Isingeniso Sokucindezela I-Pellet Ekuhlaziyweni kwe-XRF
Ukucindezela i-pellet kuyisisekelo senqubo yokulungiselela isampula ye-X-ray fluorescence spectroscopy (XRF). I-XRF iyindlela yokuhlaziya izinto eziyisisekelo lapho isampula ivezwa khona kuma-X-ray anamandla aphezulu, okubangela ukuthi ama-athomu akhiphe ama-X-ray akhanyayo esibili, aqondene nezinto ezithile. I-spectrometer ithola futhi ilinganise lokhu kukhishwa, ivumela ukuhlolwa okusheshayo, kwezinto eziningi kwamasampula aqinile, uketshezi, kanye nophuphu.
Ukulungiswa kwe-pellet ecindezelwe kuqinisekisa ukuthi amasampula empuphu ahlanganiswa abe ama-disc aminyene, afanayo. Le ndlela inciphisa izikhala zomoya kanye nokungaguquguquki kobuso, okuthi—uma kungashiywa kungalungiswanga—kungamunca noma kusakaze ama-X-ray, okuphazamisa ukunemba kokuhlaziya. Lapho ama-powder ecindezelwa abe ama-pellet, indlela ye-X-ray edlula esampula iba yinto eqinile futhi ephindaphindwayo, okuvumela ukulinganiswa kwezinto eziyisisekelo okunembile kanye nokuzwela okuthuthukisiwe, ikakhulukazi ezintweni ezikhanyayo njenge-magnesium noma i-silicon.
Izisekelo Zezindlela Zokulungiselela I-Pellet
Izinketho Zokulungiselela I-Pellet
In i-x-ray fluorescence spectroscopy (XRF), ubuqotho besampula kanye nokulingana kunquma ngqo ukunemba kokuhlaziya kanye nokuphindaphinda. Indlela ngayinye yokulungiselela i-pellet—impuphu ecocekile, ubhontshisi ohlanganisiwe, kanye ne-pellet ecindezelwe—inikeza izinzuzo nezithiyo ezihlukile ezifanele izidingo ezahlukene zokuhlaziya.
Amasu e-pellet acindezelwe asetshenziswa kabanzi ngoba alinganisa ukunemba nokusebenza kahle. Ngokuhlanganisa ama-powder esampula aqoshiwe kahle abe ama-pellet abushelelezi, angenalutho, lezi zindlela zinciphisa ukungafani futhi zinciphise ukuhlakazeka kwangemuva, okubaluleke kakhulu lapho kutholwa izinto zokukhanya. Izinqubo zelebhu zincoma ukusebenzisa osayizi bezinhlayiya ezifanayo, ngokuvamile ezingaphansi kwama-50 µm, ukuze kwandiswe ukulingana kwesampula ngesikhathi sokucindezela nokuvimbela ukungahambisani kokuzwela kokulinganisa. Kodwa-ke, izinhlayiya ezingalingani ngokwanele noma ukucindezela okungafanele kungonakalisa ubuqotho be-pellet, okuholela ekuqhekekeni noma ekuphindaphindeni okubi ekuhlaziyweni kwe-trace element.
Izindlela zempuphu ehlanzekile, nakuba zishesha futhi zingabizi kakhulu, zivame ukuba nezinkinga zokuhlukaniswa kwezinhlayiya kanye nokushelela okungekuhle kobuso. Lezi zinselele zibonakala njengokusabalala okukhulu kanye nokuzwela okunciphile, ikakhulukazi ezintweni ezikhona ngamanani aphansi. Ngenxa yalokho, ukucindezela impuphu ehlanzekile kugcinelwe ukuhlolwa kwangaphambi kwesikhathi kunokuhlaziywa kwenani.
Ukuhlanza Okuqinile Kwamasampula Aqinile
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Indlela yokuhlanganisa ubuhlalu obuhlanganisiwe inqoba imiphumela eminingi ye-matrix ehambisana namasampula ayimpuphu ngokuncibilikisa isampula ku-flux—ngokuvamile i-lithium borate—futhi yakhe ubuhlalu beglasi obufanayo. Le ndlela iletha ukuzinza kwamakhemikhali okumangalisayo kanye nokufana, okwenza kube kuhle kakhulu ekuhlaziyweni okunembile kwezinto eziningi. Noma kunjalo, izinselele ezisebenzayo ezifana nokungcola okungenzeka kwe-flux noma ukuhlakazeka okungaphelele kudinga ukulawulwa okuqinile kwezinga lokushisa, izilinganiso ze-flux, kanye nezimo zokuxuba. Imishini yokuhlanganisa ethuthukisiwe enokuphathwa kwezinga lokushisa okuzenzakalelayo kanye nokusetshenziswa kwe-platinum crucible kunganciphisa lezi zingozi, kodwa ukulungiswa kobuhlalu obuhlanganisiwe kuhlala kudla isikhathi esiningi futhi kudinga izinsiza eziningi uma kuqhathaniswa nokucindezela i-pellet.
Ocwaningweni lwakamuva, ukucindezela i-ultrafine powder—ukuhlanganisa ukugaya okumanzi kube ngaphansi kuka-4 µm nokucindezela kwe-ultrahigh-pressure—kuye kwavela njengendlela engcono kakhulu yama-matrices ayinkimbinkimbi. Lawa ma-pellet abonisa ukwehla okuphawulekayo ekungaqinisekini kokuhlaziya kanye nentuthuko enkulu ekutholakaleni kwezakhi zokulandelela ngenxa yokuqina okuthuthukisiwe kokulingana kanye nokushelela kobuso.
Ukukhetha indlela efanele yokulungiselela ama-pellet kuncike ezicini eziningana:
- Ukwakheka kwesampula kanye nobunzima be-matrix:Izinto ezilukhuni ukuhlanganisa zizuza ngokucindezela i-fused bead noma i-ultrafine powder.
- Imigomo yokuhlaziya:Ukuzwela okuphezulu kwezinto ezilandelwayo kudinga izindlela ezinciphisa ukuhlakazeka kwangemuva futhi zithuthukise ukuphindaphinda, njengama-pellet acindezelwe noma ahlanganisiwe.
- Izindleko kanye nemikhawulo yezindleko:Ukuze kuhlaziywe okuvamile nokusetshenziswa kakhulu kwezimboni, ama-pellet acindezelwe anikeza isivinini kanye nokuvumelana ngaphandle kokuphazamiseka okukhulu kwekhwalithi yokuhlaziya.
- Ingozi yokungcoliswa:Amasu anciphisa ukuphathwa kwamasampula futhi adinga izithasiselo ezimbalwa anciphisa amathuba okungcoliswa kwe-substrate kanye nokuphazamiseka kokuhlaziya.
Ukulungiswa kokucindezela—amandla, ukujiya, kanye nenani le-binder—kubalulekile kwikhwalithi ye-pellet kuzo zonke izindlela.
Indima Nokukhethwa Kwabahlanganisi
Ama-liquid binder adlala indima ebalulekile ekwakhekeni kwama-pellet e-XRF. Umsebenzi wawo oyinhloko ukuhlanganisa amasampula ayimpuphu abe ama-pellet aqinile, ahlangene amelana nokuphathwa nokuhlaziywa ngaphandle kokuqhekeka noma ukudilika. I-binder ekhethwe kahle yandisa ubuqotho besampula futhi ivimbele ukungcola, kokubili okubalulekile kudatha ye-XRF ehambisanayo nenesisombululo esiphezulu.
I-Polyvinyl alcohol (PVA) ivelele njenge-liquid binder esebenzayo. Uma isetshenziswa ngezilinganiso ezilungiselelwe kahle (isb., isampula engu-7:1 ku-binder), i-PVA iqinisekisa ukumanzisa nokusatshalaliswa ngokulinganayo kwezinhlayiya ezincane, iveza ama-pellets ane-variance coefficients engaphansi kuka-2%. Lawa ma-pellets abonisa amandla aphezulu okusebenza, amandla azinzile kuyo yonke imijikelezo yokuhlaziya, futhi aqeda isidingo sokwelashwa okwengeziwe kwendawo.ukuhlushwa kwe-PVAkuthinta amandla aluhlaza kanye nokuqina, kusiza ukwakheka kwama-pellet aqinile ngenkathi kunciphisa izingozi zokungcola.
Ezinye izinto zokubopha ezifana ne-cellulose noma ingxube ye-wax zingasetshenziswa kuye ngezidingo zokuhlaziya kanye ne-chemistry yesampula. I-Cellulose inikeza ukuqina okwengeziwe kwemishini, kuyilapho ama-wax engathuthukisa ukuhambisana kwesampula e-hydrophobic futhi anciphise ukungqubuzana phakathi kwamathuluzi okucindezela.
Ama-liquid binders anikeza izinzuzo ezithile kune-dry binders noma i-powder binders:
- Zithuthukisa ukulingana kwama-pellet esampula ngokusabalalisa ngokulinganayo izakhi zesampula ngesikhathi sokuqiniswa.
- Ama-binder acindezela ukuhlukaniswa kwezinhlayiya, anciphisa ukungalingani okungase kunciphise ukuzwela kokutholwa kanye nokuphindaphinda kokulinganisa.
- Ngokunciphisa ukuthintana okuqondile phakathi kwesampula kanye nezindawo zokucindezela, izihlanganisi zoketshezi zivimbela ukungcola—ikakhulukazi ezifundweni zezakhi zokulandelela lapho ukuphazamiseka kwendawo kungaphazamisa imiphumela.
- Ukusetshenziswa kwe-binder okulungiselelwe kuxazulula izimbangela ezivamile zokuqhekeka kwe-pellet, kusekela ukucindezela kwe-pellet okuzinzile kanye nokunemba okuthuthukisiwe kokuhlaziya.
Izibonelo zibonisa ukuthi ukusebenzisa i-PVA enesisindo esimaphakathi se-molecular ngesimo samanzi kukhiqiza njalo ama-pellets anomswakama omuhle, ukunamathela okuqinile, kanye nengozi encane yokungcola. Ukuqaliswa kwephrothokholi okuphumelelayo ngokomisa okulawulwayo kuveza ama-pellets acindezelwe angena-substrate, okuvimbela ukwelashwa okwengeziwe kwendawo.
Ngamafuphi, ukukhetha i-liquid binder—i-PVA foremost, noma ezinye izindlela ezenzelwe isampula yamakhemikhali—kubalulekile ekufinyeleleni ikhwalithi ye-pellet ethuthukisiwe, ukunemba kokuhlaziya, kanye nokuphindaphindeka kwenqubo ku-x-ray fluorescence spectroscopy.
Izici Ezibalulekile Ezithinta Ukuqina Kokwakheka Kwe-Pellet
Ukuthuthukisa Ukuhlushwa Kwe-Binder
Ukuthuthukisa i-ukuhlushwa kwe-binderkuyisici esibalulekile ekwandiseni ukuzinza kokwakheka kwama-pellet kwe-x-ray fluorescence spectroscopy. Indlela esekelwa kabanzi ukugcina isilinganiso sesampula kuya ku-binder phakathi kuka-7:1 no-10:1 ngesisindo. Kumasampula ajwayelekile, lokhu kulingana ne-binder engu-10-14%, njenge-polyvinyl alcohol (PVA) noma i-cellulose, ekhethwa ngenxa yokuphazamiseka kwayo okuncane kwe-XRF. Lesi silinganiso sitholakala kokubili ezifundweni ezibuyekezwe ontanga kanye nezinqubo zelebhu, okubonisa ukuthi ikhiqiza ama-pellet anokulingana okufanayo, ukuhlangana okuphezulu, kanye nokuphindaphindwa kokulinganisa okuthuthukisiwe ku-spectroscopy.
Ama-pellet akhiwe ngaphakathi kwalesi silinganiso esihle kakhulu abonisa ukuqina komshini, okuvimbela ukuphuka, ikakhulukazi ngesikhathi sokuphathwa nokudluliselwa kokuhlaziywa kwe-XRF. Nokho, i-binder encane kakhulu iholela ekuqhekekeni kwama-pellet noma ekuhlukanisweni kwempuphu, kungcolise indawo yokusebenza yokulungiselela isampula kanye nezinsimbi ze-XRF. I-binder enganele nayo ihlotshaniswa nokuphindaphindeka okuphansi kokulinganisa ngenxa yezakhiwo zama-pellet ezingaguquki. Ngokuphambene nalokho, i-binder eningi iletha izinkinga eziningana. Ukusetshenziswa ngokweqile (okudlula u-14% ngobuningi) kunganciphisa ukuzwela kokutholwa kwezinto eziyisisekelo ngoba ama-binder anciphisa i-target analyte futhi anegalelo emiphumeleni ye-matrix engafuneki, okwenza kube nzima ukuthuthukiswa kokunemba kokuhlaziya. Ukugxila okuphezulu kwe-binder nakho kungaphazamisa ukuhlanganiswa kwe-pellet okusebenzayo; izifundo zemishini ziqinisekisa ukuthi ngemuva komkhawulo, i-binder eningi ingabangela ama-pellet athambile, abuthakathaka ngaphandle kokuthi ingcindezi yokucindezela ikhuliswe ngokuqinile ngesikhathi esisodwa.
Ukukhethwa kwe-binder kubaluleke ngokulinganayo. I-Polyvinyl alcohol (PVA) iyathandwa kakhulu ebuchwephesheni bokucindezela ama-pellet ngenxa yokungabonakali kwayo kwe-XRF kanye nekhono lokukhiqiza ama-pellet aqinile, ahambisanayo, esekela kokubili ukuhlaziywa okuvamile kanye nokwe-trace element. I-liquid binder yokwenza ama-pellet ngezinye izikhathi isetshenziselwa ukwenza kube lula ukuxuba kodwa kumele ilinganiswe kahle ukuze kugwenywe ukugcwala ngokweqile, okungase kuphazamise ubuqotho. Izindlela zokulungiselela ama-pellet ze-spectroscopy zincoma ukuqala ngesilinganiso esingu-7:1 kanye nokulungiswa okuhle okusekelwe ekuhlolweni kwamandla okuhlola kanye nokulinganiswa kokuhlaziya ngokumelene nezindinganiso.
Amashadi aqhathanisa izinga lokwehluleka kwe-pellet uma kuqhathaniswa nesilinganiso se-binder aqokomisa i-platinum yokuzinza ngaphakathi kobubanzi obungu-7:1–10:1, kanye nokwanda okukhulu kokuqhekeka okubonwe ngaphansi kwe-binder engu-8% kanye nokwehla okuncane kokuqina kokuhlaziya okungaphezu kuka-14% (bheka Isibonelo 1). Lokhu kugcizelela isidingo sokulinganisela phakathi kokuqina okuphezulu kakhulu kwemishini kanye namandla esignali e-XRF afanele.
Ukugaya Isampula kanye Nokuhlanganiswa Kwezinto Ezifanayo
Ukufeza ukwakheka kwe-pellet okuzinzile kudinga futhi ukugaya amasampula okunzima kanye nokuhlanganiswa kwawo. Ukunciphisa njalo usayizi wezinhlayiya kubalulekile; amasampula agaywa abe ngaphansi kwama-50 μm aveza ubulukhuni obuncane bomphezulu futhi agcwalise imigodi kahle lapho ecindezelwe, okukhiqiza ubuso be-pellet obukhulu nobubushelelezi. Izinhlayiya ezincane zinciphisa umthunzi ezindleleni ze-x-ray futhi ziqinisekisa ukuthi ukuvusa nokukhipha kwe-XRF akuvinjelwa yizikhala noma ukupakisha okungajwayelekile, okuthuthukisa ngqo ukunemba kokuhlaziya. Izinhlayiya ezinkulu, ezingafani zivame ukuhlukanisa ngesikhathi sokucindezela i-pellet, ziveza ubuningi obuguquguqukayo futhi zandisa ingozi yobuthakathaka bendawo noma ukuqhekeka kwe-pellet.
Ukuhlanganiswa okuphelele kwesampula kuqinisekisa ukusatshalaliswa okulinganayo kwendawo kokubili kwe-binder kanye ne-analyte. Lokhu kufezwa ngokuthembekile kakhulu ngokuxuba ngomshini, njengokugaya ibhola, noma ukugoba okunwetshiwe ku-homogenizer. Ngemva kokuhlanganiswa kokuqala kwesampula yomhlabathi kanye ne-binder, ukugaya okwengeziwe noma ukuguqulwa kuhlanganisa noma iyiphi i-binder enezigaba, ngakho-ke azikho izindawo ezibuthakathaka lapho i-pellet ingase iqhume khona ngaphansi kokucindezelwa. Ukusebenza kahle kwe-homogenization kuqinisekiswa ngokuthwebula izithombe ze-pellet cross-section kanye nokuhlaziywa kokuvumelana; ukusatshalaliswa kwe-binder okungalingani kuvame ukubonakala njengezindawo zokuhlanganiswa okuhlukile noma ukuhlanganiswa kwezakhi ezingalindelekile kumephu ye-XRF.
Uma usebenzisa izindlela zokulungiselela ama-pellets ze-spectroscopy, ukugcina izindlela zokuxuba kanye nezilungiselelo zokugaya kubalulekile ukuze kuphinde kukhiqizwe. Izinqubo zezimboni zincoma ukuxuba i-binder kanye ne-analyte ngemva kokugaya kwangaphambili, bese kwandiswe isikhathi sokugaya noma ukwengeza izinyathelo zokuxuba kuze kube yilapho iphethini yokusabalalisa ifana ngokubonakalayo noma ngokuhlaziya. Lesi sigaba esiphindwe kabili—ukugaya okulandelwa yi-homogenization yezinyathelo eziningi—kunciphisa kakhulu ukuguquguquka kokulinganisa futhi kuthuthukisa indlela yokuvimbela ukuqhekeka kwama-pellets, njengoba kuboniswe ezifundweni lapho amazinga okuphuka kwama-pellets ancishiswe ngesigamu ngokuxuba okulungiselelwe.
Ngamafuphi, kokubili ukuhlushwa kwe-binder kanye nokugaya/ukubumbana ngokuphelele kuyizinto eziyinhloko zokuqina kokwakheka kwe-pellet. Ziyaphelelisana: isilinganiso se-binder esingcono kakhulu asikwazi ukukhokha amasampula angalingani kahle, futhi ngisho nokugaya okuhle kakhulu kumele kuhambisane nokuqukethwe kwe-binder okulungile kwama-pellet azinzile, aqinile asetshenziswa ku-XRF yokuhlaziya. Lezi zindlela zibalulekile ekuthuthukiseni ubuqotho be-pellet yesampula, inqubo yokucindezela i-pellet ezinzile, kanye nokwenza i-pellet elungiselelwe ukuhlaziywa kwe-XRF.
Ukuqinisekisa Ubuqotho Besampula Ye-Pellet Nokuvimbela Ukuqhekeka Kwe-Pellet
Izimo Ezicindezelayo Namasu
Ubuqotho be-pellet ku-X-ray fluorescence spectroscopy buxhomeke ekucindezelweni okulinganiselayo, isikhathi sokuhlala, kanye nokusatshalaliswa kwe-binder efanayo. Ukucindezela okuhle kakhulu kwe-die engu-40 mm kuvame ukuba phakathi kwamathani angu-15 no-35. Lolu hlu ludala ama-pellet aminyene, angenama-crack ahambisana nokuhlaziywa okuvamile kanye nokwe-trace element. Nokho, ukucindezela ngokweqile kungabangela ukuqhekeka kwangaphakathi noma ukulimala kwendawo, okubeka engcupheni ukunemba kokuhlaziya.
Isikhathi sokuhlala—ukubamba ingcindezi eqondiwe umzuzu owodwa kuya kwemibili—kuqinisekisa ukuthi i-pellet ehlanganisiwe ihlangana ngokugcwele. Ukunciphisa kancane ngemva kwesikhathi sokuhlala kubalulekile; ukukhululwa kwengcindezi okusheshayo kuvame ukuholela emoyeni ovalelekile kanye nokucindezeleka kwangaphakathi, okuholela kuma-pellet aqhekekile noma aqhekekile.
Ukukhethwa kwe-binder, njenge-polyvinyl alcohol (PVA), kanye nokulungiswa kwesilinganiso kubalulekile ekuthuthukisweni kobuqotho be-pellet yesampula. Ukusatshalaliswa kwe-binder efanayo kuvimbela izindawo ezibuthakathaka kanye nokucindezeleka kwangaphakathi. Ucwaningo luqinisekisa ukuthi i-binder exutshwe kahle kanye ne-powder kunciphisa nokungcola kanye nomonakalo wemishini ovela ezinhlayiyeni ezikhululekile. I-matrix ye-binder engalingani ingabonakala njenge-pellet delaminations kanye nokuqhekeka ngemuva kokucindezela, ikakhulukazi ngemva kokukhululwa kwengcindezi okusheshayo. Ama-pellet acindezelwe ngezilinganiso ze-binder ezilungiselelwe kanye nosayizi wezinhlayiyana ezingaphansi kwama-50 µm abonisa ukuqina okuthuthukisiwe kanye nokushelela.
Izikhathi zokomisa kanye nokuphathwa ngemva kokucindezela kuthinta kakhulu ukuqina kokwakheka kwama-pellet. Ukuvumela ama-pellet ukuthi ome ngokuphelele kususa umswakama osele, okungaba buthakathaka izibopho zangaphakathi futhi kuholele ekuqhekekeni ngesikhathi sezinqubo zokuhlaziya. Ukususwa ngokucophelela kudayi kanye nokuphathwa okuncane kuvimbela ukucindezeleka komshini kanye nokuqhekeka okungenzeka.
Ukuthuthukisa Ukuphindaphinda Kokulinganisa
Ukuphindaphindwa kokulinganisa ku-X-ray fluorescence spectroscopy kuncike ekunciphiseni ukuguquguquka kwe-pellet-to-pellet. Ukulinganisa ingcindezi, isikhathi sokuhlala, kanye nesilinganiso se-binder kuwo wonke amaqoqo kuyisisekelo. Ukuhlanza okuphindaphindiwe kwama-dies kanye namathuluzi okucindezela phakathi kwamasampula kuvimbela ukungcola kokuthwala, okungaletha ukuphazamiseka kokuhlaziya kanye nokubandlulula.
Ukulawulwa kokungcola kuqiniswa ngokukhetha ama-binder afana ne-PVA, abonisa ukuphazamiseka okuncane kwe-spectral kanye nokuhlangana okuqinile kwama-pellet. Ama-powder nama-binder ajwayelekile ahlanganisa i-homogenizing—kusetshenziswa izindlela ezifana nokuxuba i-vortex noma ama-blender ajikelezayo—aveza ama-pellet anamaphrofayili okuqina ahambisanayo kanye nokunciphisa i-analyte.
Ukuze uthuthukise ukuphindaphindeka, sebenzisa njalo ukukala okulinganiselwe kwe-binder kanye nesisindo sesampula. Sebenzisa amasu okulungisa impuphu akhiqiza ubukhulu bezinhlayiya ngaphansi kwama-µm angu-50 ukunciphisa ukuguquguquka kokupakisha. Imishini efana namamitha okuqina angaphakathi kanye namamitha e-viscosity avela eLonnmeter inegalelo ekhwalithini yesampula ehambisanayo ngokuqapha izakhiwo zengxube ye-binder nesampula ngaphambi kokucindezela, ukuqinisekisa izinqubo zokwakheka kwe-pellet ezizinzile.
Izindawo zokusebenza ezihlanzekile nezilawulwayo—ezingenazo izinhlayiya eziphuma emoyeni kanye nezimpuphu ezisele—zivimbela ukungcola kwangaphandle kanye nokuphazamiseka phakathi kwama-pellet. Ukusatshalaliswa kwe-binder efanayo kanye nezinyathelo zenqubo ezijwayelekile kuphakamisa kakhulu ukuzwela kokutholwa ekukhanyeni kwe-X-ray kanye nokunemba kokuhlaziya.
Ukufeza Ukunemba Kokuhlaziya kanye Nokuzwela Okuthuthukisiwe Kokuthola
Ukufana kanye Nokufana
Ukwakheka kwe-pellet efanayo kuyitshe lesisekelo se-x-ray fluorescence spectroscopy, okuthonya ngqo ukuzwela kokuthola kanye nokunemba kokuhlaziya. Lapho izimpushana zesampula zigaywa kahle futhi zihlanganiswa nezilinganiso ze-binder ezifanele, isifunda ngasinye se-pellet sinikeza i-matrix ehambisanayo ne-X-ray yesigameko. Lokhu kufana kuqinisekisa ukuthi imiphumela yokumuncwa kanye nokuhlakazeka ihlala ingaguquki, ngakho-ke izakhi zokulandelela kanye nezinto ezincane zingatholakala ngokwethembeka kakhudlwana.
Ngokwezibalo, ukuthuthuka kokufana kuveza inzuzo emangalisayo ekuphindaphindweni kokulinganisa. Isibonelo, ukuhlaziywa okuphindaphindwayo kwama-pellets e-geological acindezelwe nge-polyvinyl alcohol (PVA) binder ekugxilweni okulawulwayo kubonisa ukuphambuka okujwayelekile ekufundweni kwezinto ezinkulu ngaphansi kuka-2%. Ekuhlolweni kwezinto zokulandelela, ama-pellets ahlanganiswe kahle anciphisa ukuguquguquka kwamandla futhi anciphise ukuphazamiseka okuvela ekuminyaneni noma kuma-gradients osayizi wezinhlayiya. Idatha yokuhlola iqinisekisa ukuthi ama-pellets acindezelwe ahlala edlula ama-powder akhululekile, ngokuzwela okuthuthukisiwe kwezinto eziphansi kokugxilisa (njenge-fluorine noma i-sodium) kanye nama-curve okulinganisa azinzile kakhulu. Njengoba ukufana kwama-pellet kukhuphuka, amaphutha angahleliwe nahlelekile avela ekuhlukeni kwesampula ayancishiswa, okuphakamisa ukuzethemba ekutholeni kokubili izinto ezinkulu nezincane.
Indima yokukhetha i-liquid binder ibalulekile. I-Polyvinyl alcohol (PVA) ngesilinganiso esilawulwa ngokuqinile inikeza ukuzinza komshini futhi iqinisekisa ukusatshalaliswa okufanayo kwezinto ze-analyte. Ukugxila okulawulwayo—ngokuvamile okungu-20-30% ngesisindo se-binder—kuvimbela ukuqhekeka, ukudilika, kanye nokuhlukaniswa kobuningi, ngakho-ke i-pellet ngayinye inikeza ukumelwa kwangempela kwesampula enkulu. Ukugaya okuncane kuya kosayizi bezinhlayiya ezingaphansi kuka-10 μm kulandelwa ukucindezela okuphezulu okuhleliwe kususa izikhala zomoya kanye nokukhubazeka kwesakhiwo, okuthuthukisa kakhulu ubuqotho bomphezulu wokuhlaziya kanye nokuphindaphinda.
Ukuqinisekiswa kwezibalo
Ukuqinisekiswa kokunemba kokuhlaziya kanye nokuzwela kokuthola kuncike ezindleleni eziqinile zezibalo. Amalabhorethri ngokuvamile athembele ekulinganisweni okuphindaphindiwe kwezinto zokubhekisela eziqinisekisiwe (ama-CRM) ukuze alinganise kokubili ukunemba (ukuphindaphinda) kanye nokuba yiqiniso (ukuvumelana namanani aqinisekisiwe). Kuma-pellet acindezelwe abonisa ukufana okuhle kakhulu, ukuphambuka kokulinganisa kwangaphakathi kosuku kanye nokwaphakathi kosuku kuhlala kungaphansi kuka-2% ezintweni ezinkulu, okuqinisekisa ukuthembeka kwemiphumela yokuhlaziywa okuvamile kanye nokulandelela. Lokhu kunemba okuphezulu kuphawuleka kakhulu uma kusetshenziswa amazinga e-PVA binder alungiselelwe: "Ubuqotho be-pellet obuthuthukisiwe kanye nokuzinza kwesampula okufinyelelwe ngezilinganiso ze-PVA ezilungiselelwe kuvumela ukulinganiswa kwe-XRF okuphindaphindwayo, okunembile okune-<2%."
Ukuqinisekiswa kwenani kudlula ngokusebenzisa ama-calibration curve akhiwe ngezinto eziningi zokubhekisela. Lokhu kusekela ukuzethemba ekunqunyweni kwezinto ezilandelanayo nezincane, ikakhulukazi kuma-matrices ayinselele adinga imikhawulo ephansi yokutholakala. Ama-laboratories ahlola nezindlela zokusebenza ezibalulekile njengomkhawulo wokulinganiswa, ukuphindaphindeka, ukuqina kwemiphumela ye-matrix, kanye nokukhetha, ukuqinisekisa ukuthi ama-pellets alungiselelwe agcina ukunemba kokuhlaziya kulo lonke ububanzi obuguquguqukayo. Ukuqinisekiswa okuqhubekayo, okuhlanganiswe nokulawulwa okuqinile kwezinguquko zokwakheka kwama-pellet, kusekela i-x-ray fluorescence spectroscopy ethembekile, ephindaphindwayo kokubili ukuqapha okuvamile kanye nezicelo zocwaningo olujulile.
Izifundo zibonisa ukuthi ukusetshenziswa ngokucophelela kwalezi zindlela zokulungiselela ama-pellet—ikakhulukazi ekuxubeni i-PVA binder, usayizi wezinhlayiya ezincane, kanye nokucindezela okuhleliwe—kuphumela kuma-pellet afanayo lapho ukusebenzisana kwawo kwe-X-ray kuhlala kufana kuzo zonke izikhathi eziningi zokuphindaphinda kanye nezikhathi zokuhlaziya ezinde. Lokhu kufana, okuqinisekiswe ngokwezibalo, kuhumushela ekuthuthukisweni okusebenzayo kokuzwela, kusekela imikhawulo ephansi yokutholakala kanye nokuzethemba okukhulu ekubikeni kwe-elemental level trace.
Ukulinganisa Okuzenzakalelayo kanye Nokulawulwa Kwe-Loop Evaliwe Ekulungiseleleni I-Pellet
Ukulawulwa komthamo okuzenzakalelayo kuguqula ngokuyisisekelo izindlela zokulungiselela ama-pellet ze-spectroscopy, ikakhulukazi kuma-lab e-x-ray fluorescence (XRF) aphezulu. Ekulungiselelweni kwesampula ye-XRF, ukungezwa okunembile nokungaguquguquki kwama-binder—kungaba i-liquid binder yokwenza ama-pellet noma i-polyvinyl alcohol (PVA) binder—kuthinta ngqo izici zokuqina kokwakheka kwama-pellet, ubuqotho be-pellet yesampula, kanye nokunemba okuphelele kokuhlaziya. Izinhlelo zokulinganisa okuzenzakalelayo zenza isisindo kanye nokwengeza kwe-binder ngokunemba okuhleliwe, okunciphisa kokubili ukuguquguquka kanye namaphutha abantu. Ukulawula okunjalo kubalulekile ekuvimbeleni ukuqhekeka kwama-pellet nokugcina ubuningi obuphindaphindwayo kanye nekhwalithi yobuso, izimpawu zokuphindaphindwa kokulinganisa ku-spectroscopy.
Izinhlelo zokulawula ezivaliwe ziphakamisa izinga ngokubheka ngenkuthalo nangokulinganisa isigaba ngasinye sokucindezela ama-pellet. Lezi zinhlelo zihlala zilinganisa amapharamitha enqubo—njengokucindezela amandla, isikhathi sokuhlala, kanye nokushisa—ngesikhathi sokwakheka kwama-pellet. Ukulungiswa kwenziwa ngokuzenzakalelayo ngesikhathi sangempela ukuze kugcinwe i-pellet ngayinye ngaphakathi kwamafasitela aqinile okucaciswa, kuthuthukiswe ukuzwela kokutholwa ku-x-ray fluorescence futhi kuncishiswe ukuhlukahluka kwe-batch. Isibonelo, ama-loop okulawula alawula izinga lokushisa lokunamathela aqinisekisa ukubopha okuhle phakathi kwezinhlayiya, okwandisa kokubili ukuqina kwama-pellet kanye nokunciphisa imfucuza ye-binder.
Ukuhlanganisa imisebenzi yokulinganisa, yokulinganisa, kanye nokucindezela okuzenzakalelayo kuyitshe lesisekelo sezinqubo zokucindezela i-pellet ezizinzile neziphindaphindwayo. Ngokwemibandela engokoqobo, ukuhamba komsebenzi kuqala ngamamojula wokulinganisa ahlelwe kusengaphambili anikeza inani eliqondile le-binder kusampula eyimpuphu. Amapulatifomu okulinganisa amarobhothi noma ama-carousel azenzakalelayo abese eqinisekisa isisindo esiqondiwe ngaphakathi kokunemba kwe-milligram, ngisho nokubala izinto eziyinselele njengezihlanganisi ze-hygroscopic noma ze-deliqueescent. Ukudluliselwa ngqo kuma-press azenzakalelayo e-hydraulic noma e-servo-driven kuqeda umjikelezo, kufinyelela amaphrofayili okucindezela afanayo kakhulu kanye nezikhathi zokuhlala ze-pellet ngayinye.
Lokhu kuhlanganiswa kuqinisekisa ukuphindaphindwa okuqinile kanye nokusetshenziswa kwamandla, okubaluleke kakhulu kuma-laboratories amakhulu e-XRF. Ngokuhlanganisa ukukala, ukufaka umthamo, kanye nokucindezela ngendlela engenamthungo, ama-laboratories angakhiqiza izinkulungwane zama-pellets ngosuku ngokungenelela okuncane komqhubi. Le nqubo iphinde isekele ukwanda kwe-modular: ama-laboratories ane-high-throughput angalungiselela iziteshi ezengeziwe zokufaka umthamo, amapulatifomu okukala, noma imishini yokucindezela ehlanganisiwe njengoba isidingo sikhula.
Ukuqapha okuqhubekayo—okuvame ukusekelwa ngamathuluzi okulinganisa angaphakathi afanaamamitha okuminyana avela eLonnmeter—ivumela impendulo yesikhathi sangempela. Le mpendulo ivala ukwenziwa kwe-pellet okulungiselelwe i-XRF ngokuthola ngokushesha ukuphambuka ekubuneni noma ekusabalalisweni kwe-binder bese iqalisa isenzo sokulungisa ngokushesha ngaphambi kokuba kwenzeke ukuphambuka kokuhlaziya.
Ukulawula okuzenzakalelayo kunikeza futhi izindawo zelebhu eziphephile kanye nokuphindaphindeka okuthuthukisiwe lapho kusingathwa izinhlobo ezahlukene ze-binder noma amasampula ayinselele. Ukuvumelana ekukhetheni i-binder ukuze kube nokuzinza kwe-pellet, okufezwa ngokusebenzisa imisebenzi yokusebenza ezenzakalelayo yesikhathi sangempela, kuhumushela ngqo emiphumeleni engcono yokuhlaziya kanye nokuqiniseka okuphezulu ekulinganisweni kwezinto eziyisisekelo.
Amashadi kanye nedatha yenqubo emsebenzini wakamuva obuyekezwe ontanga kubonisa ukuthi ukulawulwa kokulinganisa okuzenzakalelayo kanye nokulawulwa kokulinganisa okuzenzakalelayo kunciphisa kanjani ukwehluka kobuningi be-pellet kube ngaphansi kuka-1% kuma-batches amakhulu esampula. Lolu hlobo lokuzinza kokusebenza lubalulekile ekutholakaleni kwezinga lokulandelela kanye nokuqhathaniswa okuthembekile phakathi kokugijima, okuqinisa imiphumela ye-XRF esezingeni eliphezulu.
Ukuhlanganiswa okunjalo okuphelele kanye nempendulo yesikhathi sangempela manje kuchaza ubuchwepheshe obusezingeni eliphezulu kumasu okucindezela ama-pellet okuhlaziya i-spectroscopic. Ukulinganisa okuzenzakalelayo kanye nokulawula i-closed-loop akuzona nje amathuluzi okonga abasebenzi; kuyizinto eziyisisekelo ezibangela ukuphindaphindeka kokuhlaziya, ukunemba kwenani, kanye nokusebenza kahle kwelebhu okukhuliswayo.
Imibuzo Evame Ukubuzwa
Kuyini i-X-ray fluorescence spectroscopy futhi kungani ukucindezela i-pellet kubalulekile?
I-X-ray fluorescence spectroscopy (XRF) iyindlela yokuhlaziya esetshenziswa ukuhlonza nokulinganisa izakhi ngaphakathi kwento ngokulinganisa ukukhishwa kwe-X-ray okuphawulekayo kwama-athomu lapho kushukunyiswa umthombo wangaphandle. Ukucindezela i-pellet kubalulekile ngoba kuguqula amasampula ayimpuphu abe amadiski aminyene, afanayo, okuqinisekisa ukusatshalaliswa kwezinto ngokulinganayo. Ukuthamba kanye nobuqotho be-pellet ecindezelwe kunciphisa ukungalingani kwendawo okungasakaza i-X-ray, kunciphisa iphutha lokulinganisa kanye nokuguquguquka. Ukulungiswa kwe-pellet okuqhubekayo kuthuthukisa ukuzwela kokuthola, okwenza imiphumela yobuningi evela ku-XRF inembe kakhudlwana futhi iphindaphindwe.
Ukuhlushwa kwe-binder kuthinta kanjani ukuqina kokwakheka kwe-pellet kanye nobuqotho besampula?
Ukuhlushwa kwe-binder kuyisici esibalulekile ekwakhekeni kwe-pellet. I-binder encane kakhulu iholela kuma-pellet abuthakathaka athambekele ekuqhekekeni noma ekuqhekekeni, kuyilapho i-binder eningi kakhulu ingaletha imiphumela ye-matrix ephazamisa ukuzwela kokutholwa kanye nokunemba kokuhlaziya ku-XRF. Ukulinganisa isilinganiso se-binder-to-sample kuqinisekisa amandla omshini kanye nokulingana kwesampula. Isibonelo, ukwenza ngcono i-binder esekelwe kusitashi kuma-pellet e-catalyst kwandisa amandla futhi kulondoloze ubuqotho, kuyilapho ukuqina okungafanele kunciphisa ukuzinza ngisho nasemithini ephezulu ye-binder. Ukulinganisa njalo kwe-binder kusetshenziswa izinhlelo ezenzakalelayo kuqhubeka nokuzinzisa ukwakheka kwe-pellet, kulondoloza ubuqotho besampula ukuze kuhlaziywe ngokwethembeka.
Yiziphi izinzuzo zokusebenzisa i-polyvinyl alcohol (PVA) njenge-liquid binder ekulungiseleleni i-pellet?
I-Polyvinyl alcohol (PVA) isebenza njengesihlanganisi soketshezi esisebenzayo sokwenza ama-pellet. Ukuncibilika kwayo emanzini kanye nezakhiwo zayo zokumanzisa kakhulu kwenza kube lula ukuhlakazeka kwezinhlayiya kanye nokunamathelana ngesikhathi sokwakheka kwama-pellet. Ukusebenzisa i-PVA kunciphisa ingozi yokungcoliswa kwe-substrate futhi kusekela ukudalwa kwama-pellet aqinile, angaqhekeki. I-PVA enesisindo esimaphakathi ithuthukisa ukuqina, ithuthukisa amandla aluhlaza, futhi iqinisekisa ukufana ngisho nasezilinganisweni eziphansi. Izifundo zibonisa ukuthi i-PVA ayigcini nje ngokwandisa amandla okucindezela kanye nokuqina kodwa futhi igcina ukulingana kwesampula—okuyisihluthulelo se-spectroscopy enembile. Ukuguquguquka kwe-PVA kuzo zonke izinhlobo ezahlukene ze-powder kwenza kube ngcono kakhulu ezindleleni zokulungiselela ama-pellet asekelwe ku-liquid binder.
Ukuphindwaphindwa kokulinganisa kanye nokunemba kokuhlaziya kungathuthukiswa kanjani ekulungiseleleni ama-pellet?
Ukuphindaphinda kokulinganisa kanye nokunemba kokuhlaziya kuncike ekulinganiseni izinyathelo ezibalulekile: ukugaya isampula ngokuphelele ukuze kufinyelelwe usayizi wezinhlayiya ezifanayo; ukulinganisa okunembile kwe-binder kwama-pellet azinzile; kanye nokucindezela okuqhubekayo ukuze kugwenywe i-density gradients. Ukucindezela okuzenzakalelayo kunciphisa ukuguquguquka okubangelwa abantu, kuyilapho izinhlelo zokulawula ezivaliwe ziqinisekisa ukuqapha okuqhubekayo nokulungiswa kwamapharamitha okulungiselela. Ukugcinwa njalo kwama-dies kanye nokunamathela ngokuqinile kuphrothokholi kwandisa ukuthembeka. Ukuqeqeshwa kwabasebenzi kanye nokulinganisa okuqinile komsebenzi kubaluleke ngokulinganayo ukuze kugcinwe ukuphindaphindeka ekucindezelweni kwama-pellet kanye nokuthatha amasampula. Le mikhuba ithuthukisa imiphumela yokuhlaziya kuzinhlelo zokusebenza ze-XRF.
Yiziphi izinyathelo ezinconywayo zokuvimbela ukuqhekeka kwe-pellet ngesikhathi sokulungiselela ukuhlaziywa kwe-XRF?
Ukuze uvimbele ukuqhekeka, sebenzisa i-binder efanele njenge-PVA ekugxilweni okuhle kakhulu futhi uqinisekise ukuthi kuhlanganiswa impuphu kanye ne-binder ngendlela efanayo. Lawula amandla okucindezela ukuze ugweme ukucindezeleka ngokweqile futhi ulawule ukujiya kwe-pellet kanye nobunzima ukuze kube nokujiya okulinganayo. Hlanganisa isampula kahle ngaphambi kokucindezela, bese womisa kahle i-pellet ukuze ususe amaphutha esakhiwo ahlobene nomswakama. Ukugcina imishini yokugaya neyokulinganisa ihlanzekile kunciphisa ukungcola, okungase kubangele amaphuzu okucindezeleka okuholela ekuqhekekeni. Ukunamathela kule mikhuba akugcini nje ngokuthuthukisa ukuqina kokwakheka kwe-pellet kodwa futhi kuthuthukisa ubuqotho be-pellet yesampula kanye nokuphindaphinda kokulinganisa.
Isikhathi sokuthunyelwe: Disemba 11-2025
