Umatshini weSepaBean™

Ulungelelwaniso lwekholomu lunokukhusela ikholam ekubeni yonakaliswe yimpembelelo ye-exothermic xa i-solvent ikhupha ngokukhawuleza kwikholamu. Ngelixa i-silica eyomileyo ifakwe ngaphambili kwikholomu idityaniswe ne-solvent okokuqala ngexesha lokuhlukana, ubushushu obuninzi bunokukhutshwa ngokukodwa xa i-solvent iguqa kwizinga eliphezulu lokuhamba. Obu bushushu bunokubangela ukuba umzimba wentsika ube wonakaliswe kwaye ngaloo ndlela uvuza okunyibilikayo kwikholamu. Kwezinye iimeko, obu bushushu bunokonakalisa isampulu ebuthathaka kubushushu.

Mhlawumbi kubangelwa ukungabikho kweoli yokuthambisa kwi-shaft ejikelezayo yempompo.

Umthamo opheleleyo we-tubing yenkqubo, i-connetors kunye negumbi lokuxuba malunga ne-25 mL.

Iseli yokuhamba yemodyuli ye-detector ingcolisekile yisampuli ene-UV eyomeleleyo yokufunxa. Okanye inokuba kungenxa yokufunxa kwe-solvent ye-UV eyinto eqhelekileyo. Nceda wenze lo msebenzi ulandelayo:

1. Susa ikholomu edanyazayo kwaye ugungxule iityhubhu yesixokelelwano ngesinyibilikisi esinamandla sepolar emva koko silandelwe sisinyibilikisi esibuthathaka esikwipolar.

2. Ukunyibilika kwengxaki yokufunxa kwe-UV: umz. ngelixa i-n-hexane kunye ne-dichloromethane (DCM) ziqeshwe njenge-solvent eluting, njengoko umlinganiselo we-DCM usanda, isiseko sechromatogram sinokuqhubeka ukuba ngaphantsi kwe-zero kwi-Y-axis ukususela ekufunjweni kwe-DCM. kwi-254 nm ingaphantsi kunaleyo ye-n-hexane. Kwimeko yale nto yenzekayo, sinokuyibamba ngokucofa iqhosha elithi "Zero" kwiphepha eliqhubayo lokwahlula kwiSepaBean App.

3.I-flow cell yemodyuli ye-detector ingcoliseke kakhulu kwaye ifuna ukucocwa nge-ultrasonically.

Isenokuba ngenxa yokuba izihlanganisi kwintloko yesibambi sekholamu ngokunjalo nakwisiseko sidumbile yi-solvent ukuze izihlanganisi zixinge.

Umsebenzisi unokuphakamisa ngesandla intloko yomphathi wekholamu ngokusebenzisa amandla amancinci. Xa intloko yomphathi wekholomu iphakanyiselwe kumphakamo othile, intloko yomphathi wekholamu kufuneka ikwazi ukushukunyiswa ngokuchukumisa amaqhosha aphezu kwayo. Ukuba intloko yomphathi wekholomu ayinakuphakanyiswa ngesandla, umsebenzisi kufuneka aqhagamshelane nenkxaso yobugcisa bendawo.

Enye indlela kaxakeka: Umsebenzisi unokufakela ikholamu phezulu kwentloko yesibambi sekholamu endaweni yoko. Isampuli yolwelo inokutofwa ngokuthe ngqo kwikholamu. Ikholomu yokulayisha isampula eqinile ingafakwa phezulu kwikholamu yokwahlula.

1. Amandla aphantsi omthombo wokukhanya;

2. Idama lokujikeleza lingcolisekile; I-intuitively, akukho ngqungquthela ye-spectral okanye i-spectral peak incinci ukuhlukana , I-spectra yamandla ibonisa ixabiso elingaphantsi kwe-25%.

Nceda uhlambe ityhubhu nge-solvent efanelekileyo kwi-10ml / min ye-30min kwaye uqaphele i-spectrum yamandla.Ukuba akukho tshintsho kwi-spectrum, kubonakala ngathi amandla aphantsi omthombo wokukhanya, nceda ubeke isibane se-deuterium; Ukuba i-spectrum itshintshile, idama lokujikeleza lingcolisekile, nceda uqhubeke nokucoca ngesinyibilikisi esifanelekileyo.

Nceda ujonge ityhubhu kunye nesinxibelelanisi rhoqo.

Ubude be-wavelength bokubona bubekwe kwi-wavlength engaphantsi kwe-245 nm ukususela ekubeni i-ethyl acetate ine-absorption eyomeleleyo kuluhlu lokufumanisa olungaphantsi kwe-245nm. Isiseko sokukhukuliseka siya kuba sisona sibalaseleyo xa i-ethyl acetate isetyenziswa njenge-eluting solvent kwaye sikhetha i-220 nm njengobude bokubona ubude.

Nceda utshintshe ubude bewavenge. Kuyacetyiswa ukuba ukhethe i-254nm njengobude bokubona ubude. Ukuba i-220 nm kuphela kobude obulungele ukuchongwa kwesampulu, umsebenzisi kufuneka aqokelele i-eluent ngokugweba ngononophelo kwaye isinyibilikisi esigqithisileyo sinokuqokelelwa kulo mzekelo.

Coca intloko yokucoca isinyibilikisi ngokupheleleyo ukususa nakuphi na ukungcola. Sebenzisa i-ethanol okanye i-isopropanol ukugungxula inkqubo ngokupheleleyo ukuze ugweme iingxaki ze-solvent ezingenakulinganiswa.

Ukucoca intloko yokucoca i-solvent, qhawula isihluzo kwintloko yokucoca kwaye uyihlambulule nge-brush encinci. Emva koko hlamba isihluzo nge-ethanol kwaye usomise. Hlanganisa kwakhona intloko yokucoca ukuze uyisebenzise kwixesha elizayo.

Nokuba utshintshe ukusuka kwisigaba esiqhelekileyo sokwahlulwa ukuya kukwahlulwa kwesigaba esibuyiselwe umva okanye ngokuchaseneyo, i-ethanol okanye i-isopropanol kufuneka isetyenziswe njengesinyibilikisi sotshintsho ukugungxula ngokupheleleyo naziphi na izinyibilikisi ezingaxutywanga kwi-tubing.

Kucetyiswa ukuba usete izinga lokuhamba kwi-40 mL / min ukucima imigca ye-solvent kunye nazo zonke iibhubhu zangaphakathi.

Nceda ubeke umphantsi wesibambi sekholamu emva kokukhulula isikrufu.

1. Izinga lokuqukuqela kwesixokelelwano liphezulu kakhulu kwikholamu yomenyezi yangoku.

2. Iisampulu ine-solubility engalunganga kunye ne-precipitates ukusuka kwisigaba esihambayo, oko kubangele ukuvaleka kweetyhubhu.

3. Esinye isizathu sibangela ukuvaleka kweetyhubhu.