerably off from being exactly 0*5 H# no correction need bo made for normality feetor* To corroot for the normality faster of a 0*5 h x 1*012 HaOH solution, mltInly 0*1 by 1*012 (* *4048) to obtain the HaOH value of the .Ol H solution. 1* The term "acid number* is 0lenient in refer ring to the results of this test* The "aoidnumber" Is defined as the milligrams of HaOH required to titrate one gram of aroolor under the conditions described above* \" 2* The H* Robertson Company calculates the "acid number" on the basis of the milligrams of KOH Instead of HaOH# Results in terms of HaOH when multiplied by 1*402 give results in terms of KOH* Conversely, results expressed in terms of KOH when multiplied by 0*715 give results in terms of HaOH* ' ; A:";:'-/ A' 3. The acid number multiplied by lOOO gives results In parts of HaOH required per million parts of iroelor* For example, a distilled Aroolor requiring 0*014 Kgsu of HaOH per gram of Aroolor (acid number 0*014) may be also expressed as requiring 14 parts of HaOH per million parte of Aroolor* A* if the acidity be oaloulated as HCl, multiply tbs acid number by *09115 to obtain percent H01* For example! if t"he "acid num*ber" --i\s9 0*80 on c0rude Aroolor, the ecorrespondilng_ HC"l Content is 0*0 x *09115 * 0*07 $6 BOX* The acidity mey sloe bo converted to HOI per million parts of Aroclor by multiplying tho ''acid number" by 91Xf For example, a distilled Aroolor having ; an "acid number" of 0*014 is equivalent to an HOI content of *014 * 9U * 12*7 parts HCl per million parts of Aroolor* less than The acid number of distilled Aroclors should be 0, Aside from free acid as a cause for HaOH consump tion, ferrio chloride which is usually present In email amount also oonsumes HaOH in neutralization to phenolphthalein, it DSW 331913 STLCOPCB4078489 /o therefore follows that an Aroolor of very low odd number must bo olco ^ctromely low jUo ferrlo chloride* : v; , ; 'f# m the titration of erude Aroolore* if thefclaok - coloring matter eteduree the phenolphthelein end point, odd an equal volume of water end oontlnue the titration# Atbe water will not *ix with the Other liquide end the end point oan he obeervod in the water# , - ' '* - . , n v; . T - ,,t-i *.' ,'f.. l- - -*' ' - ` vK-) : ;.:i/ , v;i . S;^:v r/- -v o'- - i . ' DSW 331914 STLCOPCB4078490 ; S- BETKBMINATTON OF SPECIFIC GRAVITY The specifications to* each Aroolor should state the tenperature to* both tbs Aroolor and the water to which comparison of gravity la made* In plant practise, specific gravities of Aroolora eon* talnlng up to 54$ onlorlna are amda *t 65/65 0 while epee ifla gravities of Aroolor* containing 60 * 62 $ ohlorine are made at 0v900t 5 t specific grelities of any of the Aroolor* may be made - " at 25/25*C by use of the AB*T*M# method for road taro, asphalt cements* eoft tars pitches, aerial designation D70-*27f 1927 (described In Bureau of Standards Miscellaneous Publication He* 110, Standards and Specifications for Nometollie Mineral and their produoto, page 125.) JM . Weatphal Balance* Similar to Elmer and Am^sd Catalogue No, 16550* Plummet need not have theraomoter scale to 90c but hould not be subject to injury by use at this temperature* Cylinder* Pyres: glass hydrometer Jar 1*5* ac 6* Thermometer* TJSO thermomotor which has been checked for accuracy of scale in the range used* Heat the Aroolor to be tested to a temperature about 15 higher than the temperature at which determination is to be made* For example, if epeoiflo gravity la wanted at 65C, the Aroolor Should be heated to about oQC* Then pour the heated Aroolor Into a clean Pyrex oyUnder whloh has been warmed by setting at edge of hot plate* The cylinder should be filled with DSW 331915 STLCOPCB4078491 ';' -',>\> the Aroolor to within about 1 inch of the top* '*s.v<y -' ` >i ri.i- v-j, $M\ Junior;ln:>the ` oyllnderto air eool until the i:;:v t^o^t^ lf e^out 7 degrees above that desired# then plane - ,tbe:; s&iade#'ahot water bathwhioh is at atempereture Sbo^t, 5 . degre|f^above . $$$$* ira^lfj^tratu^;g| li|erbeaker ;e!Nrt^ Xtt 1$-. case the speolfiS gravity is to bo ..., w _.. . hath should be substituted (glybesia batik for the waterbath to avoid tho water vapor with its condense* , tion eh the westphal balance which la present if water la used , at hi# temperatures euoh a $5*0# Without disturbing the adjustment of the Westphal whloh is set to read aero with plurapiet in air, plane the oyllnder oontalnlng the Aroolor In sUoh position that the plummet is y icsaeraed In Aroolor and add weights to the beam of the westphal until the beam is again level# liM^u&aet should new be com* pleteljr iaaeraed as^ll as about X/I* of the suspension wire end the plummet should not touch the oyiinder at any point* stir the Ax'dolor with a thesaaometer at frequent intervals until the desired temperature Just is reached* At this point the weights are quickly adjusted until equilibrium Is obtained end the reading noted# Having obtained the reading for drooler at the desired .f temperature. the specific gravity Is obtained by dividing this q figure by the reading when the plummet Is Immersed la pure water at the seme temperature* she reading for water is obtain* ed in the seme manner he for Aroolor* since the reading for water is eonstant. rfovlded there tope no errors la weights or Westphal; this figure need not be determined with each Aroolor .- test* ?he figure for water whloh is used as a constant should* however# be smoked onoe a month or whenever greatest aeeuraoy is needed* The tendingsJmwater at b50 and 900 are *ospeotlft# #p# and *96?? 1 y. '^gT.V ;- v- V ,,r.; >v =.' -k *. .. t-. W mmmzM fmmm ^' 1* Assume readings as follows* k'-kX'vj.sV /'" J*, - . Westphal reading with plummet in air Westphal readilng w`it"h pl`umme`t I`n Aroolor at 65C West/phal read"llag with plummet In water at &yQ Then cp.gr. at 05/650 * ` 025 1*5288 zero 1. DSW 331916 STLCOPCB4078492 Example l Assume readings as follows* Westphal reading 3WSJ* MS& 7hea spgrt at unmet In Aroelor atJJC^O y' _ W- aero l;f$ X* The we be oheoked periodio balanos* should by valeting eaoh on an anRlytieal 2. The adjustment of the liquid to^tkeiexact ten^ewur ture desired Is moot Important. Do not allow to Oool rapidly and stir frequently enough to maintain a uniform temperature from top to bottom in the oylinder* . -y. 4'1 f. 4 IlSft: ir-vt'V' -. . >' ' -.m* ' <:. 'S' y-.;- / :. 0S\N 331917 STLCOPCB4078493 /? fu. f26>f -- d&.9*. ~ib <J\v >c - <*+*- ^ 3**el*^L /ns ^ Cs-^a- " Av. t% - ^0 Kww --' Co* -- AX/ tyfl. ^ - ui. g *. cfi /<A^> KTBRMINATION OF IRON XN AH0CL0R8 :v'* 'iy^A Iron in Arociors may be determined by extracting a benzd solution of the Arcelor with dilute hydroohlorio acid until further extractions show no appreciable Iron content, The lion inthe combined extracts i# then determined by the colorimet ric method using potassium sulfooyanate* p. ;?' ^f v jmmm. - - '- \ The amount of sample taken is governed by iron content of the sample# The amount taken should be such that up to ,OQfo g of ye is present* The amount to be taken is indicated by the following tablet * -fy-'-yy . y.-r '' T/.v-v 0*1 gram sample when *1 to ye is present *2 i:S : : : :8a *1 * JtpL #g-a a . n #Qfcj<g * * n a a 3 to 5 * Below 5 to oonta The redistilled Aroolors are low in iron, consequently sample should be taken* The black Arooiors usually 03 to *i$ ye# 0*3 gram sample Is therefore used* Transfer the weighed amount Of Sample to a clean separatory funnel of about 100 00 capacity* Add about 5 ee of benzol and shake until the sample is in solution. In the ease of large amounts {3 to 5 grams] of sample the amount of benzol Should be increased to about 10 So to insure a solution of consid- drably lower specific gravity than the hydrochloric acid used for extraction# . ...yy. y. ..-y y ' when solution is complete# add 10 ee of 1*1 iron-free BOX and shake for about 2 minutes, let stand until separation of the tso layers is complete# then draw off and preserve the acid extract. Add another 10 00 of lil Hcl and shake again# Draw eft the sold layer and combine with the first extract* Transfer the Combined extracts to a Kessler tube and dilute with distilled water to about $0 ee* Add 10 ec of Normal KCNS solution and mix* Compare the color so obtained with the color of a standard solution made by adding standard iron solution to a Kessler tube containing 20 ec of 1*1 HCl# 65 00 of water, and 10 eo of KCKS solution. The standard Iron solution is added from a bufette until the eolor of the standard solution exactly matches the color of the sample. DSW 3319t8 STLCOPCB4078494 2* a v The iron content ittnperee&t i* found toy multipl the number of ee of standard iron solution required toy the i value ef X ee of standard iron solution and toy 100 lid divi< :V toy tho weight Of Sampl# |aken# y^.-- ofsolution (lee* '2^'&&8t .1 divided toy 0#3# The result- is :: -;.::., ---- _...;-:t. standiad iron solution^ X so w stoout .00005 graa Fe, Reduce about X gran of ferric acsnonlum. alum to a powder, mix well and transfer to a weighing bottle, weigh toy difference about 0,2 area of sample into a 250 00 beaker# Add 100 ec of water and 5 00 of Eel* Transfer to a 500 00 volumetric flask, make up to volume, and six well* , weigh toy difference another portion of about 0.2 gram ferric ammonium alum into a toesker and determine iron toy ammonia preaiptation and weighing the ignited oxide or toy redue- in of the iron in BOX solution with stannous chloride followed titration against standard potassium diohremate, using LphenylarainC as indicator# From the SmOUUt of iron found in io ferric ammonium Hum the Fe value of the standard iron solution may toe Calculated# Ferric ammonium alum contains about M.M Fa* one ec of standard iron solution will contain about $#loo<9 m* Fe|^-,.;-;: r : ' ';'v V/ . ^ -V'-- , .... ' ( Potassium thiocyanate solution* normal, Dissolve 100 grams K0KS In 1 liter of water. ^ 1 Dilute hydroohlorio acid, Xil* The toe free of iron# F# f. Bakers speeial BOX is suitable tout should toe tested to insure Cheches cfiron# 0^ , ';'i. / v-v;;. . `f: mm. 1 * Two extractions with ltl HCl has been found to remove the iron from the benzol solution with sufficient complete ness* The completeness of extraction may toe oheoked toy making a third HCl extraction and toy evaporating end igniting the toenasol solution in a olean white porcelain dish* If the Iron extraction is complete the dish should Show no reddish brown Iron stain after ignition* DSW 331919 STLCOPCB4078495 / J \ 2 * Acid extractions with dilute sulfuric acid are unsatisfactory due to a much greater number of extraction* which must be made for complete remove1 of the iron* - " "5* ; v ^ I The pad thiocyanate colors fade somewhat on ; .i a' standing* For this reason color comparisons must t>e made ..... freshly developed solutions end standards* In tenting a number of samples, the extractions should he completed and the thiocyanate eolors developed at one time* The samples ean then he arranged in increasing color intensity end matched hy adding standard iron solution from a burette to the single Kessler tube used far the standard soiuUon* 4 * The volumes of the thiocyanate solutions at time of comparison should be approximately e<jual* c 5 - pirplloate determinations on samples containing *05 to f20? re aiouXa agree within *d2$* 6** Results comparable with those obtained by acid extraction may be secured by carefully igniting the sample in a clean porcelain dish and dissolving the iron oxide residue in 20 ee of 111 Holt then developing the thiocyanate color in the usual way# - V. --- T * in case the Aroolor contains large amounts of iron (above 0*5$) the amount may be determined by titration of the BOi extract with 0*05 normal potassium dichromate after reduction with stannous chloride. A sample of 2 to 5 grams may be used if the iron is to be determined by titration* 2 ,, Buifhcyanide forms the red color with iron in the ferric condition only* If ferrous iron is present it will not be Shown by the sulfooyanlde test, on aeeount of the preparation of the droolers by chlorination, it may be assumed that iron present is in the ferric condition* The presence offerrous iron in sol extract may be tested for by addition of a elution of ?otasslum fcrricyanide to a diluted portion of the extract# if errous iron is present a blue color will develop* If ferroous iron Is likely to be present In the acid extraot, the extract should be evaporated to dryness after addition of a few crystals of sodium ehlorate. The dry residue Is then dissolved in HCl and treated with sulfocyanate in the usual manner* A*B* Gerber June 10* I95O egh DSW 331920 STLCOPCB4078496 /aS' DKTBRMINATIOK OF FREEZING POINTS The methods below are those rsooramaaded "by the Research Department. ,\yT> ,, ` Sixty-eight to 7 grams of diphenyl ere placed la a 100 do Griffin-typs beaker end heated to shout 100c* The beaker is then wrapped la a towel* asking s loose layer of Sloth shout 2 inches thick around the beaker* The diphenyl le stirred with an Ansohuetz (45 IO5 scale) thermometer sad readings made every minute* until either the material is too solid to stir or until tha hulh of the thermometer le exposed* J^ The observed temperatures are corrected for seals n errors* If any* and plotted against time and a smooth line drawn through the points* The points will he found to fora a two distinct urves which join at the point at whloh the diphenyl starts to crystallize* From the time crystallization starts until the material becomes practically solid there Is a relative ly slow temperature drop* This is known as the "hold" of the ; CUrVe*:- ^ _.. : - - ....... , - . . By definition* the freezing point of the sample of ; diphenyl will he the temperature at the arithmetical mean time . ef the *fcoid* . :.v.. '. : . -N FRKKZXKG POINT OF AROCLORS ; ' For low-freezing materials such eua Aroolor 1219, the reoonmended method is as follows! t^ Seventy Ouhis centimetars sf Aroolor 1219 la placed in a 100 eo Griffin-type heaker. This heaker is placed in turn in a ISO 00 heaker* The 100 so heaker is supported by its flared rim on the rim of the larger heaker and hangs loosely in the larger heaker* The nested beakers are now placed in ah lee sludge* Initial Freezing point* The Aroolor la stirred with an Ansohuetz thermometer (so ale 10 to 550)* The temperature is read every minute and seeds of both 2-enlorodiphenyl and I*ohlorodlphenyl are added every minute until crystals begin to form in the liquid* The temperature at which erystals are DSW 331921 -is STLCOPCB4078497 ' ' `-1;- w-:*'rv.-> v...... ^- .. . .... .... /b first seen to Appear Is noted* Continue the stirring and temp* erature readings at one minute intervals until a thin Slurry Is obtained. In ease supercooling takes plaee (as it often does), a temperature rise will occur after crystals have appeared, in this event* continue the stirring and temperature readings until two or three oonoeoutive readings again snow deereasing temper- aturos* . The highest temperature attained after crystals begin to appear la taken as the "initial freezing point** In ease of no supercooling with resulaat rise in temperature* the temperature at which erystals first appear is taken as the "initial freezing point"* - /. solidification point* The 100 co beaker le then r removed from the larger beaker and placed directly in the lee sludge* Temperature reading are continued until the Aroelor becomes too thick to stir or until the bulb of the thermometer is exposed* The last reliable temperature is recorded as the solidification point* Freezing Point* The freezing point of the Aroelor is arbitrarily taken We average of the "initial freezing point" and the "solidification point"* The "initial freezing point" and the "solidification point" should be reported along with the "freezing point"* ^ -v-.-y ,-,v - i; . ;.. Check* As a oheok on the initial freezing point the beaker may be removed from the loe sludge* warmed in the hand, while the Aroelor is., stirred with the thermometer* until the temperature is 2 to 470* below the inltlel freezing point* The beaker Is then wrapped in a towel and held in the hand* Stirring is continued until the crystals in the Aroelor just malt* The temperature at this point is recorded as the final melting point* if carefully determined* the final melting point serves as a cheek on the initial freezing point and should not differ by more than a few tenths of a degree at most from the initial freezing point, jv- -- If the melting point check Is made* the average of the final melting point and initial freezing point Is taken aa the ohooked Initial freezing point* ...Noras,.,. DSW 331922 1* If carefully carried out and if the Aroolor is frequently seeded with both 2-ohlorodlphenyl end 4-ohlorodlphenyl, the determination of initial freezing point should not require checking by the melting point method* However* the Aroolor is very readily super-cooled so that unless great care STLCOPCB4078498 /7 la token, It may to ooolod several degree* below it* initial freezing point before crystallization starts# The reoult la that when crystallization does set In the temperature rises but the maximum temperature la not attained end observed intlal freezing point la therefore low* r-v ft It la for this reason that the X00 oo beaker is jackedted with a larger beaker during the determination of the Initial freezing point# The jacket serves to slow up the rate of cooling end insures a more accurate determination than the melhod there the 100 oo beaker la placed directly in the loe~sludge for the determination of initial freezing point# 5* On acoount of the Short exposed mercury column of the Anecnueta thermometers, corrections of observed temper-* atures for emergent stem are not ordinarily required# under usual conditions of test, this correction is below #X-0* If Conditions of test are such that the stem correction is large, the appropriate correction should be made and recorded as a corrected temperature# Seale corrections, if any, should always be applied# 4# Xa the determination, the stirring should be eontincus and the temperature readings made at one minute intervals throughout the test# The change from the water jacket to the loo bath should be made quickly without interruption of the one minute readings and the point of change to the lee bath should be indicated on the time temperature curve# DSW 331923 STLCOPCB4078499 STLCOPCB4078500 DETERMINATION 07 BENZOL INSOLUBLE , IN SOLID AR0QL0R3 %. Crash about 50 grama of rosin* weigh oat 1 gram lata a taped 125 so flask, add 25 so of Benzol and agitato the flask with a elroular ration for a few minutes* then add 2*> so rare of benzol, washing down the side of the flask* Allow to stand for 1 hour* fj Prepare a #3 Gooeh eruoible with an asbestos pad in the usual manner and dry to constant weight* Arrange the orueible for filtration by suction* filter the solution through the orueible* using slight suotion* tJse about $0 os of benzol to transfer the insoluble material left adhering to the sides of the flask and to wash any adhering film of resin from the sides of the crucible* Dry the eruoible and flask in an oTen at 105 H0c, oool and weigh* Add to the weight of the Insoluble material in the eruoible any Insoluble matter remaining in the flask* Report Insoluble matter as percentage of original weight of resin taken* BOTES 1* The method described abort is the one used by the H* E* Robertson company* ABO/pw 9-5.30 < :v DSW 331925 STLCOPCB4078501 -?0 ./, TAPORIZATIOM MBS AT ^ The test below le that given to u* by the h# H. _ Hobereton Company. They eall tor the 100 hour loee at I50 .4 Melt slightly more than 50 grama ot Aroolor in a suitable container, being careful not to raise the tempera ture higher than neoeseary to make the reain fluid* pour into a tared shallow glass oontalner (100 millimeter Petri diBh), ool to room temperature and weigh# ; -4', Heat for 100 hours (4 days, 4 hours) at 66c in a drying oven provided with a venting outlet tor escape of volatile matter# Remove from the oven, eool to room tempera ture mid reweigh# Report loss in weight as percentage of original weight* ~mm.,- - - ... ^ _ 1* On account of the small vaporisation loss at 660, the wei^its must be taken very carefully. It is very i^ortant in obtaining these close weights that the dish and contents be at atmospheric temperature when the weights are taken* a- , , ... . t. Robertson's first description of this test ealled for the determination of loss after 5# 100, and I50 hours of drying* From this data, they drew up curves showing loss against time. Their latest procedure calls only for the loss on 100 hours drying* abg/pw 9-6-30 -4 -'0 :. . V: . V- - .. -c? V , s-'.- vV . . . { -`V : \ " - .. . DSW 331926 STLCOPCB4078502 m iiU'hAi1- K' DIPHENYL IN CtniDE D *y}f m. or ffimim, *$j3epj. : r-Sf. oif ^0$f' to aoo grams ofiha ample to e 250 ee :. beaker* weigh beaker end dottiest* on e tough balance tonearest gram* watm beaker until contents are liquid then pour 100 to 150 gram* Into a 250 eo distilling flask with 10 Inoh distilling column attached* Reweigh beaker and 0entente, thereby obtaining by difference the weight 0f eample used* , Plaoe a 3000 or 400o thermometer in the top of the 10 inch distilling column in push a way that the top of the bulb Is even with the bottom of the side nook outlet. Distill off the diphenyl end oUeot in a woithed receiving flask until the thermometer reads 275C weigh the reeelvlng flask again and Oaloulate results* ^ # dlphonyl w1^ai|han?1^100 i pour the residue in the flask while still liquid into a casserole or pan kept for this purpose* Rinse with bensbl and allow to dry* * - ' - - - ' jmmzm. Am - f. The distilling flask is a 250 00 flask to whisk a 10 inch eolumn with side outlet near top is attached* The column has Indentations to inereass eurfaoe area* Asbestos paper should be wrapped around the eolumn* p\ mm*' 5W:V#:S ' Alleker burner is used in heating the flask* sines * high boiling point must be reached, the transits board or wire gauge on which the flask rests should have a hole nearly as large as the diameter of the flask* The flame may also be applied Aireotly to the flask without the use of any transits board or wire gauge* if nec essary, asbestos paper should DSW 331927 STLCOPCB4078503 Z'V'' to pissed et the tepf* the flask* ' ''-V...' f, V-'. St. : 100 ee dietimaeflask makes* convenient receiver for the distillate* ............ ' ' ABO/jW 9-5-30 . ; ;'' r: 1' 3' os*1918 STLCOPCB4078504 3 * u , MAGNESIUM QARBONATB TEST ` 's :...: /A ":' ' was furnished Oa by the H* H. Roberteon oo* seat 8S gram* Of Aroolor in a tPO do baaher to 1$0 o AAA 1*4 & grama of pure m&gneaiun carbonate and etlr until the mixture la ' homogeneoue, keeping the temple at 15<rCt Pour Into a clean 3 inch tin top end allow to cool, compare color with the etandarda furnished ua by the H# H* Robertson Gompany# .v ^a; ; ^ -- .- ' ,: the specifications on each Aroolor should state what examination Is to be made for appearance, color, sediment, structure, ate* - .. -. . |j ABG/pW $ l.i;i . -i:0-;>'., . -- ^ .; - . . `.Jy - ., 1 ...,, ' ' %. :-&.' ' ;. I'-'-'---:* - =:',' ': ' '/ .'.. '. .'- . :,. t, . >p- ;. -- .V ... . - f '-!>/- . ,,vi; '/: f, V .'*/; f '' <.!; w - -- 4-V: -> -; -,, ' *'^ .'. '` ' . . - - dSvm 33^929 ^ ' STLCOPCB4078505 7^ X, circular S* v.-\.".. . ....... . -"' Bureau of standards. The *": " . .:: : Tasting of Thermometers* , - ^ V./ .. - - .- . . .' -v*r\ :" '. ' O .. -.V ..-' . . - ?'' v-' - . ` < - - . - >-- ? . - -. ,, '. ' ; ., ' :'/* - - " ' * ,' r,./1 ' v * - t. ' ' : : fhoriaoiaetsa^s wre tostsd and soale corrections given far total immersion because this is a definite has la to Which observations taken with any known distribution of temper ature along the stem sen be referred* if tests were node in a given depth of taersion and room temperature, the results would not be applicable when the thermometers were used in a different bath at a different room temperature, even though the depth of immersion remained the same* mmmi In general | all corrections are determined for total Immersion, that is, for the condition where both bulb end Stem of the thermometer ere at the same temperature. If. however, the stem is emergent into space either hotter or solder than the temperature of the bulb, a stem eorreotiea must he applied to the observed reading of the thermometer# This so sailed stem Correction is very large if the number of degrees emergent and the difference of temperature between the bath and space above it art large* It may amount to more than 2GPC for measurements made with a mercurial thermometer at 400*0* The stem correction may be computed from the following formula* ' : , stem correction K x n(T <* %) V%v K* feetor for relative expansion of mercury in glass) 0*00015 to 0#00016 for centigrade thermometers, average value .OOOI55 n * length, expressed in degrees, of the mercury column emergent from the bath# T * observed thermometer reading* t * mean temperature of the emergent stem , DSW 331930 STLCOPCB4078506 IS (measured by a second thermometer i&igh i* fastened by Keen* of rubber Vanda to ife ........,.. Mr v....... the thermometer measuring the bath and the bulbof which ie at the middle of ; - ' '^r. dha ppiMtd threadof mercury)# T-- '-j- -'^ri;v;:':.-Wy .,,,,,., ., fcxample Ho* 1* Suppose 1fo*t the observed temperature * .4 i.". xas 100Qc and the thermometer taa immersed tothe 20 mark an ; ?V ' dna scale, o that 00r.*f the mercury column projected into tha air* and tha mean temperature a# the emergent atom oolume was .found to ha 25c* than* *- . staa correction 0#000155 x 80 x (100 * 25) y';' "" ' As tha atom van at a lower temperature then the bulb ater read too law, so that thia correction mat ha *au.eu w *uc observed reading to find the reading corresponding to total immersion. : .- .. ;. r.; > Example No* 2# Suppose that the observed reading was 500^0 and the thermometer waa imsaeraed to the 100 mark, ao that 400" of the meroury^oolum projected out into the airjrthe mean temperature of thejimOrgonO column waa found to he 1500, then the approidNatd value of the atem correction * 0*000155 x 4^0 * p- (jOO *. ijjO) W 21*7^0^ * .-. .. ... . # V> '. ' V- > ' . . '.. - . - ' " . '. . . . :W' 5 -- V'- - . The approximate temperature of the hath ia consequent ly 500 a#70# * 521*7* A closer approximation to the true value of the dtp Correctioa ie given hv substituting the ;***%* Mima* mm* 8%m correction * O.OOgi55 x 400 x (521*7 * 15) otei where the 'shetmoaeter passes thru* a cork aa i&,- iA W frdolmatthea..f.t.ie.o.n.n.tecraot.s-fupth-#e the degrees Cor-k* , em^ergent ehould he compu* f?% ' v?'> " . ::i . .. ^ -.J0U-'7~yy. j- '''V1'.- -'5 - v` - - scale corrections are determined hy dlreot comparison against a thermometer which has been calibrated by the Bureau of Standards* Each thermometer used for the accurate determination Of boiling or freezing points should be carefully compared at fall immersion with a standard thermometer and a reoord made of the oorreetlona which must bo made at many different points on the aeelo# DSW 331931 STLCOPCB4078507 7-1 a?U<i data mgy b* kept aa a tala* or m a curve. The idea* corrections must# of course. be well established at the temperature point* at Which th* thermometer will he chiefly used, .......................... isift : .. .'4.'' ....... s? i ' ' 1. > Sine* thermometers mayehange due to exposure to or to the alow natural contraction of the glace whioh continue for years# roe nation of the thermometer are required fro*i: time to time* "M3............................B...A.......m.......S.. KiS,m the temperature of holling liquids and consequently that ofJLtc vapor variea w|th the atmospheric pressure* t* %lor the boilingJipiht of water# the correction of atmospheric pressure eanbe obtained by adding 6*0375^0 for every sea# the prevalllng baroaetrio pressure reads below 76Q mm or subtracting 0*0375 0 for every mm* above 760 mm. For exsmpie# If the ohi^pdi. temperature reading Is 95*iC at a barmetric proscure Wf Jhe eorreeted temperature is 99*4 4 (l6 3C 0*0379) 10^ for the helling points of liquids other than water* the correction factors may he Calculated approximately if the Vapor tension at the boiling point Is known* For example* for benzol the correction factor per mm* of pressure Is 0*043*0# far xylo-l the correcti-on f-act-< p,, er *....#....H...i..0.,0. 5,,a#. f.o...r...t.urp_ e. ntine the eorreetlon factor is 0*050* Mulliken "Identification of Organic Compounds" gives 0.036o as an average correction figure which can he used on organ! llguids* > In the case Of the boiling point and distillation range of Arcelor* where the temperatures are high and the ; correction factor ia unknown# it is advisable to omit correct* ion for barometer* fhi barometric reading, however, should be recorded along with the dietmation or boiling point data* :'$V" iBS/pw 9-2-30 33793. ? STLCOPCB4078508