Yehlisa Isisekelo Somsindo Wesistimu Ye-HPLC/UHPLC futhi Khuphula Ukuzwela Nge-3D Ephrintiwe Static Mixer Entsha Yokusebenza Okuphezulu Ephakeme - Februwari 6, 2017 - James C. Steele, Christopher J. Martineau, Kenneth L. Rubow - I-athikili kusayensi ye-Biological News

Isihlanganisi esisha esishintshashintshayo se-inline static siklanyelwe ukuhlangabezana nezidingo eziqinile ze-high performance liquid chromatography (HPLC) kanye ne-ultra high performance liquid chromatography (HPLC ne-UHPLC) izinhlelo.Ukuxutshwa okungalungile kwezigaba zeselula ezimbili noma ngaphezulu kungaholela esilinganisweni esiphezulu sesignali-kuya-nomsindo, okunciphisa ukuzwela.Ukuxuba okulinganayo okumile koketshezi olubili noma ngaphezulu olunomthamo omncane wangaphakathi wevolumu nobukhulu bomzimba bengxube emile kumele izinga eliphezulu kakhulu lengxube emile ekahle.Ingxube entsha emile ifinyelela lokhu ngokusebenzisa ubuchwepheshe obusha bokuphrinta be-3D ukuze kwakhe isakhiwo se-3D esiyingqayizivele esihlinzeka ngokuxubana kwe-hydrodynamic static okuthuthukisiwe okunokwehliswa okuphezulu kwephesenti le-base wave ye-sine ngeyunithi ngayinye yevolumu yangaphakathi yengxube.Ukusebenzisa i-1/3 yevolumu yangaphakathi ye-mixer evamile kunciphisa i-sine wave eyisisekelo ngo-98%.I-mixer iqukethe amashaneli okugeleza kwe-3D axhumene anezindawo ezihlukene ezihlukene kanye nobude bendlela njengoba uketshezi lunqamula amajiyometri e-3D ayinkimbinkimbi.Ukuxuba ezindleleni eziningi zokugeleza ezihlukumezayo, kuhlanganiswe nesiyaluyalu sendawo kanye nama-eddies, kuphumela ekuxubeni esikalini esincane, se-meso kanye ne-macro.Le mixer eyingqayizivele yakhelwe kusetshenziswa ukulingiswa kwe-computational fluid dynamics (CFD).Idatha yokuhlola eyethulwa ibonisa ukuthi ukuxuba okuhle kakhulu kufinyelelwa ngevolumu yangaphakathi encane.
Sekuyiminyaka engaphezu kwengama-30, i-chromatography eyi-liquid isetshenziswa ezimbonini eziningi, kufaka phakathi ezemithi, izibulala-zinambuzane, ukuvikelwa kwemvelo, i-forensics, nokuhlaziywa kwamakhemikhali.Ikhono lokukala izingxenye ngesigidi noma ngaphansi libalulekile ekuthuthukisweni kobuchwepheshe kunoma iyiphi imboni.Ukuxubana okungalungile kuholela esilinganisweni esingesihle sesignali-kuya-nomsindo, okucasulayo emphakathini we-chromatography mayelana nemikhawulo yokuthola nokuzwela.Uma uxuba izincibilikisi ezimbili ze-HPLC, ngezinye izikhathi kuyadingeka ukuphoqa ukuxuba ngezindlela zangaphandle ukuze wenze i-homogenize izincibilikisi ezimbili ngoba ezinye izincibilikisi azihlangani kahle.Uma izincibilikisi zingaxubene kahle, ukuwohloka kwechromatogram ye-HPLC kungase kwenzeke, kubonakale njengomsindo oyisisekelo owedlulele kanye/noma ukuma kwesiqongo esingesihle.Ngokuxutshwa okungalungile, umsindo oyisisekelo uzovela njengegagasi le-sine (elikhuphukayo nelihlayo) lesiginali yomtshina ngokuhamba kwesikhathi.Ngesikhathi esifanayo, ukuxubana okungalungile kungaholela ekwandiseni nasekuphakameni kwe-asymmetric, ukunciphisa ukusebenza kokuhlaziya, ukuma okuphezulu, nokulungiswa okuphezulu.Imboni ibonile ukuthi izixube eziku-line kanye ne-tee static ziyindlela yokuthuthukisa le mikhawulo futhi zivumele abasebenzisi ukuthi bathole imikhawulo ephansi yokuthola (ukuzwela).I-static mixer ekahle ihlanganisa izinzuzo zokusebenza kahle kokuxubana, ivolumu ephansi efile kanye nokwehla kokucindezela okuphansi ngevolumu encane kanye nokuphuma okuphezulu kwesistimu.Ukwengeza, njengoba ukuhlaziya kuba nzima kakhulu, abahlaziyi kufanele basebenzise njalo izincibilikisi ezipholile ezimhlophe nezinzima ukuzixuba.Lokhu kusho ukuthi ukuxuba okungcono kuyadingeka ukuze kuhlolwe isikhathi esizayo, kuqhubeke kwandise isidingo sokuklama nokusebenza kwezixube ezisezingeni eliphezulu.
I-Mott isanda kuthuthukisa uhla olusha lwezixube ezimile ezimile ze-PerfectPeak TM ezinamavolumu amathathu angaphakathi: 30 µl, 60 µl kanye no-90 µl.Lawa masayizi ahlanganisa ububanzi bevolumu nezici zokuhlanganisa ezidingekayo ekuhlolweni okuningi kwe-HPLC lapho ukuxuba okuthuthukisiwe nokuhlakazeka okuphansi kuyadingeka.Womathathu amamodeli anobubanzi obungu-0.5″ futhi aletha ukusebenza okuhamba phambili embonini ngedizayini ehlangene.Zenziwe ngensimbi engagqwali engu-316L, idluliselwe ukungangeni, kodwa i-titanium namanye ama-alloys ensimbi angagqwali futhi angenamakhemikhali ayatholakala.Lezi zixube zinengcindezi yokusebenza ephezulu efika ku-20,000 psi.Emkhiwaneni.I-1a iyisithombe se-60 µl Mott static mixer eklanyelwe ukunikeza ukusebenza kahle kokuxubana kuyilapho kusetshenziswa ivolomu yangaphakathi encane kunezixube ezijwayelekile zalolu hlobo.Lo mklamo omusha we-static mixer usebenzisa ubuchwepheshe obusha bokukhiqiza okungeziwe ukuze udale isakhiwo se-3D esiyingqayizivele esisebenzisa ukugeleza kwangaphakathi okuncane kunanoma iyiphi i-mixer esetshenziswa njengamanje embonini ye-chromatography ukuze kuzuzwe ukuxuba okumile.Izixube ezinjalo zihlanganisa amashaneli okugeleza ezinhlangothi ezintathu axhumene anezindawo ezihlukene eziphambanayo kanye nobude bendlela obuhlukene njengoba uketshezi luwela izithiyo zejiyomethri eziyinkimbinkimbi ngaphakathi.Emkhiwaneni.Umfanekiso 1b ubonisa umdwebo oyisikimu we-mixer entsha, esebenzisa okokuminyanisa okujwayelekile komkhakha okungu-10-32 kwe-HPLC yokufaka nokuphumayo, futhi enemingcele eluhlaza okwesibhakabhaka enomthunzi wembobo yokuhlanganisa yangaphakathi enelungelo lobunikazi.Izindawo ezihlukene eziphambanayo zezindlela zokugeleza zangaphakathi kanye nezinguquko endleleni yokugeleza ngaphakathi kwevolumu yokugeleza kwangaphakathi kudala izifunda zokugeleza kwe-turbulent kanye ne-laminar, okubangela ukuxuba esikalini esincane, se-meso kanye ne-macro.Idizayini yale mixer eyingqayizivele isebenzise ukulingiswa kwe-computational fluid dynamics (CFD) ukuze kuhlaziywe amaphethini okugeleza futhi kucwengisise idizayini ngaphambi kokwenziwa kwe-prototyping yokuhlola kokuhlaziya kwangaphakathi nokuhlola insimu yekhasimende.Ukukhiqiza okungeziwe kuyinqubo yokuphrinta izingxenye zejiyomethri ze-3D ngokuqondile kusuka kumidwebo ye-CAD ngaphandle kwesidingo somshini wendabuko (imishini yokugaya, ama-lathes, njll.).Lezi zixube ezintsha ezimile zenzelwe ukwakhiwa kusetshenziswa le nqubo, lapho umzimba wokuhlanganisa udalwa kusuka kumidwebo ye-CAD futhi izingxenye zenziwe (eziphrintiwe) ungqimba kusetshenziswa ukukhiqizwa okungeziwe.Lapha, ungqimba lwempushana yensimbi oluwugqinsi olulinganiselwa kuma-microns angu-20 luyafakwa, futhi i-laser elawulwa ngekhompiyutha iyancibilika ngokukhetha bese ihlanganisa impushana ibe yifomu eliqinile.Faka esinye isendlalelo phezu kwalesi sendlalelo bese usebenzisa i-laser sintering.Phinda le nqubo kuze kube yilapho ingxenye isiqedwe ngokuphelele.Impushana ibe isikhishwa engxenyeni engaboshiwe ngelaser, kushiye ingxenye ephrintiwe ye-3D efana nomdwebo wokuqala we-CAD.Umkhiqizo wokugcina ucishe ufane nenqubo ye-microfluidic, umehluko omkhulu ukuthi izingxenye ze-microfluidic ngokuvamile zinezinhlangothi ezimbili (flat), kuyilapho kusetshenziswa ukukhiqiza okungeziwe, amaphethini okugeleza ayinkimbinkimbi angadalwa ngejometri enezinhlangothi ezintathu.Lezi zimpompi okwamanje zitholakala njengezingxenye eziphrintiwe ze-3D ku-316L insimbi engagqwali kanye ne-titanium.Iningi lama-alloys ensimbi, ama-polymers kanye nezinye izitsha zobumba kungasetshenziswa ukwenza izingxenye kusetshenziswa le ndlela futhi kuzocatshangelwa emiklamo/imikhiqizo yesikhathi esizayo.
Ilayisi.1. Isithombe (a) nomdwebo (b) we-90 μl Mott static mixer ebonisa ingxenye enqamulayo yendlela yokugeleza koketshezi lwe-mixer enemibala eluhlaza okwesibhakabhaka.
Qalisa ukulingisa kwe-computational fluid dynamics (CFD) yokusebenza kwengxube emile phakathi nesigaba sokuklama ukuze usize ukuthuthukisa amadizayini asebenza kahle nokunciphisa ukuhlola okudla isikhathi nokubizayo namaphutha.Ukulingisa kwe-CFD kwezixube ezimile kanye namapayipi ajwayelekile (ukulingiswa okungahlanganisi) kusetshenziswa iphakheji yesofthiwe ye-COMSOL Multiphysics.Ukumodela kusetshenziswa i-laminar fluid mechanics eqhutshwa yingcindezi ukuze kuqondwe isivinini soketshezi nokucindezela ngaphakathi kwengxenye ethile.Lokhu kuguquguquka koketshezi, kuhlanganiswe nokuthuthwa kwamakhemikhali kwezinhlanganisela zesigaba esihambayo, kusiza ukuqonda ukuxutshwa koketshezi oluningi oluhlukene olubili.Imodeli ifundwa njengomsebenzi wesikhathi, olingana namasekhondi ayi-10, ukuze kube lula ukubala ngenkathi kuseshwa izixazululo ezifanayo.Idatha yetiyetha itholwe ocwaningweni oluhlobene nesikhathi kusetshenziswa ithuluzi lokukhomba iphuzu, lapho iphuzu eliphakathi nendawo lokuphuma likhethelwe ukuqoqwa kwedatha.Imodeli ye-CFD nokuhlola kokuhlola kusebenzise izincibilikisi ezimbili ezihlukene ngevalvu yokusampula yesampula kanye nesistimu yokumpompa, okuholele ekufakweni kwepulaki esikhundleni sesinyibiliki ngasinye emugqeni wesampula.Lezi zinyibilikisi zibe sezixutshwa kumxube omile.Amanani 2 kanye no-3 abonisa ukulingisa kokugeleza ngepayipi elivamile (akukho mixer) kanye ne-Mott static mixer, ngokulandelanayo.Ukulingisa kwakuqhutshwa ngeshubhu eqondile engu-5 cm ubude kanye ne-ID engu-0.25 mm ukuze kuboniswe umqondo wokushintshana kwamapulaki amanzi kanye ne-acetonitrile ehlanzekile kushubhu lapho ingekho i-mixer emile, njengoba kuboniswe kumfanekiso 2. Ukulingisa kusebenzise ubukhulu obuqondile beshubhu ne-mixer kanye nezinga lokugeleza elingu-0 .3 ml/min.
Ilayisi.2. Ukulingisa ukugeleza kwe-CFD kushubhu engu-5 cm enobubanzi bangaphakathi obungu-0.25 mm ukumela okwenzeka kushubhu le-HPLC, okungukuthi uma ingekho i-mixer.Ubomvu obugcwele bumele ingxenye enkulu yamanzi.Okuluhlaza okwesibhakabhaka kumelela ukuntuleka kwamanzi, okungukuthi i-acetonitrile emsulwa.Izifunda zokusabalalisa zingabonwa phakathi kwamapulaki ashintshanayo oketshezi olubili oluhlukene.
Ilayisi.3. Ingxube enganyakazi enevolumu engu-30 ml, efakwe kuphakheji yesofthiwe ye-COMSOL CFD.Inganekwane imelela ingxenye enkulu yamanzi kumxube.Amanzi ahlanzekile aboniswa nge-acetonitrile ebomvu nehlanzekile eluhlaza okwesibhakabhaka.Ushintsho engxenyeni enkulu yamanzi alingisa imelelwa ukushintsha kombala wokuxuba uketshezi olubili.
Emkhiwaneni.I-4 ibonisa isifundo sokuqinisekisa semodeli yokuhlobana phakathi kokusebenza kahle kokuxuba kanye nevolumu yokuxuba.Njengoba umthamo wokuxuba ukhula, ukusebenza kahle kokuxuba kuzokhula.Ngolwazi lwababhali, amanye amandla omzimba ayinkimbinkimbi asebenza ngaphakathi kwe-mixer ngeke abalwe ngawo kule modeli ye-CFD, okuholela ekusebenzeni kahle kokuxubana ekuhlolweni kokuhlola.Ukusebenza kahle kokuxubana kokuhlolwa kukalwe njengokuncishiswa kwephesenti kusisekelo se-sinusoid.Ukwengeza, ukwanda kokucindezela emuva ngokuvamile kubangela amazinga aphezulu okuxuba, anganakwa ekufaniseni.
Izimo ezilandelayo ze-HPLC nokusetha kokuhlolwa kwasetshenziswa ukukala amaza e-sine eluhlaza ukuze kuqhathaniswe ukusebenza okuhlobene kwezixube ezihlukile ezimile.Umdwebo oseMdwebeni 5 ubonisa ukwakheka kwesistimu ye-HPLC/UHPLC evamile.I-mixer emile ihlolwe ngokubeka i-mixer ngokuqondile ngemva kwepompo nangaphambi kwekholomu yokujova neyokuhlukanisa.Izilinganiso eziningi zangemuva ze-sinusoidal zenziwa ngokudlula ikholomu ye-injector kanye ne-capillary phakathi kwe-static mixer nomtshina we-UV.Lapho kuhlolwa isilinganiso sesignali-kuya-nomsindo kanye/noma kuhlaziywa umumo wokuphakama, ukumiswa kwesistimu kuboniswa kuMfanekiso 5.
Umfanekiso 4. Isakhiwo sokuhlanganisa ukusebenza kahle ngokumelene nokuxutshwa kwevolumu yohlu lwabaxube abamile.Ukungcola kwetiyetha kulandela ithrendi efanayo nedatha yokungcola yokuhlola eqinisekisa ukufaneleka kwezifaniso ze-CFD.
Uhlelo lwe-HPLC olusetshenziswe kulokhu kuhlolwa kwakuyi-Agilent 1100 Series HPLC enomtshina we-UV olawulwa yi-PC esebenzisa isofthiwe ye-Chemstation.Ithebula 1 libonisa izimo zokushuna ezijwayelekile zokulinganisa ukusebenza kahle kwe-mixer ngokuqapha ama-sinusoid ayisisekelo ezimweni ezimbili zezifundo.Ukuhlolwa kokuhlola kwenziwa ezibonelweni ezimbili ezihlukene zezincibilikisi.Izinyibilikisi ezimbili ezixutshwe uma kwenzeka okuthi 1 kube yi-solvent A (20 mM ammonium acetate emanzini akhishwe nge-deionized) kanye ne-solvent B (80% acetonitrile (ACN)/20% amanzi akhishwe yi-deionized).Esimweni sesi-2, i-solvent A yayiyisisombululo se-acetone engu-0.05% (ilebula) emanzini angcolile.I-Solvent B iyingxube ye-80/20% ye-methanol namanzi.Uma kwenzeka i-1, ipompo isethelwe izinga lokugeleza lika-0.25 ml / min kuya ku-1.0 ml / min, futhi uma kwenzeka i-2, iphampu isethelwe izinga lokugeleza njalo lika-1 ml / min.Kuzo zombili izimo, isilinganiso sengxube ye-solvents A no-B sasingu-20% A / 80% B. Umtshina usethelwe ku-220 nm esimweni esingu-1, futhi ukumuncwa okuphezulu kwe-acetone uma kwenzeka i-2 isethelwe ku-wavelength engu-265 nm.
Ithebula 1. Ukucushwa kwe-HPLC Kwezimo 1 kanye ne-2 Ikesi 1 Ikesi 2 Isivinini Sephampu 0.25 ml/min ukuya ku-1.0 ml/min 1.0 ml/min I-Solvent A 20 mM ammonium acetate emanzini akhishwe nge-deionized 0.05% I-acetone emanzini akhishwe i-deionized Solvent B 80% 20l0% Aceto ACN Acetoni (80% ACN) amanzi Isilinganiso sokuncibilika samanzi angama-20% 20% A / 80% B 20% A / 80% B Umtshina 220 nm 265 nm
Ilayisi.6. Izakhiwo zamagagasi e-sine axubile akalwa ngaphambi nangemuva kokusebenzisa isihlungi se-low-pass ukuze kukhishwe izingxenye eziyisisekelo zokukhukhuleka zesiginali.
Umfanekiso wesi-6 uyisibonelo esijwayelekile somsindo oxubile oyisisekelo Esimeni 1, esiboniswa njengephethini ye-sinusoidal ephindaphindayo ebekwe ngaphezulu ekukhukhuleni kwesisekelo.I-Baseline drift iwukukhuphuka okunensayo noma ukuncipha kwesignali yangemuva.Uma isistimu ingavunyelwe ukulingana isikhathi eside ngokwanele, ngokuvamile izowa, kodwa izokhukhuleka ngendlela engaqondakali ngisho nalapho isistimu izinzile ngokuphelele.Lokhu ku-drift okuyisisekelo kuvame ukukhuphuka lapho isistimu isebenza endaweni eyimiqansa noma izimo zokucindezela okukhulu emuva.Uma lokhu kudonswa kwesisekelo kukhona, kungaba nzima ukuqhathanisa imiphumela kusuka kusampula kuye kusampula, okunganqotshwa ngokusebenzisa isihlungi sephasi eliphansi kudatha eluhlaza ukuze kuhlungwe lokhu kuhlukahluka kwefrikhwensi ephansi, ngaleyo ndlela kuhlinzekwe icebo lokuzulazula elinesisekelo esiphansi.Emkhiwaneni.Umfanekiso wesi-6 uphinda ubonise isakhiwo somsindo oyisisekelo we-mixer ngemva kokufaka isihlungi se-low-pass.
Ngemva kokuphothula ukulingisa kwe-CFD nokuhlola kokuqala kokuhlola, izixube ezintathu ezihlukene ezimile zathuthukiswa kamuva kusetshenziswa izingxenye zangaphakathi ezichazwe ngenhla namavolumu amathathu angaphakathi: 30 µl, 60 µl kanye no-90 µl.Lobu bubanzi buhlanganisa ububanzi bevolumu nokusebenza kokuxuba okudingekayo ezinhlelweni ze-HPLC zokuhlaziya eziphansi lapho ukuxuba okuthuthukisiwe nokuhlakazeka okuphansi kuyadingeka ukuze kukhiqizwe isisekelo se-amplitude ephansi.Emkhiwaneni.I-7 ibonisa izilinganiso zamagagasi e-sine ayisisekelo atholwe ohlelweni lokuhlola lweSibonelo 1 (i-acetonitrile ne-ammonium acetate njengezilandeleli) ezinamavolumu amathathu ezixube ezimile futhi azikho izihlanganisi ezifakiwe.Izimo zokuhlola zokuhlola zemiphumela ekhonjiswe ku-Figure 7 zazibanjwe njalo kuzo zonke izivivinyo ze-4 ngokuvumelana nenqubo echazwe kuThebula 1 ngesilinganiso sokugeleza kwe-solvent ye-0.5 ml / min.Sebenzisa inani le-offset kumadathasethi ukuze aboniswe ngapha nangapha ngaphandle kokugqagqana kwesignali.I-Offset ayithinti ubukhulu besiginali esetshenziselwa ukwahlulela izinga lokusebenza lomhlanganisi.Isilinganiso se-sinusoidal amplitude ngaphandle kwe-mixer sasingu-0.221 mAi, kuyilapho ama-amplitude ezixube ze-Mott ezimile ku-30 ​​µl, 60 µl, no-90 µl zehle zafika ku-0.077, 0.017, kanye no-0.004 mAi, ngokulandelana.
Umfanekiso 7. I-HPLC UV Detector Signal Offset vs. Isikhathi Sekesi 1 (i-acetonitrile ene-ammonium acetate indicator) ebonisa ukuxutshwa kwe-solvent ngaphandle kwe-mixer, ama-30 µl, 60 µl nama-90 µl amamiksi e-Mott abonisa ukuxutshwa okuthuthukisiwe (i-amplitude yesiginali ephansi ) njengoba ivolumu ye-static inyusa.(ukususwa kwangempela kwedatha: 0.13 (akukho mixer), 0.32, 0.4, 0.45mA ukuze kuboniswe kangcono).
Idatha eboniswe ku-fig.8 ziyafana nezikuFig. 7, kodwa kulokhu zihlanganisa imiphumela yezixube ezimile ze-HPLC ezintathu ezivame ukusetshenziswa ezinevolumu yangaphakathi engu-50 µl, 150 µl kanye no-250 µl.Ilayisi.Umfanekiso 8. I-HPLC UV Detector Signal Offset ngokumelene ne-Time Plot ye-Case 1 (i-Acetonitrile ne-Ammonium Acetate njengezinkomba) ebonisa ukuxutshwa kwe-solvent ngaphandle kwe-static mixer, uchungechunge olusha lwama-mixer e-Mott static, nezixube ezintathu ezivamile (i-offset yedatha yangempela ngu-0.1 (ngaphandle kokuxuba), 0.60.8, 0.6,82 9 mA ngokulandelanayo ukuze uthole umphumela ongcono wokubonisa).Ukwehliswa kwephesenti kwegagasi le-sine lesisekelo kubalwa ngesilinganiso sobukhulu begagasi le-sine ukuya ku-amplitude ngaphandle kokufakwa kwesihlanganisi.Amaphesenti okuncishiswa kwamagagasi e-sine alinganisiwe Ezimo 1 kanye no-2 afakwe kuhlu kuThebula 2, kanye namavolumu angaphakathi e-mixer emile entsha kanye nezihlanganisi ezijwayelekile eziyisikhombisa ezivame ukusetshenziswa embonini.Idatha ku-Figure 8 no-9, kanye nezibalo ezethulwe kuThebula 2, ibonisa ukuthi i-Mott Static Mixer inganikeza ukufika kokufika ku-98.1% we-sine wave attenuation, edlula kude ukusebenza kwe-mixer evamile ye-HPLC ngaphansi kwalezi zimo zokuhlola.Umfanekiso 9. Isignali yomtshina we-HPLC ye-UV i-offset ngokumelene nesakhiwo sesikhathi sekesi 2 (i-methanol ne-acetone njengama-tracers) engabonisi i-mixer emile (ehlanganisiwe), uchungechunge olusha lwabaxube be-Mott static kanye nezihlanganisi ezimbili ezivamile (ukususwa kwangempela kwedatha kungu-0, 11 (ngaphandle kokuhlanganisa. ), 0.22, 0.5 mA ngokubonisa kangcono.Izixube eziyisikhombisa ezivame ukusetshenziswa embonini nazo zahlolwa.Lokhu kufaka phakathi izixube ezinamavolumu amathathu ahlukene angaphakathi enkampanini A (I-Mixer A1, A2 ne-A3 eqokiwe) kanye nenkampani B (iMixer B1, B2 ne-B3 eqokiwe).Inkampani C ilinganise usayizi owodwa kuphela.
Ithebula 2. Izici ezishukumisayo ze-Static Mixer kanye Nekesi le-Internal Volume Static Mixer 1 Ukutholwa kwe-Sinusoidal: Ukuhlolwa kwe-Acetonitrile (Ukusebenza kahle) Ikesi 2 Ukubuyiselwa Kwe-Sinusoidal: Ukuhlolwa Kwamanzi E-Methanol (Ukusebenza) Ivolumu Yangaphakathi (µl) Ayikho Isihlanganisi - - 0 Mott% 6 % 69 30 9 Mott. 1.3% 60 Mott 90 98.1% 97.5% 90 Mixer A1 66.4% 73.7% 50 Mixer A2 89.8% 91.6% 150 Mixer A3 92.2% 94.5% 250 Mixer B1 45.8% 8% B1 44.8% I-370 Mixer C 97.2% 97.4% 250
Ukuhlaziywa kwemiphumela kuMfanekiso 8 kanye neThebula 2 kubonisa ukuthi i-30 µl Mott static mixer inokusebenza kahle kokuhlanganisa njenge-A1 mixer, okungukuthi 50 µl, nokho, i-30 µl Mott inevolumu yangaphakathi engaphansi ngo-30%.Uma kuqhathaniswa i-60 µl Mott mixer ne-150 µl yevolumu yangaphakathi ye-A2 mixer, kube nokuthuthuka okuncane ekuhlanganiseni ukusebenza kahle kuka-92% uma kuqhathaniswa no-89%, kodwa okubaluleke kakhulu, leli zinga eliphezulu lokuhlanganisa lifinyelelwe ku-1/3 yevolumu yokuhlanganisa.i-mixer efanayo A2.Ukusebenza kwe-90 µl Mott mixer kulandele ithrendi efanayo neye-A3 mixer enevolumu yangaphakathi engu-250 µl.Ukuthuthukiswa kokusebenza kokuxuba kwe-98% kanye ne-92% kuphinde kwabonwa ngokunciphisa okuphindwe kathathu kwevolumu yangaphakathi.Imiphumela efanayo kanye nokuqhathaniswa kwatholakala kubaxube B no-C. Ngenxa yalokho, uchungechunge olusha lwabaxube be-static i-Mott PerfectPeak TM luhlinzeka ngokusebenza kahle kokuxubana kunama-mixer abancintisana nabo abafanayo, kodwa ngevolumu encane yangaphakathi, ehlinzeka ngomsindo ongemuva ongcono kanye nesilinganiso esingcono sesignali-kuya-umsindo, i-Analyte yokuzwela engcono, ukuma okuphezulu kanye nesinqumo esiphezulu.Amathrendi afanayo ekusebenzeni kahle kokuxuba abonwa kuzo zombili izifundo ze-Case 1 kanye ne-Case 2.Odabeni 2, ukuhlolwa kwenziwa kusetshenziswa (i-methanol ne-acetone njengezinkomba) ukuze kuqhathaniswe ukusebenza kahle kokuxuba kuka-60 ml Mott, i-mixer efanayo engu-A1 (ivolumu yangaphakathi engu-50 µl) kanye ne-mixer eqhathaniswayo engu-B1 (ivolumu yangaphakathi engu-35 µl)., ukusebenza bekungekuhle ngaphandle kokuxuba okufakiwe, kodwa kwasetshenziselwa ukuhlaziya okuyisisekelo.Ingxube ye-Mott engu-60 ml ibonakale iyingxube engcono kakhulu eqenjini lokuhlola, ihlinzeka ngokunyuka okungama-90% ekusebenzeni kahle kokuxuba.I-Mixer A1 eqhathaniswayo ibone ukuthuthuka okungama-75% ekusebenzeni kahle kokuxuba okulandelwa ukuthuthukiswa okungama-45% kumxube we-B1 ofanayo.Ukuhlolwa okuyisisekelo kokunciphisa igagasi le-sine elinesilinganiso sokugeleza kwenziwa ochungechungeni lwezixube ngaphansi kwezimo ezifanayo nokuhlolwa kwejika le-sine Esimeni 1, okunezinga lokugeleza kuphela elishintshile.Idatha ibonise ukuthi ebangeni lamazinga okugeleza ukusuka ku-0.25 kuya ku-1 ml/min, ukwehla kokuqala kwe-sine wave kwahlala kungokungashintshile kuwo wonke amavolumu amathathu okuxuba.Ezixubeni ezimbili ezincane zevolumu, kunokwenyuka okuncane kokufinyela kwe-sinusoidal njengoba izinga lokugeleza lincipha, okulindeleke ngenxa yesikhathi sokuhlala esikhulisiwe se-solvent ku-mixer, okuvumela ukwanda kokuxubana kokusabalalisa.Ukukhishwa kwe-sine wave kulindeleke ukuthi kukhuphuke njengoba ukugeleza kuncipha ngokuqhubekayo.Kodwa-ke, ngevolumu enkulu yokuhlanganisa ene-sine wave base base attenuation, i-sine wave base attenuation yahlala ingashintshile (ngaphakathi kwebanga lokungaqiniseki kokuhlolwa), ngamavelu asuka ku-95% aye ku-98%.Ilayisi.10. Ukuncishiswa okuyisisekelo kwe-sine wave ngokumelene nezinga lokugeleza esimweni 1. Ukuhlolwa kwenziwa ngaphansi kwezimo ezifana nokuhlolwa kwe-sine enezinga lokugeleza eliguquguqukayo, kujove u-80% wengxube engu-80/20 ye-acetonitrile namanzi kanye no-20% we-20 mM ammonium acetate.
Uhlu olusha oluthuthukisiwe lwezixube ezimile ezimile ze-PerfectPeak TM ezinelungelo lobunikazi ezinamavolumu amathathu angaphakathi: 30 µl, 60 µl no-90 µl zimboza ivolumu nobubanzi bokusebenza bokuhlanganisa obudingekayo ekuhlaziyeni okuningi kwe-HPLC okudinga ukuxutshwa okuthuthukisiwe kanye nezitezi zokuhlakazeka eziphansi.Ingxube entsha emile ifinyelela lokhu ngokusebenzisa ubuchwepheshe obusha bokuphrinta be-3D ukuze kwakhe isakhiwo se-3D esiyingqayizivele esihlinzeka ngokuxubana kwe-hydrodynamic static okuthuthukisiwe ngephesenti eliphakeme kakhulu lokunciphisa umsindo oyisisekelo ngeyunithi ngayinye yevolumu yengxube yangaphakathi.Ukusebenzisa i-1/3 yevolumu yangaphakathi ye-mixer evamile kunciphisa umsindo oyisisekelo ngo-98%.Izixube ezinjalo zihlanganisa amashaneli okugeleza ezinhlangothi ezintathu axhumene anezindawo ezihlukene eziphambanayo kanye nobude bendlela obuhlukene njengoba uketshezi luwela izithiyo zejiyomethri eziyinkimbinkimbi ngaphakathi.Umndeni omusha wabaxube abamile unikeza ukusebenza okuthuthukisiwe ngaphezu kwezixube eziqhudelanayo, kodwa ngevolumu encane yangaphakathi, okuholela esilinganisweni esingcono sesignali-kuya-kumsindo kanye nemikhawulo yomthamo ophansi, kanye nokuma okuphezulu okuthuthukisiwe, ukusebenza kahle kanye nesinqumo sokuzwela okuphezulu.
Kulolu shicilelo i-Chromatography - I-RP-HPLC enobungani bemvelo - Ukusetshenziswa kwe-chromatography yegobolondo elingaphakathi esikhundleni se-acetonitrile nge-isopropanol ekuhlaziyeni nasekuhlanzweni - I-chromatograph yegesi entsha ye...
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Isikhathi sokuthumela: Nov-15-2022