Intshayelelo kwiPellet Pressing kuHlalutyo lweXRF
Ukucinezela iipellet kusebenza njengeyona ndlela iphambili kwinkqubo yokulungiselela isampuli ye-X-ray fluorescence spectroscopy (XRF). I-XRF yindlela yohlalutyo lwezinto ezisisiseko apho isampuli ivezwa kwii-X-rays ezinamandla aphezulu, nto leyo ebangela ukuba ii-athomu zikhuphe ii-X-rays zesibini, ezi-element-specific fluorescent. I-spectrometer ifumanisa kwaye ilinganise le mveliso, ivumela uvavanyo olukhawulezileyo, oluneziqalelo ezininzi kwiisampuli eziqinileyo, ezingamanzi, nezinomgubo.
Ukulungiswa kwepellet ecinezelweyo kuqinisekisa ukuba iisampulu zomgubo zihlanganiswa zibe ziidiski ezixineneyo nezifanayo. Le ndlela inciphisa izithuba zomoya kunye noburhabaxa bomphezulu, obunokuthi—ukuba abulungiswanga—bufunxe okanye busasaze ii-X-ray, nto leyo ephazamisa ukuchaneka kohlalutyo. Xa iipowders zicinezelwe kwiipellets, indlela ye-X-ray edlula kwisampulu iba nozinzo kwaye iphindaphindwe, nto leyo evumela ukuba kubekho ukulinganiswa okuchanekileyo kwezinto kunye novakalelo oluphuculweyo, ngakumbi kwizinto ezikhanyayo ezifana ne-magnesium okanye i-silicon.
Iziseko zeendlela zokulungiselela i-Pellet
Iindlela zokulungiselela iPellet
In i-x-ray fluorescence spectroscopy (XRF), ukuthembeka kwesampulu kunye nokuhambelana ngokuchanekileyo kumisela ngokuthe ngqo ukuchaneka kohlalutyo kunye nokuzala kwakhona. Indlela nganye yokulungiselela ipellet—umgubo ococekileyo, i-fused bead, kunye nepellet ecinezelweyo—inika iingenelo kunye neengxaki ezahlukeneyo ezifanelekileyo kwiimfuno ezahlukeneyo zohlalutyo.
Iindlela zepellet ezicinezelweyo zisetyenziswa kakhulu kuba zilinganisa ukuchaneka nokusebenza kakuhle. Ngokuhlanganisa iipowder zesampulu ezicoliweyo kakuhle zibe ziipellet ezithambileyo nezingenamsebenzi, ezi ndlela zinciphisa ukungafani kwaye zinciphise ukusasazeka kwemvelaphi, okubaluleke kakhulu xa kuchongwa izinto ezikhanyayo. Iiprotokholi zelebhu zicebisa ukusebenzisa ubungakanani beeparticle ezifanayo, ngesiqhelo ezingaphantsi kwama-50 µm, ukwandisa ukulingana kwesampulu ngexesha lokucinezela nokuthintela ukungangqinelani kobuzwe bokulinganisa. Nangona kunjalo, iiparticles ezingalinganiyo ngokwaneleyo okanye ukucinezelwa okungafanelekanga kunokubeka emngciphekweni ukuthembeka kwepellet, okukhokelela ekuqhekekeni okanye ekuphindaphindeni okubi kuhlalutyo lwezinto ezilandelelanayo.
Iindlela zomgubo ococekileyo, nangona zikhawuleza kwaye zingabizi kakhulu, zihlala zinengxaki yokwahlulwahlulwa kwamasuntswana kunye nokuguda komphezulu obuthathaka. Ezi ngxaki zibonakala njengokwanda kokusasazeka kunye nokuncipha kobuntununtunu, ngakumbi kwizinto ezikhoyo kumanqanaba aphantsi. Ngenxa yoko, ukucinezela ipowder ecocekileyo kugcinelwe ikakhulu ukuhlolwa kwangaphambili kunokuba kuhlalutywe ngobuninzi.
I-Xrf Pelletising yeesampuli eziqinileyo
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Indlela yokusebenzisa i-fused bead yoyisa iziphumo ezininzi ze-matrix ezifumaneka kwiisampuli zomgubo ngokunyibilikisa isampuli kwi-flux—edla ngokuba yi-lithium borate—kwaye yenze i-homogeneous glass bead. Le ndlela inika uzinzo olukhethekileyo lweekhemikhali kunye nokufana, okwenza ukuba ilungele uhlalutyo oluchanekileyo lwezinto ezininzi. Nangona kunjalo, imingeni esebenzayo efana nokungcola okunokwenzeka kwe-flux okanye ukuchithwa okungaphelelanga kufuna ulawulo oluqinileyo lobushushu, umlinganiselo we-flux, kunye neemeko zokuxuba. Izixhobo zokudibanisa eziphambili ezinolawulo lobushushu oluzenzekelayo kunye nokusetyenziswa kwe-platinum crucible zinokunciphisa le mingcipheko, kodwa ukulungiswa kwe-fused bead kuhlala kuthatha ixesha elininzi kwaye kudinga izixhobo ezininzi xa kuthelekiswa nokucinezela i-pellet.
Kuphando lwakutshanje, ukucinezela ipowder ecoliweyo kakhulu—ukudibanisa ukugaywa okumanzi ukuya ngaphantsi kwe-4 µm kunye nokucinezela okucoliweyo kakhulu—kuye kwavela njengendlela engcono kakhulu kwiimatrices ezintsonkothileyo. Ezi pellets zibonisa ukuncipha okuphawulekayo kokungaqiniseki kohlalutyo kunye nophuculo olukhulu ekufumaneni izinto ezilandelelanayo ngenxa yokuhambelana okuphuculweyo kunye nokuthamba komphezulu.
Ukukhetha indlela efanelekileyo yokulungiselela i-pellet kuxhomekeke kwiikhrayitheriya ezininzi:
- Ukwakheka kwesampulu kunye nobunzima be-matrix:Izinto ezilukhuni ukufana ziyazuza kwi-fused bead okanye i-ultrafine powder pressing.
- Iinjongo zohlalutyo:Uvakalelo oluphezulu lwezinto ezilandelelanayo lufuna iindlela ezinciphisa ukusasazeka kwemvelaphi kwaye zonyusa ukuphinda-phinda, njengee-pellets ezicinezelweyo okanye ezixutyiweyo.
- Ukufikelela kwimveliso kunye nemida yeendleko:Kwinkqubo yohlalutyo oluqhelekileyo noluphezulu lwemizi-mveliso, iipellets ezicinezelweyo zibonelela ngesantya kunye nokuhambelana ngaphandle kokuphazamiseka okukhulu kumgangatho wohlalutyo.
- Umngcipheko wongcoliseko:Iindlela ezinciphisa ukuphathwa kweesampuli kwaye zifuna izongezo ezimbalwa zinciphisa amathuba okungcoliswa kwe-substrate kunye nokuphazamiseka kohlalutyo.
Ukulungiswa kwepress—amandla, ubukhulu, kunye nobungakanani be-binder—kubalulekile kumgangatho we-pellet kuzo zonke iindlela.
Indima kunye noKhetho lweeBinders
Izibopheleli zolwelo zidlala indima ebalulekileyo ekwakhiweni kweepellet ze-XRF. Umsebenzi wazo ophambili kukudibanisa iisampuli zomgubo zibe ziipellets eziqinileyo nezidibeneyo ezimelana nokuphathwa nokuhlalutywa ngaphandle kokuqhekeka okanye ukuqhekeka. Isibopheleli esikhethwe kakuhle songeza ukuthembeka kwesampuli kwaye sithintele ungcoliseko, zombini ezi zinto zibalulekileyo kwidatha ye-XRF ehambelanayo nenesisombululo esiphezulu.
I-Polyvinyl alcohol (PVA) ivelele njengesixhobo sokubopha ulwelo esisebenzayo. Xa isetyenziswa kwimilinganiselo elungiselelweyo (umz., isampuli ye-7:1 kwisixhobo sokubopha), i-PVA iqinisekisa ukumanzisa nokusasazwa ngokulinganayo kwamasuntswana amancinci, ivelisa ii-pellets ezine-variation coefficients ezingaphantsi kwe-2%. Ezi pellets zibonisa amandla aphezulu oomatshini, amandla azinzileyo kwimijikelo yohlalutyo, kwaye zisusa isidingo sonyango olongezelelweyo lomphezulu.uxinzelelo lwe-PVAichaphazela amandla aluhlaza kunye noxinano, inceda ukwakheka kweepellets ezinamandla ngelixa inciphisa iingozi zongcoliseko.
Ezinye izinto zokubopha ezifana ne-cellulose okanye i-wax mixes zingasetyenziswa ngokuxhomekeke kwiimfuno zohlalutyo kunye ne-sample chemistry. I-Cellulose inika amandla ongezelelweyo oomatshini, ngelixa ii-wax zinokuphucula ukuhambelana kwesampuli ye-hydrophobic kwaye zinciphise ukungqubana phakathi kwezixhobo zokucinezela.
Izibopheleli zolwelo zibonelela ngeenzuzo ezithile kunezibopheleli ezomileyo okanye eziluthuli:
- Ziphucula ukulingana kweepellet zesampulu ngokusasaza ngokulinganayo izinto ezisetyenzisiweyo zesampulu ngexesha lokuxinana.
- Izibophelelo zithintela ukwahlulwahlulwa kwamasuntswana, zinciphisa ukungahambelani okunokuthi ngenye indlela konakalise uvakalelo lokufumanisa kunye nokuphindaphinda komlinganiselo.
- Ngokunciphisa ukudibana ngqo phakathi kwesampulu kunye nomphezulu wepress, izinto zokubopha ulwelo zithintela ungcoliseko—ngakumbi ezifanelekileyo kwizifundo zezinto ezilandelelanayo apho ukuphazamiseka komphezulu kunokujika iziphumo.
- Ukusetyenziswa kakuhle kwe-binder kusombulula izizathu eziqhelekileyo zokuqhekeka kwe-pellet, kuxhasa ukucinezelwa kwe-pellet okuzinzileyo kunye nokuchaneka okuphuculweyo kohlalutyo.
Imizekelo ibonisa ukuba ukusebenzisa i-PVA yobunzima obuphakathi be-molecular kwimo yamanzi rhoqo kuvelisa ii-pellets ezimanzi kakuhle, ezinamathelayo kakhulu, kunye nomngcipheko omncinci wokungcola. Ukuphunyezwa ngempumelelo kweprotocol yokomisa okulawulwayo kuvelisa ii-pellets ezicinezelweyo ezingena-substrate, nto leyo ethintela unyango oluqhubekayo lomphezulu.
Ngokufutshane, ukukhetha i-liquid binder—i-PVA foremost, okanye ezinye iindlela ezenzelwe isampuli yekhemistri—kubalulekile ekufezekiseni umgangatho ophuculweyo we-pellet, ukuchaneka kohlalutyo, kunye nokuphindaphinda kwenkqubo kwi-x-ray fluorescence spectroscopy.
Izinto Ezibalulekileyo Ezichaphazela Uzinzo Lokwakheka KweePellet
Ukuphucula Ukugxila Kwe-Binder
Ukuphucula iuxinaniso lwe-binderyinto ebalulekileyo ekuphuculeni uzinzo lokwakheka kwe-pellet kwi-x-ray fluorescence spectroscopy. Indlela exhaswa kakhulu kukugcina umlinganiselo wesampulu kwi-binder phakathi kwe-7:1 kunye ne-10:1 ngobunzima. Kwiisampuli eziqhelekileyo, oku kulingana ne-10-14% ye-binder, efana ne-polyvinyl alcohol (PVA) okanye i-cellulose, ezikhethwa ngenxa yokuphazamiseka kwazo okuncinci kwe-XRF. Lo mlinganiselo uvela kwizifundo eziphononongwe ngontanga kunye nemigaqo yelabhoratri, ebonisa ukuba ivelisa ii-pellets ezine-homogeneity efanayo, i-superior cohesion, kunye nokuphucula ukulinganiswa kwe-reproducibility kwi-spectroscopy.
Iipellets ezenziwe ngaphakathi kwesi silinganiso sifanelekileyo zibonisa ukuqina koomatshini, okuthintela ukwaphuka, ingakumbi ngexesha lokuphathwa nokudluliselwa kohlalutyo lwe-XRF. Nangona kunjalo, i-binder encinci kakhulu ikhokelela ekuqhekekeni kwe-pellet okanye ukuqhekeka kwe-powder, nto leyo engcolisa indawo yokusebenza yokulungiselela isampuli kunye nezixhobo ze-XRF. I-binder enganeleyo ikwanxulunyaniswa nokuphindaphinda okuphantsi kokulinganisa ngenxa yezakhiwo ze-pellet ezingahambelaniyo. Ngokwahlukileyo koko, i-binder egqithisileyo ivelisa iingxaki ezininzi. Ukusetyenziswa kakhulu (okungaphezulu kwe-14% ngobunzima) kunokunciphisa uvakalelo lokubhaqwa kwezinto ezisisiseko kuba ii-binder ziyayinciphisa i-target analyte kwaye zinegalelo kwimiphumo ye-matrix engafunekiyo, okwenza kube nzima ukuphucula ukuchaneka kohlalutyo. Uxinzelelo oluphezulu lwe-binder lunokuthintela ukuxinana kwe-pellet okusebenzayo; Izifundo ze-mechanical ziqinisekisa ukuba emva komda, i-binder engaphezulu inokubangela ii-pellets ezithambileyo nezibuthathaka ngaphandle kokuba uxinzelelo oluxinzelelweyo lunyuswe ngokuthe ngqo kwi-tandem.
Ukukhethwa kwe-binder kubaluleke ngokulinganayo. I-Polyvinyl alcohol (PVA) ithandwa kakhulu kwiindlela zokucinezela i-pellet ngenxa yokungabonakali kwayo kwe-XRF kunye nokukwazi ukuvelisa ii-pellets eziqinileyo nezihambelanayo, ezixhasa uhlalutyo lwesiqhelo kunye nolwezinto ezilandelelanayo. I-liquid binder yokwenza i-pellet ngamanye amaxesha isetyenziselwa ukwenza lula ukuxuba kodwa kufuneka inikwe idosi ngokuchanekileyo ukuze kuthintelwe ukugcwala kakhulu, okunokuphazamisa ukuthembeka. Iindlela zokulungiselela i-pellet ze-spectroscopy zicebisa ukuqala nge-7:1 proportion kunye nokulungiswa okusekwe kwiimvavanyo zamandla e-empirical kunye nokulinganiswa kohlalutyo ngokuchasene nemigangatho.
Iitshathi ezithelekisa izinga lokusilela kwepellet kunye nomlinganiselo we-binder zigxininisa i-stability plateau ngaphakathi koluhlu lwe-7:1–10:1, kunye nokwanda okukhulu kokuqhekeka okubonwa ngaphantsi kwe-8% ye-binder kunye nokwehla kancinci kobunzulu bohlalutyo ngaphaya kwe-14% (jonga uMzekelo 1). Oku kugxininisa imfuneko yokulinganisela phakathi kozinzo oluphezulu loomatshini kunye namandla esignali ye-XRF afanelekileyo.
Ukusila kunye noHlanganisa iSample
Ukufezekisa ukwakheka kwe-pellet ezinzileyo kufuna ukugaywa kwesampulu okuqinileyo kunye nokuhlanganiswa kwayo. Ukunciphisa ubungakanani be-particle rhoqo kubalulekile; iisampuli ezicoliweyo zibe ngaphantsi kwe-50 μm zibonisa uburhabaxa obuncinci bomphezulu kwaye zizalise imingxuma ngokufanelekileyo xa zicinezelwe, zivelisa ubuso be-pellet obukhulu nobugudileyo. Ii-particles ezincinci zinciphisa umthunzi kwiindlela ze-x-ray kwaye ziqinisekisa ukuba i-XRF excitation kunye ne-emission azithintelwa yi-voids okanye ukupakisha okungacwangciswanga, okuphucula ngokuthe ngqo ukuchaneka kohlalutyo. Ii-particles ezinkulu, ezahlukeneyo zivame ukwahlukana ngexesha lokuxinwa kwe-pellet, zivelisa uxinano oluguquguqukayo kwaye zonyusa umngcipheko wobuthathaka bendawo okanye ukuqhekeka kwe-pellet.
Ukuhlanganiswa ngokupheleleyo kwesampulu kuqinisekisa ukusasazwa ngokulinganayo kwendawo ye-binder kunye ne-analyte. Oku kufezekiswa ngokuthembekileyo ngokuxuba ngoomatshini, njengokusila ibhola, okanye ukuguqa okwandisiweyo kwi-homogenizer. Emva kokuxuba kokuqala kwesampulu yomhlaba kunye ne-binder, ukugaya okongezelelweyo okanye ukuguqulwa kudibanisa nayiphi na i-binder ene-stratified, ngoko ke akukho zindawo zibuthathaka apho i-pellet inokuqhekeka phantsi koxinzelelo. Ukusebenza kwe-homogenization kuqinisekiswa yi-pellet cross-section imaging kunye nohlalutyo lokuhambelana; ukusasazwa kwe-binder okungalinganiyo kudla ngokubonakala njengemimandla yokuxinana okuhlukeneyo okanye ukuxutywa kwezinto ezingalindelekanga kwi-XRF mapping.
Xa usebenzisa iindlela zokulungiselela i-pellet kwi-spectroscopy, ukugcina iindlela zokuxuba kunye nokuseta i-grinder kubalulekile ukuze kuphinde kuvele kwakhona. Iiprotokholi zoshishino zicebisa ukuxuba i-binder kunye ne-analyte emva kokugaya kwangaphambili, emva koko kwandiswe ixesha lokugaya okanye ukongeza amanyathelo okuxuba de kube yipatheni yokusasazwa ifana ngokubonakalayo okanye ngokuhlalutya. Eli nqanaba liphindwe kabini—ukugaya okulandelwa yi-homogenization yamanyathelo amaninzi—kunciphisa kakhulu ukuguquguquka kokulinganisa kwaye kuphucula indlela yokuthintela ukuqhekeka kwe-pellet, njengoko kubonisiwe kwizifundo apho amazinga okuqhekeka kwe-pellet ancitshiswe ngesiqingatha ngokuxuba okucwangcisiweyo.
Ngamafutshane, zombini uxinaniso lwe-binder kunye nokusila/ukufana ngokupheleleyo zizinto eziphambili zozinzo lokwakheka kwe-pellet. Ziyahambelana: umlinganiselo ongcono we-binder awunakukwazi ukuhlawula iisampulu ezingalingani kakuhle, kwaye nokuba kugrunjwe kakuhle kufuneka kuhambelane nomxholo ochanekileyo we-binder kwiipellets ezizinzileyo nezisemgangathweni ophezulu ezisetyenziswa kwi-analytical XRF. Ezi ndlela zibalulekile ekuphuculeni ukuthembeka kwe-pellet yesampulu, inkqubo yokucinezela i-pellet ezinzileyo, kunye nokwenza i-pellet ephuculweyo yohlalutyo lwe-XRF.
Ukuqinisekisa Ukuthembeka KweePellet Zesampulu Nokuthintela Ukuqhekeka KweePellet
Iimeko kunye neendlela zokucinezela
Ukunyaniseka kwe-pellet kwi-X-ray fluorescence spectroscopy kuxhomekeke kuxinzelelo oluxinzelelweyo, ixesha lokuhlala, kunye nokusasazwa kwe-binder efanayo. Uxinzelelo olufanelekileyo kwi-40 mm die ludla ngokuba phakathi kweetoni ezili-15 kunye nama-35. Olu luhlu lwenza ii-pellets ezixineneyo, ezingenaziqhekeko ezihambelana nohlalutyo lwesiqhelo kunye nolwezinto ezilandelelanayo. Nangona kunjalo, uxinzelelo olugqithisileyo lunokubangela ukwaphuka kwangaphakathi okanye umonakalo womphezulu, okubeka emngciphekweni ukuchaneka kohlalutyo.
Ixesha lokuhlala—ukubamba uxinzelelo olujoliswe kulo umzuzu omnye ukuya kwemibini—kuqinisekisa ukuba i-pellet exineneyo ifikelela ekuhlanganeni ngokupheleleyo. Ukunciphisa kancinci emva kwexesha lokuhlala kubalulekile; ukukhululwa ngokukhawuleza koxinzelelo kudla ngokukhokelela emoyeni ovalelekileyo kunye noxinzelelo lwangaphakathi, okubangela ukuba ii-pellets ziqhekeke okanye ziqhekeke.
Ukukhethwa kwee-binder, ezifana ne-polyvinyl alcohol (PVA), kunye nokulungiswa kwemilinganiselo zizinto eziphambili ekuphuculeni ukuthembeka kwe-pellet yesampulu. Ukusasazwa kwee-binder ezifanayo kuthintela iindawo ezibuthathaka kunye noxinzelelo lwangaphakathi. Uphando luqinisekisa ukuba i-binder exutywe kakuhle kunye nomgubo ikwanciphisa ungcoliseko kunye nomonakalo wezixhobo ezivela kumasuntswana akhululekileyo. I-matrix ye-binder engalinganiyo inokuvela njenge-pellet delaminations kunye nokuqhekeka emva kokucinezelwa, ngakumbi emva kokukhululwa koxinzelelo ngokukhawuleza. Ii-pellets ezicinezelweyo ezine-binder ratios ezilungisiweyo kunye nobukhulu bee-particles ezingaphantsi kwe-50 µm zibonisa ukuqina okuphuculweyo kunye nokuguda.
Amaxesha okomisa kunye nokuphathwa emva kokucinezela kuchaphazela kakhulu ukuzinza kokwakheka kwe-pellet. Ukuvumela ii-pellets ukuba zome ngokupheleleyo kususa umswakama oseleyo, onokuthi ubuthathaka iibhondi zangaphakathi kwaye ukhokelele ekuqhekekeni ngexesha leenkqubo zohlalutyo. Ukususwa ngononophelo kwi-die kunye nokuphathwa okuncinci kuthintela uxinzelelo loomatshini kunye nokuqhekeka okunokwenzeka.
Ukuphucula Ukulinganiswa Kokuphinda Kuphindwe
Ukuphinda kulinganiswe kwakhona kwi-X-ray fluorescence spectroscopy kuxhomekeke ekunciphiseni ukuguquguquka kwe-pellet-to-pellet. Ukulinganisa uxinzelelo, ixesha lokuhlala, kunye nomlinganiselo we-binder kuyo yonke ibhetshi sisiseko. Ukucocwa okuphindaphindiweyo kwee-dies kunye nezixhobo zokucinezela phakathi kweesampuli kuthintela ungcoliseko lokuhamba, olunokungenisa ukuphazamiseka kohlalutyo kunye nokukhetha icala.
Ulawulo longcoliseko luqiniswa ngokukhetha izinto zokubopha ezifana ne-PVA, ezibonisa ukuphazamiseka okuncinci kwe-spectral kunye nokuqina kwe-pellet cohesion. Ii-powders kunye ne-binders ezihlala zihambelana rhoqo—zisebenzisa iindlela ezifana nokuxuba i-vortex okanye ii-rotary blenders—zivelisa ii-pellets ezineeprofayili zokuxinana ezihambelanayo kunye ne-analyte dilutions.
Ukuze uphucule ngakumbi ukuphinda-phinda, sebenzisa rhoqo idosi elinganisiweyo ye-binder kunye nobunzima besampuli. Sebenzisa iindlela zokulungiselela umgubo ezivelisa ubungakanani beesuntswana ezingaphantsi kwe-50 µm ukunciphisa ukuguquguquka kokupakisha. Izixhobo ezifana neemitha zoxinano oluphakathi kunye neemitha ze-viscosity ezivela kwiLonnmeter zinegalelo kumgangatho wesampuli ohambelanayo ngokujonga iimpawu zomxube we-binder kunye nesampuli ngaphambi kokucinezela, ukuqinisekisa iinkqubo ezizinzileyo zokwakheka kwe-pellet.
Iindawo zokusebenza ezicocekileyo nezilawulwayo—ezingenazo iinxalenye eziphuma emoyeni kunye neempuphu ezisele—zithintela ungcoliseko lwangaphandle kunye nokuphazamiseka phakathi kweepellet. Ukusasazwa kwe-binder efanayo kunye namanyathelo enkqubo emiselweyo aphakamisa kakhulu uvakalelo lokufumanisa kwi-X-ray fluorescence kunye nokuchaneka kohlalutyo.
Ukufezekisa Ukuchaneka Kohlalutyo kunye Nokuphucuka Kokuqaphela Ukuqonda
Ukufana kunye nokufana
Ukwakheka kwepellet efanayo sisiseko se-x-ray fluorescence spectroscopy, echaphazela ngokuthe ngqo ukuvavanyeka kunye nokuchaneka kohlalutyo. Xa iipowder zesampulu zicoliwe kakuhle kwaye zihlanganiswe nge-optimal binder ratios, indawo nganye yepellet inika i-matrix ehambelanayo kwi-X-rays yesiganeko. Oku kufana kuqinisekisa ukuba iziphumo zokufunxa kunye nokusasazeka zihlala zihleli, ngoko ke izinto ezincinci kunye nezincinci zinokufunyanwa ngokuthembekileyo ngakumbi.
Ngokwezibalo, ukuphuculwa kokufana kuvelisa inzuzo emangalisayo ekuphindaphindweni komlinganiselo. Umzekelo, uhlalutyo oluphindaphindwayo lweepellets zejoloji ezicinezelwe nge-polyvinyl alcohol (PVA) binder kwi-controlled concentration lubonisa ukuphambuka okuqhelekileyo kwi-major element readings engaphantsi kwe-2%. Kwi-trace element assays, iipellets ezihambelana kakuhle zinciphisa ukuguquguquka kobunzulu kwaye zinciphisa ukuphazamiseka kwi-density okanye i-particle size gradients. Idatha yovavanyo iqinisekisa ukuba iipellets ezicinezelweyo zihlala ziphumelela ngaphezu kwee-loose powders, kunye novakalelo oluphuculweyo lwezinto ezixineneyo eziphantsi (ezifana ne-fluorine okanye i-sodium) kunye ne-highly stability calibration curves. Njengoko i-pellet uniformity isanda, iimpazamo ezingahleliweyo nezicwangcisiweyo ezivela kwi-sample heterogeneity ziyancitshiswa, okuphakamisa ukuzithemba ekufumaneni zombini izinto eziphambili kunye nezilandelelanayo.
Indima yokukhetha i-liquid binder iphambili. I-Polyvinyl alcohol (PVA) kwi-ratio elawulwa ngokungqongqo inika uzinzo loomatshini kwaye iqinisekisa ukusasazwa okufanayo kwezinto ze-analyte. Uxinzelelo olulawulwayo—ngesiqhelo yi-20–30% ngobunzima be-binder—luthintela ukuqhekeka, ukuqhekeka, kunye nokwahlukana koxinano, ngoko ke i-pellet nganye inika umfanekiso ochanekileyo wesampulu enkulu. Ukusila okucolekileyo ukuya kubukhulu beentwana ezingaphantsi kwe-10 μm kulandelwa kukuxinana koxinzelelo oluphezulu ngokwezigaba kususa izithuba zomoya kunye neziphene zesakhiwo, nto leyo ephucula ngakumbi ukuthembeka komphezulu wohlalutyo kunye nokuphindaphinda.
Ukuqinisekiswa kwezibalo
Ukuqinisekiswa kokuchaneka kohlalutyo kunye novakalelo lokufumanisa kuxhomekeke kwiindlela eziqinileyo zezibalo. Iilabhoratri zihlala zixhomekeke ekulinganisweni okuphindaphindiweyo kwezinto eziqinisekisiweyo (ii-CRM) ukuze zilinganise ukuchaneka (ukuphindaphinda) kunye nobunyani (ukuvumelana namaxabiso aqinisekisiweyo). Kwiipellets ezicinezelweyo ezibonisa ukufana okuphezulu, ukuphambuka kokulinganisa kwangaphakathi kosuku kunye nokwangaphakathi kosuku kuhlala kungaphantsi kwe-2% kwizinto eziphambili, okuqinisekisa ukuthembeka kweziphumo zohlalutyo oluqhelekileyo nolulandelelwano. Olu lwazi luphezulu luphawuleka ngakumbi xa kusetyenziswa uxinaniso lwe-PVA binder oluphuculweyo: "Ukunyaniseka kwepellet kunye nokuzinza kwesampuli okufunyenweyo ngemilinganiselo ye-PVA ephuculweyo kwenza ukuba imilinganiselo ye-XRF ephindaphindwayo nechanekileyo ibe notshintsho olungaphantsi kwe-2%.
Ukuqinisekiswa kobungakanani kuqhubeka ngokusebenzisa ii-calibration curves ezakhiwe ngezinto ezininzi zokubhekisela. Ezi zixhasa ukuzithemba ekumiselweni kwezinto ezilandelelanayo nezincinci, ingakumbi kwiimatrices ezinzima ezifuna imida ephantsi yokubhaqwa. Iilabhoratri zikwavavanya iikhrayitheriya zokusebenza ezibalulekileyo ezifana nomda wokulinganiswa, ukuphindaphinda, ukuqina kwimiphumo ye-matrix, kunye nokukhetha, ukuqinisekisa ukuba ii-pellets ezilungisiweyo zigcina ukuchaneka kohlalutyo kuluhlu olubanzi oluguquguqukayo. Ukuqinisekiswa okuqhubekayo, okudibene nolawulo oluqinileyo lwezinto eziguquguqukayo zokwakheka kwe-pellet, kuxhasa i-x-ray fluorescence spectroscopy ethembekileyo, ephinda-phindwayo yokujonga rhoqo kunye nezicelo zophando olunzulu.
Izifundo zibonisa ukuba ukusetyenziswa ngononophelo kwezi ndlela zokulungiselela iipellets—ingakumbi ekuxubeni i-PVA binder, ubungakanani be-particles ezincinci, kunye noxinzelelo olucwangcisiweyo—kuphumela kwiipellets ezifanayo apho ukusebenzisana kwazo nge-X-ray kuhlala kuhleli rhoqo kwiikopi ezininzi kunye namaxesha ohlalutyo olongezelelweyo. Oku kufana, okuqinisekisiweyo ngokwezibalo, kuthetha ukuphucuka okunokwenzeka kobuntununtunu, ukuxhasa imida yokufumanisa ephantsi kunye nokuzithemba okukhulu kwingxelo ye-trace-level elemental.
Ukulinganisa ngokuzenzekelayo kunye noLawulo oluValekileyo loLungiso lwePellet
Ulawulo lwedosi oluzenzekelayo luguqula ngokusisiseko iindlela zokulungiselela i-pellet kwi-spectroscopy, ngakumbi kwiilebhu ze-x-ray fluorescence (XRF) eziphezulu. Kulungiselelo lweesampuli ze-XRF, ukongezwa ngokuchanekileyo nangokuhambelanayo kwee-binders—nokuba yi-liquid binder yokwenza i-pellet okanye i-polyvinyl alcohol (PVA) binder—kuchaphazela ngokuthe ngqo izinto ezizinzileyo zokwakheka kwe-pellet, ukuthembeka kwe-pellet yesampuli, kunye nokuchaneka kohlalutyo ngokubanzi. Iinkqubo ze-dosing ezizenzekelayo zenza ubunzima kunye nokudibanisa i-binder ngokuchanekileyo okucwangcisiweyo, okunciphisa ukuguquguquka komntu kunye neempazamo. Ulawulo olunjalo lubalulekile ekuthinteleni ukuqhekeka kwe-pellet kunye nokugcina uxinano oluphindaphindwayo kunye nomgangatho womphezulu, iimpawu zokuphindaphindwa kokulinganisa kwi-spectroscopy.
Iinkqubo zolawulo ezivaliweyo ziphakamisa umgangatho ngokujonga ngokukhutheleyo kunye nokulungelelanisa inqanaba ngalinye lokucinezela i-pellet. Ezi nkqubo zihlala zilinganisa iiparameter zenkqubo-ezifana namandla okucinezela, ixesha lokuhlala, kunye nobushushu-ngexesha lokwenziwa kwe-pellet. Uhlengahlengiso lwenziwa ngokuzenzekelayo ngexesha langempela ukugcina i-pellet nganye ngaphakathi kweefestile ezichanekileyo zeenkcukacha, ukuphucula uvakalelo lokubona kwi-x-ray fluorescence kunye nokunciphisa ukuguquguquka kwebhetshi. Umzekelo, ii-loops zokulawula ezilawula ubushushu bokunamathela ziqinisekisa ukubopha okufanelekileyo phakathi kwamasuntswana, ukwandisa ukuqina kwe-pellet kunye nokunciphisa inkunkuma ye-binder.
Ukudibanisa imisebenzi yokulinganisa, ukukala, kunye nokucinezela ngokuzenzekelayo yeyona nto ibalulekileyo kwiinkqubo zokucinezela iipellet ezizinzileyo neziphindaphindwayo. Ngokwendlela yokusebenza, umsebenzi uqala ngeemodyuli zokulinganisa ezicwangcisiweyo kwangaphambili ezihambisa ubungakanani obuchanekileyo be-binder kwisampulu yomgubo. Iiplatifomu zokulinganisa iirobhothi okanye ii-carousels ezizenzekelayo emva koko ziqinisekisa ubunzima ekujoliswe kubo ngaphakathi kokuchaneka kwe-milligram, zize ziqwalasele nezinto ezinzima ezifana nee-hygroscopic okanye ii-deliqueescent binders. Ukudluliselwa ngqo kwii-press ze-hydraulic okanye ze-servo ezizenzekelayo kugqiba umjikelo, kufezekisa iiprofayili zoxinzelelo ezifanayo kakhulu kunye namaxesha okuhlala kwipellet nganye.
Olu manyano luqinisekisa ukuphinda-phinda okuqinileyo kunye nokukhupha okusebenzayo, okubaluleke kakhulu kwiilebhu ezinkulu ze-XRF. Ngokudibanisa ukulinganisa, ukudosa, kunye nokucinezela ngendlela engenamthungo, iilebhu zinokuvelisa amawaka eepellets ngosuku ngokungenelela okuncinci komqhubi. Le nkqubo ikwaxhasa ukwandiswa kwemodyuli: iilebhu ezikhupha okusebenzayo okuphezulu zinokumisela izikhululo ezongezelelweyo zokufaka idosi, amaqonga okulinganisa, okanye oomatshini bokushicilela abadibeneyo njengoko imfuno ikhula.
Ukubeka iliso rhoqo—kudla ngokuxhaswa zizixhobo zokulinganisa ezikwimigca efanaiimitha zoxinano ukusuka eLonnmeter—yenza impendulo ngexesha langempela. Le mpendulo ingena kwi-pellet eyenziwe kakuhle ye-XRF ngokubona ngokukhawuleza ukuphambuka kuxinano okanye ukusasazwa kwe-binder kwaye iqalise isenzo sokulungisa ngokukhawuleza ngaphambi kokuba kwenzeke ukuphambuka kohlalutyo.
Ulawulo oluzenzekelayo lukwabonelela ngeendawo zelebhu ezikhuselekileyo kunye nokuphucula ukuphindaphindeka xa kusingathwa iintlobo ezahlukeneyo ze-binder okanye iisampuli ezinzima. Ukungaguquguquki ekukhetheni i-binder ukuze kuzinze i-pellet, okufezekiswa ngokusebenzisa imisebenzi ezenzekelayo yexesha langempela, kuguqulela ngokuthe ngqo kwiziphumo ezingcono zohlalutyo kunye nokuzithemba okuphezulu kwi-elemental quantification.
Iitshathi kunye nedatha yenkqubo kumsebenzi wakutshanje ophononongwe ngontanga zibonisa indlela ulawulo lwedosi oluvaliweyo kunye nolawulo lwedosi oluzenzekelayo olunciphisa ngayo umahluko kwi-pellet density ukuya ngaphantsi kwe-1% kwiibhetshi ezinkulu zeesampulu. Olu hlobo lozinzo lokusebenza lubalulekile ekufumaneni inqanaba lokulandelela kunye nothelekiso oluthembekileyo phakathi kweziphumo, zixhasa iziphumo ze-XRF ezisemgangathweni ophezulu.
Ukuhlanganiswa okubanzi kunye nempendulo yexesha langempela ngoku zichaza indlela yanamhlanje yobuchwepheshe bokucinezela iipellets zohlalutyo lwe-spectroscopic. Ukulinganisa ngokuzenzekelayo kunye nolawulo oluvaliweyo azizozixhobo zokonga abasebenzi kuphela; zizinto ezisisiseko eziqhuba ukuphindaphinda kohlalutyo, ukuchaneka kobungakanani, kunye nokusebenza kakuhle kwelebhu okunokulinganiswa.
Imibuzo ebuzwa rhoqo
Yintoni i-X-ray fluorescence spectroscopy kwaye kutheni kubalulekile ukucinezela i-pellet?
I-X-ray fluorescence spectroscopy (XRF) yindlela yokuhlalutya esetyenziselwa ukuchonga nokulinganisa izinto ezikwizinto ngokulinganisa uphawu lwe-X-ray yokukhutshwa kweeathom xa zivuselelwa ngumthombo wangaphandle. Ukucinezela ipellet kubalulekile kuba kuguqula iisampulu zomgubo zibe ziidiski ezixineneyo, ezifanayo, ukuqinisekisa ukusasazwa ngokulinganayo kwezinto. Ukuthe tyaba kunye nokuthembeka kwepellet ecinezelweyo kunciphisa ukungalungelelani komphezulu okunokusasaza ii-X-ray, kunciphisa impazamo yokulinganisa kunye nokuguquguquka. Ukulungiswa kwepellet rhoqo kuphucula uvakalelo lokufumanisa, okwenza iziphumo zobungakanani ezivela kwi-XRF zichaneke ngakumbi kwaye ziphinde ziphindeke.
Uxinzelelo lwe-binder luchaphazela njani uzinzo lokwakheka kwe-pellet kunye nokuthembeka kwesampuli?
Uxinaniso lwe-binder luyinto ebalulekileyo ekwakhiweni kwe-pellet. I-binder encinci kakhulu ikhokelela kwii-pellets ezibuthathaka ezinokuthi ziqhekeke okanye ziqhekeke, ngelixa i-binder egqithisileyo inokungenisa iziphumo ze-matrix eziphazamisa uvakalelo lokufumanisa kunye nokuchaneka kohlalutyo kwi-XRF. Ukulinganisela umlinganiselo we-binder-to-sample kuqinisekisa amandla oomatshini kunye nokuhambelana kwesampulu. Umzekelo, ukuphucula i-binder esekelwe kwisitatshi kwii-pellets ze-catalyst kwandisa amandla kunye nokuthembeka okugciniweyo, ngelixa ukuxinana okungafanelekanga kunciphisa uzinzo nokuba kukwi-binder dosages ephezulu. Ukulinganisa rhoqo i-binder kusetyenziswa iinkqubo ezenzekelayo kuzinzisa ngakumbi ukwakheka kwe-pellet, kugcina ukuthembeka kwesampulu ukuze kuhlalutywe ngokuthembekileyo.
Zithini iingenelo zokusebenzisa i-polyvinyl alcohol (PVA) njengesixhobo sokubopha ulwelo xa kulungiswa i-pellet?
I-Polyvinyl alcohol (PVA) isebenza njengesihlanganisi solwelo esisebenzayo ekwenzeni i-pellet. Ukunyibilika kwayo emanzini kunye neempawu zayo zokumanzisa kakhulu kwenza kube lula ukusasazeka ngokupheleleyo kwe-particle kunye nokunamathela ngexesha lokwenziwa kwe-pellet. Ukusebenzisa i-PVA kunciphisa umngcipheko wongcoliseko lwe-substrate kwaye kuxhasa ukudalwa kwee-pellets eziqinileyo, ezingaqhekekiyo. I-PVA enobunzima obuphakathi be-molecular iphucula uxinano, inyusa amandla aluhlaza, kwaye iqinisekisa ukufana nokuba kumanqanaba aphantsi. Izifundo zibonisa ukuba i-PVA ayinyusi nje kuphela amandla okuxinzelela kunye nokuzinza kodwa ikwagcina i-homogeneity yesampulu—isitshixo se-spectroscopy echanekileyo. Ukuguquguquka kwe-PVA kwiimatrices ezahlukeneyo zomgubo kwenza ukuba ibe yeyona ifanelekileyo kwiindlela zokulungiselela i-pellet esekelwe kwi-liquid binder.
Ingaphuculwa njani indlela yokulinganisa ukuphinda kulinganiswe ngayo kunye nokuchaneka kohlalutyo xa kulungiselelwa iipellet?
Ukuphinda kulinganiswe kunye nokuchaneka kohlalutyo kuxhomekeke ekulinganisweni kwamanyathelo abalulekileyo: ukugaywa kwesampulu ngokupheleleyo ukuze kufunyanwe ubungakanani obufanayo besuntswana; ukuphononongwa ngokuchanekileyo kwe-binder yee-pellets ezizinzileyo; kunye noxinzelelo oluqhubekayo lokucindezela ukuze kuthintelwe i-density gradients. Uxinzelelo oluzenzekelayo lunciphisa ukuguquguquka okubangelwa ngabantu, ngelixa iinkqubo zolawulo oluvaliweyo ziqinisekisa ukujonga rhoqo kunye nokulungiswa kweeparamitha zokulungiselela. Ukugcinwa rhoqo kwee-dies kunye nokubambelela ngokungqongqo kwiprotokholi kwandisa ukuthembeka. Uqeqesho lwabasebenzi kunye nokulungiswa okungqongqo komsebenzi kubaluleke ngokulinganayo ukugcina ukuphindaphindwa kokucinezela ii-pellet kunye neesampuli. Ezi ndlela ziphucula ngokuqinisekileyo iziphumo zohlalutyo kwizicelo ze-XRF.
Ngawaphi amanyathelo acetyiswayo ukuthintela ukuqhekeka kwepellet ngexesha lokulungiselela uhlalutyo lwe-XRF?
Ukuze uthintele ukuqhekeka, sebenzisa i-binder efanelekileyo efana ne-PVA kuxinzelelo olufanelekileyo kwaye uqinisekise ukuba umxube we-powder kunye ne-binder uyafana. Lawula amandla okucinezela ukuze uphephe uxinzelelo olugqithisileyo kwaye ulawule ubukhulu be-pellet kunye nobunzima ukuze i-density ilingane. Lungisa isampuli kakuhle ngaphambi kokuba uyicinezele, kwaye uyomise kakuhle i-pellet ukuze ususe iziphene ezinxulumene nokufuma. Ukugcina isixhobo sokusila nokulinganisa sicocekile kunciphisa ungcoliseko, olunokubangela iindawo zoxinzelelo ezibangela ukuqhekeka. Ukunamathela kwezi ndlela akugcini nje ngokuphucula uzinzo lokwakheka kwe-pellet kodwa kuphucula ukuthembeka kwe-pellet yesampuli kunye nokuphindaphinda komlinganiselo.
Ixesha leposi: Disemba-11-2025
