1, kev txheeb xyuas ntawm hydroxypropyl methyl cellulose txoj kev
(1) Siv 1.0g ntawm cov qauv, rhuab dej (80 ~ 90 ℃) 100mL, do tsis tu ncua, thiab txias rau hauv cov kua dej khov hauv da dej; Muab 2mL ntawm cov kua rau hauv lub raj kuaj, maj mam ntxiv 1mL sulfuric acid tov ntawm 0.035% anthrone raws phab ntsa raj, thiab tawm rau 5 feeb. Lub nplhaib ntsuab tshwm ntawm qhov sib txuas ntawm ob lub kua.
(2) Siv qhov tsim nyog ntawm cov slime uas tau hais los saum toj no siv rau hauv kev txheeb xyuas ntawm (ⅰ) thiab hliv rau ntawm iav phaj. Tom qab cov dej evaporates, ib zaj duab xis ductile yog tsim.
2, hydroxypropyl methyl cellulose tsom xam ntawm cov txheej txheem tshuaj npaj
(1) Sodium thiosulfate txheem tov (0.1mol / L, siv tau: ib hlis)
Kev npaj: Boil txog 1500mL dej distilled thiab txias kom txog thaum npaj siv. Qhov hnyav 25g sodium thiosulfate (nws qhov hnyav molecular yog 248.17, thiab sim ua kom raug li ntawm 24.817g thaum hnyav) lossis 16g anhydrous sodium thiosulfate, yaj hauv 200mL ntawm cov dej txias saum toj no, dilute nws mus rau 1L, thiab muab tso rau hauv xim av. lub raj mis, muab lub raj mis tso rau hauv qhov tsaus ntuj, thiab lim nws siv tom qab ob lub lis piam.
Calibration: Nyhav 0.15g ntawm siv poov tshuaj dichromate ci kom qhov hnyav tas li, raug rau 0.0002g. Ntxiv 2g poov tshuaj iodide thiab 20mL sulfuric acid (1 + 9), co zoo, muab tso rau hauv qhov tsaus ntuj rau 10min, ntxiv 150mL dej thiab 3ml 0.5% starch qhia tov, titrate nrog 0.1mol / L sodium thiosulfate tov, cov tshuaj hloov los ntawm xiav. kom ci ntsuab ntawm qhov kawg taw tes. Potassium chromate tsis tau ntxiv rau qhov kev sim dawb. Cov txheej txheem calibration tau rov ua dua 2 ~ 3 zaug thiab qhov nruab nrab tus nqi raug coj mus.
Cov molar concentration C (mol / L) ntawm sodium thiosulfate txheem tov yog xam raws li nram no:
Qhov twg, M yog qhov loj ntawm potassium dichromate; V1 yog qhov ntim ntawm sodium thiosulfate noj, mL; V2 yog qhov ntim ntawm sodium thiosulfate noj hauv kev sim dawb, mL; 49.03 yog qhov loj ntawm potassium dichromate sib npaug rau 1mol ntawm sodium thiosulfate, g.
Tom qab calibration, ntxiv me ntsis Na2CO3 los tiv thaiv microbial decomposition.
(2) NaOH txheem tov (0.1mol/L, siv tau: ib hlis)
Kev npaj: Kwv yees li 4.0g ntawm NaOH ntshiab rau kev soj ntsuam tau hnyav rau hauv lub beaker, thiab 100mL distilled dej ntxiv rau yaj, ces pauv mus rau 1L volumetric hwj, thiab cov dej distilled ntxiv rau teev, thiab muab tso rau 7-10 hnub kom txog thaum. calibration.
Calibration: Muab 0.6 ~ 0.8g ntawm cov ntshiab poov tshuaj hydrogen phthalate qhuav ntawm 120 ℃ (qhov tseeb rau 0.0001g) rau hauv 250mL conical khob, ntxiv 75mL distilled dej kom yaj, ces ntxiv 2 ~ 3 tee ntawm 1% phenolphthalein qhia, titrate nrog cov saum toj no npaj sodium hydroxide tov kom txog rau thaum nws yog liab me ntsis, thiab qhov kawg taw tes yog tias cov xim tsis ploj nyob rau hauv 30S. Sau qhov ntim ntawm sodium hydroxide. Cov txheej txheem calibration tau rov ua dua 2 ~ 3 zaug thiab qhov nruab nrab tus nqi raug coj mus. Thiab ua ib qho kev sim dawb.
Qhov concentration ntawm sodium hydroxide tov tau xam raws li hauv qab no:
Qhov twg, C yog qhov concentration ntawm sodium hydroxide tov, mol / L; M sawv cev rau qhov loj ntawm potassium hydrogen phthalate, G; V1 yog qhov ntim ntawm sodium hydroxide noj, mL; V2 sawv cev rau qhov ntim ntawm sodium hydroxide noj hauv kev sim dawb, mL; 204.2 yog cov molar loj ntawm poov tshuaj hydrogen phthalate, g ib mole.
(3) Dilute sulfuric acid (1 + 9) ( siv tau: 1 hli)
Nyob rau hauv stirring, ua tib zoo ntxiv 100mL concentrated sulfuric acid rau 900mL distilled dej, ntxiv maj mam, thaum stirring.
(4) Dilute sulfuric acid (1 + 16.5) ( siv tau: 2 lub hlis)
Nyob rau hauv stirring, ua tib zoo ntxiv 100mL ntawm concentrated sulfuric acid rau 1650mL ntawm distilled dej, ntxiv maj mam. Do thaum koj mus.
(5) Starch qhia (1%, siv tau: 30 hnub)
Qhov hnyav 1.0g soluble starch, ntxiv 10mL dej, do thiab txhaj rau hauv 100mL boiling dej, boil me ntsis rau 2 feeb, tso nws, thiab coj lub supernatant mus siv.
(6) Starch qhia
0.5% starch qhia tau los ntawm kev noj 5mL ntawm npaj 1% hmoov txhuv nplej siab qhia thiab diluting nws mus rau 10mL nrog dej.
(7) 30% chromium trioxide tov ( siv tau: 1 hli)
Qhov hnyav 60g ntawm chromium trioxide thiab yaj hauv 140mL dej yam tsis muaj teeb meem organic.
(8) Potassium acetate tov (100g / L, siv tau: 2 lub hlis)
10 g ntawm anhydrous potassium acetate nplej tau yaj hauv 100mL daws ntawm 90mL glacial acetic acid thiab 10mL acetic anhydride.
(9) 25% sodium acetate tov (220g / L, siv tau: 2 lub hlis)
Dissolve 220g ntawm anhydrous sodium acetate hauv dej thiab dilute rau 1000mL.
(10) Hydrochloric acid (1: 1, siv tau: 2 lub hlis)
Sib tov cov concentrated hydrochloric acid nrog dej ntawm 1: 1 ntim piv.
(11) Acetate buffer tov (pH = 3.5, siv tau: 2 lub hlis)
Dissolve 60mL acetic acid hauv 500mL dej, tom qab ntawd ntxiv 100mL ammonium hydroxide thiab dilute rau 1000mL.
(12) Lead nitrate npaj tov
159.8mg ntawm txhuas nitrate yog yaj nyob rau hauv 100mL dej uas muaj 1mL ntawm nitric acid (density 1.42g/cm3), diluted rau 1000mL dej thiab sib tov zoo. Kev npaj thiab khaws cia cov tshuaj no yuav tsum tau ua nyob rau hauv cov iav tsis muaj hlau lead.
(13) Cov tshuaj txhuas txhuas ( siv tau: 2 lub hlis)
Kev ntsuas qhov tseeb ntawm 10mL ntawm cov tshuaj txhuas nitrate npaj tau diluted nrog dej rau 100mL.
(14) 2% hydroxylamine hydrochloride tov (Lub sij hawm siv tau: 1 hli)
Dissolve 2g ntawm hydroxylamine hydrochloride hauv 98mL dej.
(15) Ammonia (5mol / L, siv tau: 2 lub hlis)
175.25 g ntawm ammonia yog yaj hauv dej thiab diluted rau 1000mL.
(16) Cov kua sib xyaw (lub sijhawm siv tau: 2 lub hlis)
Sib tov 100mL glycerol, 75mLNaOH tov (1mol / L), thiab 25mL dej.
(17) Thioacetamide tov (4%, siv tau: 2 lub hlis)
4g thioacetamide tau yaj hauv 96g dej.
(18) Phenanthroline (0.1%, siv tau: 1 hli)
Dissolve 0.1g o-phenanthroline hauv 100mL dej.
(19) Acid stannous chloride ( siv tau: 1 hli)
Dissolve 20g stannous chloride hauv 50mL concentrated hydrochloric acid.
(20) Potassium hydrogen phthalate standard buffer tov (pH 4.0, siv tau: 2 lub hlis)
10.12g ntawm poov tshuaj hydrogen phthalate (KHC8H4O4) yog raug hnyav thiab qhuav ntawm (115 ± 5) ℃ rau 2 ~ 3h. Dilute rau 1000ml nrog dej.
(21) Phosphate standard buffer solution (pH 6.8, siv tau: 2 lub hlis)
3.533g ntawm anhydrous disodium hydrogen phosphate thiab 3.387g ntawm poov tshuaj dihydrogen phosphate qhuav ntawm (115 ± 5) ℃ rau 2 ~ 3h tau raug hnyav thiab diluted rau 1000mL nrog dej.
3, hydroxypropyl methyl cellulose pawg cov ntsiab lus txiav txim
(1) Kev txiav txim siab ntawm cov ntsiab lus methoxy
Kev txiav txim siab ntawm cov ntsiab lus methoxy yog ua raws li qhov decomposition ntawm hydroiodate acid los ntawm cua sov nrog ib qho kev ntsuam xyuas uas muaj methoxy los tsim volatile methane iodide (boiling point 42.5 ° C). Methane iodide yog distilled nrog nitrogen hauv autoreaction tov. Tom qab ntxuav kom tshem tawm cov khoom cuam tshuam (HI, I2 thiab H2S), iodine methane vapor yog absorbed los ntawm potassium acetate acetic acid tov uas muaj Br2 los ua IBr thiab ces oxidized rau iodic acid. Tom qab distillation, cov tshuaj nyob rau hauv lub txais yuav pauv mus rau iodine fwj thiab diluted nrog dej. Tom qab ntxiv formic acid kom tshem tawm ntau tshaj Br2, KI thiab H2SO4 ntxiv. Cov ntsiab lus methoxy tuaj yeem suav tau los ntawm titrating 12 nrog kev daws ntawm Na2S2O3. Qhov sib npaug ntawm cov tshuaj tiv thaiv tuaj yeem qhia tau raws li hauv qab no.
Cov cuab yeej rau kev ntsuas cov ntsiab lus methoxy yog qhia hauv daim duab 7-6.
Hauv 7-6 (a), A yog 50mL puag ncig-hauv qab khob txuas nrog lub catheter. Lub bottleneck yog vertically nruab nrog ib tug ncaj cua condensing raj E, txog 25cm nyob rau hauv ntev thiab 9mm nyob rau hauv lub cheeb. Sab saum toj kawg ntawm lub raj yog khoov rau hauv lub khob capillary raj nrog lub qhov hluav taws xob downward thiab 2 hli nyob rau hauv txoj kab uas hla. Daim duab 7-6 (b) qhia cov cuab yeej txhim kho. 1 yog cov tshuaj tiv thaiv lub raj mis, uas yog 50mL puag ncig-hauv qab khob, thiab cov yeeb nkab nitrogen nyob sab laug. 2 yog ntsug condensing yeeb nkab; 3 yog lub tshuab ntxhua khaub ncaws, muaj cov kua ntxhua khaub ncaws; 4 yog lub raj nqus dej. Qhov sib txawv loj tshaj plaws ntawm cov cuab yeej thiab cov tshuaj pharmacopoeia yog tias ob lub absorbers ntawm txoj kev tshuaj pharmacopoeia tau muab tso ua ke rau hauv ib qho, uas tuaj yeem txo qhov poob ntawm qhov kawg nqus dej. Tsis tas li ntawd, cov kua ntxhua hauv lub tshuab ntxhua khaub ncaws kuj txawv ntawm cov tshuaj pharmacopoeia, uas yog cov dej distilled, thiab cov cuab yeej txhim kho yog kev sib xyaw ntawm cadmium sulfate tov thiab sodium thiosulfate tov, uas tuaj yeem yooj yim adsorb cov impurities hauv cov roj distilled.
Instrument pipette: 5mL (5), 10mL (1); Qhov hnyav: 50 ml; Iodine ntsuas lub raj mis: 250mL; Txheeb xyuas qhov sib npaug.
Reagent phenol (vim nws yog ib qho khoom, yog li nws yuav raug fused ua ntej noj); carbon dioxide los yog nitrogen; Hydroiodate acid (45%); Kev tsom xam ntawm ntshiab; Potassium acetate tov (100g / L); Bromine: analytically ntshiab; Formic acid: analytically ntshiab; 25% sodium acetate tov (220g / L); KI: analytical purity; Dilute sulfuric acid (1 + 9); Sodium thiosulfate txheem tov (0.1mol / L); Phenolphthalein qhia; 1% ethanol kua; Starch qhia: 0.5% starch hauv dej; Dilute sulfuric acid (1 + 16.5); 30% chromium trioxide tov; Organic-dawb dej: ntxiv 10mL dilute sulfuric acid (1 + 16.5) rau 100mL dej, kub rau boiling, thiab ntxiv 0.1ml0.02mol /L poov tshuaj permanganate titer, boil rau 10min, yuav tsum kom liab; 0.02mol/L sodium hydroxide titration solution: Raws li Suav Pharmacopoeia appendix method, 0.1mol/L sodium hydroxide titration solution yog calibrated thiab raug diluted rau 0.02mol/L nrog boiled thiab txias distilled dej.
Ntxiv li 10mL ntawm cov tshuaj ntxuav rau hauv lub tshuab ntxhua khaub ncaws, ntxiv 31mL ntawm cov tshuaj uas tau npaj tshiab nqus rau hauv lub raj nqus dej, teeb tsa cov cuab yeej, hnyav li 0.05g (qhov tseeb rau 0.0001g) ntawm cov qauv qhuav uas tau qhuav kom qhov hnyav tas li ntawm 105. ℃ rau hauv cov tshuaj tiv thaiv lub khob, thiab ntxiv 5mL hydroiodate. Cov tshuaj tiv thaiv lub raj mis txuas nrog ceev ceev rau cov rov qab condenser (lub qhov ncauj sib tsoo yog moistened nrog hydroiodate), thiab nitrogen yog pumped rau hauv lub tank ntawm tus nqi ntawm 1 ~ 2 npuas ib ob. Qhov ntsuas kub tau tswj tau maj mam kom lub zog ntawm cov kua boiling nce mus rau ib nrab ntawm qhov siab ntawm lub condenser. Lub sij hawm cov tshuaj tiv thaiv nyob ntawm tus qauv, ntawm 45min thiab 3h. Tshem lub raj nqus dej thiab ua tib zoo xa cov tshuaj nqus mus rau hauv 500mL iodine flask uas muaj 10ml ntawm 25% sodium acetate tov kom txog thaum tag nrho cov ntim nce txog 125mL.
Nyob rau hauv tas li co, maj mam ntxiv formic acid poob los ntawm kev poob kom txog thaum lub daj ploj. Ntxiv ib qho poob ntawm 0.1% methyl liab qhia, thiab xim liab tsis ploj rau 5 feeb. Tom qab ntawd ntxiv peb tee ntawm formic acid. Cia nws zaum ib pliag, ces ntxiv 1g ntawm poov tshuaj iodide thiab 5mL ntawm dilute sulfuric acid (1 + 9). Cov tshuaj tau titrated nrog 0.1mol / L sodium thiosulfate txheem tov, thiab 3 ~ 4 tee ntawm 0.5% starch qhia tau ntxiv nyob ze ntawm qhov kawg, thiab titration tau txuas ntxiv mus txog thaum xim xiav ploj.
Nyob rau tib lub sijhawm, ib qho kev sim dawb tau ua.
Kev suav tag nrho cov ntsiab lus methoxide:
Qhov twg, V1 sawv cev rau qhov ntim (mL) ntawm sodium thiosulfate txheem tshuaj noj los ntawm cov qauv titration; V2 yog qhov ntim ntawm sodium thiosulfate tus qauv kev daws teeb meem siv hauv kev sim dawb, mL; C yog qhov concentration ntawm sodium thiosulfate txheem tov, mol / L; M hais txog qhov loj ntawm cov qauv qhuav, g; 0.00517 yog 0.1mol / L sodium thiosulfate ib 1ml sib npaug rau 0.00517g ntawm methoxy.
Tag nrho cov ntsiab lus methoxy sawv cev rau tag nrho methoxy thiab tus nqi hydroxyproxy ntawm kev suav methoxy, yog li tag nrho alkoxy yuav tsum raug kho los ntawm cov ntsiab lus hydroxyproxy kom tau txais cov ntsiab lus methoxy. Cov ntsiab lus ntawm HYDROXYPROPOXY yuav tsum tau kho ua ntej rau kev tsim tawm los ntawm kev ua haujlwm ntawm HI nrog HYDROXYPROPYL nrog K = 0.93 (TSIS TAU TXAIS LUB SIJ HAWM LOS NTAWM LUB SIJ HAWM TSHIAB). Yog li ntawd:
Kho cov ntsiab lus methoxy = tag nrho cov ntsiab lus methoxy - (hydroxypropoxy cov ntsiab lus × 0.93 × 31/75)
Qhov twg tus lej 31 thiab 75 yog cov molar pawg ntawm methoxy thiab hydroxypropoxy pawg, feem.
(2) Kev txiav txim siab ntawm cov ntsiab lus hydroxypropoxy
Cov pab pawg hydropropoxy nyob rau hauv cov qauv reacts nrog chromium trioxide los tsim acetic acid. Tom qab distilled los ntawm cov tshuaj autoreaction, cov ntsiab lus ntawm chromic acid yog txiav txim los ntawm titration nrog NaOH kua. Vim hais tias ib qho me me ntawm chromic acid yuav raug coj tawm hauv cov txheej txheem distillation, cov tshuaj NaOH kuj tseem yuav tau noj, yog li cov ntsiab lus ntawm chromic acid no yuav tsum tau txiav txim siab ntxiv los ntawm iodimetry thiab txiav tawm los ntawm kev suav. Qhov sib npaug ntawm cov tshuaj tiv thaiv yog:
Cov cuab yeej thiab cov tshuaj reagents Cov cuab yeej ua tiav rau kev txiav txim siab ntawm pawg hydroxypropoxy; Lub raj mis Volumetric: 1L, 500mL; Ntsuas lub tog raj kheej: 50mL; Peev: 10ml; Iodine ntsuas lub raj mis: 250mL. Basic burette: 10mL; Sodium thiosulfate txheem tov (0.1mol / L); Dilute sulfuric acid (1 + 16.5); Dilute sulfuric acid (1 + 9); Starch qhia (0.5%).
7-7 yog ib qho khoom siv rau kev txiav txim siab ntawm cov ntsiab lus hydroxypropoxy.
Nyob rau hauv 7-7 (a), D yog 25mL ob-caj dab distilling hwj, B yog 25mm × 150mm chav generator raj, C yog ib tug khiav kev twb kev txuas raj, A yog ib tug hluav taws xob cua sov roj da dej, E yog ib tug shunt kem, G yog lub khob ntim nrog lub khob ntsaws, qhov kawg sab hauv txoj kab uas hla yog 0.25-1.25mm, muab tso rau hauv lub khob distilling; F yog ib lub raj condensing txuas nrog E. Nyob rau hauv cov cuab yeej txhim kho pom nyob rau hauv FIG. 7-7 (b), 1 yog lub reactor, uas yog 50mL distillation flask; 2 yog lub taub hau distillation; 3 yog 50mL iav funnel los tswj kev ceev ntawm cov dej organic; 4 yog cov yeeb nkab nitrogen; 5 yog cov yeeb nkab condensing. Qhov sib txawv tseem ceeb tshaj plaws ntawm cov cuab yeej hloov kho thiab cov tshuaj pharmacopoeia yog qhov sib ntxiv ntawm lub iav funnel los tswj tus nqi ntawm cov dej ntws, kom tus nqi ntawm distillation tuaj yeem tswj tau yooj yim.
Cov kev sim hauv cov qauv ntawm 105 ℃ ziab kom qhov hnyav tas li yog li 0.1 g (0.0002 g), raug hais hauv lub raj mis distillation, ntxiv 10 ml ntawm 30% chromium trioxide tov, lub distillation flask rau hauv roj da dej khob, roj da dej theem. zoo ib yam nrog chromium trioxide kua nto, ntsia khoom, qhib dej txias, nitrogen, ntawm peb lub Hoobkas los tswj tus nqi ntawm nitrogen txog ib npuas ib ob. Tsis pub dhau 30min, cov roj da dej tau rhuab mus rau 155 ℃ thiab khaws cia ntawm qhov kub thiab txias kom txog thaum cov tshuaj sib sau mus txog 50mL. Lub distillation tau nres kom tshem tawm cov roj da dej.
Ntxuav cov phab ntsa sab hauv ntawm lub txias txias nrog dej distilled, muab cov dej ntxuav thiab cov distillate rau hauv 500mL iodine lub raj mis, ntxiv 2 tee ntawm 1% phenolphthalide qhia, titrate nrog 0.02mol / L sodium hydroxide tov rau pH nqi ntawm 6.9 ~ 7.1. , thiab sau tag nrho cov naj npawb ntawm sodium hydroxide noj.
Ntxiv 0.5g sodium bicarbonate thiab 10mL dilute sulfuric acid (1 + 16.5) rau lub raj mis iodine thiab cia nws sawv ntsug kom txog thaum tsis muaj carbon dioxide tsim. Tom qab ntawd ntxiv 1.0g potassium iodide, ntsaws nws nruj nreem, co nws zoo thiab tawm hauv qhov tsaus rau 5 feeb. Tom qab ntawd ntxiv 1mL 0.5% starch qhia thiab titrate nws nrog 0.02mol / L sodium thiosulfate mus rau qhov kawg point. Sau cov ntim ntawm sodium thiosulfate noj.
Hauv lwm qhov kev sim dawb, cov naj npawb ntawm sodium hydroxide thiab sodium thiosulfate titrators noj tau raug sau tseg.
Kev suav ntawm hydroxypropoxy cov ntsiab lus:
Qhov twg, K yog daim duab kho coefficient ntawm qhov kev sim dawb paug: V1 yog qhov ntim ntawm sodium hydroxide titration noj los ntawm tus qauv, mL. C1 yog qhov concentration ntawm sodium hydroxide txheem tov, mol / L; V2 yog qhov ntim ntawm sodium thiosulfate titration noj los ntawm cov qauv, mL; C2 yog qhov concentration ntawm sodium thiosulfate txheem tov, mol / L; M yog cov qauv loj, g; Va yog qhov ntim ntawm sodium hydroxide titration noj hauv kev sim dawb, mL; Vb yog qhov ntim ntawm sodium thiosulfate titration noj nyob rau hauv qhov kev sim dawb paug, mL.
4. Kev txiav txim siab ntawm noo noo
Instrumental analytical tshuav nyiaj li cas (qhov tseeb rau 0.1mg); Lub raj mis ntsuas: txoj kab uas hla 60mm, qhov siab 30mm; Qhuav qhov cub.
Txoj kev sim ntsuas ntsuas qhov hnyav ntawm tus qauv 2 ~ 4G (
Post lub sij hawm: Sep-08-2022