Document 1ganVppmrn18v4LQMZL6EQomX

\ # LEAD INDUSTRIES ASSOCIATION. INC. 1*2 HAOIIOH AVCNUC NtW YORK. N.Y. 10017 rtur**ot<i-4tcA co< 04 *4I sC*u m ihoaHoaN. r+% i-m MNhlfN W MfCN. WHS MOM O trM. Ml H >*** u iiMiiaiT IKiV^tl *< 0AVIO M COMA I ((<** * IW t*v*4* Mty ?5, 19^7 To: All Hesters of tin Lead Health and Safety Ccssaittee Re: AIHA Blood laad Coaporlaat study Attached you vlll flod * copy of a paper, presented at the I967 American Industrial Hygiene Conference, which describe* ths blood-load casparlscn (tudy conducted by tin Analytical Chemistry Sect loo of tin American Industrial Hygiene Association. You vlll note that the result* of this study lodlcate serious disagree ments both betveen laboratories sod vlthla the eaas laboratory. Accordingly, It has been decided that a co4 surrey la cecetaary to resolve these differ ences and to eliminate any questloo of uniformity which night have been * Introduced by aiding number* of snail staples to sake up the composite* need .y In the first reference specimens. for your Information, our organisation Is joining in providing financial support for the repeat study. In addition, ve plan to give our neefcer compa nies sufflcleot ad ranee notice, so that any who vlah to nay participate la the second surrey. r t-~c./C*,--~.r .i JCl/jr Att. Janet C. Rocnas Assistant Director lealth and Safety V/v4 v r-*V?` jf j ! 1 . J :] . -' 3 .3 BIUCTOI emsio* or ixjxsniAL h t c id o IKOIASA STAT1 BOAtt Of HZAlTX 1)10 VIST K1CHICA# STRUT IMOIAKATOU5, l.VBIAXA rtancr o u iik m ILOOO UAO OOMTAA1SOM STUOf AIMA AXAiYTICAt OIKI STAY COOUTIU | E ttfuyr.'" .inyflwyi 4Wi- ..... .......Malle./.luv.i Introduction The Uft elagla analytical test for determining a worker's exposure to load li a blood lood uul/ili. This tst ku proves effective la tbs prevention of cllalcsl lead poisoning. Xoraally a worker c m bo removed from further Industrie! exposure to lead before cllalcsl s/aptoat of poisoning becose evident. furthermore, in many plants particularly the ooes eaploylng oaly a saall nuaber of employees, a physician la brought into the Industrial aodlclne program for the first tlaa tinea It la * * > necessary for kta to dm the blood for load aaalytla. Accuracy it a prlae requisite If blood lead levels of Industrial workers are to ba used at aa lodes of exposure and workers are to be transferred to nos-lead exposure jobs at a result of tMt analytical test. If lead levels are erroneously reported low, worker* are glvea a falsa teas* of security and excessive lead exposures will continue wltb eventual 5 cases of clinical lead polsonln|. If lead lavela ere erroneously reported - 1 .. high, workers are gives e false scare of potential polsoalag. They are unnecessarily transferred to noa-ltad exposure jobs aost oftea wltb tbe lost of tamings. Tbe potential production and industrial relatloa problems / which Industry then faces should not be alnlalled. Tbe blood lead test be of tremendous value te both industry and labor, but such tests MUST M Hccwuat. t, 'v la Order that this study be u realistic aj possible, blood trem worker* with lnluitrUl ttpotun to 1i i4 wtt accumulated ul AmliM for analysis to participating laboratories without artificially spiking those tables with an loorjtnic teed compound. The purpose of this study was actually tvo*fold: It afforded each participating labor** tor/ as opportunity to coopare Its result* with those of other laboratories anal/ilng slallar blood staples; and. It gsve * broad prospective to the efficacy of blood-lead analysis. & -y-'J1-*?.- '-"iJSWj^MisgieutfigioaMjsp^j^jpaes^ IIbc o only * lull portion of a blood spec lata as received Is required for lead analysis ss perforaed In tha Indiana Industrial Hyg1en# Laboratory, that blood which reaalned was pourod fro* Its Vscutsinsr and bottisd according to tha level of laad found in tho staple and the anti* coagulant protnt, bo it poUsilua ozalata or EDTA. Tba blood la tbsss bottlas mi kept refrigerated and varied la ago fro* ono week to oro tkM ono yoar. Load analyses wort aadt on tbo blood ia each storage container i and aa eitlaate was aadt of tbo roluao of blood stored la each container. / Free this iafomatloe, four pooled lots wort eado up with appro*Uto coacontrations (by calculations) of 0.0); 0.01; 0.07 and 0.09 eg load per 100 al. of whola b'.wod. All pooled loti wtre plactd ia s bottle largo enough to sccoaodste tbo entire lot. Each pool was filtered through s piece of clean loeJ-frte cheese cloth placed la a S.S as. tvehner funnel ia order to remove any coagulated eattrlal which nay have been iatreduced ia tba original blood, in Yacutalaero, or which say havo forued after pooling of the blood. Very little coagulated notarial waa observed la any of the pools. ._ San. Portions of the poet were transferred to t 121 nl. ftssk (fitting flask) free which the blood was drawn Into Seckton and Pickenses 1)200 Vecvtalaers (lead-free, 10 al. capacity) through a 200 XI' disposable 5- f i . f t - . , -.a I jj I j '-f `?P<ljpnj>ppPPI^ Nuj* we im41i , Whan tha flaak kKiH aapty, It nt rtf111*4 by pouring tk* poolad blood fro* tha bottla c*ulttii| tha pool. Etch Vacutalnar mi glvaa a nunbar ao thtt lta contents ami place la tha science of fill lag would b know*. Wur# tha voltaaa of blood la tha pool paralttod tha raOhral of tha required ouahar of Vacutalnar* of blood aa controls, tha controls war* tolactad as follows!' a. tha first, aiddl* and last Vacutalnar drtva frca tha first filling flask of tha pool. b. tha aiddl* vacutalnar of tha Jrd, 1th, 7th, bth, ate. filling flask of tha pool. . tha last Vacutalnar of blood draws fros tha ant Ira pool. I All Vscutsleor control samples wtra analysed V apactrcgrsphlc analysis and also by tha apectrophotcaatrlc dlthlton* aithod. 7h* ><* variation found In any on* pool was _ 0.OOS ng. laad. That* analytes Indiestad that tha pools wart unifora la laad cootaat and that tha Yacutalnara of blood twppllad tha participating 1aborttorlaa waro also ualfors la thalr laad coataat. Slnca thara was no avldanca that tha laad coatant lncraasad or dtertasod aa tha Vacutalnar* war* filltd froa tha pools, flvo Vscutalnars of blood waro saat by first cist* nail to each participating laboratory lanadlataly following conplatlon of controls' snalyaas. Two of tha Vacutsiaars last to aach laboratory-contained blood froa ana pool whlla tha raulslif'^ thraa Vacutalnar* contalnad blood froa aach of tha othaf thraa pools. -, ' ' ` mmmm A imo ms sent to tech ^rtldpitU| laboratory on September JO, 1PM advising the* that five blood i;k U<d i were belnj shipped to than os'Otis dsto. It ms sutstttod that th*io seaples bo analysed Oft October 10, 10M, or if this ms not possible that they bo eaal/ted st osrllost dato after October 10. Tbe s m also stated that tbs bloo4 sasplos bolus shipped ears fro* workers with Industrial lead exposures. Oxelated blood had been accumulated and pooled without "aplhlns* for this study. Since many industrially esposed workers had been treated fr tine to ' ^ tine with Yerseoate (COXA) It was expected that the blood specleans would contain tone SOTA. The blood in the Vacutalners should bo thoroo{hly nixed ' prior to roaovel for analysis. # .i. Allhoush the pertlclpatlnf laboratories were advised that they could use any nethod of analysis which thay desired. It ms sutseited that they use the net hod of analysis noraaily performed la their laboratory. * Each laboratory was assisted an Identification number known only to > the partlclpetins laboratory end the Project Chairmen. The tpeclnen aueber oa each Yacutelner Me e coded nunber (each ruaber was rastly different), asking It Uposslble for the perttelpetln| laboratory to ascerteie the speclflt blood pool represented In each seapte. The fact that each laboratory Received two Yacutalner* of blood froo aa Identical poo) was a tlesely swarded secret W : vW-; ' '*3* wiklck mi not fawn by y portUIpotlaj laboratory, Ik iu ii ot tha co44 auakorla* l;it uaai, it m Mt potllb!* tor liUntoriti to affectlvaly coopera tiiir rmlti with other laboratories prior to tubalttlng that# to frojact Oval nun. -.' ' / r T. / "W^*MSs ^Bgwu;yjygag^ : ."? >: K;*8!'as: /' litft v*' 1*"'-" V' -v*V'-*'- ' * '* .. w '- > '. .'..-. . ~--r" - losults of Studies The coaplete blood-lead riiultt of oil the partlclpatlnj labore- terles are ikow to Table I. Tbo multi froa laboratories which mri reported u altllgraas of lut per 100 cc. of whole blood were converted to ailllfraas of load par 100 (rui of whole blood la order to compare tbo analytical multi. Tablo 11, Is a compilation of all multi reported to Hood A la aaaaoTlcally etcendln| ordor. Tbo float results of 29.2 was dolotod for statistical analysis. Tbo aoaa value reported was 0.019 with a standard dovlatloa of 0.0171. v Tbo results roportod oa pool blood I aro flvea la Tablo 111. Tbo value of S.4 llatad la tbo tablo baa boon dolotod for statistical analysis. Tbo aoaa value roportod for blood I was 0.0SI with a standard dovlatloa of 0.0741, Tablo IV shows tbo laboratory rosults roportod for pool blood I. r With a valuo of 1.4 dolotod, tho aoaa values roportod was 0.044 with a Standard dovlatloa of 0.0141. $ swm All tho values roportod for Hood C ( D which aro froa tho aoaa blood pool aro listed la Tablo V. Tbo aoaa valuo roportod was 0.071. li i Tablo VI! Is a auntiry of remits roportod oa blood CIO accordtni to^. tho deviation between tho remits of tho two samples roportod. Althou|h i. 21 loborotorlo* roportod tho esae result oa sach of tholr two oaaplot. I i J r i- \ ~ It 1* intonating to not* that tha blood land concantrationt raportad variad 0.000 and S.t migrant of load par 100 |ru> of blood. 1/ txcludlftj tbo two laboratorlas reporting tha graatait variation la the result* of their two aaaplaa, tha difference reported waa 0.01S with a atandard daviatloa of 0.020. Tabloa VII, VIII and IX indlcata tha blood laid ratulta reported according to netbod of preparation, separation and estimation. Tablt X how* tha range of blood laad valuta raportad according to nethodt of estimation. Tha avaraga (aaan) blood laad raaulta raportad according to nethodt of estimation ara givaa in tabla XI, 3^ >- Conclusions Tko wide variation la blood-lead levels reported on each pool seaple Is stuck greeter this c m be tolerated. Although ik ! cbeulst end each laboratory participating la tbit Study believes tbslr results to b accurate. It is obvious that mb / rasults reported sra unquestionably lacorract. In fact, oa tba basis of this study. It would appaar that sons laboratories km no business attempting to parlor* trace analytes. Of particular Interest are tba rasults reported on blood CIO which are r. saaplas fro* one blood pool. Table VI Indicates tkat 23 laboratories^ \ found Identical lead concentrations In aeck of tbalr two saaplas fro* tkls sa*e blood pool. Although tbesa laboratories were able to reproduce tbalr results, the lead concentrations reported varied fro* 0.00 to S.O eg. lead c* < per 100 pet, of whole blood. Ires If these two extreeea end also ridiculous figure* are dropped, we still find a lead variation froa 0.03 to 0.12. .i Tkls study nay point up one or nor* of the follovioj deficiencies! ) Soso laboratories nay not be staffed wltk personnel properly' '.a trained and experienced In trace analysts. It vet apparent tkat so*e laboratory personnel la this study were confuted ever the teres allllgraas sad alcrofreat, .* i k) So** leboraterles nay not have or are not utilising the proper te stake blood lead analytes. '.'3 '-5 ' k > .. a ..* ^___ | **3kt i e) Son# laboratories, although proparly equipped sod staffed, nay not kar* suitable analytical procedures for these typos - .} f SMlytat. } Most Individual laboratories nay find It necessary and advantageous to tale a good long and bard loot at their aethods, technique* and standards. Xt Is a recognlted fact that referee or special type of analysis normally get special treatment la aoit laboratories. It nay be Interesting -\ to sunelae lbe results of a study of tbls type were the sasples analysed In each participating laboratory at a routlns type aaaple. -i i / i i. 5- JUJJl WPP, ' ]% 4 Tte blood*lead cwpirlioii study should be repeated, Tho blood for soother study should b purchased In quantity fro* donors with Industrial exposure to load rather than saline tip pools by nixing a lists nates of Individual blood speclaens. Only froth blood should bo nsod on future studios. All lsboratorlos vho plan to partlclpats should first study tholr stathods tad techniques. It aay bo sdvlsabls to prooots aaothor typo of trscs analysis ~ rsfsroo study la ordar to ascortais over-all rollsblllty of laboratory competency. ' Should futuro studios Indicate that a ilsotblo h u bbor of laboratories do ltd competency In troco anxlytls, It say bo ccctsury that provltloas bo aado by A1HA to furnish roforoo taapios to laborstorlos routlnoly so lhay aay porlodlcally chock tho accuracy of certain typos of analyses which they art making. It nay alto bo necessary to five consideration to licencingor fronting approval to laboratories for aaklnf certain types of analyses. / / r } SpMiaia Mo. Laid Content (Uaa appropriate eolunn) | Pb/100 cc blood f 7b/100 tl blood . Onto spocUeaa tocelvad AVAIYSIS 1XTQWXT1QH A. Preparation ( cback o m Itao) 1. Dijeatloa (Not taken to a retidut) IS 2. AiMa j ; i. k. Dry w.t n11r 2. Protein Precipitation 4 4. bleed uatd without aUeiatlea 1 >. lulitlo* or Separation of U*J ( ckeck appropriate ltM) 1. Precipitation 1 2. Li traction . tti|nt 1. Mt Hi tone 27 "J 2. APDC T~ : 2. Other *T k, SoIt tot ' 1. Chloroform 24 2. Carton Tat 2. Mitt 4. Other 2. X* Separation 17 V C, Salination ( check M lt*) 1. *j Color a. Vtiual 1 k. ColerUeter or Spectrephotoaeter Tl' 2. Titration I ' 2. Pel ar( r pS 4 4, Atc*l< AbaorptTe* > 2. tpMitriri^k " a. flU 4 k. tlrxrfftJtr 2 4. Other 0 ; *- ;r. ( S;-- , ' Si*.-. TAILS I. 'COMPLETE 4LOOO LEAD RESULTS OP PARTICIPATING LABORATORIES k|, L**d p*r 100 pi. Ittrtl* Blood Ut>. No. i 2 2 4 4 7 4 10 11 12 14 IS 14 14 1* 20 21 22 '1 22 24 24 24 27 24 29 SO SI 22 SS 24 24 24 40 41 42 44 4S 44 44 40 Blood A 0.022 .044 .022 .045 .042 .024 .022 .070 .014 .022 .027 .024 .021 .050 .074 .052 .017 .022 .051 .011 .022 .010 .022 .044 .017 24.2 .054 .000 .024 .024 .020 .120 .000 .022 .040 .014 .027 .042 .024 Blood 4 0.010 .022 .074 .051 .070 .040 .0S1 .022 .054 .027 .052 .044 .044 .024 .041 .052 .074 .120 .074 .044 .047 .024 .040 .012 .054 .047 S.4 .042 .021 .021 .050 .052 .042 .000 .021 .014 .044 .01# .047 Blood CIO 0.021 0.027 .044 .054 .054 .042 .047 .070 .120 .150 .047 .0*7 .054 .059 .044 .074 .0*4 .102 .022 .054 .050 .051 .042 .042 .054 .041 .024 . 047 .071 .050 .044 .027 .092 .115 .120 .022 .042 .040 . 049 .040 .04* .045 .0*7 .071 .02* .021 .000 .074 .074 .07* .024 . 04* 4.4 2.4 .044 .077 .02* .024 .04# .070 .071 .075 .047 . 044 .100 .120 .000 .000 .0*2 .04* .074 .012 .127 .041 .072 .042 . 04# .07* .07# Blood B 0.070 .049 .07* .04* .095 .102 .074 .100 .122 .094 .077 .077 .077 .079 .024 .0*7 .142 .020 .027 .0*0 .07* .0*2 .0*2 .024 .044 .094 .070 4.4 .0*7 .029 .090 .079 .100 .000 .0*2 .10* .721 ,04* .0*2 .129 UlSJg 1 v' >"i:r <**-' r l ; I llood luvlu bgr Uterittrlti ?| 2 UK Ho. SO SI 52 S3 S4 SS SO S7 SI s to 11 IS 14 M Hood A 0.024 .040 OJS .M2 .032 .041 .034 .010 .030 .034 .025 .040 .260 .037 .010 Hood 1 0.0S1 .OSS .OSS .M9 .041 .061 .059 .020 .046 .067 .040 .052 .164 .059 .025 Hood CIO 0.059 0.061 .054 .062 .067 .067 .097 .116 .025 .072 ' .050 .060 .064 .067 .061 .061 .053 .060 .050 .051 .052 .063 .061 .067 .134 1.05 .065 .066 .053 .063 Hoed B 0.07S .074 .066 .129 .071 .102 .099 .M3 .069 Ml .056 .074 .172 .093 .070 i Ubmtory JUiultf Rport4 k;' Lm4 fr 100 t* Vbol* Mood Mood A *-'v. e l 0.000 0.000 0.021 0.022 0.010 0.012 0.040 0.040 0.04S . 0.064 :`: 0.010 0.022 0.021 0.012 0.012 0.040 0.042 0.044 r 0.010 0.010 0.021 0.021 0.012 0.011 0.04S 0.041 0.070 0.012 0.011 0.024 0.014 0.014 0.074 0.014 o.oso 0.1M 0.017 0.024 0.014 0.0S1 0.240 i- 0.017 0.027 O.Olt 0.011 O.Olt 0.074 0.014 0.014 29.2 0.016 v 0.014 0.024 4 i 0.017 i t * ! 1 V r 1 l mmm tr f[ :,v 'cY:: " i 0.000 0.012 0.014 0.010 0.010 0.024 o.o:s 0.026 0.024 0.024 TAOLU III. Utorttory Rttultt R*port*4 Kf. Ud f*r lOOjai. hola 41oo4 Hood I 0.012 0.011 0.017 0.040 0.041 0.041 0.044 0.044 0.046 0.044 0.047 0.044 o.oio 0.011 0.0S1 0.011 0.011 0.011 0.012 0.012 0.012 0.011 0.011 0.011 0.014 0.014 0.014 0.014 0.014 0.040 0.040 0.042 0.061 0.041 0.044 0.047 0.047. 0.070 0.074 0.074 0.044 0.110 0.164 1.4 * } .^e^ouijwiiWHiUt.ui ryrifr '1 t s \ 0.000 0.000 0.000 0.011 0.02$ 0.021 0.021 0.021 0.021 0.0S1 0.011 0.01$ 0.014 0.01$ 0.017 0.017 TA1LI r. laboratory Rmlti Koportod * l**4 pr lOOfU. trholo >loo4 0.041 0.0S 0.047 0.041 0.041 O.OSO 0.010 0.010 0.010 0.010 0.011 0.012 0.011 0.011 0.014 0.016 0.016 0.014 0.011 0.011 0.010 0.010 Ioo4 C I P 0.060 0.060 0.060 0.060 0.061 0.061 0.061 0.061 0.061 0.061 0.061 0.062 0.062 0.062 0.062 0.061 0.064 0.06S 0.061 0.061 0.061 0.066 0.066 0.066 0.066 0.066 0.067 0.067 0.067 0.067 0.067 0.067 0.067 0.061 0.06* 0.060 0.060 0.060 - 0.070 0.070 0.071 0.071 0.071 0.072 0.072 0.074 0.074 0.074 0.074 0.07$ 0.076 0.076 0.077 0.07 0.044 0.0*7 0.012 0.017 0.100 0.101 0.11$ 0.11* 0.120 0.120 ^ v 0.120 0.127 0.114 0.110 1.01 S.6 1.4 i ; i ? 1, c L f. K ! `` r. 'H ----. ... : - '' a- wwya--wg; Sii*pS?# *^T4\ t t' 25 laboratorie* Mfwrtid Sui Itiulti on Each of Thelr Two'Saaplea, With The following Concentration* Reportsj J Duoitr of U.frmmlti Lead Concentration 1 0.00 2 0.05 I 0.05 0.0* a 0.02 5 o.oa 1 0.12 1 5.6 15 Laboratories Reported Results Oa Etch Of Their Two Saxplts Which Varied 1/ Only 0.0i Kith The following Concentration! Reported: i Kuaber of laboretoriee Lead Concent ratio* 2 0.02-0.04 1 0.04-0.0$ 4 0.OS-0.06 a 0.06-0.02 5 0.02-0.04 I Laboratories tiportti Results oa Each of Their Two laaplat which varied by only 0.02 *{., With The following Concentrat loos Reported: P, Kunber of Laboretoriee Lead Coocentretlo* 1 0.01-0.0$ 5 0.05-0.02 1 0.02-0.0* 1 0.04-0.10 2 0.10-0.12 2 Laboratories Reported Results on Each of Their Two Staple* which varied by 0.05 e|. or Here, With The follovlnf Content ret loos Reportedl huaber of UJiaxuaxUi 1 i 1 t 1 1 l Uit.CanMftU.ulai 0.00-0.0 2 o. oi-o. II 0.01-0.0* 0.01-0.02 o.cn-o.o# 0.11-0.It O.ll-l.Ot t- .. .Wi.rfc .fc..,,..* . 11,. . , . l .I.-) .A . ---------.-fc -;.., . . . ...... TAILS m. ILOOO LEAD RESULTS REPORTED ACCORDING TO XETHQO OP PREPARATION Digaation; Extraction with >11 th l lone; Solvent - chiorofora. Extinction by Visual Color 39.2 S.6 J.6 - S.6 S. Digestion; Sant* Average Extraction with dlthltose; Solvent . chloroform Satlnatlon by Color Spectropbotometar .0*1 .0*1 .067-.070 .06* .0** .01* .0S6-.061 .077 .1*0 .11*-.120 .0*0 .0*0 .0*2 .042-.064 .07* .040 -- .074 .10* .0*4 .0*7 .07*-.079 .119 .040 .0*2 .061-.067 .074 .0*0-.040 .044-.1*0 .0*6-.120 0S0-.1J9 .0** .06* .074 .0*2 Digestion; Extraction with dithixone; Solrant - chloroform Satlnatlon by Titration .000 .000 .000-.000 .000 Digestion; Extraction with AP5C; Solvent - XUJC. Extinction by Atonic Absorption .011 .026 .04$ .0*3 Digestion; No Separation of Lea*. Satlnatlon by Spectrachealeal - Plln .064 .07* .0*4-.062 .07* .0*4 .0*1 .06*-.077 .017 Digestion; No Separation of Lead. Salination by Spectmchemleel - Direct Header .01* .0*1 .0*4-.0*9 .074 Dry Aahlnji Pang* Average Extraction with dlthltona; Solvent - chloroform ...Satlnatlon by Color Spectrophotometer .0*2 .041-.0*6 ,049 .027 .041 .067-.042 .077 .0*1 .042 .060-.044 .07* .017 .047 .054-.041 .070 .040 .0** ,0*4-.042 .074 .014 .067 .0*0-.0*1 .01* .017-.0*1 ,.0*2-.0*7 .0*6-.04* .0*9-.0*4 .0*4 .012 .0** .07* : ______________ i --:" ....... Dry Ashing; Extraction with dlthltona; Ho Solvent LllteS. EatUatlon by Polerogreph .012 .041 .025-.072 .071 Dry Axblngi Mo Separation of lead. EatUatlon by felarograpfc .050 .041 -- -.071 * .054 Dry Ashing; Mo Separation of Lead. Ettlaatlon by Spectroche*leal . film .005 .070 .120-.ISO .005 .150 .055 .100-.120 .100 - 1 1 Vat Aehlng; Extraction with DltMtone; Solvent - Chloroform, Eatlnation by Vlaual Color. .017 .059 .055-.06* .095 Vat Aahlng; Eaag a Avaraja Extraction vlth DltMtone; Solvent - Chloroform. EatUatlon by Color - Spectrophotometer .021 .024 .021..047 .079 .02* .051 .050-.044 .0*7 .051 .074 .017-.092 .142 .017 .074 .051-.041 .057 .012 .044 .040-.049 .0*0 .012 .040 .047..071 .0*1 .010 .021 .012 ... .02*-.Oil .000-.074 .014 .044 .054 .054 .074-.074 .094 .024 .051 .049-.070 .090 .014 .050 .071-.075 ... .021 .051 .041-.044 .0*5 .045 .059 .045-. 049 ' .0*2 .024 .051 .059-.041 .075 .041 .044 .050-.040 .102 .014 .059 .044-.047 .099 .040 .052 .041-.047 .07* 010*.044 .012-.074 .000-.092 .014..142 .011 .050 .054 .0*4 Vat AaMng; Eatraetlon with DllMione; Solvent Chloroform. Itllaatlon by folarogreph ,000 ,021 .02*..014 .019 Vet AaMng; talreetlon with DltMtone; Solvent Carbon Tetrachloride tiMaation by Color - Spectrophotometer .0*2 .0*9 .097..114 .129 an.'iei, " WJM1 j~ .v b."?v '...a ` J'S?.a.'gB'-get-Vjyv"'1-* ~ Extraction with A?DC; Solvent - Chiorofora Estimation by Atonic Absorption .055 .05$ .067-. 067 .0*6 Extraction with AEOC Solvent - KISJC Estimation by Atonic Absorption .056 .046 .OS0-.O6O .069 So Extraction Descent list ad; Solvent - Other Estimation by Atonic Absorption .070 .OS* .054-.105 .123 So Separation of lead IstUatloo by Atonic Absorption .042 .060 .067-.0*7 .102 No Separation of lead Estimation by Polarofnph .014 .014 .015-.127 .251 So Separation of Lead Estimation by Spectrochanlcnl ElIn .022 . 052 . 050-.Oil .077 33s Erotela freelpltatlon; Extraction with AECC; Solvent - KIM Estimation by Atonic Absorption -.025 .019 .02*-.057 .070 .022 .055 .061-.074 .100 Erotela Precipitation; So Separation of lead . Estimation by Specirocbenlcsl - Olract leader .010 .020 .061-.061 . .0*5 .010 .025 .0S5-.065 .070 Hood Used Without Alteration; Ertclpltatlen of Lead; Other Descent.^ rI Estimation by Atonic Absorption .025 .019 .Oil-.057 ,070*e Hood Used Without Alteration; No Separation of Lead 'Estimation by Spectroche*teal file ,0)1 .04* .041-.072 .046 1 *-- ---eUUL-y1?* '-T"*.1 V**" ;*< ,~"j JXa. TAILS mi, 11000 LEAD JESUITS REPOTTED ACCORDING TO MTTHOO 07 SEPARATION ^rKlflUtlMJ Hood Ut*d Without Alteration; Solvent - Other Eltlaallon by Atealc Absorption .OU .017 .to)-.014 .004 Extraction with Dlthltotve; Solvent - Oi loro fora; Rreparatloa-Dijeatlon Iitlnatlca by Visual Color 20.2 l.i }.(.{.( S.S Extraction vlth DltMtone; Solvmt - O)lorofora; 7r<p*r*tloa-Dl|**tlM . ))Est nation by Color - Spectrophotoaatar 0 .011 .067-.070 .044 .0)4 .040 .0)4-.041 .077 ... .1)0 .11)-.120 .0)0 .070 .0)2 .042-.044 .070 .040 ... -- -.074 .104 ,0 V* .047 .074-.070 .1)7 .07S .040 .017..04) .on R**t* .on..oo .040..no .017-. 120 .0)0-.1)7 Avtraj* .on .044 .074 .010 Extraction trlth Olthitooe; Solvmt-Qtlorofora; TrnuitlM - D1|**i 1m .000 .000 .000-.000 .000 Extrtctloa vlth tltMioit; SolrtAt.O lorofora; Prep* ratio* - Dry Athia* Ettlaatloa by Color Spactroohotoaeter ... .0)2 .04)..014 .047 .027 .041 .047..042 ' .077 .on .042 .040..044 .071 .017 .047 .0)4-.041 .070 .040 .on .0)4-. 042 .074 .on . .047 .on-, on .044 S*o** .017..on ,0)7. .047 .0)4..044 .04?..044 ^* Avar*** .on .0)2 .0)4 .074 W- titrtctloa vlth Olthliona; Stv*l-Chtorofora; Preparation - f*t AsHln* lillaatlo* by Visual Color .0)7 .0)4 .04)..044 .07) i i; Kxmctloa with DUKImm; Solvnt-O>lorofor*; fxtpArttloa - Wat Arblst IttUailoa by Color Spctroyboto*t*r .021 .024 .024-.047 .07* .02* .05* .050-.064 .047 .05* .074 .0*7..092 .142 .017 .02* .01*-.04* .057 .012 .04* .060-.069 .040 .032 .060 .067-.071 .04* .010 .012 .024*.011 .054 .023 .000-.074 .064 .044 .054 .074-.076 .094 .024 .054 .051 .050 .069-.070 .071-.075 ...090 .02* .051 .065-.064 .04* .045 .05* .065-.06* .0(2 .024 .051 .059-.061 .075 .04* .044 .050-.060 .102 .014 .05* .066-.067 .099 .040 .052 .061-.067 .074 luji .010-.064 .012-.074 .000-.092 .0*4-.142 Arr(* .0*3 .050 .05* .07* i bimtlM vlU Pit hi *> ; SIvat-OUorofor; 7r*j*rtlMi - lt AtUt| littvaUoq by Polarofrsyh i / .000 .02* .07S-.054 .05# Ltrctlen trlth PltMron*; Solvtat - Crbon TetrcMri4; 7r*yrxloa - *t AiMn* llllutloo by Color - SjxclropiiotOMtw .042 .04* .097-.11* .12* btncllM with DltMion*; )*o Solvtnt llitod; Trt^ntlM Dry Itllat IttlMtlM by Pottrojripb .0*2 .041 .025-.072 .07* litmtlM *10* *>CC; Solvtat - Oilarofora; Irt^mtlM - * Ahl$ litlutiM by Atomic Abrorytloa .01* .01* .047-.047 .0*4 litrxlion with A7DC; Solvtnt Mill; Prrptritloft - Vt AtXlnf I*Uu Hm by Atoale Abtorytloa .01* .04* .013-. 060 . 04* wltb A7t<; 5tvt Milt; 7r*?rtltxv tllUilloa by At<rl Abiarytloa .011 .01* .02*-.017 .022 .011 .044-.074 7rM*l frKtpluilM .070 .100 : W*'!' No Separation; Preparation . Kit AsMnj Estimation by Atonic Absorption .070 .01* .014..101 .172 No Separation; Triparitlm - Dl(t*tloa Estimation by Spectrochcnlcal - 711a .064 .076 .016-.062 .07* .024 .062 .06*-. 077 . 0*7 No Stpiritla; Preparstloo . Dljastlon Eat 1mtIon by Spectrochenlcal - Direct Header .026 .021 .02*-.OS# .074 No Separation; Tripantto* - Dry MMnj Estimation by Tolarojrapb .020 .041 .. ..071 .024 No Separation; Treparation-Dry A shin; Estimation by Spectrochcnlcal - 71 In .062 .070 .120-.120 .0*2 .120 .062 .ICO-.120 .100 No SifinliM; TriptritlM - >it AiMaj Estimation by Atomic Absorption .042 . 060 . 067..0*7 .070 .011 .0*4-.102 ,102 .122 No >p4ratlo; Preparation . Vat UM>| Estimation by Spect roc>.ealeal - 711a .022 .M2 .010- .051 .077 No Spirit Im; Ereparatioa - Protala Precipitation Estlnatlon by Spec t rocbam Ua 1 - Direct leader .010 .010 .070 . 022 .0*1-.061 . 017-. 062 . .0*2 . 070 No Separation; Preparation Hood Used Vltbout Alteration tattmatian by SpectrocHaaleal - Pita .022 .046 .061..072 .06* ; .s 1 0 TAM4 IX. LOOO LEAD mum mp o h t e d ACOOilDI.SC TO METHOD Of ESTIXfcTJO* Tlivil Color; Preparation - Dlfettloa Ijr Dlthltono - Chloroform btrwtlM 19.2 S.4 S.4-S.4 S.4 VIfuel Color; Prevention - Vet Axhlni )jr DltMtona - Chloroform extraction 017 .059 .045-.064 .09) Color - Spectrophotometer; Preparation - Dilution )/ Olthlione - Chloroforn Extraction .05) .051 .047-.070 .04) .054 .044 .054-.041 .077 .. .150 .11$-.120 .050 .050 .052 .042-.044 .079 .040 .. -- -.074 .10) .054 .047 .074-.079 .119 .c:i .040 .C12-.04S 05) tM|* O25-.O40 .040-.150 .057-.120 Average .05) .044 .074 .0)0 3 o leO* V- J 5 r.\ i' K ' r, i fr." P i S'"" '`St* *i Hum mi ,<gdue i < CeloT~Sp+ctropboloa*tr; Prepentlon - Pry Ashing 9y Oithiton* Chloroforn (xtrsctlon .032 .049*.056 .069 .027 .049 .062*.062 . .077 .041 .062 .060-.066 .074 .017 .047 .036*.049 .070 .040 .053 .056*.062 .074 .034 .067 .050*. 059 .0(6 U*|t .017*.051 .032*.067 .036*.066 .069*.09* .034 .052 .056 .07* 9 1 or-Spoc tropKot o+*t *r ; Preparationi Vet Ashing * iy Dithlxoftt - Chlorofom Extractioa .021 .024 .021*.047 .079 .024 .053 .050*.066 .097 - .043 .074 .037*.092 .162 .017 .029 .033*.043 .057 .032 .046 .060*.069 .090 .032 .060 .067*.071 .0*3 .010 .012 .029*.031 .034 .021 .000*.074 .06* .06* .036 .074..676 .096 .026 .051 .069*.070 .090 .03* .050 .071-.075 -- .021 .OSl .063*.066 .0(3 .043 .049 .063*. 069 .0(2 .026 .051 .039-.Oil .075 .046 .06* .030*.060 .102 .034 .059 .066*.067 .099 .040 .032 .061*.067 .074 .260 .164 .134*1.05 .172 lUnge .010*260 .012*.164 .000-1.05 .034*.172 Ami| .046 .036 .099 .090 ly deleting 1 *t ree of rtniltl iler* tenge Avenge .010*.06* .012*.074 .033 .050 .000*.092 .059 .034*.162 .0*4 0lr-!^(trc^)iiciitri Prep*ritlod Vet Ashing 9y Pit hi lone - Cmrboa TetrechlorUe Lursctloa .0*2 .0*9 .092*.11* .129 .* Tttrlioi Preperetloa - Mgestifra y Plthiton* > CM Off for* tstrectle* .000 . 000 . 000*.000 . 000 . --A-r.'. -- *--- - * ------ --- V ' Attijid^tiaJh>*^iJr^iii*ri-T. ^--ifii iW-rrr^iirVr--r-"--^----- - t.u ?isse.s^ss5f(!. -v'. Polarograph; Preparation - Dry Ashing My Dlthitone Extraction - Mo Solvent LIit*4 .052 .041 .025*. 072 .071 Polerograph; Preparation - Dry Ashing Uo Load Sop* rat lea. .0S0 . .Ml ....071 .054 Polarogreph; Preparation - Pot Axh 1 ng y Dlthlioaa - Chloroform Extraction .000 . 024 . 024*.054 . 050 Polerograph; Preparation - Wat Ashing Mo Lead Separation .014 . 014 . 015-. 127 . 251 - Atomic Absorption; Preparation - Digestion by APPC - HIH Extraction .011 .024 -- ..MS .045 Atonic Absorption; Preparation Wat Ashing by ATDC Chloroform Extraction .055 . 055 . 067.. 0*7 .044 Atonic Absorption; Preparation * Wet AiMng by APCC . Hilt Extraction .054 .M4 .050-.060 .042 Atonic Absorption; Preparation - Wet Ashing by Other Sol rant Extraction .070 . 05* .054-.105 .122 Atcailc Absorption; Preparation >*t Ashing Mo Load Separation .M2 .060 . 047..047 .101 Atonic Absorption; Preparation Protein Precipitation by.APDC - Hilt Zitrectlon .071 ,01 .021-.057 .072 .055 ,044-.074 .100 Atonic Absorption; Hood UaeJ without Alteration Precipitation of Lead .014 .057 ,055-.054 .044 .j ,070* i1 :,v / # i 'Pi^ ^ r iill*-^ |---f^-'^- 1tf fPri -!- [ min j ir J.I1B_r^T ^r JpoctrcxUoicol - Fll* (floto); freporotloa - MjMtlo* Mo Soporotloo of U1 ,006 .074 .056-.065 .07 .054 .045 .065,.077 .0*7 Spoctrochcalcol - flJ (7 Ut ); 7rrprtl<va - Ory Aihlo* Mo S>uitlM of Ui4 .065 .070 .120-.ISO .091 .110 .065 .100-.120 .100 Spoctrocboalcal - 71 lo (Plot*); Prtporotion - Wot A*Mnj Mo S*prtlon of too* .025 .055 , 050-.051 .077 Spoctrocbralcol - fll* (Hot*): u,#d *l**wt AltorotloM Ko Soporttlon of Loo* .015 .04* .061-.072 .06* SjwctrocKeotcol - 01r*<ior *rt*or; Froforotlo* - OlgootlM Mo StMrtiUii of too* .01* .051 .05*-.059 .074 SjsoctrtxiralCil Oiroct 9rir; frv*rtloa - frotoln frotlpUotlos Mo Soporotioa of too* .010 .020 .0*1-.0*1 .0*5 .010 . 025 . 055-.0*5 . 070 l ik]" "`f-.-- * '-- ******* * ^ ^ a^"U`^'li***M*`*^ ^ + i i 'VP^JBVp-gy11 *.ry r--if.J %3* ' .< -'- - '*..m -itj .- 'l l : --Jj.i-.iZLjija;-!...... . -> - ,:.V .... . ...... HAKE OP 4LOOO LEAS USULTS Ripomo ACCORDING TO KCTVIOW OP 1STIHATI0* Xthod Sp*ctrophoto*tn " (C*It OM Ub) Atcalc AbporytloM S^ctntbaUtl - P1U * - Direct lu^ir iiood a 010-240 010-612 000-oso 011-070 022-110 010-014 llood 017-164 012-040 014-041 019-060 046-074 020-0JI llood C 1 D 000-1.OS 000-116 015-127 024-101 0SO-1SO 055-06S llood I 014-172 014-129 014-251 069-172 064-100 070-041 k - jggijg^ 1 wggi14'"!Ui-4tgw>.','. ; . -sa* ! ^ctip!toMt(r 9ol*r(Vif>!t Atoalc AbrpUi i;xtr<)>wlcil fill Mnc( A**<l*r Ilnxl A 055 024 012 049 019 9 J oo-d 9 054 051 042 042 052 10<xl CIO 045 0S5 041 012 040 lift** I 042 104 091 OM 074 -j ,, :*;J ei " bps i ?Sfc