1. Indlela yokuhlonza i-hydroxypropyl methylcellulose
(1) Thatha u-1.0g wesampula, shisa u-100mL wamanzi (80~90℃), gudluza ngokuqhubekayo, bese upholisa endaweni yokugeza eqhweni kuze kube uketshezi olubonakalayo; faka u-2mL woketshezi eshubhuni yokuhlola, bese wengeza kancane u-1mL ka-0.035% i-anthrone sulfuric acid eduze kwesisombululo sodonga lweshubhu bese uyishiya imizuzu emi-5. Iringi eluhlaza ivela esibonakalayo phakathi koketshezi olubili.
(2) Thatha inani elifanele lamafinyila asetshenziselwa ukuhlonza (I) ngenhla bese uwathela epuleti lengilazi. Njengoba amanzi ehwamuka, kwakheka ifilimu ye-ductile.
2. Ukulungiswa kwesisombululo esijwayelekile sokuhlaziya i-hydroxypropyl methylcellulose
(1) Isixazululo esijwayelekile se-sodium thiosulfate (0.1mol/L, isikhathi sokuqinisekisa: inyanga engu-1)
Ukulungiselela: Bilisa amanzi angaba ngu-1500mL, upholile futhi ubeke eceleni. Kala u-25g we-sodium thiosulfate (isisindo se-molecular singu-248.17, zama ukunemba cishe cishe ngo-24.817g uma ukala) noma u-16g anhydrous sodium thiosulfate, uhlakaze ngo-200mL wamanzi okupholisa angenhla, hlambulula ku-1L, ulibeke ebhodleleni elinsundu. bese ubeka Gcina endaweni emnyama, hlunga futhi ubeke eceleni ngemva kwamasonto amabili.
Ukulinganisa: Isisindo esingu-0.15g sereferensi ye-potassium dichromate bese ubhaka esisindweni esingaguquki, esinembile sibe ngu-0.0002g. Faka u-2g we-potassium iodide no-20mL sulfuric acid (1+9), xukuza kahle, bese ubeka ebumnyameni imizuzu eyi-10. Engeza amanzi angu-150mL kanye nesisombululo senkomba yesitashi esingu-3ml esingu-0.5%, bese u-titrate ngesisombululo se-sodium thiosulfate esingu-0.1mol/L. Isixazululo siyashintsha sisuka kokuluhlaza okwesibhakabhaka sibe luhlaza okwesibhakabhaka. Iphenduka ibe luhlaza ngokukhanyayo ekugcineni. Ayikho i-potassium chromate engeziwe ocwaningweni olungenalutho. Inqubo yokulinganisa iphindwe izikhathi ezingu-2 kuya kwezi-3 futhi inani eliphakathi liyathathwa.
I-molar concentration C (mol/L) yesisombululo esijwayelekile se-sodium thiosulfate ibalwa ngokuya ngale fomula elandelayo:
Kufomula, uM yinqwaba ye-potassium dichromate; I-V1 umthamo we-sodium thiosulfate esetshenzisiwe, mL; I-V2 umthamo we-sodium thiosulfate esetshenziswe ekuhlolweni okungenalutho, mL; I-49.03 yi-dichromium elingana ne-1 mol ye-sodium thiosulfate. Ubuningi be-potassium acid, g.
Ngemva kokulinganisa, engeza inani elincane le-Na2CO3 ukuze uvimbele ukubola kwe-microbial.
(2) Isixazululo esijwayelekile se-NaOH (0.1mol/L, isikhathi sokuqinisekisa: inyanga engu-1)
Ukulungiselela: Kala cishe u-4.0g we-NaOH ehlanzekile ukuze uhlaziywe ebhekhani, engeza u-100mL wamanzi acwecwe ukuze uncibilike, bese udlulisela ku-1L ye-volumetric flask, engeza amanzi acwecwe kuphawu, bese uliyeka izinsuku ezingu-7-10 kuze kube yilapho ukulinganisa.
Ukulinganisa: Beka i-0.6 ~ 0.8g ye-potassium hydrogen phthalate ehlanzekile (enembile ku-0.0001g) omisiwe ku-120 ° C ku-250mL Erlenmeyer flask, engeza u-75mL wamanzi acwecwe ukuze uhlakaze, bese wengeza amaconsi angu-2 ~ 3 we-phenolph engu-1%. Titrate nge-titrant. Gcoba isixazululo se-sodium hydroxide elungiselelwe ngenhla size sibebomvu kancane, futhi umbala ungafi phakathi kwamasekhondi angu-30 njengendawo yokugcina. Bhala umthamo we-sodium hydroxide. Inqubo yokulinganisa iphindwe izikhathi ezingu-2 kuya kwezi-3 futhi inani eliphakathi liyathathwa. Futhi wenze ucwaningo olungenalutho.
Ukuhlushwa kwesisombululo se-sodium hydroxide kubalwa ngale ndlela elandelayo:
Kufomula, i-C iyinhlanganisela yesisombululo se-sodium hydroxide, i-mol/L; U-M umele ubuningi be-potassium hydrogen phthalate, G; I-V1 - umthamo we-sodium hydroxide esetshenzisiwe, mL; I-V2 imele i-sodium hydroxide esetshenziswe ekuhloleni okungenalutho Ivolumu, mL; 204.2 isisindo se-molar ye-potassium hydrogen phthalate, i-g/mol.
(3) Nciphisa i-sulfuric acid (1+9) (isikhathi sokuqinisekisa: inyanga engu-1)
Ngesikhathi ugqugquzela, engeza ngokucophelela u-100 mL we-concentrated sulfuric acid ku-900 mL wamanzi acwecwe bese wengeza kancane ngenkathi uvuselela.
(4) Nciphisa i-sulfuric acid (1+16.5) (isikhathi sokuqinisekisa: izinyanga ezi-2)
Ngenkathi ugqugquzela, engeza ngokucophelela u-100 mL we-concentrated sulfuric acid ku-1650 mL wamanzi acwecwe bese wengeza kancane. Govuza njengoba uhamba.
(5) Inkomba yesitashi (1%, isikhathi sokuqinisekisa: izinsuku ezingama-30)
Kala u-1.0g wesitashi esincibilikayo, engeza u-10mL wamanzi, ugovuze futhi uthele ku-100mL wamanzi abilayo, ubilise imizuzu engu-2, uyeke, bese uthatha i-supernatant ukuze uyisebenzise kamuva.
(6) Inkomba yesitashi
Thatha u-5 mL wesisombululo senkomba yesitashi esilungisiwe esingu-1% bese usihlanza ngamanzi sibe ngu-10 ml ukuze uthole inkomba yesitashi engu-0.5%.
(7) 30% isixazululo se-chromium trioxide (isikhathi sokuqinisekisa: inyanga engu-1)
Kala u-60g we-chromium trioxide bese uyincibilikisa ku-140mL wamanzi angenayo i-organic.
(8) Isixazululo se-Potassium acetate (100g/L, sisebenza izinyanga ezi-2)
Chaza u-10 g we-anhydrous potassium acetate granules ku-100 mL wesixazululo esingu-90 mL we-glacial acetic acid kanye no-10 mL we-acetic anhydride.
(9) 25% isisombululo se-sodium acetate (220g/L, isikhathi sokuqinisekisa: izinyanga ezi-2)
Chaza 220g anhydrous sodium acetate emanzini futhi nciphisa ku-1000mL.
(10) I-Hydrochloric acid (1:1, isikhathi sokuqinisekisa: izinyanga ezi-2)
Hlanganisa i-hydrochloric acid egxilile namanzi ngesilinganiso sevolumu ye-1: 1.
(11) Ibhafa ye-acetate (pH=3.5, isikhathi sokuqinisekisa: izinyanga ezi-2)
Chaza u-60mL we-acetic acid ku-500mL wamanzi, bese wengeza u-100mL we-ammonium hydroxide bese unciphisa ku-1000mL.
(12) Isixazululo sokulungiselela i-nitrate yokuhola
Chaza i-nitrate engu-159.8 mg emanzini angu-100 ml aqukethe i-nitric acid engu-1 mL (ukuminyana 1.42 g/cm3), hlambulula ku-1000 mL wamanzi, bese uxuba kahle. Kulungiswe kahle. Isixazululo kufanele silungiswe futhi sigcinwe engilazini engenamthofu.
(13) Isixazululo esijwayelekile esiholayo (isikhathi sokuqinisekisa: izinyanga ezi-2)
Kala ngokunembile u-10mL wesixazululo sokulungiselela i-nitrate yomthofu bese wengeza amanzi ukuze unciphise ku-100mL.
(14) 2% isixazululo se-hydroxylamine hydrochloride (isikhathi sokuqinisekisa: inyanga engu-1)
Chaza u-2g we-hydroxylamine hydrochloride ku-98mL wamanzi.
(15) I-Amonia (5mol/L, isebenza izinyanga ezi-2)
Chaza amanzi angu-175.25g ammonia bese unciphisa ku-1000mL.
(16) Uketshezi oluxubile (ukusebenza: izinyanga ezi-2)
Xuba u-100mL we-glycerol, u-75mL wesisombululo se-NaOH (1mol/L) kanye no-25mL wamanzi.
(17) Isixazululo se-Thioacetamide (4%, sisebenza izinyanga ezi-2)
Chaza u-4g we-thioacetamide ku-96g wamanzi.
(18) I-Phenanthroline (0.1%, isikhathi sokuqinisekisa: inyanga engu-1)
Chaza u-0.1g we-phenanthroline ku-100mL wamanzi.
(19) I-Acidic stannous chloride (isikhathi sokuqinisekisa: inyanga engu-1)
Chaza u-20g we-stannous chloride ku-50mL we-concentrated hydrochloric acid.
(20) Isixazululo sebhafa esijwayelekile se-Potassium hydrogen phthalate (pH 4.0, isikhathi sokuqinisekisa: izinyanga ezi-2)
Kala ngokunembile u-10.12g we-potassium hydrogen phthalate (KHC8H4O4) bese uyomisa ku-(115±5)℃ amahora angu-2 ukuya kwangu-3. Nciphisa ku-1000mL ngamanzi.
(21) Isixazululo sebhafa esijwayelekile se-Phosphate (pH 6.8, isikhathi sokuqinisekisa: izinyanga ezi-2)
Kala ngokunembile u-3.533g anhydrous disodium hydrogen phosphate kanye no-3.387g we-potassium dihydrogen phosphate omiswe ku-(115±5)°C amahora angu-2~3, bese uhlanza ku-1000mL ngamanzi.
3. Ukunqunywa kokuqukethwe kweqembu le-hydroxypropylmethylcellulose
(1) Ukunqunywa kokuqukethwe kwe-methoxyl
Ukunqunywa kokuqukethwe kweqembu le-methoxy kusekelwe ekuhlolweni okuqukethe amaqembu e-methoxy. I-Hydroiodic acid iyabola lapho ishiswa ukuze ikhiqize i-methyl iodide eguquguqukayo (iphuzu elibilayo elingu-42.5°C). I-Methyl iodide yahlanjululwa nge-nitrogen kusixazululo sokuziphendulela. Ngemva kokugeza ukuze kukhishwe izinto eziphazamisayo (HI, I2 kanye ne-H2S), umhwamuko we-methyl iodide umuncwa isixazululo se-acetic acid ye-potassium acetate equkethe i-Br2 ukuze yakhe i-IBr, bese i-oxidized ibe iodic acid. Ngemuva kokukhishwa kwe-distillation, okuqukethwe kwe-receptor kudluliselwa ebhodleleni le-iodine futhi lihlanjululwe ngamanzi. Ngemuva kokwengeza i-formic acid ukususa i-Br2 eyengeziwe, i-KI ne-H2SO4 yengezwe. Okuqukethwe kwe-methoxyl kungabalwa ngokuhlanganisa u-12 ngesixazululo se-Na2S2O3. I-equation yokusabela ingavezwa kanje.
Idivayisi yokulinganisa okuqukethwe kwe-methoxyl ikhonjiswe kuMfanekiso 7-6.
Ku-7-6(a), A iyiflask eyindilinga engu-50mL exhunywe ku-catheter. Kuneshubhu lokujiya lomoya eliqondile E elifakwe mpo ebhodleleni, elingaba ngu-25cm ubude no-9mm ububanzi bangaphakathi. Ingxenye engenhla yeshubhu igotshwe ibe yithubhu ye-capillary engilazi enobubanzi obungaphakathi obungu-2 mm kanye nendawo yokuphuma ibheke phansi. Umfanekiso 7-6(b) ubonisa idivayisi ethuthukisiwe. Umfanekiso 1 ubonisa i-reaction flask, okuyiflask eyindilinga engu-50mL, eneshubhu le-nitrogen kwesokunxele. 2 iyishubhu ye-condenser eqondile; 3 i-scrubber, equkethe uketshezi lokuwasha; 4 iyishubhu yokumunca. Umehluko omkhulu phakathi kwalolu cingo kanye nendlela ye-Pharmacopoeia ukuthi izimunca ezimbili zendlela ye-Pharmacopoeia zihlanganiswa zibe yinto eyodwa, okunganciphisa ukulahlekelwa uketshezi lokugcina lokumuncwa. Ngaphezu kwalokho, uketshezi lokugeza ku-scrubber nalo luhlukile endleleni ye-pharmacopoeia. Ingamanzi acwecwe, kuyilapho idivayisi ethuthukisiwe iyingxube yesisombululo se-cadmium sulfate kanye nesisombululo se-sodium thiosulfate, okulula ukumunca ukungcola kwegesi ehlutshiwe.
I-pipette yensimbi: 5mL (izingcezu ezingu-5), 10mL (ucezu olu-1); I-Burette: 50mL; Ibhodlela levolumu ye-iodine: 250mL; Ibhalansi yokuhlaziya.
I-phenol ye-reagent (ngoba iqinile, izoncibilika ngaphambi kokuphakela); i-carbon dioxide noma i-nitrogen; i-hydroiodic acid (45%); izinga lokuhlaziya; isixazululo se-potassium acetate (100g/L); i-bromine: ibanga lokuhlaziya; i-formic acid: ibanga lokuhlaziya; 25% isisombululo se-Sodium acetate (220g/L); I-KI: ibanga lokuhlaziya; hlambulula i-sulfuric acid (1+9); isixazululo esijwayelekile se-sodium thiosulfate (0.1mol/L); inkomba ye-phenolphthalein; 1% isisombululo se-ethanol; inkomba yesitashi: 0.5% Isixazululo esinamanzi sesitashi; hlambulula i-sulfuric acid (1+16.5); 30% isixazululo chromium trioxide; amanzi angenawo ama-organic: engeza u-10mL we-sulfuric acid ehlanjululwe (1+16.5) ku-100mL wamanzi, ukushisa kube abilayo, bese wengeza u-0.1ml we-permanganic acid engu-0.02mol/L i-Potassium titer, ubilise imizuzu eyi-10, kufanele ihlale ibomvana; I-0.02mol/L i-sodium hydroxide titrant: Linganisa i-0.1mol/L sodium hydroxide titrant ngokwendlela yesithasiselo se-Pharmacopoeia yaseShayina, bese uhlambulule ngokunembile ube ngu-0.02mol ngamanzi abilisiwe napholile ancibilikisiwe/L.
Engeza cishe u-10mL woketshezi lokuwasha eshubhuni yokuwasha, engeza u-31mL woketshezi olusanda kulungiswa lokumuncwa eshubhuni yokumunca, faka ithuluzi, ukale cishe u-0.05g wesampula elomisiwe elomisiwe ukuze libe nesisindo esingaguquki esingu-105°C (okunembe kuya ku-0.0001 g), engeza ukusabela kokuthi ℃ Ebhodleleni, engeza u-5 mL we-hydroiodide. Ngokushesha xhuma ibhodlela lokusabela ku-condenser yokutakula (manzisa imbobo yokugaya nge-hydriodic acid), bese umpompa i-nitrogen ethangini ngesilinganiso samabhamuza angu-1 ukuya kwangu-2 ngomzuzwana.
Isikhathi sokuthumela: Feb-01-2024