Document 8RaqkNEg9z5py61Ka0ZdXvaJ5

Lead Industries Association, Inc. 202 Mtdtoon Avanu# New York. N. Y. 10017 T#!*phoo: (212) 670^020 January 29, X974 SUBJECTt DRAFT STANDARD fOR OCCUPATIONAL EXPOSURE TO INORGANIC LEAD TO THE OFFICIAL MEMBERS OF THE LEAD INDUSTRIES ASSOCIATION, INC. i Although the attached material la now being received by the p,rpi|x?rn of the LIA Environmental Health Committee, I am aura aomo of you will wi?*h to have your own file copy of thia Department of Iwibor draft Standard. Comment and Muggeal.iona on thia draft are solicited by the Department'* <ji f i <:r >j ! M andards. S1hcorrly, .!! : 1m, A i I . tmurnt JAt-fUs rorno l`. Smith . rotary *. General Manager Lead Industries Association, Inc. ?? Mxtiton Ntw York. N V 10017 Tdaphon* (717) S3? 7373 f nvifonmontal Health Depot meat January 1H, TO: LTA Ivnvlromentnl Health Cormlttee KH3M: Donald R. Lynam, Ph.D. DUJHfcCT: Department of Labor Dtanl/ud for Occupational Exposure to Inory/ini': had riorihlomen: Enclosed in n draft of the I>f>artmrnt of Labor Standard for Oecufkitlonat KxfkT.aur*- to InorpTinlc lead. TO!:) draft waa obtained from Dr. .Jotm 0*lb 1 I, Office of Standards, on January 10th when Dr. O'Neil met with the Irylustrlai Health Corrmlttec of the Mattery fourrl] International. Dr. O'Neil ask'd that ty document be reviewed and onrrnts he submitted to hln. it la i m>tias /yd that this 1.". a draf d y ismt. 'y. pith a'-d t'.d tie Department of Labor want'd to ev.iiu.it'- tty bnn'ict of t'y nri|e""I ' ta: > lari 'in the workplace lyfore iasulru' a final dorumerit. He stated that tir D nart- rrynt of Libor would like to visit, plants In order to evaluate the stan i.a:-l. He stated that the visits could Ik ? made without Initiating futy conn) 1 an'.''- action iriyirdlens of coniltlora, since such visits would be In conjunction with tty? wrltlnr of standards rather than compliance actions. Dr. OM.'e'i. Indicated ttk'it the De|>artment of Labor would like to visit a numtyr of lead operations by Invitation. !. O'll'd 1 ;irivl ry'l ttk'it tty D'p.'irtiiyrit of Lihor did riot plan to have e. Advisor/ C<mn|tt"e for tty lead staryl.ar!:, ::!rc" ttylr ex;yrlerye v/lt.n Advisor/ f'yinil t.t*had rril. bo'-n p-kid. !t a).'-.Tr':', ttiat. thy !yp.ir* "/ :iV ;.i(Mr pro|y/ses to u.'i'.- Ltd:; nrcli-'L'il: jri <>!' ev.T I uafl rip, propos'd stai/lTsd: . 'Dy Department of Ikilior types to determine by this valuation: 1. If all provisions of tty doeunent .are ty'-hd or If additional t 1 - j v 1: 1 * -j .. arv rufjiilrrslV . If the standards arx- applied us written, will the objectives of prot'-'ti.u: tty worker be met? 1. Are sore provisions of tty standard stringent but yet lricffeet 1 v In protecting the worker? Cont'd ./.UIII. 1J v , j 1 fix' ini.l'-ir privli)i<>ici of th" ilx:ument an-: J. T)/; standard for nlrtxmie concentration:! fur lead 1:; o.l'j ur/in'. ?. Hie employer shall provide or male- avallable /a hlr, own cost., biological monitoring to nil employees subject to exjxjsure to Inorganic lead. a. The blood lead limit la 80 ug/lOOg. b. Urine nay be uned Instead of blood. However, If a concentration of lead In urine exceeds 0.<>0 mg/ml, a blood sample Is required within two weeks. Ur. O'Nell Indicated that tlie employer 1:; required to mal"- aval laid'- i,i . ...d.-at monitoring, alttwugh tlv iirployce lr, not. rx-qulrt'd to sulimK to t,loior,l, monitoring. Ur. O'Neil Indicated that lie would like to Have a critique of tlx; doeunx.-r,'.. Ml"fl u,,. work Jr, cornl"L.vl the f'lml rkcimTif will h- wrltt.-ri , publ In the Federal Heglster, public hearings hold If rcqueste<J, conr;nt per-lai provided, and tie hepnrtment. of l/tbor would Uien review i.'k - total record to come up with a final docunent. ,j I think it In moat Important that the LIA Envlrorrnentnl Health CarTmlU.ee lave a meeting to dlscunn the proposed standard. We would appreciate any corrments that you might, fvive. .'dneorel.y, lumld I:. lyrvmi, i'h.in Aralr.t.'int Director I'lriv 1 mrrnenl a 1 Ilea | t.i. DRAFT i DEPARTMENT OP LABOR Occupational Safety and Health Administration {29 CPR Part 1910) Standard for Occupational Exposure to Inorganic Lead Notice of Propoaed Rulamaklng Pursuant to Section 6(b) of the Williams-Steiger Cccupat ion.i 1 Safety and Health Act of 1970 (84 Stat. 1393; 29 U.S.C. 635), Secretary of Labor's Order No. 12-71 (36 F.R. 8754) and 29 CFR Part 1911 (36 F.R. 17506), It la hereby propoaed to adopt a new standard to protect the health of employees In occupational exposure to Inorganic lead. The National Institute for Occupational Safety and Health (NIOSH), U. S. Department of Health, Educotlon, and Welfare published and aubmlttcd to the Secretary of Labor, puiaunnt to the Williaaa-Stelger Occupational Safety and Health Act of 1970, criteria for a recomendcd standard on occupational exposure to inorganic lead. The proposed standard la baaed for the most pert on recommendations In the criteria document of NIOSH. The proposed standard compiles with sections 6(b)(5), 6(b)(7) and 8(c) (3) in fulfilling the requirements of the Act for a comprehensive standard. Written comments concerning the proposal may be mailed to tha Office of Standard*, Room 509,Railway Labor Building, Washington, D. C. 20210 within 60 `aya after the publication of this notice In the FEDERAL REGISTER. The deta, vlewa, and arguments will be available lor public Inspection and copying at DRAFT DEPARTMENT OF LABOR Occupational Safety and Health Administration (29 CFR Part 1910) Standard for Occupational Exposure to Inorganic Lead Notice of Proposed Rulemaking Purauant to Section 6(b) of tha Wllllams-Stclger Occupctlonnl Safety and Health Act of 1970 (84 Stat. 159?; 29 U.S.C. 655), Secretary of Lebor'e Order No. 12-71 06 F.R. 8754) end 29 CFK Pert 1911 (J6 F.R. 17506), It la hereby proposed to adopt a new atendard to protect the health of employees In occupational exposure to Inorganic lead. The National Inatltute for Occupational Safety and Health (N10SH), 1). S. Department of Health, Education, and Welfare publlahed end submitted to the Secretary of Labor, pursuant to the Vllllams-Stelger Occupational Safety and Health Act of 1970, criteria for a recosmendcd standard on occupational exposure to Inorganic lead. The proposed atendard Is baaed for the moat part on recommendations In the criteria document of N10SI1. The proposed standard compiles with sections 6(b)(5), 6(b)(7) and 8(c) (3) In fulfllllnf the requirements of the Act for a comprehensive standard, Written coassent a concerning the proposal aiay be mailed to the Office of Standards, Room 509,Railway Labor Building, Washington, D. C. 20210 within 60 ('aye after the publication of this notice In the FEDERAL REC1STER. The data, views, and arguments will be available for public Inspection and copying at the Office of Standard*. Pursuant to 29 CPU 1910.11 (b) and (c) , interested pernoni, ay. In addition jto filing written mattar aa provided jbovi', file objections to tha propoaol requesting an Informal hearing with raapect thereto in accordonce with the following conditions: (1) i The objection* tuat Include the noma and address of tho objactorj (2) The objactlona eiuat b* postmarked on or before tin 30th day after the data of publication of thla notice of proposed Tula**king; (3) The objactlona ttuat apaclfy with particularly the provlalon of tha proposed rule to which objection la taken,and must atata tha grounds therefor; (4) tach objection nuat he separately Btatod and numbered, and (5) Tha objactlona musl be accompanied by n summary o( tl evidence proposed to be adduced at the requested heating. Upon consideration ol the records ol the hearing!), If any, together with any other written date, views, or arguments received In response to this notice, the Aaslatant Secretary may adopt the proposal with or without changes or modify the proposal In light of the consent* received. Accordingly, It Is heteby proponed to amend J*rt 1910 of Title 29 of the Code of Federal Kcgulatlous, ns net forth below: 11910.93 (AMENDED] 1. Table 02 In 11910.93 (F.R. 22142, October If), 1972) In -2- propoaed Co be amended by deleting tbe lollowlng: ***** Lead and lea Inorganic . . . 0.2 aig/M^ compound* (7.37.11-1969). AAA## 2. A new aactlon 1910.93 - la propoaed to be added to Part 1910, read aa follow*! *1910.93 Inorganic Lead. (a) Scope. Thl* aactlon applies to all place* of nap) oyn.cnt where dutta or fume* of Inorganic lead are preaent or may be preaent In the air. Where employee* are subject to exposure to Inorganic land at or below half the permissible limit specllled In paragraph (c) of this section. Compliance with the following paragraphs of this section la not required, except for paragraph* (f)(l)(li), (f)(2) and (g)(1). (b) Definitions. For the purpose of tills section. 0) "Inorganic lead" Includes lead oxides, retalllr lead, and lead salts (including organic salts such as lead soaps). (2) "Exposure to inorganic lend" mean* exposure nbovr b.-ilf the permlaslble limit specified In paragraph (c) of thin sect ton. (c) Porirlaalble exposure to inorganic lead. The airborne concentrctlon of Inorganic lead to which any employee may be exposed shall not exceed 0.13 mllllgraai per cubic meter of air (0.15 stg/M^) de terralned aa a l ime-we 1 ghted-avernge (TWA) expoi.uie for an 8-hour day. -3- i'viKJ m ",a m \;& t ;& [nopoucd to he ac: .<!<*<' by deicilng t b < f u) i owl h k l.tad and its inorganic ^*2 ntg/* expound* (737.11-1969). gy i. LIA1367 1 ;\, .^'V.:. .--* . : .- ; :.' 7 ' ` , - .*- : . , i.i^'^.i,-'"'",'o b'1, .Z:** **>. ^>7*0. . *``,s ` *S ' -aY ; ' t ^ ) . f. orv **C< ion 1910.93 - 1 proposed f .' ' r t>.\,\<d f'. j'j-.i ! read et. f ol lov r $19 30.93 Inorganlr l.rad. (a) Scope. TM auction applies to nil plates of cr-pl- *' * where dueta or furoea of Inorganic lead arc present or cay he pi ent In the air. Where cirployeta arc subject to exposure to ! nnj ^nlc lend at or be 1 <*v half l he pr n:: 11, #. J M < 1 1 rr 11 a p<* i, 1 J :i i . *;: * .-i yr n { h (c )of t h 1 a t. c * f 1 un . ( :r t ) \ n i,; u 1 ! !. r h < f o ) 1 < v 5? , pal tK ph of this section j* not rc<ju i i rd , </.;? f o: pni.-jj:-- i). (f)(2) and (g)(1). (b) Def i nit font. For the purpose tf this section. (1 ; "Inoiganlc lead" includes lead oxides, ortnllli lead, and Je.id alts (including organic aaltn auch at* l***.! c<ip!.). (3) "bxpopure to inorganic lend" nc/nu. cxpoMiTt ctlwvr i. I t !<,}! I r ! lr j I H jii-r 1 f 1 ed 1 ti pa 1 .< yt n pi (i ) ol t h i t- i. t () IV lr 1 at. lb ) - ryjiOi.utr to 1mi !,'< lead. The j 1 r b- i i 'i,no;ilni| Ion of 1 t o 'i y n n 1 < 1 end t < wh 1 < ); r: v r-p 1 < -v -c !-./< v v . j <'> 't! n)i n ] 1 not% t r o! 0.1'; in i ] ' j p t n r- pi * r nlip lor t v i < > 1 * 1 : '(;/K'j dele r*\ : nf |>.c. -- . iO** ''.j' LIA13672 v (d) Method* of sampling snd analyain. Method* of Honpllng nd analysis ahall be auch that Inorganic lend at a concentration of 0.15 mg/cu a con be determined with an accuracy of 4 15 per cent In a one hour air sample. (1) Sampling. Lead dust or (uoco ahall b* collected on 0.45 or 0.60 alcroaeter poroalty cellulose aesfcran* filter* Mounted In either 2 or 3 piece filter caasettra. Air ehall be drawn through the filler by means of a pump at a rata of 2 liter* per mlnutas (not lac* than 1 nor aor* than 4 liter* per alnutt). A minimum sample of 100 lilera ahall be collected. Clectroatatlc precipitators and other collection methods and taapllng ratal ahown to give equivalent result* may be used. (2) Analytical method. The reference dithlrone method as pacified in Appendix A, or atonic absorption spectrophotometry or any nethod ahown to be equivalent In precision and accuracy to the dlthlxon* net hod ahall be uead for the analynia of the lead In air and biological aanples. (a) Envlronnantal r-onltoring. (1) Genera) requirements. (1) Where exposure levels of employees to lead Is not known the employer ahall have an Industrial hygiene survey done, to determine the employee's exposure to Inorganic lead and environmental levels In workroom areas. The program shall be carried out within C months of tha effective date of thl* section. (11) Vorkrooa artas where It ha* been determined on the basil of an Industrial hygiene aurvey, that environmental levels of lead do not exceed half the pcmlaslble limit specified In -4- 4 pnrcgrqph (c) of this section nhoil not bo conui doted to U'iv i exposure to inorgsnlc lead. (2) Frequency of sampling. (1) Wheru there lu cxpo-.tiii to Inorganic lead the monitoring program shall consist of poif.on.il breathing tone samples. Monitoring shall bt done on a periodic basis, but at least every six months, or whenever there is s chmtgc in exhaust ventilation, process, or operation that ray nfftM the employee's exposure to lead. (if) If breathing ton* leveln arc at or above the permiMill- Unit tpcclfied in paragraph (c) monitoring ahall b done cvci y 3 months. This increased frequency of monitoring ahall be continued at laaet 6 tonthe (l.e. two core quarterly monitoring periods) after the last campling that demonstrated levels nt nr above the parmiaslblt limit specified In paragraph (c) of thK ectIon. (Hi) Periodic olr oampling hall be performed to coincide with pcrlodir biologic sampling, 1.*., ahnll be performed vjthii. two vecVit of biologic sampling. (3) Breathing zone samples. Breathing zone*, samples ihoJl be collected to permit conctruction of an 8-hour lime-weigbt < d- average expoaurc of employees. The following number of 1 er. ahall be collected and analyzed, nn a minimum! baaed on the maxlmum number of employees in any given work urea: Number of Employees Frpor.ed Nmnhcr of Snnp 1 ej* (O Ul) 1-20 20 - 100 SOX of the number of rtijtloyn . 10 HAMplcti J>)UH of i he -5- txccnh -V n nv< r 1 GO r 1 ovr r . (4) Employee pb&rrvt Ion or ror\ i t o ? i n y . AMected < n.-p 1 ny< or their represent*!!ve*, shall be given opportunity to observe any monitoring required by this paragraph and shall have nccof> to the records thereof. (f) Met hod of cont rol . (1) Fnglncn in}; > on t r < 1 . Fng j nn i > u controls shall be used to maintain the airborne lend rnnmK r ,i( nn, vhcre feasible, below the permissible limit r.perifitd In pc t /i jo .i ph (e) of this section. (1) F.r.hauat nyt> x c o j > . Where a loco) exhaust ventilation and dust collection syaten la used It shall be designed and maintained to prevent tha accumulation of lend duet and fume. (11) Rcclrculation of air. Air from the exhaust ventilation system* ahall not be recirculated Into the wurl root:*, and rhnll net be discharged outside- the plant In such a iwinnor on to < t fusti an alt pollution problem. (2) HouHfkeeping. (i) All o x Umia ] imrf.:.h.->]l ! cvflntalned lire of nr ennui ;it ion of Inurg.mlt l.*d dual, if with their dispersion Into the air there would be .m excewr* J vc coticer * tration. Leeks and spills shall bo cleaned up . noon n<> pn?;>. IM* to prevent dispersion of lead Into the air. (il) Vacuuming, wet sweeping or other rTthodw which do not generate airborne lead shall he uacri for cl ra n i n g t he wurl'plnci . lio dry sweeping or blowing shall t<* pr rtrl f t <*d . (ill) Materials which euiy (-on t nu<l tin t r t (, uoi l orni with -A~ Inorganic lead duat ahull ba properly stored and disposed of to prevent auch ocrurrancc, (g) Sanitation practlcaa. (1) Food facllltlea. Food preparation, diapanalng (Including vending machines), and ontlng ahall b* prohibited in lead work tircae In compliance with 11910.141(g), (2) Locker facilities. Work and atreet clothing ahnll not be atored In the awe locker In compliance with (1910.141(c). (3) Shower facllltlea ahall be provided In acco-dance with (1910.141(d)(3) and uted by enploytea who are exposed to air borne concentrations of lead above the parol salble llnlt specified In paragraph (c) of this aectlon, or when work clothing or exposed body surfaces becoos contaoinated with Inorganic lead duat. (h) Personal protective equlpnent. (1) Respirators. Coop 1 lance with the exposure Unit specified In paragraph (c) of this section nay not be achieved by the use of respirators or shift rotation of employees, except: (1) During the tier period necessary to Install the engineering controla required by paragraph (f) of thla aectlon. (11) In work situations In which the methods prescribed In paragraph (f) of thla aectlon ere cither technically not feasible or feasible to an extent insufficient to reduce the airborne concen trations of inorganic lead below the limit specified In parogra ph (c) of thla aectlon. (ill) In emergencies; or (lv) Occasional brief exposures of a nonroutlnc nature above the Holt specified In paragraph (c) of thin section. (v) Wharo both reeplrntora and pereonnel rotntion nrc 1 lowed by eubdlvlelona (1), (11) or (111) of thla ubporor.rnpl, and both are practicable, pereonnel rotation ahall be preferred and uaad. / (2) Whara a raaplrator la permitted by aubparagraph (1) of thia paragraph, It ahall be aelected from among thoac approved by the National Inatitut* for Occupational Safety and Health, Department of Health, Education, and Welfare, and the Mining Enforcement and Safety Admlnletratlon, Department of the Inter for under the provlaiona of 30 CFR Part 11 (37 F.R. 6244, Harch 1972) and ahall be uaed In accordance with aubparagraph (3) of thla paragraph. (3) The employer ahall provide rcaplratora when required Ly thla aection, and ahall aeeurc that employeca uee the rceplrnion. provided. Table I ahall be uaed for the aelectlon of rcapirntort at concentratlona of airborne Inorganic lead above the limit epeclfled In paragraph (c). LIA13677 TABI.E I Requirement! for Respirator linage at Concentration! Above the Fcrmlasibla Exposure limit Exposure Inorganic lead duet 8 Hr TWA lee* than 1.5 Respirator Type A, B leaf than 15.0 C greater than 15.0 D Inorganic lead fuse leaa than 1.5 F le*a than 15.0 F greater than 13.0 D *A - Reusable filter-typo alr-purlfylng duet reaplrator B - tingle-use duet reaplrator C - Powered alr-purlfylng poaltlvc-preaaura duet reaplrator D - Type C poaltlve-preeaure aupplled air reaplrator E - Reusable filter-type alr-purlfylng fume reaplrator T - Powered alr-purlfylng poaltlve-preeaure fumo reaplrator (A) Employees experiencing breathing difficulty while using reaplrator* ahall be referred to a phyalclan for evaluation. Thlr. valuation ahall investigate If the employee* had adequate venti latory capacity and any evidence of obstructive lung disease. Employees with Inadequate ventilatory capacity or evidence of obetructivc lung dleeasc dull not wear typea A, B, and K reaplratora. (5) The employer shall ratabllah a reaplrator program in accordance with th requirement# of iubparagrapha (b)(1) through (b)(10) of 11910.134 of thla Part. 9- - (6) If both fuatea and dual ara praaent the reconwended uaage raaplrator la that for Time. (7) Usage of a vaaplrator apaclflcd for uae In higher concentration* of lead la permitted In atmosphere* of lower concentration. (8) Eoployaea ahall be given instructions on the unc of raaplrator* aaalgnad to than, cleaning of the reaplratore, and hov to teat for leakage. (9) Protective clothing. (1) Each employee subject to contamination by contact of clothing or exposed body surfaced with Inorganic lead, or to airborne concentrations ol Inorganic lead above the Halt specified In paragraph (c) of this section ahall wear coveralls or alaiflar full body work clothing and head covering during working hours In these areas. Eaployees not subject to contamination by contact of clothing or body surfaces with lead but subject to "exposure to Inorganic lead" at or below the Halt specified In paragraph (c) of thi* section ahall change into aultabla work clothing before atarilng work, and ahall remove work clothing before leaving work. This work clothing need not afford full body coverage. (II) Work clothing contaminated with lead dust ahall not be cleaned by blowing or shaking. When practicable, work clothing ahall be vacuumed before reaoval. (III) Whan work clothing becomes contaminated with Inorganic lead It shall be changed for clean work clothing on the next shift or next day's work. .'V *' ,'r -'> " v-* 4vS.y , ~-:.'%,.*< -;A-",>*< ~-*>.> .j ,.' ,,tvtr.*W.irM3*"'-4.Vwj..--.*-..r-,'.~- * LI A13 6 79 (I) ^.-ir * *x cnployrrfl_of h nr a t d * M * * l<_ftd (1) 1 '< k cc.pl oyOc r * poo c d to ] # #i I 1 (I r < c i e t go r>f y p i < r -' ' > r * , , j t t !.of tci f t 1 <: 11 f- e fif! (no iii;i {cnii f r ; v tt f e *J ac or r > or e . f r-, 1 <, y >' r ha 1 I hr d v 1 h 16 au t. o rv ft 11*b11 11 y of a ueh i r 1 o i rvi f i fa .-!:)<< * h t* 1 1 \ -1 V r pi f *?'. Ill*- 41 n ij m h a 1 1 It a < c t: h n 11 > j e t < r, i < y r < f e 1 pirn- of t'ri[']uy:-iv*i!i whole j * .h ! j h uaod. (J) M*dJ_r*3 . ( ) I FMoln^s.i! I^ni t or Ir;];. \I) 'Hu- vv.y'<>', < t Khali provide ot wake available at hla coot biological Eton f t or 11->, to all etrployeec subject to "exposure to lnoigT*. ic lend. Tt -'ont.iaiu of i*atrpl ing and analysis of whole blo-d, r a 11 e? i.n! ' 1 1 v < : vi r f ne for 1 e* n <J content. Such wonfturing 'h.-ill hr pc i ! < r r,* <! ! < f!,M:u i , . v.t> t- tn;> i oyr v a 1. wo i \. t an u:.n'' t r j i ' 'v ; - >' r*f < ' hruu c c pt ab 1 r ftbMOJpllc.n of letf por-htp > t ! h V of {.< 1 M(n 1 np la d riDonst rn t et! at li-vol*, of 0 . (h1-. n. f 1 1 J ^r a r.a <-i lr.i'1 pel litrT of urine (with urine >p<-rlf c p.r.ivlf;- u-r r er t m! to 1.02^) or (/renter. Procedure# fot snupllnp, tu! muilyi.Ift of blou<f or urine shall be aa deocrlbed In Appendix A and auhparugrnph (d)(2). (if) P 1 v ` ` : ' ' i M i <. r/i" ' 11 ! !i.m j i ]<-ar* rihall hov*- t* 1 r* 1 og 1 r 1 r i, f f i : 1 i. j, U"H w Vii 11 :> h ) * ! t< t hi r. iv * j y <* r#>nths r;o that rath ce.p 1 oyer jduill lt/tvc blood a. .a u i '; t, . r: d r t a 1 y a j fi r;tn 1' ft v n t 1 /ib 1 e t r > h 1 u yt ,is jy. A eero n*ve] 1 ij found to ho 0.08 rv.J 1 1 1 p,i u* p*i 100 grown id v.hulr blocal or -33- I *?/P: 44440 +* J** grcntci . U this aacond blood aample 'oniiirt.u n*. I'niiMilve lend ot 0.08 willigra** of lead per 100 gratia of whole blood , nr greater, b % apa to reduce the employee11. ahnorpt Jon of lead n).b 1 i be taVcn. JUepe to be considered IncUi-V J r.pr < v rr m t ( J :-v :.T 1 t out r o)h ,Kijr fvr ent <-l p* i m>u J 1 ' ' ' ? ; 1 - 1 - ; h/g Ifm- , and vif.e of adiM r. i M : t i vr cm.itwbm ' <J 1 < .) J t.--i ;v. t lot* for pusaibl* lead poisoning a lull 1 be L-.'de t,\u 11 /* !.* J < . (1M) Urine sample. If urine sampling end annlyi.it; .no choacn instead of bloixi tatEpling and annlyr.ia to nntitjfy the biological raonltorlng requirement, each employe*; shall have urin< ampHop, and analyal* Bade available at f> wmtht. 'p-'t urine specimen?. of about 100 tnl . aha 11 be i ol ]m t rd dating vui i day, and urine ftpatiwne vlt.h a epecilK gravity lean than 1.010 ahull be dlacnrded and another sample obi aim'd. Jt nn enq )*> y< '; urine lead level la found to be 0.70 f.g/iliei <*: yteator, > a < 1 to specific gravity of 1 , 01: A, a blood u ai: pi e t> ha ) 1 be ob t ; ; ' > analyted within / weran. (iv) Abtto?e;al level ft of_env i i mn c i t u 1 i-i bj o) i.jyi i ji 5 _j nj ! <_ * If the concentration of airborne Inorganic Wad exceeds the llr.lt prescribed in paragraph (r) of thin i,n t i-n, the interval of !>*<- logical t.oni'oring nlj/ill hr hlv*-! j . < . , blood analysis i.h.u I b, ain'!;i( led quarterly, with r nrh ott;* J oy amp ] ed i mrd --e .mua 1 1 v , (, III I'wilvnll filial) be conducted quartet)*, .<n m.rh rinp ) oyee . Jt.J tm tenure! frequency uluili Ire i out i*nin' f'i it I e/ M (, iMmthn aim- the high environments! J ev< 1 li been Iu -w m, (v) Biologic monitoring shall alto be made available where there la raaaon to believe that operations produce unusual exposure excursions or that envlronaiantal staples do not adequately describe the eaployee't exposure to inorganic lead. / (2) Medical examinations. (1) Central requirements. The employer ohall provide or male medical examinations available t hja coat to employees under any of the following conditions: (a) When the airborne concentrations of Inorganic lead exceed the llailt prescribed In paragraph (c) of this section. (b) For eaployees vlth an unacceptable absorption of lead as Indicated by biological monitoring. () When administrative controls Involving rotation oi personnel or respiratory protection are uoed. (11) These medical examinations shall be provided or made available prior to employee placement In areas where the airborne concentration of Inorganic lead exceeds the limit specified in paragraph (c) of this section, and annually therenitcr. Current employees who meet the requirements for a medical examination it. aubdlvlatona (J)(2)(), (Jb), or (c_), and who have not received such examination within one year of the effective date of thin standard shall have such medical examinations conducted within 6 months of the affective date of this section and annually thereafter. (ill) The medical examinations shall include a physical examination, complete blood counts, blood lead determinations, routine urinalysis (specific gravity, hllMr< and protein deierroltmt ions, 15- cttd oi ros roj i c examlnatlone), and rfr.oi J o / any aigns or r< of plurablam, If present. (iv) Whrc urtn i selected instead of blood for biologic mon 11oringf the preplacement examination uball eleo include *> urinary lead determination. K*ch employe* whe abcorbr, un/n < ;>' )* amounts of lead ce Indicated by biologic monitoring ahal 1 b< examined ab soon a* practicable after such abborptirn In drrv.i. traced and confirmed, and at leaat every 3 month*, thereafter ' :. t f ! hla blood or urine lead levels have returned to normal, i.c. balov O.OflO og/100 g of blood or 0.20 mg/lltcr or urine, If clinical evidence* of plumblaa la developed from theac medic.*! examinatton*, the worker thAll be kept under a phyaiclanf. care, in accordance with applicable Workman's Compensation pro v 1 r. J r r.*., until the worker haw completely recovered or raxiual irprovemen? haa occurred. (k) Kacordkcepi up. (1) Knvlronmcnt a 1 records. Record*. hall be maintained for all campling schedule* to include the aaiopling and analytical methods, type of respiratory protection in uac (If applicable), and tire concentration of Inorganic ) c*id in pernonal breathing zone samples, and work area aamplcn. R-ecord* shall be maintained no that they can be cl attained by employee. tech employee shall tic* able to obtain informal ion on lia own environmental exposure. The record;* nhnlJ bo kept for at 1 east 3 yeaia . (2) Medical records. Medical records aboil include infor mation on all biological monitoring rind medical examination!'. -14- These record* shall be kept Cm ot lonat 1 year* following the l*t occupational exposure to Inorganic land, (3) The medical record* *h*ll be available to the medical representative* of th atnployar, of th* Aaulatant Secretary of Labor for Occupational Safety and Health, of the Director of NIOSH, Department of Health, Education, *nd Velfar*, and, ot the employee's request, to th* employee's physician. (1) Caution sign*. (1) Potting. Caution sign* ahall be provided and displayed at each location vhar* airborne Inorganic lead concentration* *r* likely to occur which exceed one-half the limit apecifled In paragraph (c) of thie section. (2) Sign specification* (i) Th* caution algn required ahall display th* following legend with letter slrea, atylcn, and contrasting color* of a visibility to permit coo.prehonsion of the warning at a distance of no lese than 10 feet. Signa ahall he replaced when they are not readable at a distance of 10 feet. LEAD AREA CAUTION Follow Supervlaora Instruction* On Precaution* To Obaerve (11) When the concentration of airborne Inorganic lead exceed* th* Unit epeclfled In paragraph (c) of thi* section, all requirement* of eubdlvlelon (2)(1) of this paragraph shall be compiled with, except th* sign shall display th* following legendi LEAD DANCER High Concentration of Fun* or Dust Wear Proper Respirator APPENDIX A REFERENCE DIT1I1Z0NE METHOD FOR ANALYSIS OF LEAD IN AIR AND BIOLOCICAL SAMTLLS Tha fol loving direct lone for analysis of lead ire taken frot tha flrat part of the report, "The 'USPHS' Metnod for Determining Lead In Air and In Biological Materials" by Keenan, Bycre, Sultinan and Hyalop.1 Additional Information on the reproducibility and accuracy of tha method la given In other portion* of the repent. 1. REACENTS 1.1 Analytical grade reagenta are used. Purification It. eaaantlal when analytlng biological tlaeuea and fluids because of the vary low levels of lead In these materials; purification of reagents nay not be required for air samples containing quantities of lead sufficiently greater than that present In the reagent blank. A reagent blank sample 1* carried through the entire procedure with each set of unknown samples (air, biological, or other type) and lta analyred lrod content is subtracted freer, each analytical result to calculate the net quantity of lead In each unknown sample. 1.2 A boiling rod la uaed or prevent bumping In tbc flunks when dletllllng reagents. This la prepared by cutting 3 or 4 u> O.D glaaa tubing to a length which la one cm greotcr than the height of the flask. The tubing la Reeled at a a pot about one cm above the bottom end which le flrc-pollshcd but left open. Before each use, the liquid la shaken out ol the bottom nrctIon 1 Keenun, n.f.., Byers, I)., Snltzman, B.E., llyslop, F.L: The ' USI'II.'I' Method of Determining lead In Air And In Biological Materials. Am. Ind. l!yg. Aaaoc J 20:4fil-91, 1903. A ud l li t: J C 1 l V in til*- 1 1 0 V . Ah t h stream of air and vapor bubbles iasuan f rorr' l be open Hpucc, t'i. , providing nuclei (or aovooth boiling. 1.3 Doubla-diatil1td vater - To distilled vntti In .m all borosilleate-glaae still add a crystal each of potassium j>errf.angar.; i and barium hydroxide and redistill. Use for rengent and hiolof.i< '< 1 sample solutions unless tests indicate that n i np.) e -d i f. t i 1 1 ed v/itr is satisfactory; finj -distilled w.itcr Jo ui.ually adequate fm d r t er mi na t lono on air sample. 1.4 Nitric Acid, Concentrated - Rediutill in an all boror.i- licate-glasa still the ACS rsagent grade acid, 69.02 minimum, specific gravity 1.42. Use an electric heating jacket on the boiling flask to minimize danger of its breakage, and a boil ini, rod to prevent bumping, which otherwise would he Levcrr. Dirceid the Mrst '0 r.l of distillate; thit may be combined with t lo se i d allowed to remain in the flask n t the end of the d 1 r t 1 ) , .i , o, and used for vai.hlng glansuarr. The reagent in convenient!) dispensed from r i.uwill aufomntli burette. ho pir/iuv should l- uned on the stopcock. 1.5 Nitric Ac id, 1:99 - Dilute 10 ml of the rrd i a111 1 ed , concentrated acid to one liter with douhled-dinti11ed water. 1.6 Ammonium Hydroxide, Concentrated - Distill in an nil boronillcntr-glass Btill 3 liters of the ACS rougrnt grade, 7H.92 minimum specific, gravity 0.8957 at 60*K, into 1.5 11 tern of dml)< distilled voter, contained in n 7--3 It t* r reagent hottlc which 1 , chilled In n fr* bar it. Continue the distillation until the bottle ,/V "-5 *< V'*'- He * & * J nl**-. , .( :' L1M3686 the. c.. <;,i'5 n;< > m.1<*- deeply in the w/Uet In (: net Ivn , i ' i',irw M. 1t- f >>; <. i j n t1 t l> c It ( n \ \ nvi * d u i ; ! io : i n . ! . ' fr r- ?*-V d i t`: i l 1 A t V . V; I : ; ; < i; . . t t If . y in ^ ; IWu m - J .' .- >>.{. rr.bh to the b''Mn;. of :' r*; yh Tf'tp.ciit bottle. The 4MfionlA n if abftoibed lit dc oh ) c-d. 1 M ill*' : ,.ff ;' ^>C ,.v*i water until th aolwllon reach^n t he deniicd epee if ic ^invity. i|f: \.) Ch 1 oro f oi n, - Um: n biend viih t\ r, ( ) t er e r> X nn ?h< l-d-i : * .*OJ th.nl (hr r h 3 u ;>f < > r r>p/ ft ee ft t hr .V < r J < >ii Ch < in 1 / > 'n'< i< I ; t < < '; r< u i % /ih \ 1 1 I y 1 ` r ut-i` 1 n d 1 l h ] i on* ; i1: < b*i < o . i 1 r -'d 1 I i -i: , 1 hatch of rhlondorn rhou]d be po 5 < h,ii. e d It, pi.to- . unt ai o* r ni, and ahoulcl be tea ted n follow in the j abn1 n i / y to :.o m that it in aa t 1 u f uc t o ry for piaparinj; \ h< 'i 11 i ?.<>u r,olutJ<-u. add a r.inutc qvjnntlty of dit!rlionc to n povl1<;n of tilt ihlnrrlnn In a toot tube, hflV.<* gently, then ntopper with a cork. 7b< frtint gret-n color ho\jld br r> t n T1 * lot on** <i.v. Our *x }o r'1 :; < hn ft J t id i < n t r ! t !,;il f )ir ! 1 iin, , lit: rroiifi . 1 < ut y,r i wflt j etit rt! in view of tin- * i < ini t ..t i I ub i 1 1 l y n i o i fn^'ii t f,r :id(* n . l.M Kxt r art 1 on l)i t h i roric - Dinno)vr ] (> rj; ol diphenyl l h i o - 1.9 Standard Plthlrons - Dissolve B ij of dlphenythlocarbarone In one liter of chloroform. Store In a brown botlli In the refrigerator but allow to warm to room temperature before using. Age for at laaat one day, then standardize as described In the procedure. Reatandardire every few months. 1.10 Sodium Citrate - Dissolve 125 g of the 2 NajC^lljOj. 11 H-,0 salt In sufficient distilled voter to provide a solution ncnily 500 eil In volume. Adjust the pH to 9-10, using a very small quantity of phenol red Indicator solution (strong red color) and fresh. pHydrlon test paper to check the pH. Extract In n large separatory funnel with a 100 mg per liter solution of dithlrone and finally with the extraction dithlrone reagent until a groin extract Is obtained with the latter reagent. Add a small volort of lead-free citric acid until an orange color (pll 7) oppinr;.. Extract the excess dithlrone repeatedly with chloroform until a colorless extract la obtained. Remove the last traces of chlorolori* 1.11 Hydroxylamlne Hydrochloride - Dissolve 70 g of tin- i.r.H in distilled water to provide s volume of 65 ml. Add s few drops of sr-cresol purple indicator, then add ammonia until the indicator turns yellow (pH 3). Add s sufficient quantity of a 42 nolutlon of sodium dlethyldithiocarbmaste to combine with metallic Impurities then mix. After a few minutes extract repeatedly with chloroform until the excess carbamate reagent has been removed, so indicated by the absence of a yellow color in the final chloroform extract tasted with a dilute copper solution. To the aqueous solution of the hydroxylamlne hydrochloride add redistilled, 6N hydrochloric acid until the indicator turns pink, and adjust the volume to 100 a>l vith double-dlatllled water. 1,12. Potassium Cyanide - (Dancer! Highly pol nonour;! I ) To 50 g of potassium cyanide In a beaker, odd sufficient d!/.il!)<<! water to make a sludge. Transfer trbe sluice to a separately funnel previously marked to show 100 ml volume. Add a small amount of dietilled weter to the beaker and warm. (Potassium cyanide coola tha aolution aa it diaaolves, thua retarding the aolutlon procer. a.) Add thie warm water to the eeparatory funnel but do not permit contents to exceed the 100-ml mark. Shake, tl.cn let etend until the contents come to room temperetutc. A practically saturated solution results. 1.12.1 Extract the lead by shaking repeatedly with portions of the extraction dlthlxone solution until the lead lias baan removad. Tart of the dlthlione dissolves In the aqutoun plume but enough remains in the chloroform to color it. A green extract Indicates that all the lead lie a been completely extracted. Hoot of the dithlrone in the aqueous phase is then removed by repeated extractions with pure chloroform, Dilute the concentrated rolutlon of potassium cyanide with double-distilled water to 500 ml. It should not be necessary to filter the solution. If the ditrctlom. are followed prcclccly. Extraction in carried out before dilu tion because the higher pH of the dilute solution is less favorable. 1.12.2 (NOTE: A colorlciin solution uouully results if above directions ere followed. Occasionally aging resultn in e brown color or precipitate due to polymerltation of hydrogen cysnlda. Thin doaa not Interfere with ue of the If It. i c taiifnliy decanted. Old potassium cyanide reagent mo y lohe enough e f r <-nj; 1! i to cause insufficient complexlng of largo amounts of zinc.) 1.13 Airmo n fa-cyanide HI xture - Mix 200 ml ol the purified 10X potassium cyanide reagent with 1 !>0 nl of nlMllled a won 1 or:, hydroxide (specific gravity 0.9, cor r rspond 1 rp to 26.4X NM^; <ir.<! dilute to one liter with double-d 1 a 111 led v.it t i . If tin ?<., i. ;< .* specific gravity of the nax&onla la not 0.9, m.< the equivalent volume ae calculated from a tabic of specific gravity vs. percentage aration la. 1.14 Standard Lead Solution - Dissolve 1 . *>984 g of pure lead nitrate in one liter of 1:99 nitric acid to provide a strong Mock aolution containing one mg Pb per ml. Plpct exactly 20 n.l Into a 5O0-mJ volumetric flask and rake to ns\rk with 1:99 r, 111 1 < /k . Id to give a dilute stock, aolution containing 40 \sy. Pb per i.) . (A standard lead aolution, 10 u& Pb/ml, was stable- in 1:99 nilMt acid for three years.) Prepare n working solution, containing 2 yg Pb per ml, just before it is needed by pipetting j ml of the dilute otock aolution into a 100-ml volumetric flank and s .-iking to mark with 1:99 nitric acid. 1.3* Phenol Red - 0,3 X aqueous solution. 1.16 Ash 1 rig Aid Acid - Dissolve ?b g po t ;i. t. ium sulf/ite In aulflcient rcdlMlJlcd concentrated nitric ncid lo make 100 n) . 1.17 Wh1 t e Pet to] .i t um - Supplied Jn t\ i'J/im. )<ir, foi greasing stopcocks. To check on the purity, put n pinch oi this pc t ro 1 a l ura in a beaker, add n f i*w mill filtern r> f the 1.1 mul.ii d m <11T M / one inti swirl. If the dUMron* It no h*np r green n!in few Kilimlcfc, the DsAtclif) ia unea t 1 * f a c ( or y r.i < Mr.i; i.toj-ii- 2. APPARATUS 2.1 A Beckouin Model DU Spoctrophotomet'r hns been u j u m! in this laboratory since this Instrument becarue available in the l?40'e. However, the Beckman Model B and tlie Rausch and Lorob Sprctronic 20 have been shown to give comparable results for blood lead detorninat Ions, provided tliat appropriate standard! rations are conducted with each instrument. Other laborntor !<?., whose rruulta are reported in ihlr. paper, have ptssumsbly h m ' a diversity of available photoirctcx r* and spect t uphe t ore f i r . h. our laboratory, 2? x 125 run matched teat tuber* are unrd In mo*,f spec t rophot orect r J c procedural employing the Model DU, which J* fitted with a tube holder which doea not Interfere with ih< u m of the instrument with regular tell*. Ihcae aiv tubcu me ui.ed in the Model B fitted wit)* a teat lube adaptor. A 1/A-liwli tub. supplied by the manufacturer, i* ward In the haunch nnd I-orh Spectronlc 20. 2.2 boronll Irate f;lh*vrc In ward t hougboui the procedure (except ior vac ut a 1 fie rn used for blood iwirp 1 1 ng) . Ashing 1 n performed in 125- or 250-ml J'bJliipfe brakriw. Automatic burette are used for tho addition of roost reagent*. The extractions mr conducted In the Squibo-type, 125-eil separatory funnels support i. In electrically operated vhskeru provided with timer avilchcM, The stopcocks of the iiopuratnry funnel i* niv groaned wjtli white petrolatum (purchased In a glass Jar rather limn In a moiuJ i nr. or tube) unlcee Teflon stopcocks, which require no grease, are used. Ml glsasvaro should be reserved for trace analysis only to ovoid poaalble groan contamination. 2.3 Soak all ashing beakers In a detergent solution (Mumm .or Duponol Is suitable) Immediately after each mingc to prevint any Material from drying on the surfaces. Rinse C-10 tiiwr, with hot water and atora In a dust-proof drawer or cabinet until needed Use the following acid cleaning, lrad-lreclng techniques Inroad 1st ely before tha next use of the glassware: Rinse the sshing baakera with s saturated solution of sodium dichrorrr.tc In concentrated sulfuric acid, leave a 1-2 ml portion in the beaker or flask (proportionally less in a smell voluactrlc flask!). Add obout 5-10 ml of warm tap utter and allow the hot solution to flow over all Inner surfacet to remove the last trscen ol gre.n.i . Rinse with three or fout portion* of cold tap watir. Rinse with ons portion of either concentrated >r 1:1 nitric acid, m. ptiftii.. (This wash nitric acid may ba used repeatedly until it loan. 11 i. otrength) Then rinse aucccsalvely with three or four portions each of tap water, distilled and double-distilled water. bet the beakers upright on the bench and cover with a clean dustcase or a large piece of filter paper (or otherwise protect from dust). Under no circumstances It. glassware turned mu,He down to drain on a towel or checaccloth placed on a lnhorntnry bench. Use an oven operating at 105 C If dry glasawara Is required. 2.4 Separatory funnel* arc rinsed with top wntcr Immed 1 .*i < 1 after uee. If a high lead rumple woa present ot if a visible precipitate remains on t lie inside, Jt in rinsed with a small portion of 1:1 wash nitric acid (which is ! 3 a < .i r dud) , follow* -d ty tap water. The stoppered funnels in e ( < r *i in d< > t;h ] r - <1 < < V Yacks. Immediately before use, stopcocks nn- regreneed Si t, * < ary. Then the funnels are rinsed wi lit wash acid, four times uj tap water, and four tinea with distilled water. Lech rinse is accomplished by ahaking with the atopper, then draining through the etopcock with two or three turn*. 2.5 Spectrophotometer tuben are rirn-vn foot tlmu, ctu h with tup and distilled water Immediately after use. They nr- pl/j<< upright in a large beaker end dried In an oven at 105 C, then stored under a dust-cover. Occasionally they arc cleaned with d lehr on-at r~*ul f ut J i n< Id and nltr 1 . s< Jd ;if, <ics > l bed sbnv< . 2.5.1 (NOTH: With thin method <>f donning gl;iM w.w < we have never encountered c ront-c on t *ni j il / t 1 <>n f ton1 rluoniur?:, lc.nl or froo any other trace element being deter dm d routinely In thi laboratory.) 3. ANALYTICAL I1 ROCLDl'HL 3.3 Uijim the sample anh (prepared described In the following section:;) with ? ml of cone.< tit ml rd nltile arid for .i few mlnut.rn, then odd 7j oil of dlntllled water, healing cm the hotplate until n clear solution lu obtained. 3.2 Cool to loom temperature.. Add to the solution In the -10- beaker one ml of hydroxylamlne hydrochloride, 4 irl of sodium citrate (10 ol It required for t urine sample) , one drop of phono 1 red Indicator, and titrate to a strong red color with concentrated aenonia reagent. Add a few drop* cxcesa of nmnunl.i to moke sure that the pH It between 9 and 10, using resh pHydrlon teet paper to check the pH, 3.2.1 (WOTEt Phenol red htt a weak orange-red color in etrong acid, yellow In weak acid, and a red color in alkaline eolution. Do not mistake the firet color for that produced In alkaline medium!) 3.3 Transfer the nemple quantitatively with doubledletilled water rlnalnge to a 125-ml Squibb separatory funnel containing } ml of the potaealum cyanide reagent. 3.4 Add 3 ml of the extraction dlthltone and ahako two mlnutet, after releasing the Initial praaaura by momentarily opening the stopcock of the Inverted aeparatory funnel. Allow tha chloroform layer to aettle. 3.5 Draw off moat of the extraction dlthlrona into n aecond funnel containing exactly 30 ml of 1199 nitric acid. 3.6 Add a aacond 5-ml portion ol axtractlon dlthlrone to the f1 rat funnel and ahake aa before. Allow the layers to separate and combine the cxtracta In tha aacond funnol, Continue thia proccaa with frcali portiona of axtractlon dlthlrona until ihe reagent remains green, A rough estimate of the load proaonl In the earnple may he made on the bneia of 20 pg for each cltarry-red 5-ml extract portion. m LI A1369A "11 - / (t;A -11- 3.7 .MioV.t* tin- i.rcc,i\<\ funnel im l wo p.lr.ul c h to t i nun! cl the lend o ;lic 1:9V nJfrli; ,v M layer. Allow tin- layers Id acpoiAtf. Hi near'd I hr chloroform layer. 3.8 Shake the nitric Acid eolation with ppi ox 1 nat i y 5 til of reagent chlot of ot n. tine lei keltic, brain the settled C h lor o form through the stopcock bore aft completely as por.sihlr without loaa of the nqucf un layer. Evaporate the lent chop of chloroform clinging to the upper aurface of the liquid, 3*8,1 (NOTE 1: Start a z*ro leod otwndnrd at the beginning of t. h i e step by placing 30 o. 1 of 1:9V nitric n<Jd it. ii separatory funnel. This zero leaf* standard will ho used t <> iici the sped rophotuOAt cr at zero absorbance for each uvtlvu nf wamplea being analyzed.) 3.8.2 (NOTE ?: If (he quantity o! loud cMir./iln! for any cample exceeds the ?5 ug range of the c n lor 1 net r j c bctijminatlon, pipet an appropriate aliquot of the nitric acid solution at the end of utep 7 Into a clean rrparatory funnel containing j trl 1:99 nitric acid to minimize errors caused by poasiMf of t hr fitoj.mcV, add nufiii lent additional I'.'l'i u J t r Jr arid to 1'inVc 30 trd tntft) volume, and continue with step 8.) 3.8.3 (NOTE 3: Start lead standards at title point if required. Wd 5-rrl portions of 1:99 nitric acid to each of four separatory fttnnpU, then 2.5, 5.0, 7.3, and 12.5 ml of dilute fitaiuoid lead aolutlon (? ug Pb/ml) from a buret u*, respectively to the ccparntory funneln, finally add the* proper quantify oi K99 nlttic n< id to make total volume 30 ml in e.uh. Cunt into ?*& with step 0.) 3,9 Add 6,0 P'1 of .he arnBf>n In-1 y pn 3 dc* nhlui c, f x./i' I i) ml of the standard dlthiKonc, and shake two rlnulcr*. Allow [hr layers to separate. Drain the chloroform layer containing t hr lead dlthitonato Into c clean, dry lest tube, and corV the tube iedlately. 3.30 Decant thin solution carefully Into a dry phM <>r' t i lube leaving the water behind. If any war.or apotw are vhM ]c in the optical light path, transfer again to another phot o t k 't er tube . 3.11 Set the spctrophotoftetor at a wavelength of 910 on.. 3.12 5t the lnstrueent at i*ro absorbance* using the *t o lead ntsndsrd solution. 3.13 head the absorbances of the sanplos end of the rc'K( hi anV.. 3.1^ Calculate the load content of ruth by rrul t jpl > ii y ) abeox lan< < hy 11 * o ct nnda i d ) 7 at 1 on (which \t. th ol<[ < ' the a t puda i d 1 r nt ion plot in till lo^mri) of lead per unit < * f abfiorhance.) Subtract t he blank value fror the pinna lead <or-tont of each aac.pl* to obtain the net amount of lead expressed in micrograira. A. S'PKOAL MATKK1AI.S FOR bbOOl) SAMJ'l.INh 4.1 Vacul ai nc rt>, Becion~n 1 r V 1 tujnn , Kd. 20-rl or 10 i- ) , t otrsp 1 r 11* with stoppers arc uued for blw>-J . /irr p ] 1 n g, 7h* v .ih j UJnorr. are lined repeatedly and are lend f i r-d by t !i- t erhn 1 `jm- described pieviously. blood la i *rnovi*<l frou. tin- v k utainci and (.lie stoppciB, slier rocli use, by soaking In cold ,np wat.et . Wlu n no further visible trace of blood terrains on these Items, they are soaked overnight In the determent solution. They ore then rinsed repeatedly with hot tap water to remove alkaline timln i,,i! . The vacutnlncra are then aubjecced to the chronic and nitric arid cleaning procedure*. The stopper* are soaked for 20- to 30-mlnutc periods, three times, with single distilled water mid finally three tinea with double distilled water. The lead-freed vamtainera are dried at 105*C, fitted with clean stoppers, and Mured In s drawer reeerved for thcei. layers of cheeie-r lot h at e placed between the eeperate leyere of vacutalners and the drawer i i. sealed with masking tape to prevent the admittance of any dust. They arc evacuated Just before shipment to the field. A vscuur tester It used both In the laborstory and field tc test for lost of vacuum, which usually will not occur until steppers have >> r, used several tides, 4. 1 Vscuum Tester, High frequency, 1'lsher Cat. No. 1-17b, or equivalent. 4.3 Needles, Bee t on-Dl ck 1 neon , Gauge 20, one and one-lie): Inches In length, stainless steel, B-D No. 3200 N. As these needles are used repeatedly, check the tips for burrs by drawing then across the thumb nail. When burro develop cither discard the needles or file off the burrs. After filing, they must be if cleaned, Vscutalner needles sre sosked In a dilute detergent aolution. A Beet on-Dl ck 1 nson Needle Cleaner, No. 3200 C In ui.ed to lorcc detergent solution and subsequent rinse water through the need let*. Nccldcn orr nubj cc t rd to t hoi otigh r lnwlnj.; with dlrtilled water. They nre then placed in h i r:r 11 uhm and rltlur autoclnvrd or heated for tvo hour* in a drying oven operut i i,g at ]flO*C. The flier Stubrn nre then fitted with rubber top*.. 4.4 lit e r 1 t ubc t, , Bee t un - I' i V i iihofi , No, 3 2 f;o 1/, with rubber rapri. 4.5 Stillct* for No, 3200 N needier, 20 Cau^e, two .m-! oevrn-eight* Inches long. 4.5,1 (These CO it etna or- available Iron, the Bc m Dickinson Company, Rutherford, New Jerwey.) 5. COU.tCTINO Abb ASH2NC, M.OOb bAMJ'LKh 5.1 Collect c 10-ftil twinple oi who)* ( )<(><!. using a ).' free vucutnlnrr and a sterilized, Mninl<* 'tnl n*-rd]<'. Jr. the ] rtbor nl ory, transfer tin i.nrplr to n vMgf.r-*, ,><! Ir*-, 175-n.l bornwilicate Phillips beaker. No a ) 1'jnot i ng f,f t h i t J>r X ir i., 1 b 11 , t\, tio ; t < ! the 11 .id J /. pr se( it, ! ! < < ) <. t . Mf'l ft ni nf t lie weight of the blood Nuu.pl c to tin* lu.irrM Ci.01 gram, weighing rapidly to rlnlmjre r vpo \ ,t i (or.. Add of ashing aid acid r capon t . Add 7 nj) ii i m- lituio! n J t r 1 < ,i t J d . (Thin a wiling aystem permits the nn/ilyM to- 1 /indie u l.n j;c inndej oi r. amp 1 e /, a t a time aw the blond riot bir.iV* up r r,n! j 3 y nod *. "m >' * | lily wltbmit bun-ping and without ! ng fbe oiii'itmi! t h miI icti of the aimlyitt.) PJa<<* the i. ample/, on <i bofpl/Ue operating about 130 C and evaporate Juwt to dryness. Affei 11* < water is driven off In t tic initial evapornt loti to dryness, Veep tho bonVcr covered vitli lead-free ualchglasa to lncrcoac t he reflux action of the concentrated acid. Thla serves to w.-mh aollda dowd f row'the aldoa to the hotter rone nt the hot tow, nod alao reducaa the amount of acid needed. Cool the beaker brlefjy and than add auccaaalve portlona of the nitric acid ranging frow 7 ml down to 0.3 ml aa the aahing procaada. Do not renove the watchglaaa at any time but aeroly slide It back sufficiently to facilitate each new addition of the acid. Each time, aa aoon o h the residua becomes light colored, heat on a 400 C hotplate luct long, enough to blacken tho residue, then remove end cool the nar.ple Throughout the remainder of the anhing procedure, ultrrnately heat the aample with a few dropa of nitric acid on the 130 C hotplate and bake the rewldee for the few mlnutea required m darken It on the 400 C hotplate. Finally, the residue will pale yellow or light brown (due to Iron content) after heating for 3-10 minutes at the high temperature. Avoid exccaa b.rkln,; .1 thla stage, aa the oah will become dreotrpoaed to a difficulty soluble form. It la now ready for Bolutlon and analysln. Kcpcrt result a aa mllllgrama of lend per 100 gramn of whole blood. 6. COLLECT INC AND ASHING UR INK SAMPLES 6.1 Use lead-free, narrow-mouthed, reagent-type, boror.lll- cate, 230-ml bottlea provided with standard taper r Ibh h ttopprni to collect grab namplee of urine. Add 2.0 ml of a 371 formalin solution aa a preservative, shaking the bottle 10-12 timet, after the contribution of the urine to mix the specimen with the -)(>- formalin thoroughly* 6,1.1 Alternatively, urine spec 1 orm, may be rolled*- in 125-rol polyct hylcnn bottle*; containing . preaervativ* J 00- 200 nig of hDTA (acid f o t tn) per bottle. Ihjf. 1 r, convenient and r r on(iml c n 1 f or h 1 p p 1 np, a amp lea ronf; 1 d r i n 1) 1 r b 1 f. t a ?tc r \ . f.,2 If f be mine ample 1. clear arid only one or tv;.- d.iy old, mriihurc a f>0 ml portion Into a ginduntdi cylinder. }!ovev-:, If the aample is older, much ot the lead may be *n a aedind.t or on the walla of the bottle and runt be dissolved before aliquot ir Transfer the entire spec imon to a glata-Glopperr d graduated ryllnder, record the volune, rinse the nanplc bottle v/ltl three ecjill portions of eonrentratre) nitric acid and add t.lveae rinr.Jnga to the cylinder. Klx thoroughly (Caution! Old >anph: r.ay loan, over.) Note the total volume and i mnvc .in equivalent to Vj r] of mine for .inn I y u 1 c . 11 .-urd c? the a ) i *, ' ' portion to a lead-free, hoi oi* i ] j < .it e i'hljllps be.tWr add !i t t 3 of redial 11 led i mu n,; i /iin! n I l r 1 r a i J <! . J v .ipi .i ,, t . Joel to dryness on a hotplate updating at about 110 (. ( ou ` , add sufficient nitric arid to noialen the rn. and cover tin beaker with a lead-free vatrhghiRH. Heat on the IK) C hotplate and then alternately bake for a lew minuter* am! dlgeM wltli minimal atmnmta of nitric acid (no drr,ti Jbr<; jn t ) m ..idling, rolhod lot h 1 uod ) im! I ) a wli 1 t r* f, J d ue l <-n;i 1 nr. .11 t * i the final hiding for V-wl minute?* at the high t enipe' n t or * . `Jhe aample Is. now ready for nolutlon and amilyeie. Report roMilts nn ml 1 1 1 j;r a u ? of lend per liter of urine. 7. PROCEDURE FOR AIR SAKTLES 7.1 It la convanlent to wash out eantplc<i in electrost.-iiie precipitator tubes with redistilled ethanol, uaing n special policeman made with a rubber disc cut to fit the tube like a plat on, and tranaferring the sample through a short icon funnel Into a 250-ml Ph 111 ip- beaker; gontly evaporate Just do dryness, (Ethanol la helpful In removing greauy deposits on the wnlh of the precipitator tube. Some chemlets may prefer hot 1 to 52 nitric acid to transfer the sample.) Transfer Implngcr samplei. or membrane filter samplea to Phillips beakers. If little nr.h la expected (usually for Impfnger or membrane filter samples), add 2 ml of sailing aid acid reagent. (The presence of this unit will prevent Iona of lead by glaring onto the surface of the beaker during ashing.) Othcrvlte add 1-2 ml nitric odd. Evaporate to dryness. Continue ashing vlth nitric acid nt s nodcrate hint until organics ore destroyed. 7.2 Dissolve the ash in 2 ml of concentrated nitric old and distilled voter and then tronsfer quantitatively to n 100-r.l volumetric flash and make to mark. Pipct n suitable aliquul into a separatory funnel, containing about 5 ml of doublo-d 1 st 111 < <1 water, add sufficient additional doublc-dio1111ed water to rake the total volume about 25 oil, and apply the Analytical Procedure, starting with step 2. In step 3, an the sample is already in u separatory funnel, oxtroly add the cyanide. The amount of lend present In the aliquot may be estimated as described in Step (>. If it io leas than a few mlcrograam, an additional allquol may be by, ; ' i ;=. ,-v: * VvI'--; LIA13701 -1B- oddrd to tlit same funnel, and the )i!l rendj out rd with inonil.i. The cxi r /if t lo.i la then continued, and extract i, <<>rl.loii! wit! t !i< collected previously In the second lunncl. 1! llir < 1.1 ! m.'i t < a mount of loud cxccedn the range of the mctlu.d (?') c.li rri;r."" l , an aliquot as described In Hole 2, ntep ft. 7.3 When calculating the results, moke allowance lot t).< totnl number of allquotu. If convenient, aliquot the reo/.uri blank In the same manner o that the correction represent i. tl.e same nnountu of nohlng and extractfor. reagents an arc pro: < nt in the sample. However, the blank correetlon Is usually i.n.il 1 for air aanplcs. Report results as mllllgraes of lend pet (n!.n meter of air.