Document 1g8qbEpq19vJ3y1wOEeBM8M0j

BATES LABELS 0C07-SWP-O43S00 THROUGH 0007-SWP-043SCL NOT USED IN THIS PRODUCTION - Dcj," s c h et 'j l b o f smtna^xw y0. 86 Issued by Eaint Besearch Division Detroit, Michigan July 15, 1933 STABILITY TEST LEADED ZINC ASP OTHER BASIC LEAD SOLPPA'ng PlmraHTR QSESRA1 This test should be regarded as ien+ative. This test x b Based cn the reaction which takes place when Basie Lead Sulphate pigments, such as Leaded Zincs and. Sublimed White Lead, are rubbed up in Glycerine, producing a pinkish discoloration, more or less pronounced, depending on the particular pigment, grade of Glycerine, temperature and light conditions^ Some Basic Lead Sulphate pigments which develop this color ation rapidly show a similar tendency in certain vehicles when exposed in paste form to ultraviolet iigh^-, and much more slowly on exposure to sunlight in a paint film. This "Glycerine test' is easily performed and serves to distinguish Basic Lead Sulphate pigments which are relatively light stable from those which are relatively unstable. 1 In order to avoid misleading.^results- the tes^ moBt^iS;. ^conducted under carefully controlled conditions and. against ^standard :'of,`proven stability in various vehicles'under ultraviolet' c?f-' ions, in *1 L#h<mia%BE0ar. of ihiTt^63Wt:;i-gSes'sai'ti6llijh'tlhhlV^hot'rbrl'abt r ___ . - 8 le<t 1,8 uaed'nt normal. |jM>plate;,carTying the smear is then placed in an inM/11''SOd'tiiTfor'"one hour. At the expiration of " 'from the oven and cool at room temperature for 0007-SWP-043602 0007-SWP-000126946 Schedule of Examination No 86 . Sh'et A fresh postc- of Ox gocm- cue g]yi,'*rJ.ne ic now o V made r..id laid down against the heated and coo'.ed smear This paste mist "be freshly made and not a portion of the firs- paste held over Examine, tion is then made for change m r.olorr,r.ioT> of the particular pigment in the heating with Glycerine Due consideration mast "be given the flatting effect of the heat on the to the change m the u Oj . oni';' is considered. Each pigment is examined agiinst itself The use of the standard is a check on the test and noi on the sample under test I:. properly conducted there will he no change (or at most a fain appr.rc.r. darkening due to flatting of vehicle rather rkan of the pigment) with the standard pigjaeat. The discoloration if any, may te re'..'Orted on. a numerical system using the standard ligh* sensitivity char in estimating. G - No change 8". - Very 'faint darkening 01 pink <j2 ,, Easily detectable darkening or pink (F = Decided darkening or pink Or - Cbnsljienable darkening or pink Q5 - Salmbifred or fellow led - 'it-". 0007-SWP-000126947 ors c h t o p is micmyiog Ho. 43 leaned by Cleveland. Technical Servian Dipt., Voombor 21, 1934. a w a it s is qr w h it e p a iw t s (?i outre romca) {Thl Sohednle la derived frow Chaptera XTI Mi Zfll of Dr. Hoilay* a book, *Analyla of Paint and Tarnieh Products*, edition of 1912) 1. OQAIITATITg IIUWIB In the Majority of oaaaa a complete goalltatle* analystt of the plgaoste praaant la hardly north the tine It regalear, aa there la hot little tlaw load In following the regular foaatltetlve sohewa. If, however, a fualltative analrale la da aired, the foiloaring antline alll be found raffIciest in noet lnetencea, the reamval of tee vehiele previous to these tart a being nniereteoi. (2ee Schedule of XmatnaAlm lo. U) Carbonatea Iffamniwi tin eeaaaatrated hydroahlorio eat* laUtatu mtwtM, or hyTtgtn oalpMde If ate* sulphide be praaant, the tetter being distinguished by ita oir and by the tsmoo blackening a place of filter payer noietened with land aeatelo. *mt*3* loll abate aistare flea ttadu, dilute with Mlbf enter, titter; An isaaluKfca realtea nay la baryte a, alllea, clay, r ether al Ueetaa,; 'dBHrt tme barytea mow teat, udag^n alatt-- wire. A ohnranterlat&a yMMiliriaMtlir bterwi:;-. ' feat a naall portion of the aald filtrate for edMwi sulphorlis add with too darwps of barlan ddtrlii. foot another mall portion of the add filtrate with sulphurie add. A'" mit ywH)Htrta at-aaw if oo rtaatei >ndlii lead. ^ JlM /'>-r^v1ikraonR moll parkin of the acid filtrate and add a fee drape of potacalc*forraoymatde. *&*&* precipitate with a bin!ah tinge indicate. *ino. 0007--SWP--043604 N23220.01 0007-SWP-000126948 Schedule of SttBlnttioB Xo. 42. 2 U/21/2i Cal don The remaining portion of the acid. flitrot la miK alkaline nth ammonia and hydrogen sulphide passed in for fl-ro ainntss. filter and tost filtrate for calcium with wmenlUB oxalate, setting aside In a oars plaos. Means slma if ter oosplstely precipitating the calcium add. a fee drops of hydrogen sodina phosphate. 4 preolpltate on standing indicates the presents of magnesium compounds. The identification of the fonts in which^|hs lead may oeeor can only be determined by the yaautltatlve aohese If both sulphates and carbonates are present. smmxMxm iw a u b ib or i o t mm 9, Tyrg mv Teigh 1 gnus af the dry plgasnt into a 280 o.c. heahsr. Add 20 e.o. of strong hydroohlerie add, boil 5 dentes, add 20 .. nf hot eater, teat 10 dautes longer, settle, filter while hat, and mash thoroughly with boiling stir. The mashing shanH he began the Instent the solution lat filtered tbrmogh, In order fce swli any oryetalllsatiom of lead nhlorlda in the perma of the filter peper. that faimed the crystals can gaily be dissolved with difficulty and ellh tte'tN''tftedNMi mf aUh mater, mfcdah, as elated, mast ha at boiling tuagmra* . This apsrattmn to host rmndnsWd by the aid of saotlon. Casein and other paradncte of * ahallar matara are nese si easily steed in the aamfacturs of nixed paints in ooasjdorabio goantities, ami tbe analyst should always ha on the leofcast for tbo pesslblo praecaea of thoao whstaaces. IBm-diflam-le made Just alkaline mith mean sis, than Jest said t litarns sd%h hrdrsChlsrlsrndt. ft to smry neaensery that the aatah* ha aaly barsly add, ttd- ingiimih' fall gaaatUy T free maid mill temp considerable lead rrm ptfIjatjteft,' Mat hara arf> barely elhallne, nkUh is indented by the predyitattan of the land, the eeluttea io brought to a faintly add oanCttiLaa by uaDtg^gltis hydrashlavlo add (l ta 10). Dilute to about 880 o.o. Coal, pass la hytrngm tetUldia gas, acting the calar of the prscdpitata: if gray, some illno la being throon dana; if reidlah blank, the solution is too add. Add a foe drops of dlhrtsaitt ar smaonla ns the aase requires. Settla, filter, and mash with eold matsr. flwt .. of nitrls add and 28 o.o. at aator, heat *ntly/fRtiii/dte lead basall dissolved, am shown by ths residual sulptar having a riltir liiwll hyTliii ll `fl herd enough thoroughly to disintegrate the <M wgagBS anted la dlseolvtag the lead contained la the eiiljwnT^ go oatteet ttea into a hall mith the aid of a stirring -go a fall hanker and treat mith a few cable centimeters concentrated ttttrlousli, and teat until dissolved, than pour hack into the largsr beaker. 0007-SWP-043605 0007-SWP-000126949 Schedule of xrlnet1on So, 42. 3 11/31/24 Pour solution and filter paper on to a ruction funnel provided with a platino* con*. If any fine particle# pas* through, pour the filtrate hack again. Thle procedure permits the washing of the filter mass with a very Mil amount of water, thne earing considerable time In the sub sequent evaporation. If the above apparatus is not available, filter through paper In the ordinary way, washing carefully. Add 5 o.c. of dilute sulphuric acid to filtrate, and evaporate until sulphur trloxide fumes appear. Cool, add 35 c.c. of water, 25 c.c. of alcohol; allow to stand one-half hour with occasional stirring; filter, using Qooch crucible, wash with diluts alcohol, dry, heat gently over ordinary lasp, and weigh as lead sulphate. 3. CALCTPM the filtrate containing the sine, calcium, and possibly magnesium Is made slightly alkaline with ammonia, a few drops of a mercuric chloride solution (l to 10) added, and a stream of hydrogen sulphide gas passed Into the solution for about ten minutes. tbs addition of the mercuric chloride renders the precipitate granular and very ea^r to filter, and entirely obviates the difficulty of filtering a slimy xino sulphide precipitate. In the analysis f tints wber# the sine cannot be titrated until it hat been freed from Iren, the addition of the mtreurlo ohleride will not aan.se any trouble, as treatment with hydrochloric mold results in the solution of the sine only, the meroorio sulphide being insoluble In hydrochloric acid. Settle, decant, filter, and wash. Evaporate the filtrate from above precipitate to about 150 c.a., make alkaline with ammonia, add ammonium oxalate (00 o.o. for 1 gram of lime), usually 90 e.c. la sufficient, and set In a warm place for two or three hours, /liter, wash, ignite, and weigh as oalotum oxide, or titrate precipitate with paraamipanfee by platting filter and the thoroughly washed, preclpltat* in a 400 o.o. beaker, add ing 900 e.c. of boiling water and 30 o.o. of dilute sulphuric acid, and titrate with standard tenth-norsel pota*si w permanganate. /liter paper mast bo removed frsm the solution before titrating. 1 o.o. tenth-normal permanganate = 0.0039 gram C*0 1 o.c, tenth-normal permanganate = 0.0000 gnsa CaCO^. \ Barium carbonate is still to be found in certain mixed paints, and it Is advisable to teat for tbs presence of soluble barium with a few drop* ef sul phuric acid before precipitating the ealelua. 4. mwaaiPM The filtrate from the oaldust oxalate should he teeted for magnesium by treating with hydrogen sodium phosphate. Allow to stand one-half hour, add 25 c.c. of ammonia, allow to stand one hour, then filter on to a Goooh crucible, wash with dilute ammonia, ignite, and weigh. Veight precipitate x 0.7575 weight magnesium carbonate. 0007-SWP--043606 0007-SWP-000126950 Schelde Of KoalottlM K. 43. -4- U/ZL/34 sa...gKj|DS Standard fine eolntlca X&stolm 10 pw of steal0*1X7 pars si no in bydrooblorie said in * graduated litsr flesk, *dd 80 gnat of nnlna chloride, and ask# op tn 1 liter. 1 e.e. = 0.01 gemn eine or 0.01940 gram slao osids. Standard pMmlni ferroemnido solntioa Dissolve 40 to 48 gnats of crystalline<1 potatslwn fsrrooTaalle in water, sate to 1000 0.0. tttwdti nitrate solatia* 81ssalve 15 grass of wui nitrate in 100 c.o. af water. ****?<*#"* ,WW ,.** f* 4rtBtH tin wains of tte pcttaeslwaa ferrosyaal.de ooteaiaa, piptw 88 e.e. ftfjn-4at a 400 a.o. boater. Rlato aasM sat ante * a faintly Mdd condition atfct tednstelorle anid, aaiTjten mM 8 o.n. Mt*** f tte nnansatmial *nl*, 4ilto fe a total TstaatguMilriK a , tet-te# C., and tlteate ms foilaoo; tear off (best 10 OiSi 4f;-t*n nine solatia* late asall Mar attft ost aelga, m tte ure- 4 tf*ttasl tentAi tear. flattest ioi-a-*-*<aP, a'.**t#8fr iter-asla- i^itete saltskla* w*n jtecslain Ofton tte mi pelat tea tea jnmt tte krte.MltB 3, IS 10.O.O. of water, roy tte standard sine tte naan depth sf color on the __________is oarwfnliy osrriod oat, tte prooetare teing L'dntaradtetlnn, tte re salts will be focal satisfactorily . t 0007-SWP-043607 0007-SWP-000126951 Schedule of Examination Bo. 43. 5- 11/21/ 34 6. LEAP SULPHATE Dissolve 0.5 gram In a alight excess of dilute hydrochloric bold. Dl3'>te to 200 a.c. and add a piece of aluminas foil which about coror the bottom of the beaker. It ! Important that this b hold at the bottom by a glass rod. Boll gontljr until the load lo precipitated. Completion of thlo is ahown by tha load ceasing to coat or cling to the alxmlmn. He cant through a filter, pressing tho load sponge Into oak# to fros It from solution. Add to filtrate a slight excess of barium chlorldo solution, allow precipitate to oottlo for on hoar on hot plats, filter, wo eh, Ignite , and weigh ae barlm ralphate. Calculate to lead sulphate by multiplying by 1,3 at a factor, unless calcium eulphate le preeont, in which caeo it le advisable to woks uee of Thoapeon'e eoparatlon. In tha absence of barium sulphate tho combined sulphuric add easy be oatlmatod by H, Momhardt's method: Grind 1 gram of pigment with 1 gram of sodium carbonate rory Intimately In on agate mortar. Boll gently for tan minutes, the eaefclned eulphnrle add, and in the cate at colors containing chromate the chromic add, will pass into solution and may be estimated in the filtrate In the usual aanntr. If necessary colleot the Insoluble portion on a filter, dry, detach, and triturate e second time. 1, BASIC CAgBOflgE Of 1BI frHItS UMB) After deducting the amount of lead present In the pliant as sulphate at lead, calculate the (met of the lead as white load by multiplying the remaining eulphate by 0.803, unlese eublimed lead Is snspeotad to be present, in which case the ounfelned lead oxide met be taken into consideration. 'iJZ'JVjZ The Insoluble residue from the original hydrochloric add treatment may contain baryte e, rnagneslm el licet*, ellloa, and clay. Ignite filter paper and residue until white, weigh as total insoluble matter; grind In agate mortar with about 10 times its weight of soda* oarbemate, fuse for 1 hour la a platinum crucible, and dieeolra out In hot water. Barium sulphate The solution from the fusion le filtered. The residue consists of barium carbonate, magnesium carbonate, etc., and Is washed with hot water. The filtrate and washings are sawed. Pieros filter paper and wash precipitate into clean banker with hot dilute hydrochloric odd; finish washing with hot water, heat to boiling, add 10 c.e. of dilate eulphnrle add to predpltate barium, filter, Ignite, and weigh as barium eulphate. Silica Tha filtrate from the barium sulphate le added with care to the filtrate reserved In t*** preceding paragraph, maklng distinctly add; evaporate to complete dryness, oool, add 15 c.c. of hydrochloric aald, heat to boiling, cool, settle, filter. Ignite, and weigh ae silica. 0007-SWP-043 608 0007-SWP-000126952 Schedule of Xxamlnatloa Ho. 42. Alenina 6 11/ 21/ 24 Tbo filtrate from the iliaa will contain all of ths almlna axespt that which was dissolved In tha or1glial treatnsut with hydrochloric acid, This 1 guite constant, varying from .004 to .006 gna Pr grow of clay. Ths add flitrata, ara sad* slightly alkaline with aswala, and bollad until odor 41 sappsars. Bottls, flltar, wash, lgnits, and wwlgh as alusdna. Haight alowlna z 3.6373 - wolght olay. Weight olay * .4647 = weight of silica In slay. Any differsac* greater than 6 par asnt nay ha oonaldarad as fra a or addad silica, according to Soott. _ Calcine and Keans tjun odds# If qualitative tost shows prsssneo of ne&edus In lnsolnhls rail das fro* ths first faydrocklsrlc add treatment. it was prssant probably as Mgnsul-aa si 11 oats. Treat filtrate fro* ths almlnxn hydrazlds for c*ldT* sad aagnsi&tn oxides. Magnetic* si 11 oats contains 3 to 6 per oont combined water. h mmm Instead of re sorting to faatoa with aodlwa iwrtowts, the insslwhlo reddue, which should ha weighed sp las clean platlma* crnolbls, say 1m trastad with several drops of pwra oonoontratad hydrofluoric add and sulphuric add and bedad gently on a aaad hath water tha head, wot^ only wofftstart haat slswty to tabtttlM tha stilts and ssOphnrle aold. Itssatn ant in water aaldaletad irlth add. The rsstdM, ohtdkla fetttni attphuta, tt fittarad ttt-mid nttaj^ai as neh. tha flltrata will osnts&n any ihMas, 0*1du*. sod wagnsstwa Ptepfel Oddah stay ha estlnatsd and oalanlatad as axldao as abwv* daswrlbad. 'tha WWMi ndght of tha harlwn anlphats, alnstna, detw, and asgastsa addsis ahhtgsjiftad frw tha sdgjM of tha Ittsefehln rodtea naad ft*** tea walgfet of dUea. Thl'fjji>0*tloa is ante ahartsr than recanting ta a fndaa and a pally as aanifats. \1 Occasionally paints ara aat with nhloh contain oalo&na anlphats, oalolun earhanata, aolphata of load, and ahlts load Chaslo carbonate of lead), in which ease It la naesssary to ante a separation of tha oaldum {cspwsto, ddah nay ha affeated by DasgsM's asthod as fallows: * 1 gran of ths asaqtla n*a aUd lt *-*. sf a sdxMua af-sdna.flirts alcohol (66 par oast) and one part of (innoaliratal ndtria add. 6tlr, end -allow ta stand 60 ainokaa. Asoant an * flltar nmt.yiiteil.iaw ttMUHt *lth mi* jdMHilaahol nixtam'ycar tints, silwttill -ta tttiian aarhoaata nUl go into aefetian, whlla tha aaloAnaaulphata nr gypsou ranoiaa utttOeeXtaL; AddfiUaxxtt ***** tha ateaidne in tta hatter; dissolve la^M^^^Un&ddth aamdax* wttar * infer* tbs solution of tha ealdw. tuw2p*vjia siibdnals, past la hydrogen vs&phlte for 10 minutes, boil, settle, ^flltfrwj&fh* filtrate and weblogs ara concentrated to about 150 c.c. and ths telttte%Y*eivit*tad with aasionlnw oxalate In ths unal manner, Tbs Ignited preelpl- tata la oalowlatad to hydrated calcium sulphate. 0007-SWP--043609 0007-SWP-000126953 Schedule of Examination Bo. 43. 7 12/21/34 ii. ssrmmar or c ah bg k d io x id e ih t h e p b b s z b c z o f z ih c s t o p h iis Thle Method, devised by Mgnahwrdt, la often useful in determining complex mixture* of pl^tenta. One gnus of the pigment la ground for several ml rmtaa in a aamreth glass sorter with an ezceaa of bichromate of potash, using considerable pressure; the mixture is then placed in the carbon dioxide gener ator and the carbon dioxide liberated and estimated in the usual manner. 13. CALCDIATI0K5 the ignited precipitate of calcium oxide obtained from the portion insoluble In the aaid-alaohol mixture is subtracted frost the total caloiun weighed at oxide; the remaining oalcion oxide 1 calculated to salslut carbon ate. The total carbon dioxide it determined in a portion of the sample, the portion due to the calcium carbonate is deducted from the total amount, and the remainder calculated to baeio carbonate of lead. The combined sulphuric acid due to the sulphate of lime ie deducted from the total combined sulphuric add, and the remainder calculated to sulphate of lead. Wt. calcium oxide x 3.0715 = hydrated calcium sulphate. Wt. oaloleai oxide x 1.7*4 = calcium carbonate, Wt. calcium carbonate x 0.440 = carbon dioxide, Wt. carbon dioxide x 8.0058 = basic o&rbomte of lead, Wt. of hydrated sulphate of lime x 0.4541 = combined sulphuric acid, Wt. of combined sulphuric acid x 3.788 = sulphate of lead. AKALIB 13 tff WHITS PAIHTS ACCOM Wt TO THCTtPBOW (3. Soe. China. Ind., June 30, 18ttl Bohames for the separattea of the constituents front each other end into thmir preximate combinations depend on the constituent a present, and we ean treat this subject in no better way than by taking typical cases, which we new da. 13. hiKPia 1 is a mixture of barytes, whits lead, and sine oxidw. Two 1-gram portions are weighed out. One is dissolved in acetic acid and filtered, the Insoluble matter Ignited and weighed as barytes, the lead in the soluble portion precipitated with bichroautte of potash, weighed In Gooch crucible as qhiwte, and calculated to white lead. Tbs other portion is dissolved in dilute nitric acid, sulphuric acid added 1& excess, evaporation carried to fums, water added, the sine sulphate solution filtered from barytes sued lead sulphate and precipitated directly as oarbenate, filtered, ignltwd, and weighed as oxida. 0007-SWP-043 610 0007-SWP-000126954 chaduls of laalotlan Ho. 43. a U/21/34 14, SAMPLE 3 1* a mlxturs of Wryta * and *0-001104 sublimed whit* lead. H*lgh oat three 1-grwm portions. In on* determine zinc oxide, as In case 1. Treat a second portion with boiling aeetlo acid, filter, dsterstln* lead in filtrate, and calculate to lead oxide. Treat third portion by boiling with aold ammonium acetate, filter. Ignite, and weigh residue as barytes; determine total lead In filtrate, deduct from it the lead a oxide, and calculate tie remainder to sulphate. 8ubllaed lead contains no hydrate of lead, and Itt relative whiteness is probably due to the oxide Of lead being contained with the sulphate as basic sulphate. Its analysis should be reported In terms of sulphate of lead, oxide of lead, and oxide of sine. 15. 3AMPH 3 lea mixture of barytes, sublimed fead, and white lead. Determine barytes, sine oxide, lead soluble in aaetle add and in ammonlm aoetats, as in cas# 3; also, dstermlo* Carbonlfl acid, which oalculata to whit* lead, deduct lead in whit* lead from tbs lead soluble In aoetlo add, and calculate the remainder to lead oxide. 16. 811CJX 4 le a mixture of barytes, whits lead, and carbonate of lime. Determine baryte a and lead soluble in aaetle aold (whit* lead), as in ease 1, In filtrate from lead chromate precipitate lima a* oxalate, weigh aa sulphate, and salaulat* to carbonate. Chromic aold dose not interfere with the predpitatlom of lime as oxalate from aoetlo aold solution, 17, aAMPUt 6 is a mixture of barytes, white lead, Uno oxide, and oarbonate of lima. Determine baryte* and whit* lead as in case 1. Dissolve another portion In moatlo add, filter, and pass aulphnreted hydrogen through the boiling solu tion, filter, and pr* dpi tat# lime in filtrate a* oxalate; die solve mixed sulphides of load and sine in dilute nitric add, evaporate to fossa with eulptarle acid, separate, and determine sins oxide, a* in ease 1. 18. Sj|gU g is * mixture of barytes, whits load, sublimed lead, and saxtennt* of Urns. Determine barytes, lead soluble in aoetlo add and in ammonium acetate, as in case 8, lime and sine odds, as In case 5, and oarbonle add. Calculus* lime to osrbomst# of lime, dsduct oarbodo add In it from total carbonic add, oalculat# tht rsmalndsr of it to whits lead, deduct lead in whits lead from lead soluble in aoetlo aold, and calculate the rasaimder to odd* of lead. 19, 8AMP18 7 contain* as Insoluble matter, barytss, china olay, and silica. After igniting and weighing the insoluble matter, carbonate of soda 1 added to It and the mixture fused, ffcs fused mass is treated with water end the Insoluble portion filtered off and mashed. Chi* Insoluble portion is dis solved in dilate hydrochloric acid, and the barium preswat precipitated with miphBwiff aold In excess. Ths barium sulphate Is filtered cat, ignited, weighed, and if this weight doss not differ materially - say by 3 per oaat - from the weight of the total Insoluble matter, tha total Insoluble matter is reported as barytes. If the difference is greater than this, add the filtrate from tha 0007-SWP-043611 0007-SWP-000126955 ASA LYSIS OF 0H1TB-EAIETS-{PlflttEIft POfiTlOld &V- *k:"- TIT/HUNK. DXJJ& . Ji-S -i5^-* - ^ Oi too CUT if A \.i.& < ,. . *,A'-i. *CV: *l. c;> l ? '.V- J-w i 1 * .-T& 11 4.. - . J-. COOl dilute"*}th water, and filter. 7c > or_ 20 o. of the fil'Cisjjj' in a test tube add " c.c. hydrogej. poroj.td^ A ciistifi&jL.. coloration indicates the presence of Tit&nox Bothing-sf*!' in a White Pair.t inttrferes with thirt test. ys. 1 !<.< o Iq ; Increases with, the amount ef^Tltanlum present and is not al' by.either an eioeas of,^^rogeb;i>eroxide or sulphuric acid"1 However, the amount of sulphuric arid present cruet be at 1 5% by volume.' It is we'lX:to test out the hydrogen peroxide used in making thin test on a e*.*ple know-. ?- .,-or.tsi- Titaniums. _ (^ay 100? dry), as inaccurate results are obtained in the -p---1--- senoe. of..hydroflourl c acid, consequently it is not permissi - 1^^.o4by>gn-peroxide'Afo'rMhla teat which hae been prep'- 'frbpbaritia 'peroxide by mean's of hydrofluoaiiioio acido , ' furthermorei`chromic, vanadic and stlyMio acids muot not present-SlBOS they also.give, colorations with hydrogen p* The pretence of snail amounts of iron does not affect the :xw^V|Sl!ftrttany^ore thaniaKtrn.es -of iron-would not be -prej 'inia^hi^igfPlgnient. . If> however, phosphoric acid is addl_ t# hndfslfirlo' solution it..betomes decolorised and from such sOJLptl^nijSfiihc determination of the presence of Titanium w -Thls-:rsao,tion is delicate to 000005 l|0xid present^o*^ sulphate-In 50 os. of solution; >.rransfe5fe Pyrdx'bdaker, ad Jt'cfd''and' 7 to 8 ''grabs- of ^ JfT"Mix heat on hot plate until;, bid are voivsdf,-and then continue the be"' spams ujjUii/sipBticn is complete (usually., Utso) or ,it/.lii^>parent that the residue'is ..sulpha ta. ,-^jfitoel,;,' * " .let settle, filter tftroj . ** Itrate to 20Q o.c. and aid about , ,, ... . %fep. gr. o.c'!' -c lc*r ' - nilt; $&(by .volume) eulph-cric e.~: > Ib-'" lash out a Jcpf!< EfiCMid and water, I*:- 0007-SWP-043612 u .\^:s!5S-j s b: 0007-SWP-000126956 waahirft not ooro than one or two^ir,<ps of O.IK,pr^^an8it*Si'oObtain a pint color) Eaptjp' `-the re ceiver and "put in it 2S c.?. (measured Taduate) oi ferrio sulphate solution, (See reagent^ pared Titanium solution v. izi.c-sa-. f.e-iuod the pr-e *i*- *' " -,V*V - (i/- itun.50 ^*.c# ex' u^;] the xaciucss at.',a';*pGe<i__of about 100 c.c, pex-inutp* - *i *! '(a)- f&Wlh^Kth the Titaaiun solution %~w .msseMfe' vs-Vi*' .(3)- lash out ifith^lOQ o,c. pulpboric ucil. .. /i'.- > ' ' ;-*' ' (4)- Tiaally run'.through about 100 a.e. oi water,'. dre - Should be taken-that the raductor is always filled with solution or -at ter to the upp? . A-,ei of the tine, Gradually.j'jsleasothc suction, wash thoroughly the gj ^jnereed ir, the ferric suiphate.-aolutij fecitl' fe- .- solution. One .. _ - " 'potasalua 'p'elfibhhg^fl^ta equals 0..00*:31 grams *1 tani urn ,,:s , ..u'toro008Qlgratts.*it*-niu* Oxide. Run a blank.dater* ;J)t ""' ` -- - ...................... ... . leu 1st .. ..^{ihWfinali,reading to Titanium dioxide. This, ::'; p&X.Xnolufai&tPfo, chromium, arsenic, and'-aa/^otber .^t^-^;*uh^tjtoijf^]h'.'ie reduoed byrXico and apdd^Ut^nOrie e|sd%^>o present ex.cepti:as a trah4^^^%bii CTwnyreg^&^spet-; oocmOn' Tltanlum.plgaSif * .'V 4 -i^^*a^^^i^l|8^dntalnlng 25^4Titanlua 0jfi ... ... W-W--------..... v s k -.!V * { SfeorWfeRife-BuiPmTy so l o t row - a soiutm;ochi_ Ii^^kiK(-Mper^gent.-1 ron a* ferric sulphate is deeirdd'addrj ' b^MW^WMP^dlloir*': vrTapssg^ir.-f *:-fS ;. 4dd about fiO o.e. of .sulphuric..at EST t& F'oi ^fs.oltsjlr'*P4 ,-Xllts.**jjMis bit's si perfiaigartate until a faint pi nr color' ' Lnutas. (to exiiiro -*r,y forr c u b irofl fWeent; fe<*<*r"-. 0007-SWP--043613 0007-SWP-000126957 dlaastet of about 19 asa, Ifcon the spiral, or glass b*.*lc, 3 ic plaoei a plug of glaa? and than thin la/or c as'^sto* such as is ussi for fCreech ' _ .-I eltfc . "'* - \n filial *ith ' i rinc >?*hln 5 r.i no c a u b j olfanlns it with a l'ittia 1 /'if i v'ulvrilo w-iiil - j - ^ i* j *i .> this oonditlOhftho *inc is scarcely sietid u;> on at al t>/ hydrochloric aqld, bat le capable ef caiur-t/g *i, isc:: c . Titaniua solutioh just a.a affaotivaly aw If it war net. ga^atad. On top of tha eolunai of *tno is placed * '1- glafts wool to serve aa a flitar. - > BiMTSSSSST s avt. ' un__ ti /techiC^^9 0007-SWP-043614 0007-SWP-000126958 ''/'H- f- *y*t*r- .* Weigh accurately a.5 grass of pigment, transfer to a 8B0-r-- ' c. c. irlonKr-ttr flask, moisten with a. fn* dr-:ps of aleohol* &i<l about 3C0 c.o. of 2ft to f.'vttic oo-jd, (20 r., o, - rAkCiO1 .a *aw v'^ * * V. < .igorcufll/ and. . ltt itarvJ faar 30 nla. at roots temperature, shaking oaoe?'^*- every five minutes. Then let stand at root temperature irk, at least fire hours, preferably overnight, filter throSpl'-* a dry paps/ into a 250 0.3. gr-'-a<.iR.t?d rolusetric flask* ; - - Wash residue with 3jC to 3Jfr acetic acid and fli] voluio$ flaek-.to mar* with 3)C to 3%>c*tic acid. Transfer c.0. Of the filtrate (corresponding to 1 gram) to a c-0. beater. To the olear solution add 30 e. 0, of (1:3), 100 c.c " water, and ?,, small pi eon of litmus paper; add strong ammonium hydroxide until alkaline, render Just add with hydrochloric* acid, then add 3 o conoenji^kted hy.drochlo^id, neat Nearly to bcilinj and titrate with potasaHtt^ferro-cyanide oolutlon as i running total *fne. Calculate the percentage of sinc^ oxide (any zinc carbonatf;_.or zinc* sulphate la includof the aino oxide). Subtract thia result from fchs-jjsjrooi of total -jUna as sine oxide and oalouiat# the diffe#* to xin'o'eulpM da. "r` I ; wit-f.--. W^VSHTtlKSCKISEW ;aSsi A-..sSs 0007--SWP-043615 0007-SWP-000126959