Document wKRex0LnVpqaMenVK9MyjxXYJ

p r o j e c t mr -8 ; THE DETERMINATION OF SMALL QUANTITIES OF LEAD IN URINE submitted by -- ~ W. F. von Oettingen, M.D., Ph.D* Director.... :, ...L.. Haskell Laboratory of Industrial Toxicology - Wilining toil, Delaware rr'- ^ .. ' .;S/ DUP040001784"7T la order to decide a$>o& a aotfeod for the 4tj?aia*tioa of lead %n oris* which should he suitable for group the following aetfcedg mm $tntUi , all of which 'am based apea the ma of dit&loeo* (ilpheg^lfhloo*^^ eolatloft fore# *-i^#aMed colored coaplex cUthM*" ' 1* Behrea# att faeger* Xtse&r* g*oaeptl* Med*,, jgf, iBt 1936. HI . Bo## and.luoaa. S, Biol*. &.. U* S8# 1B8B* foapseit &d &&*?*&,' Siahe* f*r M* MW*#- iir 4* fil&tns, l?illottgfe'0f*8.-l^aa#- *yad. .' lad* lag* mmv: i* ieelBopf sad larger* . . .. fetschr* ges* vxptU Bed** m# r JW* * flater, Soblasso, laalb sad' S&Llar* Xnd. lag* Qhm* mtt'l* t&*> , &SS, .&ABB with the## ^ sethod#...the ..aM^...jof..looi..1#.,.cltifc..doteralaad..... fcjr caapariag the inteaeitgr .&*oolori^oter^ egniipt;-'#.; :#teadapt^:or=^,#iifcaiai 'r the afeaorptioa- of light la m spoctropliotomstor,; or fey 'GmPminlng %m omt of dithisone repaired for tim ^rntplm^th-r. dlthlsoae haring hoea staadwriUaed ageiaet * toom sasiiat of losd* , Ihi first aetfaod otadied. as* .'that of flMari. fllloajldsy^- ^ KrtiMr sod inith, which tsfeaaed apoa of lead with a staadord dithisoao solution*. "ifcdo^' howeror, did cot ,\ * ' lead Itself eery fdvmfeljr to oar profcle* bettHUMt. its results DUP040001785 were m% aeemrete maiagk for tko. Amamfeltie* of lead fetnagt iM nrim#* ad %mmm the mu of a 4#ro karette or seesrai alerts....... bare**** s?snl4 regntre am elaborate sot ap* to ooa^&ot4 for ellmismi mode* the aetM of fteelfcopf ansi tasger #* not stm4ie& ,. M-retairea tie no# of * sp##tropliton#tr* an Imstrsttiomfcmot^------ 1 available in Boat eiiaieal laboratories* fit# aeMtefte-'/ef lebreas sm&, T&oger, .of Tm&mtt sad. im&ersea, s4 of linter* EoMmsm, lamb and Miller* whltrfe. are baaed on coloriaetrie comparison*" wore sfodled.in detail eng t&* aetbeft of ftebreus mii tmm was nioptod *itb miner eodifiest&eos*. .... ' ...... . , &t. first detareiiiatie&a wsro. mado .to find _ red color of tb l@sd complex inueiaft dlreetlf altfe tfe* tiem of load* this we# done fejr tafelnt sample# comt&imla#- varied* amounts of. lead as lead nitrate and eoaparlaf t&em .ftgaiaiafc- a ateadard containing 0*0S sag* of " lead# tfte following reenlt# in dicate that' -the color dees -.~yj'. standard etmieiolng .OfOi--g* ' @f-, !#&-- -.:. Saaplc lo* .1 u .8 4 ' ft 3 -? ft ' lend taken- teadfeand . Wot. . . m* **. . - ft*; 0.190 ' 9.390 0*080 0*080 0*040- 0.080 0*080 0.080 0.106 * 0*0 Q*m$ ~0*000 'OaOftOT. : * MOOT : , 0*0406 '4MHMS"v . - ..------- . t.081 - *'0f(Mftr.... - '...- 0*0000: -0*001- 0*0fl0 + SiW v.^,; DUP040001786'- The ;oad4%isii til urine tas studied next*: this was ' :' carried out by the baleiaatlan. method as snf$sbi by Behrens and f&egsr*- The lead Is precipitated as chloride and ear*ed: ' down by entrainment with * precipitate of calcium oxalate* .... After calcination, the -precipitate- fa dissolved in nitric lihd--ihe- lead extracted with dibbiame* Ihe ' ;&6b' were obtained by adding lead as lead nitrate t&, tfo&'W&fr... show that this method is. quits accurate* . .''_.. Standard containing Q*0mg, of lead Sample ' head added'r head-fh^d . So, g* 1 ' 0.060 - &*$&*- , * . /.. v 0*060 :.,,0*04P,,. % . 0*060 0*046:v' 4 . 0*060 0*0402 - 0*060 0*020' ' 0 0*100 - . ,0*0084- 7 .0*060 " "0*044 6 ' 0*060 . 0*0615 0 : - 0*060; 0*0200 10 0*060 . 0*025 11 '. 0*100 0*0... 12 0*050 IS 0*100 . 0*1012 :. 14 . 0*060 . is :, 0*060; > .ft**** -jsf3Bfiur,yffitTai m:im ' 4nftitt& Q*l(fS8r,-Ti^S:*S.. . i*r A n B|T -i--j . a V. O''*" ' ' '- !J3H=rair_~ 0*000110*001 : 0*001 0*006 0*0016 0*0004 - 0*006'.'. 3$sm i 0*0060 ;V80M mm^. It was- found that the median error in these.; determinatiaas; was - 1.6 per cent* with maximal variations of - 10 and * 12 per cent, and an average error''-.of about Another method of'oxidation wusec sett and Andersen/ was tried. She urine is 'is dishes, calcinated, using nitric acid to remove the last traces......... of carbon, and then extracted by the method used above. DUP040001787 .. Two ^aUe-rniw tions ga:f &&4 ftsl=t ;-*&# S&jg * . -w-7 *iw3r* j MW * ** + * > v VfiS^rf<'t"s&vV-^&iW '& j*:* A' H *- 'P'ja&k ^^UWW* ' " - rv->*4fe *'J v-s& ,, 'V 'V*`'*' ??5o* 0*060 ataee 'f#&ji4k.a astis^d viisi not ?a.t$p oirof' fell oro^^kir us n&:3 di3efclas*4 v` S' , / vt 3d- - -vl g?L% ; TV-T' ` - r th# aotftcKl for ti 1#*4 with dlthlaoae, ^ecoriia 5Sms ;5$0::lii"tO&tiOi3.H6# is &- tcm. Bam-mx*tn xtaad eoa&ereliiX dit&Ueoe la m 09% of eartwa tetrachloride* labraot *Xt& three m ee# . . portion* of-0*S pm coat mmmim fepdreadd**. this 4X# soires th& dlfcMsoa but act the istporitlee* .feject the earbea tetrachloride layer ead aeafcreiXse the atgneea* -layer to' Utaas with 1 I hydrochloric acid# Sxtraet-- . jnarified difthime with several IS m* portieaa of earbsa- - tetrachloride sad dilate the total extract to 100 ee* . The _ solotioa should bo k*pt Ut * pyreae flash la the jp*wr frlgarator sad m&e op fyeefc every third 4ey# m* lead standards. Q*l# pi# of eeeeyetejilei^ is- de ap to one liter with redistilled.. -r r ^t''Xm4 free nitric sett ere aided- te a i0O-"e#v all|4oi^1:- whieh. is storei-ia a pyrex Teasel* . Standard X X cc* contains 0*1 -eg* of lead*. ' < etasdard 11 1 ee* contains 0*01 eg# of lead* Had# by , dilating 10 ee* of dtaadard X to 100 so* heagenta containing mm Wmm 0*01 to ' 0*00E-:'ai:*.T-ofr' X#e4 gBist be-rejected#.-.; ' 'Fiat# a suitable ensatlty of urine' (100 ee ` to 1000 m* / depending upon the mmmtmti&u&f lead) in a bearer sad `acidify with ftOetie acid* than aid f a# of' a $ pey -&* solution and with stirring slowly' add `id eo* -of & Lii3L t.ion af wsaojiiuia oxalate* . Xa this way the lead is pr^elpitcited by entriiapen* with the ealeiw oxalate precipitate# let it." DUP040001789 ; ***ad aigiii'aad nam tfe* sapssa&tsafc %lm%& W wsttsit'". %%m amt day* - the omlata j*ti#ttet is ell#etby i^I-lag. m is ttssinft Sbs with yailatlllad **' dtratsiaisig a . tm &mp ttf sstcurstsd aioa salat siati* tlw psesipi* "t*b is tvaastsm* t a .pesasXaiii raetbls, b befcies* a - sil&?s . 7dlifc sltiagfe raywa&U sssaits mem fetalaes! aitik ----- ---- ;jisiiif***, tm pmsipl%*% U then Med m m $m& bath &t M '.'= ' mA tfcsa *ielaed la a saffl tummm at iQS* $ mtl^ tbs rasicJa la silroly wMt (sASfeeast* od xld*}* f&. ;"' sitfc tm least' possible mtvmt IM 'Wmk still, sad tbs slatie*i: aix#d rntm %&'M*. ..jfoitJ a_t:adlm itrst almti* lls d*o$s of &a ;"^^^s|^lfersa0sl pmrpis *" bfoatfeyi*! bias' i*r solatisa is nat*ollsd wits mh mm&u fhs; soimMaa is- - i?e&t % *4jMtaftti7 fdnasi.t d*$s;# a Ei .pear aat.pQtsia- eyaaM# soiatles .* added* fits ttixigw# Is then stm&m migmm&f-- fr-t- to 0 slants* with boat *'.** if pOTifMaSi dittoes^ gfas^etfeegt tmvm &ia#id is drain off md 'tt*r -.-nr - -. >0&: -----yf^ diaiaiafead portiona ef fe&;dltMssae mill..s furtitw r#&; iS5 toloy .apps&f's' la tts# eba tsirssijisid* tths is&d la- %M.- -is sapl#talr'*tsstsd fw tbs squsoa* .mlatloa sad' tb# jrslloir...... saps&istsst liquid is d&sft&sdsd* , f:-; ;tbs.;J?d 'ditgtlMnt acrlstlaty-attar .Msg w*sjii$'i%tfr Wli "0*6 pern em% stnoaina' bydroaids salati^-Teoatild^p^Sf 1 to "9 drops f potassitti eysalds (t ssasy* *ajr- sans** sjf-lfifc **g*at) Is ad tap to % dsfiaits roliaa witb oasfeast t^tmeMotide: ': sad #a*^3P Is a dlSK^iartss against- a afcasd&M p^py?ed m7t|s:n._rE DUP040001790-.r* way# - fb* eteeOer* .efeetfM fee estreated at tma mm tie#' m the o*aple*' from a m%table tpaattitgr r iS steaderd* iftii# s#lmtl#ft' i3 not l?i tie myeKsleii of eater o&n. be *# m&vei..:fey filtevthg, tferongfe a dr?, filter paper# , ffe# serial**' sfeoalC b#^ eoaf3?4 witbta 1 bear after extreetScni feeeeaee tfee ..;sawfc fee first eleamed aiife aitiroaia-amM'tLri' eted (leaning aalatloa) fallowed fey tap water* dilute aitrlo acid*Mused witfe redistilled-water* tm rererex samples aiiaalta^aeusiy:'does' a#l;r^MsfeSai|yiiy^''fv^ttwf m owi a^^|iir,; 14, _ fraparaMa--#f tfee precipitation * .'v'-::z>^v .-- ^' - :v. ? "' wm&nm'Hdf'7fcfa#^ :'c^ . w-^.~Z-Z..: ?-.- :--vv:::..;. . -*- >. - . * * we******^. #,... L> fiB&trifagatiQtt end. transfer to rating dia&es *:** IS M*- en the aeoend-'day*- :-' r" * ' ' _ __i feoara# " -i transfer. to. .muffle fme** * * S aiimtt#* ^aXetuatiw*- la tfee -naffla fiumaao. until *t issorsln^* ~maeeXMni-feMdu# &m eelerimetr&r 7>v^--.7r~-v:; .-v'^'.y^j;-- -; ' ;v'::? ~ - .` prepared In' ifee: and are raady for aao, tfao doterainatlon requlr^iu, tfeerefore* ` :fyav'l#7^er'S|^ hm of aatol tlat mi ana fee fiMsfeed ^atlWPe^lNiihrh a* the evening of tb* first dejrcr-Tr^:^ ftgy peraott witfe ; #Bftiyti fee able to' Oo tfee. Oetaj^inatioiA of .ieait;.:iiiH: -777# ootiiaoO- afeof# ami that the eetfeoi to aaitafele for tfe# remttne ::;:;::~:r' anaSyal# eir'ieaA Jte nrtae# ",;:;:7tgg fi;in- DUP0400017917#