1. Indlela yokuchonga ye-hydroxypropyl methylcellulose
(1) Thatha i-1.0g yesampulu, fudumeza i-100mL yamanzi (80 ~ 90℃), ugxobhoze ngokuqhubekayo, kwaye upholise kwibhafu yomkhenkce de ibe lulwelo lwe-viscous;beka i-2mL yolwelo kwityhubhu yovavanyo, kwaye ngokucotha ukongeza i-1mL ye-0.035% ye-anthrone sulfuric acid ecaleni kwesisombululo sodonga lwetyhubhu kwaye uyishiye imizuzu emi-5.Iringi eluhlaza ivela kujongano phakathi kwezinto ezingamanzi ezimbini.
(2) Thatha umlinganiselo ofanelekileyo wencindi esetyenziselwa ukuchonga ku-(I) ngasentla kwaye uyigalele kwipleyiti yeglasi.Njengoko amanzi ephuphuma, ifilimu ye-ductile ifom.
2. Ukulungiswa kwesisombululo esiqhelekileyo sokuhlalutya i-hydroxypropyl methylcellulose
(1) Isisombululo esisemgangathweni se-sodium thiosulfate (0.1mol/L, ixesha lokuqinisekisa: inyanga eyi-1)
Ukulungiselela: Bilisa malunga ne-1500mL amanzi adibeneyo, upholise kwaye ubeke bucala.Ukulinganisa i-25g ye-sodium thiosulfate (ubunzima bayo be-molecular yi-248.17, zama ukuchaneka malunga ne-24.817g xa ulinganisa) okanye i-16g ye-sodium anhydrous thiosulfate, yinyibilikise kwi-200mL yamanzi okupholisa angentla, nciphisa kwi-1L, uyibeke kwibhotile emdaka. kwaye ubeke Gcina kwindawo emnyama, hluza kwaye ubeke bucala emva kweeveki ezimbini.
Ukulinganisa: Ubunzima be-0.15g yereferensi ye-potassium dichromate kwaye ubhaka kubunzima obuqhubekayo, obuchanekileyo kwi-0.0002g.Yongeza i-2g ye-potassium iodide kunye ne-20mL sulfuric acid (1 + 9), xubha kakuhle, kwaye ubeke kwindawo emnyama imizuzu eyi-10.Yongeza i-150mL yamanzi kunye ne-3ml 0.5% isisombululo sesalathisi sesitashi, kunye ne-titrate kunye ne-0.1mol / L isisombululo se-sodium thiosulfate.Isisombululo sitshintsha ukusuka eluhlaza ukuya eluhlaza okwesibhakabhaka.Ijika ibe luhlaza oqaqambileyo ekupheleni.Akukho potassium chromate yongezwa kuvavanyo olungenanto.Inkqubo yokulinganisa iphinda iphindwe kabini ukuya kwii-3 kwaye ixabiso eliphakathi lithathwa.
Uxinzelelo lwe-molar C (i-mol / L) yesisombululo esisemgangathweni se-sodium thiosulfate ibalwa ngokwefomula ilandelayo:
Kwifomula, uM bubunzima be-potassium dichromate;I-V1 ngumthamo we-sodium thiosulfate esetyenzisiweyo, i-mL;I-V2 ngumthamo we-sodium thiosulfate esetyenzisiweyo kwilingo elingenanto, mL;I-49.03 yi-dichromium elingana ne-1 mol ye-sodium thiosulfate.Ubunzima be-asidi ye-potassium, g.
Emva kokulinganisa, yongeza inani elincinci le-Na2CO3 ukukhusela ukubola kwe-microbial.
(2) Isisombululo esisemgangathweni se-NaOH (0.1mol/L, ixesha lokuqinisekisa: inyanga eyi-1)
Ukulungiselela: Ukulinganisa malunga ne-4.0g ye-NaOH ecocekileyo yokuhlalutya kwi-beaker, yongeza i-100mL yamanzi adibeneyo ukuze uchithe, uze udlulisele kwi-flask ye-volumetric ye-1L, yongeza amanzi adibeneyo kwi-mark, kwaye uyishiye iintsuku ezi-7-10 de kube ukulinganisa.
Ukulinganisa: Beka i-0.6 ~ 0.8g ye-potassium hydrogen phthalate ecocekileyo (echanekileyo kwi-0.0001g) yomiswe kwi-120 ° C kwi-flask ye-Erlenmeyer ye-250mL, yongeza i-75mL yamanzi adibeneyo ukuze uchithe, uze ungeze i-2 ~ 3 amaconsi e-1% ye-phenolph.Titrate nge-titrant.Gxuma isisombululo se-sodium hydroxide elungiselelwe ngasentla ide ibe bomvu kancinane, kwaye umbala awupheli kwimizuzwana engama-30 njengendawo yokuphela.Bhala umthamo wesodium hydroxide.Inkqubo yokulinganisa iphinda iphindwe kabini ukuya kwii-3 kwaye ixabiso eliphakathi lithathwa.Kwaye wenze umfuniselo ongenanto.
Ukuxinwa kwesisombululo sesodium hydroxide kubalwa ngolu hlobo lulandelayo:
Kwifomula, i-C yingxubusho yesisombululo se-sodium hydroxide, i-mol / L;M imele ubunzima be potassium hydrogen phthalate, G;I-V1 - umthamo we-sodium hydroxide esetyenzisiweyo, i-mL;I-V2 imele i-sodium hydroxide esetyenziswe kuvavanyo olungenanto uMqulu, mL;I-204.2 yi-molar mass ye-potassium hydrogen phthalate, i-g/mol.
(3) Nciphisa iasidi yesulfuric (1+9) (ixesha lokuqinisekisa: inyanga eyi-1)
Ngelixa uvuselela, yongeza ngononophelo i-100 mL ye-sulfuric acid egxininisiweyo kwi-900 mL yamanzi adibeneyo kwaye wongeze ngokukhawuleza ngelixa uvuselela.
(4) Nciphisa i-asidi ye-sulfuric (1+16.5) (ixesha lokuqinisekisa: iinyanga ezi-2)
Ngelixa uvuselela, yongeza ngononophelo i-100 mL ye-sulfuric acid egxininisiweyo kwi-1650 mL yamanzi adibeneyo kwaye wongeze kancinci.Gxuma njengoko uhamba.
(5) Isalathisi sesitatshi (1%, ixesha lokuqinisekisa: iintsuku ezingama-30)
Yenza umlinganiselo we-1.0g yestatshi esinyibilikayo, yongeza i-10mL yamanzi, ugxobhoze kwaye ugalele kwi-100mL yamanzi abilayo, ubilise imizuzu emi-2, yiyeke, kwaye uthathe i-supernatant ukuze isetyenziswe kamva.
(6) Isalathisi sesitatshi
Thatha i-5 mL yesisombululo esilungisiweyo se-1% yesitatshi kwaye uhlambulule ngamanzi kwi-10 mL ukufumana isalathisi se-0.5%.
(7) 30% isisombululo sechromium trioxide (ixesha lokuqinisekisa: inyanga eyi-1)
Yenza i-60g yechromium trioxide kwaye uyinyibilikise kwi-140mL yamanzi angenayo i-organic-free.
(8) Isisombululo sePotassium acetate (100g/L, sisebenza iinyanga ezi-2)
Dissolve i-10 g ye-anhydrous potassium acetate granules kwi-100 mL yesisombululo se-90 mL ye-glacial acetic acid kunye ne-10 mL ye-acetic anhydride.
(9) I-25% isisombululo se-sodium acetate (220g / L, ixesha lokuqinisekisa: iinyanga ze-2)
Dissolve 220g anhydrous sodium acetate emanzini kwaye uhlambulule kwi-1000mL.
(10) I-Hydrochloric acid (1:1, ixesha lokuqinisekisa: iinyanga ezi-2)
Hlanganisa i-hydrochloric acid egxininisiweyo kunye namanzi kwi-volume ratio ye-1: 1.
(11) Isithinteli se-acetate (pH=3.5, ixesha lokuqinisekisa: iinyanga ezi-2)
Dissolve i-60mL ye-acetic acid kwi-500mL yamanzi, uze udibanise i-100mL ye-ammonium hydroxide kwaye udibanise kwi-1000mL.
(12) Isisombululo sokulungiselela i-nitrate
Dissolve 159.8 mg lead nitrate kwi-100 mL yamanzi aqukethe i-1 mL nitric acid (ubuninzi be-1.42 g / cm3), nciphisa kwi-1000 mL yamanzi, kwaye udibanise kakuhle.Kulungiswe kakuhle.Isisombululo kufuneka silungiswe kwaye sigcinwe kwiglasi engenalo ilothe.
(13) Isisombululo esisemgangathweni (ixesha elisemthethweni: iinyanga ezi-2)
Yenza umlinganiselo ngokuchanekileyo we-10mL yesisombululo sokulungiselela i-nitrate yelothe kwaye wongeze amanzi ukuze udibanise kwi-100mL.
(14) 2% isisombululo se-hydroxylamine hydrochloride (ixesha lokuqinisekisa: inyanga eyi-1)
Dissolve 2g ye-hydroxylamine hydrochloride kwi-98mL yamanzi.
(15) Ammonia (5mol/L, isebenza iinyanga ezi-2)
Nciphisa i-175.25g yamanzi ammonia kwaye udibanise kwi-1000mL.
(16) Ulwelo oluxutyiweyo (ukusebenza: iinyanga ezi-2)
Hlanganisa i-100mL ye-glycerol, i-75mL yesisombululo se-NaOH (1mol / L) kunye ne-25mL yamanzi.
(17) isisombululo se-Thioacetamide (4%, sivumelekile kwiinyanga ezi-2)
Dibanisa i-4g ye-thioacetamide kwi-96g yamanzi.
(18) I-Phenanthroline (0.1%, ixesha lokuqinisekisa: inyanga eyi-1)
Ukunyibilikisa i-0.1g ye-phenanthroline kwi-100mL yamanzi.
(19) I-Acidic stannous chloride (ixesha lokuqinisekisa: inyanga e-1)
Dissolve 20g yestannous chloride kwi-50mL ye-concentrated hydrochloric acid.
(20) Isisombululo esisemgangathweni se-potassium hydrogen phthalate (pH 4.0, ixesha lokuqinisekisa: iinyanga ezi-2)
Ngokuchanekileyo ukale 10.12g ye potassium hydrogen phthalate (KHC8H4O4) kwaye uyomise ku (115±5)℃ iiyure ezi-2 ukuya kwezi-3.Nciphisa kwi-1000mL ngamanzi.
(21) Isisombululo somgangatho we-Phosphate buffer (pH 6.8, ixesha lokuqinisekisa: iinyanga ezi-2)
Ubunzima obuchanekileyo be-3.533g ye-anhydrous disodium hydrogen phosphate kunye ne-3.387g ye-potassium dihydrogen phosphate yomiswe ku-(115±5)°C ngeeyure ezi-2 ~ 3, kwaye ixutywe kwi-1000mL ngamanzi.
3. Ukumiselwa komxholo weqela le-hydroxypropylmethylcellulose
(1) Ukumiselwa komxholo we-methoxyl
Ukuzimisela komxholo weqela le-methoxy kusekelwe kuvavanyo oluqukethe amaqela e-methoxy.I-Hydroiodic acid iyabola xa ifudunyezwa ivelise i-olatile ye-methyl iodide (iqondo lokubila elingu-42.5°C).I-Methyl iodide yachithwa nge-nitrogen kwisisombululo sokuziphendulela.Emva kokuhlamba ukususa izinto eziphazamisayo (i-HI, i-I2 kunye ne-H2S), umphunga we-methyl iodide ufunxa isisombululo se-acetic ye-acetate ye-acetate ye-potassium equkethe i-Br2 ukwenza i-IBr, ethi emva koko i-oxidized kwi-iodic acid.Emva kwe-distillation, iziqulatho ze-receptor zidluliselwa kwibhotile ye-iodine kwaye ihlanjululwe ngamanzi.Emva kokongeza i-asidi ye-formic ukususa i-Br2 engaphezulu, i-KI kunye ne-H2SO4 yongezwa.Umxholo we-methoxyl unokubalwa ngokulinganisa i-12 kunye nesisombululo se-Na2S2O3.I-reaction equation ingabonakaliswa ngolu hlobo lulandelayo.
Isixhobo sokulinganisa umxholo we-methoxyl siboniswe kuMfanekiso 7-6.
Kwi-7-6 (a), i-A yi-50mL i-flask ejikelezayo ejikelezayo edibeneyo kwi-catheter.Kukho umbhobho womoya othe ngqo we-E ofakwe ngokuthe nkqo kwi-bottleneck, malunga ne-25cm ubude kunye ne-9mm yangaphakathi ububanzi.Isiphelo esiphezulu sombhobho sigotywe kwi-glass capillary tube kunye nobubanzi obungaphakathi be-2 mm kunye ne-outlet ejongene nezantsi.Umzobo 7-6(b) ubonisa isixhobo esiphuculweyo.Umzobo we-1 ubonisa i-reaction flask, eyi-50mL ye-flask ejikelezayo ephantsi, kunye netyhubhu ye-nitrogen ngakwesobunxele.I-2 yityhubhu ye-condenser ethe nkqo;I-3 yi-scrubber, equlethe ulwelo lokuhlamba;4 yityhubhu yokufunxa.Umahluko omkhulu phakathi kwesi sixhobo kunye nendlela ye-Pharmacopoeia kukuba i-absorbers ezimbini zendlela ye-Pharmacopoeia idityaniswe ibe yinto enye, enokunciphisa ukulahlekelwa kolwelo lokugqibela.Ukongezelela, i-liquid yokuhlamba kwi-scrubber nayo ihluke kwindlela ye-pharmacopoeia.Ngamanzi adibeneyo, ngelixa isixhobo esiphuculweyo singumxube wesisombululo se-cadmium sulfate kunye nesisombululo se-sodium thiosulfate, ekulula ukufunxa ukungcola kwi-gas distilled.
I-pipette yesixhobo: 5mL (iziqwenga ezi-5), i-10mL (iqhekeza eli-1);Burette: 50mL;Ibhotile yevolumu ye-iodine: 250mL;Ibhalansi yohlalutyo.
I-Reagent phenol (kuba iqinile, iya kunyibilika ngaphambi kokutya);carbon dioxide okanye initrogen;i-hydroiodic acid (45%);ibakala lohlalutyo;isisombululo se-acetate ye-potassium (100g / L);bromine: ibakala lokuhlalutya;i-asidi ye-formic: ibakala lokuhlalutya;I-25% isisombululo se-Sodium acetate (220g / L);KI: ibakala lokuhlalutya;nciphisa i-asidi ye-sulfuric (1+9);isisombululo esiqhelekileyo se-sodium thiosulfate (0.1mol / L);isalathisi se-phenolphthalein;I-1% isisombululo se-ethanol;isalathisi sesitatshi: 0.5% Isisombululo samanzi sesitatshi;nciphisa i-asidi ye-sulfuric (1 + 16.5);30% isisombululo sechromium trioxide;Amanzi angenawo i-organic: galela i-10mL ye-sulfuric acid encibilikayo (1+16.5) ukuya kwi-100mL yamanzi, ubushushu ukubilisa, kwaye wongeze i-0.1ml ye-0.02mol/L permanganic acid i-Potassium titer, ubilise imizuzu eyi-10, kufuneka ihlale i-pink;I-0.02mol / L i-sodium hydroxide titrant: Ukulinganisa i-0.1mol / L ye-sodium hydroxide titrant ngokwendlela ye-Appendix yaseShayina ye-Pharmacopoeia, kwaye uhlambulule ngokuchanekileyo kwi-0.02mol ngamanzi abilisiwe kunye ne-cooled distilled / L.
Yongeza malunga ne-10mL yokuhlamba ulwelo kwi-tube yokuhlamba, yongeza i-31mL yolwelo olusandul 'ukulungiswa kwi-tube yokufunxa, faka isixhobo, ulinganise malunga ne-0.05g yesampulu eyomileyo eyomisiweyo kwi-105 ° C echanekileyo kwi-0.0001 g), yongeza impendulo ku-℃ kwibhotile, yongeza i-5 mL ye-hydroiodide.Ngokukhawuleza udibanise ibhotile yokusabela kwi-condenser yokubuyisela (unyakazise i-port yokugaya nge-hydriodic acid), kwaye upompe i-nitrogen kwi-tank ngesantya se-1 ukuya kwi-2 bubbles ngomzuzwana.
Ixesha lokuposa: Feb-01-2024