I-inline static mixer entsha eguquguqukayo yakhelwe ngqo ukuhlangabezana nezidingo eziqinile ze-high performance liquid chromatography (HPLC) kanye ne-ultra high performance liquid chromatography (HPLC kanye ne-UHPLC). Ukuxubana okungekuhle kwezigaba ezimbili noma ngaphezulu ezihambayo kungabangela isilinganiso esiphezulu sesignali-kuya-kumsindo, okunciphisa ukuzwela. Ukuxubana okuqinile okufana kwama-fluid amabili noma ngaphezulu anevolumu yangaphakathi encane kanye nobukhulu obungokomzimba be-static mixer kumelela izinga eliphakeme kakhulu le-static mixer efanele. I-static mixer entsha ifinyelela lokhu ngokusebenzisa ubuchwepheshe obusha bokuphrinta be-3D ukudala isakhiwo esiyingqayizivele se-3D esihlinzeka ngokuxubana okuqinile kwe-hydrodynamic okuthuthukisiwe kanye nokunciphisa okuphezulu kakhulu kwe-base sine wave ngeyunithi ngayinye yevolumu yangaphakathi yengxube. Ukusebenzisa i-1/3 yevolumu yangaphakathi ye-common mixer kunciphisa i-basic sine wave ngo-98%. I-mixer iqukethe iziteshi zokugeleza ze-3D ezixhunyiwe ezinezindawo ezihlukene ze-cross-sectional kanye nobude bendlela njengoba uketshezi ludlula ama-geometries ayinkimbinkimbi e-3D. Ukuxubana ezindleleni eziningi zokugeleza ezi-tortuous, kuhlanganiswe ne-turbulence yendawo kanye ne-eddies, kuphumela ekuxubeni ezikalini ezincane, ze-meso kanye neze-macro. Lo mxube oyingqayizivele wenzelwe ukusebenzisa ukulingisa kwe-computational fluid dynamics (CFD). Idatha yokuhlola eyethulwe ikhombisa ukuthi ukuxuba okuhle kakhulu kufezwa ngevolumu yangaphakathi encane.
Sekuyiminyaka engaphezu kwengu-30, i-chromatography yoketshezi isetshenziswe ezimbonini eziningi, okuhlanganisa imithi, izibulala-zinambuzane, ukuvikelwa kwemvelo, i-forensics, kanye nokuhlaziywa kwamakhemikhali. Ikhono lokulinganisa izingxenye ngesigidi noma ngaphansi libalulekile ekuthuthukisweni kobuchwepheshe kunoma yimuphi umkhakha. Ukusebenza kahle kokuxuba kuholela esilinganisweni esibi sesignali kuya kumsindo, okuyinto ecasulayo emphakathini we-chromatography ngokwemikhawulo yokuthola kanye nokuzwela. Lapho uxuba izinyibilikisi ezimbili ze-HPLC, ngezinye izikhathi kuyadingeka ukuphoqa ukuxuba ngezindlela zangaphandle ukuze uhlanganise izinyibilikisi ezimbili ngendlela efanayo ngoba ezinye izinyibilikisi azihlangani kahle. Uma izinyibilikisi zingaxubene kahle, ukuwohloka kwe-chromatogram ye-HPLC kungase kwenzeke, kuzibonakalise njengomsindo wesisekelo oweqile kanye/noma ukuma kwe-peak okubi. Ngokuxuba okubi, umsindo wesisekelo uzovela njengegagasi le-sine (elikhuphukayo neliwelayo) lesignali yokubona ngokuhamba kwesikhathi. Ngesikhathi esifanayo, ukuxuba okubi kungaholela ekukhuleni nasekuphakameni okungalingani, kunciphisa ukusebenza kokuhlaziya, ukuma kwe-peak, kanye nesisombululo se-peak. Imboni iqaphele ukuthi izingxube ezi-in-line kanye ne-tee static ziyindlela yokuthuthukisa le mikhawulo nokuvumela abasebenzisi ukuthi bafinyelele imikhawulo ephansi yokuthola (ukuzwela). I-mixer emile efanele ihlanganisa izinzuzo zokusebenza kahle kokuxuba, ivolumu ephansi yokufa kanye nokwehla kwengcindezi ephansi kanye nevolumu encane kanye nokusetshenziswa okuphezulu kwesistimu. Ngaphezu kwalokho, njengoba ukuhlaziya kuba nzima kakhulu, abahlaziyi kumele basebenzise njalo izinyibilikisi ezi-polar nezinzima ukuzixuba. Lokhu kusho ukuthi ukuxuba okungcono kuyimfuneko ekuhlolweni kwesikhathi esizayo, okwandisa isidingo sokuklama nokusebenza okuhle kakhulu kwe-mixer.
Muva nje iMott isungule uhla olusha lwezixube eziqinile ze-PerfectPeakTM ezinelungelo lobunikazi ezinezivolumu ezintathu zangaphakathi: 30 µl, 60 µl kanye no-90 µl. Lawa masayizi amboza ububanzi bezinto eziguquguqukayo kanye nezici zokuxuba ezidingekayo ezivivinyweni eziningi ze-HPLC lapho kudingeka khona ukuxuba okuthuthukisiwe kanye nokuhlakazeka okuphansi. Wonke amamodeli amathathu anobubanzi obungu-0.5″ futhi aletha ukusebenza okuhamba phambili embonini kumklamo ohlangene. Zenziwe ngensimbi engagqwali engu-316L, ezingasebenzi ngenxa yokungangeni, kodwa i-titanium kanye nezinye izinsimbi zensimbi ezingagqwali futhi ezingangenisi amakhemikhali nazo ziyatholakala. Laba baxubi banengcindezi yokusebenza ephezulu efika ku-20,000 psi. Ku-Fig. 1a kunesithombe se-60 µl Mott static mixer eyenzelwe ukuhlinzeka ngokusebenza kahle kokuxuba ngenkathi isebenzisa ivolumu encane yangaphakathi kunezixube ezijwayelekile zalolu hlobo. Lo mklamo omusha we-static mixer usebenzisa ubuchwepheshe obusha bokukhiqiza okungeziwe ukudala isakhiwo esiyingqayizivele se-3D esisebenzisa ukugeleza okuncane kwangaphakathi kunanoma yimuphi umxube osetshenziswa njengamanje embonini ye-chromatography ukuze kufezwe ukuxuba okuqinile. Ama-mixer anjalo aqukethe iziteshi zokugeleza ezihlanganisiwe ezinobukhulu obuthathu ezinezindawo ezahlukene ze-cross-section kanye nobude bezindlela ezahlukene njengoba uketshezi luwela izithiyo zejiyometri eziyinkimbinkimbi ngaphakathi. Ku-Fig. Isithombe 1b sibonisa umdwebo we-schematic we-mixer entsha, esebenzisa ukufakwa kokucindezela kwe-HPLC okujwayelekile kwemboni okungu-10-32 kokungena kanye nokuphuma, futhi inemingcele eluhlaza okwesibhakabhaka enombala we-patent internal mixer port. Izindawo ezahlukene ze-cross-section zezindlela zokugeleza kwangaphakathi kanye nezinguquko ekuqondeni kokugeleza ngaphakathi kwevolumu yokugeleza kwangaphakathi kudala izindawo zokugeleza okuguquguqukayo nokune-laminar, okubangela ukuxubana ezikalini ezincane, ze-meso kanye neze-macro. Umklamo walo mxube oyingqayizivele usebenzise ukulingisa kwe-computational fluid dynamics (CFD) ukuhlaziya amaphethini okugeleza nokulungisa umklamo ngaphambi kokwenza i-prototyping yokuhlola ukuhlaziya kwangaphakathi kanye nokuhlolwa kwensimu yamakhasimende. Ukukhiqiza okungeziwe kuyinqubo yokuphrinta izingxenye ze-geometric ze-3D ngqo kusuka kumidwebo ye-CAD ngaphandle kwesidingo somshini wendabuko (imishini yokugaya, ama-lathe, njll.). Lawa ma-mixer amasha aqinile aklanyelwe ukukhiqizwa kusetshenziswa le nqubo, lapho umzimba womxube udalwa kusuka kumidwebo ye-CAD futhi izingxenye zenziwe (ziphrintiwe) ungqimba ngengqimba kusetshenziswa ukukhiqiza okungeziwe. Lapha, kufakwa ungqimba lwempuphu yensimbi oluyi-microns ezingama-20 ubukhulu, bese kuthi i-laser elawulwa yikhompyutha incibilikise ngokukhetha bese ihlanganisa impuphu ibe yifomu eqinile. Faka olunye ungqimba phezu kwalolu ungqimba bese ufaka i-laser sintering. Phinda le nqubo kuze kube yilapho ingxenye isiqediwe ngokuphelele. Impuphu isuswa engxenyeni engaboshiwe nge-laser, kushiye ingxenye ephrintiwe nge-3D ehambisana nomdwebo wokuqala we-CAD. Umkhiqizo wokugcina ufana kancane nenqubo ye-microfluidic, umehluko omkhulu ukuthi izingxenye ze-microfluidic zivame ukuba nezinhlangothi ezimbili (eziyisicaba), ngenkathi kusetshenziswa ukukhiqizwa okungeziwe, amaphethini okugeleza ayinkimbinkimbi angadalwa nge-geometry enezinhlangothi ezintathu. Lawa ma-faucet okwamanje atholakala njengezingxenye eziphrintiwe nge-3D ngensimbi engagqwali engu-316L kanye ne-titanium. Iningi lama-alloy ensimbi, ama-polymers kanye nezinye izinto zobumba zingasetshenziswa ukwenza izingxenye kusetshenziswa le ndlela futhi zizocatshangelwa emiklamo/imikhiqizo yesikhathi esizayo.
Ilayisi. 1. Isithombe (a) kanye nomdwebo (b) womxube oqinile we-90 μl Mott obonisa ingxenye ephambene yendlela yokugeleza koketshezi lomxube enombala oluhlaza okwesibhakabhaka.
Sebenzisa ukulingiswa kwe-computational fluid dynamics (CFD) kokusebenza kwe-static mixer ngesikhathi sesigaba sokuklama ukusiza ukuthuthukisa imiklamo ephumelelayo nokunciphisa ukuhlolwa kwe-trial-and-er okubizayo okuthatha isikhathi futhi okubizayo. Ukulingiswa kwe-CFD kwabaxubi be-static kanye namapayipi ajwayelekile (ukulingiswa okungena-mixer) usebenzisa iphakheji yesofthiwe ye-COMSOL Multiphysics. Ukumodela usebenzisa i-pressure-driven pressure fluid mechanics ukuqonda ijubane loketshezi kanye nengcindezi ngaphakathi kwengxenye. Lokhu kuguquguquka koketshezi, kuhlanganiswe nokuthuthwa kwamakhemikhali kwama-compounds esigaba esihambayo, kusiza ukuqonda ukuxubana koketshezi oluhlanganisiwe oluhlukene oluhlukene. Imodeli ifundwa njengomsebenzi wesikhathi, olingana nemizuzwana eyi-10, ukuze kube lula ukubala ngenkathi kuseshwa izixazululo ezifanayo. Idatha yethiyori itholakale ocwaningweni oluhlobene nesikhathi kusetshenziswa ithuluzi lokuphrojektha le-point probe, lapho iphuzu eliphakathi nendawo yokuphuma lakhethwa khona ukuze kuqoqwe idatha. Imodeli ye-CFD kanye nokuhlolwa kokuhlola kusebenzise izinyibilikisi ezimbili ezihlukene nge-valve yokusampula elinganayo kanye nesistimu yokupompa, okuholela epulakini yokufaka esikhundleni se-solvent ngayinye emgqeni wokuthatha isampula. Lezi zinyibilikisi bese zixutshwa ku-static mixer. Izibalo 2 no-3 zibonisa ukulingisa ukugeleza ngokusebenzisa ipayipi elijwayelekile (elingenawo umxube) kanye ne-Mott static mixer, ngokulandelana. Ukulingisa kwaqhutshwa kuthubhu eliqondile elingamasentimitha angu-5 ubude kanye ne-0.25 mm ID ukuze kuboniswe umqondo wokushintshana kwama-plug amanzi kanye ne-acetonitrile emsulwa kuthubhu ngaphandle komxube oqinile, njengoba kuboniswe kuMfanekiso 2. Ukulingisa kusetshenziswe ubukhulu obuqondile bethubhu kanye ne-mixer kanye nesilinganiso sokugeleza esingu-0 .3 ml/min.
Ilayisi. 2. Ukulingisa ukugeleza kwe-CFD epayipini elingu-5 cm elinobubanzi bangaphakathi obungu-0.25 mm ukumela okwenzeka epayipini le-HPLC, okungukuthi uma kungekho mshini wokuxuba. Ubomvu obugcwele bumelela ingxenye enkulu yamanzi. Okuluhlaza okwesibhakabhaka kumelela ukuntuleka kwamanzi, okungukuthi i-acetonitrile emsulwa. Izindawo zokusabalalisa zingabonakala phakathi kwama-plug ashintshanayo oketshezi olubili oluhlukene.
Ilayisi. 3. I-mixer engaguquki enomthamo ongu-30 ml, efakwe kumodeli kuphakheji yesofthiwe ye-COMSOL CFD. Inganekwane imelela ingxenye enkulu yamanzi ku-mixer. Amanzi ahlanzekile aboniswa ngombala obomvu kanye ne-acetonitrile emsulwa ngombala oluhlaza okwesibhakabhaka. Ushintsho engxenyeni enkulu yamanzi alingisiwe lumelelwa ushintsho kumbala wokuxuba uketshezi olubili.
Ku-fig. 4 kukhombisa ucwaningo lokuqinisekisa imodeli yokuhlobana phakathi kokusebenza kahle kokuxuba kanye nevolumu yokuxuba. Njengoba ivolumu yokuxuba ikhula, ukusebenza kahle kokuxuba kuzokhula. Ngokwazi kwababhali, amanye amandla ayinkimbinkimbi asebenza ngaphakathi kwe-mixer awakwazi ukubalwa kulo modeli we-CFD, okuholela ekusebenzeni kahle kokuxuba okuphezulu ezivivinyweni zokuhlola. Ukusebenza kahle kokuxuba kokuhlola kwalinganiswa njengokunciphisa kwamaphesenti ku-base sinusoid. Ngaphezu kwalokho, ukucindezela komhlane okwandisiwe kuvame ukuholela emazingeni aphezulu okuxuba, angacatshangelwa ekulingiseni.
Izimo ezilandelayo ze-HPLC kanye nokusethwa kokuhlolwa kusetshenziswe ukukala amagagasi e-sine aluhlaza ukuqhathanisa ukusebenza okuhlobene kwama-mixer ahlukene aqinile. Umdwebo ku-Figure 5 ukhombisa ukwakheka kwesistimu ye-HPLC/UHPLC ejwayelekile. I-mixer ezinzile ihlolwe ngokubeka i-mixer ngqo ngemuva kwephampu nangaphambi kwekholomu ye-injector kanye ne-separation. Izilinganiso eziningi ze-sinusoidal zangemuva zenziwa ngokudlula ikholomu ye-injector kanye ne-capillary phakathi kwe-mixer ezinzile kanye ne-UV detector. Lapho kuhlolwa isilinganiso sesignali-kuya-kumsindo kanye/noma kuhlaziywa ukuma kwe-peak, ukucushwa kwesistimu kuboniswe ku-Figure 5.
Isithombe 4. Isakhiwo sokusebenza kahle kokuxuba uma kuqhathaniswa nevolumu yokuxuba yezinhlobo ezahlukene ze-static mixers. Ukungcola okungokwemfundiso kulandela umkhuba ofanayo nedatha yokungcola yokuhlola eqinisekisa ubuqiniso be-CFD simulations.
Uhlelo lwe-HPLC olusetshenziswe kulolu vivinyo kwakuyi-Agilent 1100 Series HPLC ene-UV detector elawulwa yi-PC esebenzisa isofthiwe ye-Chemstation. Ithebula 1 libonisa izimo ezijwayelekile zokulungisa zokulinganisa ukusebenza kahle kwe-mixer ngokuqapha ama-sinusoids ayisisekelo ezifundweni ezimbili zamacala. Ukuhlolwa kokuhlola kwenziwe ezibonelweni ezimbili ezahlukene zamakhemikhali. Amakhemikhali amabili axutshwe esimweni soku-1 kwakuyi-solvent A (20 mM ammonium acetate emanzini acwebezelwe) kanye ne-solvent B (80% acetonitrile (ACN)/20% amanzi acwebezelwe). Esigabeni sesi-2, i-solvent A yayiyisisombululo se-acetone engu-0.05% (ilebula) emanzini acwebezelwe. I-solvent B iyinhlanganisela ye-methanol engu-80/20% namanzi. Esigabeni soku-1, ipompo yabekwa esilinganisweni sokugeleza esingu-0.25 ml/min kuya ku-1.0 ml/min, kanti esimweni sesi-2, ipompo yabekwa esilinganisweni sokugeleza esingaguquki esingu-1 ml/min. Kuzo zombili izimo, isilinganiso sengxube ye-solvents u-A no-B sasingu-20% A/80% B. I-detector isethwe ku-220 nm esimweni 1, kanti ukumuncwa okuphezulu kwe-acetone esimweni 2 kusethwe ku-wavelength engu-265 nm.
Ithebula 1. Ukucushwa kwe-HPLC Kwamacala 1 no-2 Icala 1 Icala 2 Isivinini sephampu 0.25 ml/min kuya ku-1.0 ml/min Isixazululo 1.0 ml/min Isixazululo A 20 mM ammonium acetate emanzini acwebezelwe 0.05% I-Acetone emanzini acwebezelwe Isixazululo B 80% I-Acetonitrile (ACN) / 20% amanzi acwebezelwe 80% i-methanol / 20% amanzi acwebezelwe Isilinganiso sesisombululo 20% A / 80% B 20% A / 80% I-B Detector 220 nm 265 nm
Ilayisi. 6. Imidwebo yamagagasi axubile alinganiswe ngaphambi nangemva kokusebenzisa isihlungi esidlula phansi ukususa izingxenye zokukhukhuleka eziyisisekelo zesignali.
Isithombe 6 siyisibonelo esijwayelekile somsindo wesisekelo oxubile ku-Case 1, oboniswa njengephethini ye-sinusoidal ephindaphindayo ebekwe phezu kwe-baseline drift. I-Baseline drift iwukukhula noma ukwehla kancane kwesignali yangemuva. Uma uhlelo lungavunyelwe ukulingana isikhathi eside ngokwanele, luvame ukuwa, kodwa luzohamba ngokungahleliwe ngisho noma uhlelo luzinzile ngokuphelele. Lokhu kudonsa kwesisekelo kuvame ukwanda lapho uhlelo lusebenza ezimweni ze-gradient ejulile noma ezimweni zokucindezela okuphezulu emuva. Uma lokhu kudonsa kwesisekelo kukhona, kungaba nzima ukuqhathanisa imiphumela kusuka kusampula kuya kusampula, okunganqotshwa ngokusebenzisa isihlungi se-low-pass kudatha eluhlaza ukuze kuhlungwe lokhu kuguquguquka kwemvamisa ephansi, ngaleyo ndlela kuhlinzekwe ngesakhiwo sokuzulazula esine-baseline eyisicaba. Ku-Fig. Isithombe 6 sibonisa futhi i-story yomsindo wesisekelo womxube ngemuva kokusebenzisa isihlungi se-low-pass.
Ngemva kokuqeda ukulingiswa kwe-CFD kanye nokuhlolwa kokuqala kokuhlola, kwathuthukiswa abaxubi abathathu abahlukene be-static kusetshenziswa izingxenye zangaphakathi ezichazwe ngenhla ngamavolumu amathathu angaphakathi: 30 µl, 60 µl kanye no-90 µl. Lolu hlu luhlanganisa ububanzi bamavolumu kanye nokusebenza kokuxuba okudingekayo kwezicelo ze-HPLC eziphansi zokuhlaziya lapho ukuxuba okuthuthukisiwe kanye nokuhlakazeka okuphansi kudingeka khona ukukhiqiza izisekelo eziphansi ze-amplitude. Ku-Fig. 7 kukhombisa izilinganiso eziyisisekelo ze-sine wave ezitholwe ohlelweni lokuhlola lweSibonelo 1 (i-acetonitrile kanye ne-ammonium acetate njenge-tracers) ngamavolumu amathathu abaxubi be-static futhi kungekho abaxubi abafakiwe. Izimo zokuhlola zokuhlola zemiphumela eboniswe ku-Figure 7 zigcinwe zinjalo kuzo zonke izivivinyo ezine ngokwenqubo echazwe kuThebula 1 ngesilinganiso sokugeleza kwe-solvent esingu-0.5 ml/min. Sebenzisa inani le-offset kumasethi edatha ukuze aboniswe eceleni ngaphandle kokugqagqana kwesignali. I-Offset ayithinti ubukhulu besignali esetshenziselwa ukwahlulela izinga lokusebenza lomxube. Isilinganiso se-amplitude ye-sinusoidal ngaphandle kwe-mixer sasingu-0.221 mAi, kuyilapho i-amplitude yabaxubi be-Mott abangashintshi ku-30 ​​µl, 60 µl, kanye no-90 µl yehle yaya ku-0.077, 0.017, kanye no-0.004 mAi, ngokulandelana.
Umfanekiso 7. I-HPLC UV Detector Signal Offset vs. Isikhathi Secala 1 (i-acetonitrile ene-ammonium acetate indicator) ekhombisa ukuxubana kwe-solvent ngaphandle kwe-mixer, ama-mixer e-Mott angu-30 µl, 60 µl kanye no-90 µl abonisa ukuxubana okuthuthukisiwe (i-amplitude yesignali ephansi) njengoba ivolumu ye-mixer engaguquki ikhuphuka. (ukushintshaniswa kwedatha yangempela: 0.13 (akukho mixer), 0.32, 0.4, 0.45mA ukuze kuboniswe kangcono).
Idatha eboniswe ku-Fig. 8 iyafana nese-Fig. 7, kodwa kulokhu ifaka imiphumela yabaxubi abathathu be-HPLC static abasetshenziswa kakhulu abanevolumu yangaphakathi engu-50 µl, 150 µl kanye no-250 µl. Ilayisi. Isithombe 8. I-HPLC UV Detector Signal Offset vs Time Plot for Case 1 (Acetonitrile kanye ne-Ammonium Acetate njengezinkomba) ekhombisa ukuxubana kwe-solvent ngaphandle kwe-static mixer, uchungechunge olusha lwabaxubi be-Mott static, kanye nabaxubi abathathu abavamile (i-data offset yangempela ingu-0.1 (ngaphandle kwe-mixer), 0.32, 0.48, 0.6, 0.7, 0.8, 0.9 mA ngokulandelana ukuze kube nomphumela wokubonisa ongcono). Ukunciphisa amaphesenti e-base sine wave kubalwa ngesilinganiso se-amplitude ye-sine wave kuya ku-amplitude ngaphandle kwe-mixer efakiwe. Amaphesenti okuncishiswa kwe-sine wave okulinganisiwe kwamacala 1 no-2 abhalwe kuThebula 2, kanye namavolumu angaphakathi e-static mixer entsha kanye nabaxubi abajwayelekile abayisikhombisa abavame ukusetshenziswa embonini. Idatha ekuZithombeni 8 no-9, kanye nezibalo ezethulwe kuThebula 2, zibonisa ukuthi i-Mott Static Mixer inganikeza ukuncishiswa kwe-sine wave okufika ku-98.1%, okudlula kakhulu ukusebenza komxubi ojwayelekile we-HPLC ngaphansi kwalezi zimo zokuhlola. Isibalo 9. I-HPLC UV detector signal offset versus time plot yecala 2 (i-methanol kanye ne-acetone njenge-tracers) ekhombisa ukungabikho komxubi oqinile (okuhlanganisiwe), uchungechunge olusha lwabaxubi abaqinile be-Mott kanye nabaxubi ababili abavamile (i-data offsets yangempela ingu-0, 11 (ngaphandle komxubi.), 0.22, 0.3, 0.35 mA kanye nokuboniswa okungcono). Abaxubi abayisikhombisa abavame ukusetshenziswa embonini nabo bahlolwe. Lokhu kufaka phakathi abaxubi abanezinhlobo ezintathu zangaphakathi ezihlukene ezivela enkampanini A (i-Mixer ekhethiwe A1, A2 kanye ne-A3) kanye nenkampani B (i-Mixer ekhethiwe B1, B2 kanye ne-B3). Inkampani C ilinganise usayizi owodwa kuphela.
Ithebula 2. Izici Zokuxuba Ezingaguquki kanye Nomthamo Wangaphakathi Ikesi Lokuxuba Okungaguquki 1 Ukubuyiselwa Kwesinoyidi: Ukuhlolwa Kwe-Acetonitrile (Ukusebenza Kahle) Ikesi 2 Ukubuyiselwa Kwesinoyidi: Ukuhlolwa Kwamanzi Kwe-Methanol (Ukusebenza Kahle) Umthamo Wangaphakathi (µl) Akukho Mxubi – - 0 Mott 30 65% 67.2% 30 Mott 60 92.2% 91.3% 60 Mott 90 98.1% 97.5% 90 Umxubi A1 66.4% 73.7% 50 Umxubi A2 89.8% 91.6% 150 Umxubi A3 92.2% 94.5% 250 Umxubi B1 44.8% 45.7% 9 35 Umxubi B2 845.% 96.2% 370 Umxubi C 97.2% 97.4% 250
Ukuhlaziywa kwemiphumela kuMfanekiso 8 kanye neThebula 2 kukhombisa ukuthi i-30 µl Mott static mixer inokusebenza kahle kokuxuba okufanayo ne-A1 mixer, okungukuthi i-50 µl, nokho, i-30 µl Mott inomthamo wangaphakathi ongaphansi ngo-30%. Uma kuqhathaniswa i-60 µl Mott mixer ne-150 µl yangaphakathi ye-A2 mixer, kube nokuthuthuka okuncane ekusebenzeni kahle kokuxuba okungu-92% uma kuqhathaniswa no-89%, kodwa okubaluleke kakhulu, leli zinga eliphakeme lokuxuba lafinyelelwa ku-1/3 yevolumu ye-mixer. Ukusebenza kwe-90 µl Mott mixer kwalandela umkhuba ofanayo ne-A3 mixer enevolumu yangaphakathi engu-250 µl. Ukuthuthuka ekusebenzeni kokuxuba okungu-98% no-92% kwabonwa futhi ngokunciphisa okuphindwe kathathu kwevolumu yangaphakathi. Imiphumela efanayo kanye nokuqhathaniswa kwatholakala kubaxubi B no-C. Ngenxa yalokho, uchungechunge olusha lwabaxubi abangaguquki i-Mott PerfectPeakTM lunikeza ukusebenza kahle kokuxuba okuphezulu kunabaxubi abancintisana nabo abafanayo, kodwa ngevolumu encane yangaphakathi, enikeza umsindo wangemuva ongcono kanye nesilinganiso esingcono sesignali kuya komsindo, i-Analyte yokuzwela engcono, ukuma kwe-peak kanye nesinqumo se-peak. Izitayela ezifanayo ekusebenzeni kahle kokuxuba zabonwa kuzo zombili izifundo ze-Case 1 kanye ne-Case 2. Kwi-Case 2, kwenziwa izivivinyo kusetshenziswa (i-methanol ne-acetone njengezinkomba) ukuqhathanisa ukusebenza kahle kokuxuba kwe-60 ml Mott, i-mixer efana ne-A1 (ivolumu yangaphakathi engu-50 µl) kanye ne-mixer efanayo B1 (ivolumu yangaphakathi engu-35 µl). , ukusebenza kwakukubi ngaphandle kokufakwa kwe-mixer, kodwa yasetshenziselwa ukuhlaziya okuyisisekelo. I-mixer ye-Mott engu-60 ml ibonakale iyi-mixer engcono kakhulu eqenjini lokuhlola, inikeze ukwanda okungu-90% ekusebenzeni kahle kokuxuba. I-Mixer A1 efanayo ibone ukuthuthuka okungu-75% ekusebenzeni kahle kokuxuba kwalandelwa ukuthuthuka okungu-45% ku-mixer efanayo ye-B1. Ukuhlolwa okuyisisekelo kokunciphisa i-sine wave ngesilinganiso sokugeleza kwenziwa ochungechungeni lwabaxubi ngaphansi kwezimo ezifanayo nokuhlolwa kwe-sine curve ku-Case 1, kanti izinga lokugeleza kuphela elishintshile. Idatha ibonise ukuthi ebangeni lamazinga okugeleza kusukela ku-0.25 kuya ku-1 ml/min, ukwehla kokuqala kwe-sine wave kwahlala kungaguquki kuwo wonke amavolumu amathathu okuxuba. Kumaxubi amabili amancane omthamo, kukhona ukwanda okuncane kokugoba kwe-sinusoidal njengoba izinga lokugeleza lehla, okulindeleke ngenxa yesikhathi sokuhlala esengeziwe se-solvent ku-mixer, okuvumela ukwanda kokuxubana kokusabalalisa. Ukususwa kwe-sine wave kulindeleke ukuthi kwande njengoba ukugeleza kuncipha kakhulu. Kodwa-ke, kumthamo omkhulu wokuxuba one-sine wave base attenuation ephezulu kakhulu, i-sine wave base attenuation yahlala ingashintshi (ngaphakathi kobubanzi bokungaqiniseki kokuhlola), ngamanani asukela ku-95% kuya ku-98%. Ilayisi. 10. Ukunciphisa okuyisisekelo kwesilinganiso se-sine wave uma kuqhathaniswa nesilinganiso sokugeleza esimweni 1. Ukuhlolwa kwenziwe ngaphansi kwezimo ezifana nokuhlolwa kwe-sine ngesilinganiso sokugeleza esiguquguqukayo, kufakwe u-80% wengxube engu-80/20 ye-acetonitrile namanzi kanye no-20% we-20 mM ammonium acetate.
Uhla olusha oluthuthukisiwe lwezixube eziqinile ze-PerfectPeakTM ezinelungelo lobunikazi ezinezivolumu ezintathu zangaphakathi: 30 µl, 60 µl kanye no-90 µl luhlanganisa ububanzi bokusebenza komthamo kanye nokuxuba obudingekayo ekuhlaziyeni okuningi kwe-HPLC okudinga ukuxuba okuthuthukisiwe kanye nezitezi eziphansi zokuhlakazeka. I-static mixer entsha ifinyelela lokhu ngokusebenzisa ubuchwepheshe obusha bokuphrinta be-3D ukudala isakhiwo esiyingqayizivele se-3D esihlinzeka ngokuxuba okuqinile kwe-hydrodynamic okuthuthukisiwe kanye nokunciphisa okuphezulu komsindo wesisekelo ngevolumu yeyunithi ngayinye yengxube yangaphakathi. Ukusebenzisa i-1/3 yevolumu yangaphakathi ye-mixer evamile kunciphisa umsindo wesisekelo ngo-98%. Lezi zixube zakhiwa iziteshi zokugeleza ezihlanganisiwe ezinezinhlangothi ezintathu ezinezindawo ezahlukene eziwela phansi kanye nobude obuhlukene bendlela njengoba uketshezi luwela izithiyo zejiyometri eziyinkimbinkimbi ngaphakathi. Umndeni omusha wezixube eziqinile uhlinzeka ngokusebenza okuthuthukisiwe ngaphezu kwezixube ezincintisanayo, kodwa ngevolumu yangaphakathi encane, okuholela esilinganisweni esingcono sesignali-kuya-kumsindo kanye nemikhawulo ephansi yokulinganisa, kanye nokuma okuphezulu, ukusebenza kahle kanye nesisombululo sokuzwela okuphezulu.
Kulolu daba i-Chromatography – I-RP-HPLC enobungani nemvelo – Ukusetshenziswa kwe-chromatography yegobolondo eliyinhloko ukuze kuthathelwe indawo i-acetonitrile nge-isopropanol ekuhlaziyweni nasekuhlanzweni – I-chromatograph entsha yegesi ye…
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