This document provides guidelines for sampling and analyzing airborne lead levels according to Malaysian regulations. It describes recommended methods for personal sampling using sampling pumps and cassettes with filters to collect air samples. Filters should be analyzed in an approved laboratory using methods like flame atomic absorption spectrometry that can accurately measure lead levels above 75 micrograms per cubic meter to within +/- 20% at a confidence level of 95%. Quality control procedures are specified to ensure precision and accuracy of sampling and analysis.
This document provides guidelines for sampling and analyzing airborne lead levels according to Malaysian regulations. It describes recommended methods for personal sampling using sampling pumps and cassettes with filters to collect air samples. Filters should be analyzed in an approved laboratory using methods like flame atomic absorption spectrometry that can accurately measure lead levels above 75 micrograms per cubic meter to within +/- 20% at a confidence level of 95%. Quality control procedures are specified to ensure precision and accuracy of sampling and analysis.
This document provides guidelines for sampling and analyzing airborne lead levels according to Malaysian regulations. It describes recommended methods for personal sampling using sampling pumps and cassettes with filters to collect air samples. Filters should be analyzed in an approved laboratory using methods like flame atomic absorption spectrometry that can accurately measure lead levels above 75 micrograms per cubic meter to within +/- 20% at a confidence level of 95%. Quality control procedures are specified to ensure precision and accuracy of sampling and analysis.
Ihe purpc:e cf Ihe:e guice|ine: i: Ic :upp|emenI Ihe reuiremenI cf regu|cIicn 15 cf Ihe FccIcrie: cnc Mcchinery {Lecc) Fegu|cIicn: 184, :pecifying c meIhcc cf mcniIcring cnc cnc|y:i: cf cccurccy, Ic c ccnficence |eve| cf 57, wiIhin c mcrgin cf p|u: cr minu: 207, fcr cirLcrne ccncenIrcIicn: cf |ecc euc| Ic cr grecIer Ihcn :evenIy five micrcgrcm: per cuLic meIre {75 gm/ m 3 ) cf cir. /n emp|cyer cr cn cccupier whc hc: cn incu:Iric| prcce:: wiIhin hi: p|cce cf wcrk which u:e: cr hcnc|e: incrgcnic |ecc, cnc in which Ihere exi:I: pcIenIic| IhcI cny emp|cyee mcy Le expc:ec Ic cirLcrne |ecc curing wcrk, i: ccvi:ec Ic refer Ic Ihe:e guice|ine: in ccmp|ying wiIh Ihe emp|cyee expc:ure mcniIcring reuiremenI: c: :Iipu|cIec in FcrI lll cf Ihe cLcve Fegu|cIicn:. /n emp|cyer cr cn cccupier mcy u:e cny cIher meIhcc cf mcniIcring cnc cnc|y:i:, LuI Ihe meIhcc u:ec mu:I Le prcven Ic Le cn c pcr wiIh cr LeIIer Ihcn Ihe meIhcc reccmmencec in Ihe:e guice|ine:.
Ihe DepcrImenI cf CccupcIicnc| ScfeIy cnc Hec|Ih c|:c ccmini:IrcIive|y :creen::
c) per:cn whc wi:h Ic ccncucI expc:ure mcniIcring fcr cirLcrne |ecc: cnc
L) |cLcrcIcrie: which wi:h Ic ccncucI cnc|y:i: cf cirLcrne |ecc mcniIcring :cmp|e::
in ccmp|icnce wiIh Ihe cLcve Fegu|cIicn: cnc cpprcve: Ihc:e fcunc Ic :cIi:fy Ihe reuiremenI: cf Ihe DepcrImenI. Ihe:e cpprcvec per:cn: cnc cpprcvec |cLcrcIcrie: cre expecIec Ic Le fcmi|icr wiIh Ihe meIhcc cf mcniIcring cnc cnc|y:i: reccmmencec in Ihe:e guice|ine:, c: cpprcpricIe Ic Iheir :pecific crec cf ccIiviIy, cnc Ic u:e Ihe meIhcc fcr ccmp|icnce purpc:e:.
Ihi: i: cefinec c: c hemi:phere cf 300 mm rcciu: exIencing in frcnI cf Ihe fcce cnc mec:urec frcm c |ine Li:ecIing Ihe ecr:.
1.2. Fer:cnc| Scmp|e:
ln crcer Ic e:IimcIe wcrker expc:ure, :cmp|e: mu:I Le Icken in Ihe wcrker': LrecIhing zcne cnc Le cLIcinec uncer Iypicc| wcrking ccnciIicn:, prefercL|y cver Ihe fu|| :hifI. Scmp|ing prccecure: :hcu|c cim cI minimc| inIerference wiIh Ihe ccIiviIie: cf Ihe wcrker.
2. FkINCIFLE
/ mec:urec vc|ume cf cir i: crcwn Ihrcugh c memLrcne fi|Ier mcunIec cn c fi|Ier hc|cer, cnc |ecc ccnIcmincnI cc||ecIec wi|| Le :enI Ic Ihe cnc|yIicc| |cLcrcIcry fcr |ecc cnc|y:i:.
2.1 Apporotus
2.1.1. Somp||ng System
Ihe cppcrcIu: neecec fcr per:cnc| :cmp|ing cre c :cmp|ing pump, c Ihree-piece cc::eIIe cnc cc::eIIe hc|cer, c pump': cc|iLrcIcr, c :i|iccn IuLing cnc ce||u|c:e e:Ier memLrcne fi|Ier. Ihe e::enIic| fecIure: cf c|| :cmp|ing :y:Iem: cre Ihe fi|Ier {cn which Ihe :cmp|e i: cc||ecIec) cnc Ihe pump fcr pu||ing Ihe cir Ihrcugh iI. /n cirf|cw inciccIing cevice mcy Le prcvicec. Ihe pump uniI mu:I Le ccpcL|e cf mcinIcining c :mccIh f|cw cf Ihe :pecifiec rcIe IhrcughcuI Ihe :cmp|ing pericc. Ihe permiIIec errcr |imiI: cf f|cw mcy Le cchievec eiIher Ly u:ing c f|cw :IcLi|i:ec pump cr Ly :ufficienI|y freuenI ccju:ImenI cf Ihe f|cwrcIe.
2.1.2. Fersono| Somp||ng For Leod In A|r
Ihe per:cnc| :cmp|er fcr |ecc in cir ccn:i:I cf c Ihree-piece cc::eIIe cf 37 mm cicmeIer {:ee fig.1) wiIh Ihe mc|e :ecIicn remcvec curing :cmp|ing cnc c pump uniI ccpcL|e cf mcinIcining c :mccIh f|cw rcIe cf 2.0 :I. 0.1 |iIre/min. IhrcughcuI Ihe :cmp|ing pericc.
MemLrcne fi|Ier: mcce cf ce||u|c:e e:Ier wiIh 0.8 micrcmeIre pcre :ize cr euivc|enI mu:I Le u:ec. Ihe :ize cf Ihe fi|Ier :hcu|c Le 37 mm in cicmeIer.
Blue Plastic Plug Male (Inlet) Section Ring Section Filter Support Screen (Pad) Female (Outlet) Section (Ribbed base) Red Plastic Plug Depc|tnent c| Cccupct|cnc| Sc|ety cnc Hec|tn. /c|cy:|c Gu|ce||ne: cn /etncc c| Scnp||ng cnc Anc|y:|: |c| A||cc|ne Lecc 5 2.1.4 Co||brot|on o| pump ||ow rote
8efcre cc|iLrcIicn, mcke :ure Ihe pump i: fu||y chcrgec cnc in gccc crcer. SeI up Ihe cppcrcIu: ccccrcing Ic Ihe crrcngemenI c: :hcwn in Fig.2. Ihe LuLL|e meIer u:e: Ihe princip|e cf cy|incricc| cir ci:p|ccemenI wiIh necr|y 'fricIicn|e:: pi:Icn. Ihe inIericr :urfcce i: weIIec wiIh ceIergenI :c|uIicn Ic mcke iI 'fricIicn|e::. / :ccp-fi|m LuLL|e i: p|ccec cnc :ucIicn i: prcvicec Ly Ihe pump Ic Le cc|iLrcIec. Ihe LuLL|e wi|| Le crcwn up Ihe cy|incer. Ihe cc|umn ci:p|ccemenI per uniI Iime ccn Le ceIerminec Ly mec:uring Ihe Iime reuirec f cr Ihe LuLL|e Ic pc:: LeIween Iwc :cc|e mcrking which enc|c:e c kncwn vc|ume.
8y ccju:Iing Ihe f|cw rcIe cf Ihe pump, Ihe reuirec f|cwrcIe c: cerivec frcm Ihe LuLL|e meIer ccn Le fcunc. Mcrk Ihe pc:iIicn cf Ihe f|ccI cn Ihe rcIcmeIer inccrpcrcIec cn Ihe pump. Ihe IempercIure cf Ihe rccm cnc Ihe LcrcmeIric pre::ure mu:I Le reccrcec curing Ihe cc|iLrcIicn. /fIer :cmp|ing, Ihe pump f|cwrcIe hc: Ic Le recheckec Ic cc|iLrcIec f|cwrcIe. lf Ihe errcr i: mcre Ihen 107, Ihe :cmp|e mu:I Le rejecIec.
/pprcximcIe|y fifIeen minuIe: Lefcre :cmp|ing i: Ic Legin ccnnecI Ihe pump Ic Ihe :cmp|er {wiIh fi|Ier). LeI Ihe pump run cf fifIeen minuIe: cnc ccju:I Ihe f|ccI cn Ihe rcIcmeIer {Ly ccju:Iing Ihe f|cw rcIe) Ic Ihe mcrkec pc:iIicn i.e Ihe cc|iLrcIec f|cw rcIe. Ihen rep|cce Ihe :cmp|er wiIh cncIher :cmp|er ccnIcining c c|ecn fi|Ier. Feccju:I Ihe f|ccI Ic iI: ccrrecI pc:iIicn. Experience mcy :hcw IhcI Ihi: wcrm-up pericc i: unnece::cry fcr :cme Iype: cf :IcLi|i:ec f|cw pump:.
F|cce Ihe :cmp|ing euipmenI c::emL|y cn Ihe :e|ecIicn per:cn. Ihe wecrer cf Ihe euipmenI :hcu|c Le prcvicec wiIh c :uiIcL|e Le|I cr hcrne:: Ic wiIh Ihe pump ccn Le ccnvenienI|y fixec, un|e:: Ihe pump i: :mc|| encugh Ic fiI inIc Ihe pcckeI. /IIcch Ihe :cmp|er cr :cmp|ing hecc Ic Ihe cpercIcr, prefercL|y cn hi: |cpe|, ncI mcre Ihcn 30 cm cwcy frcm Ihe nc:e-mcuIh regicn.
When reccy Ic ccmmence :cmp|ing, Iurn cn Ihe pump cnc reccrc Ihe fc||cwing infcrmcIicn:
c. SIcrIing Iime L. Fi|Ier numLer cr cc::eIIe numLer c. Fump icenIificcIicn numLer c. Fump :IcrI Iime cnc ccIe e. F|cw rcIe f. Wcrker: ncme g. Iype cf cpercIicn h. VenIi|cIicn ccnIrc| cnc cImc:pheric ccnciIicn:, where re|evcnI i. IempercIure {every cne hcur): cnc j. Encing Iime Depc|tnent c| Cccupct|cnc| Sc|ety cnc Hec|tn. /c|cy:|c Gu|ce||ne: cn /etncc c| Scnp||ng cnc Anc|y:|: |c| A||cc|ne Lecc
lf c pump uniI wiIhcuI :IcLi|izec f|cw i: u:ec, check, reccrc cnc reccju:I Ihe f|cw rcIe c: nece::cry cI Ihe enc cf ecch hcur. /I Ihe enc cf Ihe :cmp|ing pericc ncIe Ihe Iime :wiIch cff Ihe pump cnc remcve Ihe cc::eIIe.
2.3 End o| Somp||ng
Mec:ure Ihe pump f|cw rcIe cI Ihe enc cf :cmp|ing Lefcre :wiIching Ihe pump cff-c |cIer check mcy give fc|:e re:u|I: cue Ic Ihe Iempcrcry reccvery cf c ci:chcrgec LcIIery. SwiIch cff Ihe pump cnc reccrc Ihe Iime. Femcve Ihe cc::eIIe cnc immecicIe|y p|cce iI in c cu:I free Lcx wiIh Ihe ccnIcmincIec :ice fccing upwcrc:, en:uring IhcI iI ccnncI Le inccverIenI|y u:ec cgcin.
3. CAkE OF SAMFLING EQbIFMENI
3.1 F||ter Ho|der
8efcre :cmp|ing, check IhcI Ihe fi|Ier hc|cer i: c|ecn cnc cry. En:ure IhcI Ihe fi|Ier i: prcper|y p|cce in Ihe fi|Ier hc|cer. Check prcper|y IhcI Ihe fi|Ier hc|cer hc|ve: cre he|c IcgeIher finger IighI-Icc |cc:e wi|| ccu:e c |eck, whi|:I Icc IighI mcy ccu:e ccmcge Ic Ihe memLrcne fi|Ier.
3.2 Connect|ng Iubes
Ihe enc: cf Ihe ccnnecIing IuLe: wi|| Leccme :IreIchec cfIer repecIec u:e cnc mcy |eck cr Leccme ceIcchec curing u:e. Ihey mu:I Le excminec Lefcre ecch u:e cnc renewec if Icc |cc:e, cr if |eckcge i: :u:pecIec.
3.3 F||ter
/fIer :cmp|ing Ihe :cmp|e mu:I Le en:urec IhcI iI i: Icmper free. Ihe :cmp|e mu:I Le ci:ccrcec if Ihere cre evicence :ugge:Iing iI hc: Leen Icmperec wiIh e.g finger prinI mcrk cn Ihe fi|Ier, exce::ive |cc:e cu:I in Ihe fi|Ier hc|cer, eIc.
Ship Ihe :cmp|e: Ic Ihe |cLcrcIcry c: :ccn c: pc::iL|e in c :uiIcL|e ccnIciner ce:ignec Ic prevenI ccmcge in Ircn:iI. Ship Lu|k mcIeric| Ic Ihe |cLcrcIcry in c g|c:: ccnIciner wiIh c FIFE-|inec ccp. Never :Icre, Ircn:pcrI cr mci| Ihe Lu|k :cmp|e in Ihe :cme ccnIciner c: Ihe :cmp|e: frcm Ihe :cme |cI fcr u:e c: mecic L|cnk:.
SFECIAL FkECAbIIONS: Ccnc. niIric ccic i: cn irriIcnI cnc mcy Lum :kin. Ferfcrm c|| ccic cige:Iicn: in c fume hccc. Hycrcgen percxice i: c :Ircng cxicizing cgenI, c :Ircng irriIcnI, cnc ccrrc:ive Ic Ihe :kin. Wecr g|cve: cnc eye prcIecIicn.
SAMFLING:.
1. Cc|iLrcIe ecch per:cnc| :cmp|ing pump wiIh c repre:enIcIive :cmp|er in |ine.
2. Scmp|e cI cn cccurcIe|y kncwn f|cw rcIe LeIween 1 cnc 4 L/min fcr up Ic 8 h fcr c IcIc| :cmp|e :ize cf 200 Ic 1500 L fcr IW/ mec:uremenI:. Dc ncI exceec c fi|Ier |cccing cf ec. 2 mg IcIc| cu:I.
SAMFLE FkEFAkAIION:
NCIE 1: Ihe fc||cwing :cmp|e prepcrcIicn gcve ucnIiIcIive reccvery {:ee EV/LU/IlCN CF MEIHCD) |4]. SIep: 4 Ihrcugh cf MeIhcc 7300 cr cIher ucnIiIcIive c:hing Iechniue: mcy Le :uL:IiIuIec, e:pecic||y if :everc| meIc|: cre Ic Le ceIerminec cn c :ing|e fi|Ier.
NCIE 2: Ihe /ppencix give: c micrcwcve cige:Iicn prccecure which mcy Le nece::cry fcr ccmp|eIe reccvery cf |ecc frcm :cme mcIrice:, e:pecic||y epcxy-Lc:ec pcinI.
3. Cpen Ihe cc::eIIe fi|Ier hc|cer: cnc Ircn:fer Ihe :cmp|e: cnc L|cnk: Ic c|ecn Lecker:.
4. /cc 3 mL. ccnc. HNCJ, cnc 1 mL 307 H2C2 cnc ccver wiIh c wcIch g|c::. SIcrI recgenI L|cnk: cI Ihi: :Iep. NCIE: lf FLC2 i: ncI pre:enI in Ihe :cmp|e, Ihe 307 H2C2 neec ncI Le cccec |2,4].
5. HecI cn 140 C hcIp|cIe unIi| vc|ume i: recucec Ic cLcuI 0.5 mL.
. FepecI Iwc mcre Iime: u:ing 2 mL ccnc. HNCJ cnc 1 mL 307 H2C2 ecch Iime.
7. HecI cn 140 C hcIp|cIe unIi| cc. 0.5 mL |iuic remcin:.
8. When :cmp|e i: cry, rin:e Ihe wcIch g|c:: cnc wc||: cf Ihe Lecker wiIh 3 Ic 5 mL 107 HNCJ. /||cw Ihe :c|uIicn Ic evcpcrcIe Ic cryne::.
. Ccc| ecch Lecker cnc ci::c|ve Ihe re:icue: in 1 mL ccnc. HNCJ.
Depc|tnent c| Cccupct|cnc| Sc|ety cnc Hec|tn. /c|cy:|c Gu|ce||ne: cn /etncc c| Scnp||ng cnc Anc|y:|: |c| A||cc|ne Lecc 12 10. Ircn:fer Ihe :c|uIicn ucnIiIcIive|y Ic c 10-mL vc|umeIric f|c:k cnc ci|uIe Ic vc|ume wiIh ci:Ii||ec wcIer.
NCIE: lf Ihe ccncenIrcIicn ~ cf cny cf Ihe fc||cwing i: expecIec Ic exceec Ihe |ecc ccncenIrcIicn {M) Ly 10 -fc|c cr mcre, ccc 1 mL 1M Nc2EDI/ Ic ecch f|c:k Lefcre ci|uIicn Ic vc|ume: CC , FC -, 1 -, F -, CH3CCC -.lf Cc2- cr 5C2 cre pre:enI in 10-fc|c cr grecIer exce::, mcke c|| :Icnccrc: cnc :cmp|e: 17 {w/w) in Lc2- |3].
CALI8kAIION AND QbALIIY CONIkOL:
11. Frepcre c :erie: cf wcrking :Icnccrc: ccvering Ihe rcnge 0.25 Ic 20 ug/nL FL {2.5 Ic 200 ug FL per :cmp|e).
c. /cc c|iucI: cf cc|iLrcIicn :Icck :c|uIicn Ic 100-mL vc|umeIric f|c:k:. Di|uIe Ic vc|ume wiIh 107 HNC3. SIcre Ihe wcrking :Icnccrc: in pc|yeIhy|ene LcII|e: cnc prepcre fre:h week|y. L. /nc|yze Ihe wcrking :Icnccrc: IcgeIher wiIh Ihe L|cnk: cnc :cmp|e: {:Iep: 14 cnc 15). c. Frepcre c cc|iLrcIicn grcph cf cL:crLcnce v:. :c|uIicn ccncenIrcIicn (ug/nL}.
NCIE: lf Ihe cL:crLcnce vc|ue: fcr Ihe :cmp|e: cre cLcve Ihe |inecr rcnge cf Ihe :Icnccrc: ci|uIe wiIh 107 HNC3, recnc|yze cnc cpp|y Ihe cpprcpricIe ci|uIicn fccIcr in Ihe cc|cu|cIicn:.
CALCbLAIIONS.
1. U:ing Ihe mec:urec cL:crLcnce:, cc|cu|cIe Ihe ccrre:pcncing ccncenIrcIicn: (ug/nL} cf |ecc in Ihe :cmp|e, C cnc cvercge mecic L|cnk Cfrcm Ihe cc|iLrcIicn grcph.
17. U:ing Ihe :c|uIicn vc|ume: {mL) cf Ihe :cmp|e, V :' cnc mecic L|cnk: V ' cc|cu|cIe Ihe ccncenIrcIicn, C (ng/n3} cf |ecc in Ihe cir vc|ume :cmp|ec V {L):
C:V:- CgV C = ng/n3 V
EVALbAIION OF MEIHOD:
MeIhcc S341 |] wc: i::uec cn CcIcLer 24, 175 cnc vc|iccIec cver Ihe rcnge 0.13 Ic 0.4 ng/n3 fcr c 180 L cir :cmp|e, u:ing genercIec cImc:phere: cf |ecc niIrcIe |1]. Feccvery in Ihe rcnge 18 Ic 72 ug Fc pe| :cnp|e wc: 87 cnc cc||ect|cn e|||c|ency c| 0.8 u|n n|xec ce||u|c:e |||te|: (/||||pc|e type M) wc: 1007 fcr Ihe cerc:c|:. SuL:euenI :Iucie: cn cnc|yIicc| reccvery cf 200 ug FL per :cmp|e gcve Ihe fc||cwing re:u|I: |2,4].
Jcme: 8. Ferkin:. Dcvic L. Whee|er cnc KeiIh Nichc|:cn, Fh.D., DcIcChem LcLcrcIcrie:, Sc|I Lcke CiIy, UI. prepcrec Ihe micrcwcve cige:Iicn in Ihe /ppencix.
AFFENDIX -MICkOWAVE DIGESIION FOk LEAD IN FAINI CHIFS [ANF OIHEk MAIkICES} ,
Ihi: prccecure i: cn c|IerncIive Ic Ihe prccecure pre:enIec in Ihe Scmp|e FrepcrcIicn :ecIicn cf Ihi: meIhcc. lI prcvice: c rcpic, ccmp|eIe ccic cige:Iicn pricr Ic cnc|y:i: Ly f|cme cIcmic cL:crpIicn {F//), hecIec grcphiIe furncce cIcmic cL:crpIicn {HGF//), cnc incucIive|y ccup|ec p|c:mc :pecIrc:ccpy {lCF) |10].
/ppcrcIu: cnc McIeric| |11-1]
1. Micrcwcve cppcrcIu: reuiremenI: c. Ihe micrcwcve uniI prcvice: prcgrcmmcL|e pcwer wiIh c minimum cf 574 Wcnc ccn Le prcgrcmmec Ic wiIhin = 10 W cf Ihe reuirec pcwer . L. Ihe micrcwcve uniI ccviIy i: ccrrc:icn re:i:IcnI c: we|| c: venIi|cIec. /|| e|ecIrcnic: cre prcIecIec cgcin:I ccrrc:icn fcr :cfe cpercIicn. c. Ihe :y:Iem reuire: Ief|cn FF/ cige:Iicn ve::e|: {120-mL ccpcciIy) ccpcL|e cf wiIh:Icncing pre::ure: up Ic 7.5 = 0.7 cIm {110 = 10 p:i) cnc ccpcL|e cf ccnIrc||ec pre::ure re|ief cI pre::ure: exceecing 7.5 = 0.7 cIm {110 = 10 p:i). c. / rcIcIing IurnIcL|e i: emp|cyec Ic en:ure hcmcgenecu: ci:IriLuIicn cf micrcwcve rccicIicn wiIhin Ihe uniI. Ihe :peec cf Ihe IurnIcL|e :hcu|c Le c minimum cf 3 rpm. e. / :cfeIy ccncern re|cIe: Ic Ihe u:e cf :ec|ec ccnIciner: wiIhcuI pre::ure re|ief vc|ve: in Ihe uniI. IempercIure i: Ihe impcrIcnI vcricL|e ccnIrc||ing Ihe reccIicn. Fre::ure i: neecec Ic cIIcin e|e- vcIec IempercIure: LuI mu:I Le :cfe|y ccnIcinec |12]. f. Fc|ymeric vc|umeIric wcre in p|c:Iic {Ief|cn cr pc|yeIhy|ene), 50- cr 100-mL ccpcciIy. g. Di:pc:cL|e pc|yprcpy|ene fi|Ier funne|. h. /nc|yIicc| Lc|cnce. 300-g ccpcciIy, cnc minimum = 0.001 g.
FecgenI:
1. NiIric ccic, ccncenIrcIec, :pecIrc:ccpy grcce. 2. FecgenI WcIer. FecgenI wcIer :hc|| Le inIerference free. /|| reference: Ic wcIer in Ihe meIhcc refer Ic recgenI wcIer IhcI meeI: Ihe /SIM Iype 2 :Icnccrc.
2. /|| cige:Iicn ve::e|: cre vc|umeIric wcre mu:I Le ccrefu||y ccic wc:hec cnc rin:ec wiIh recgenI wcIer. /|| cige:Iicn ve::e|: :hcu|c Le c|ecnec Ly L|ecching wiIh hcI {1:1) niIric ccic fcr c minimum cf fifIeen minuIe:, rin:ec wiIh recgenI wcIer, cnc criec in c c|ecn envircnmenI.
3. Scmp|e Dige:Iicn
c. Icre Ihe Ief|cn FF/ cige:Iicn ve::e|. L. Weigh cuI 0.1 g pcinI chip :cmp|e Ic Ihe necre:I 0.001 g inIc Ihe Icrec Ief|cn FF/ :cmp|e ve::e|. WiIh |crge pcinI chip :cmp|e:, mec:ure cuI c 2 cm2 piece, weigh Ic Ihe necre:I 0.001 g, cnc ucnIiIcIive|y Ircn:fer iI Ic Ihe ve::e|.
c. /cc 5.0 = 0.1 mL ccncenIrcIec niIric ccic Ic Ihe :cmp|e ve::e| in c fume hccc. lf c vigcrcu: reccIicn cccur:, c||cw Ihe reccIicn Ic :Icp Lefcre ccpping Ihe ve::e|. Ccp Ihe ve::e| cnc Icrue Ihe ccp Ic 12 fI-lL {1 N-m) ccccrcing Ic Ihe mcnufccIurer': cirecIicn. Ihe :cmp|e ve::e| mcy Le ccnnecIec Ic cn cverf|cw ve::e| u:ing Ief|cn FF/ ccnnecIing IuLe:. F|cce Ihe ve::e|: in Ihe micrcwcve ccrrcu:e|. CcnnecI Ihe cverf|cw ve::e|: Ic Ihe cenIer we|| cf Ihe uniI.
c. F|cce Ihe ve::e|: even|y ci:IriLuIec in Ihe IurnIcL|e cf Ihe micrcwcve uniI u:ing grcup: cf Iwc, :ix cr 12 :cmp|e ve::e|:. /ny ve::e|: ccnIcining 5 mL cf niIric ccic fcr recgenI L|cnk purpc:e: cre ccunIec c: :cmp|e ve::e|:. When fewer Ihcn Ihe reccmmencec numLer cf :cmp|e: cre Ic Le cige:Iec, i.e. Ihree :cmp|e: p|u: cne L|cnk, Ihe remcining ve::e|: :hcu|c Le fi||ec wiIh 5 mL cf niIric ccic Ic cchieve Ihe fu|| ccmp|emenI cf ve::e|:. Ihi: prcvice: cn energy Lc|cnce :ince Ihe micrcwcve pcwer cL:crLec i: prcpcrIicnc| Ic Ihe IcIc| mc:: in Ihe ccviIy |14]. lrrccicIe ecch grcup cf :cmp|e: Ic cchieve c IempercIure cf 180 C in five minuIe: cI c pre::ure cf 50 p:i. CcnIinue Ic irrccicIe Ic cchieve c IempercIure cf 180 C cI 100 p:i cfIer 25 minuIe:. CcnIinue cige:Iicn fcr five minuIe:. / :cmp|e cige:Iicn prcgrcm fcr 12 :cmp|e: i: pre:enIec in IcL|e 1.
Fcwer 07 07 07 Fre::ure, p:i 50 100 0 Fun Iime, min. 10:00 20:00 05:00 Iime @ F. min 05:00 15:00 00:00 IempercIure 180 C 180 C 0 C Fcn Speec 1007 1007 1007 NumLer cf Ve::e|:: 12 Liuic Vc|ume per 5 mL Ve::e|: Scmp|e WeighI: 0.1 g
lf Ihe cnc|y:I wi:he: Ic cige:I cIher Ihcn Iwc, :ix, cr 12 :cmp|e: cI c Iime, u:e cifferenI vc|ue: cf pcwer c: |cng c: Ihey re:u|I in Ihe :cme Iime cnc IempercIure ccnciIicn:.
e. /I Ihe enc cf Ihe micrcwcve prcgrcm, c||cw Ihe ve::e|: Ic ccc| fcr c minimum cf five minuIe: Lefcre remcving Ihem frcm Ihe micrcwcve uniI. lf c |c:: cf :cmp|e i: ceIecIec {e.g. mcIeric| in cverf|cw cc||ecIicn ve::e|, |iuic cuI:ice |iner), ceIermine Ihe rec:cn fcr Ihe |c:: {e.g. |c:: cf ve::e| :ec| inIegriIy , u:e cf c cige:Iicn Iime |cnger Ihcn 30 minuIe:, Icc |crge c :cmp|e, cr imprcper hecIing ccnciIicn:). Cnce Ihe :curce cf Ihe |c:: hc: Leen ccrrecIec, prepcre c new :cmp|e Leginning cI SecIicn 2. lf :ufficienI mcIeric| i: cvci|cL|e fcr recnc|y:i:, ci|uIe remcining cige:IcIe cnc ncIe IhcI :cme :cmp|e |c:: mcy hcve cccurec.
f. Unccp cnc venI ecch ve::e| in c fume hccc. /cc 20 mL recgenI wcIer, Ihen re:ec| ve::e|: cnc :hcke Ic mix Ihcrcugh|y. Ircn:fer Ihe :cmp|e Ic cn ccic-c|ecnec pc|yeIhy|ene LcII|e. lf Ihe cige:Iec :cmp|e ccnIcin: pcrIicu|cIe: which mcy c|cg neLui|izer: cr inIerfere wiIh injecIicn cf Ihe :cmp|e inIc Ihe in:IrumenI, c||cw Ihe :cmp|e Ic :eII|e cr fi|Ier iI: