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: