Kusanthula ndi kuyesa kwa hydroxypropyl methyl cellulose

1, kuzindikiritsa njira ya hydroxypropyl methyl cellulose

(1) Tengani 1.0g ya chitsanzo, madzi otentha (80 ~ 90 ℃) 100mL, gwedezani mosalekeza, ndi kuziziritsa mumadzi owoneka bwino mumadzi oundana; Ikani 2mL yamadzimadzi mu chubu choyesera, pang'onopang'ono onjezerani 1mL sulfuric acid solution ya 0.035% mpando wachifumu pakhoma la chubu, ndikusiya kwa 5min. Mphete yobiriwira imawonekera pa mawonekedwe pakati pa zakumwa ziwirizi.

(2) Tengani kuchuluka koyenera kwa matope omwe atchulidwa pamwambapa omwe amagwiritsidwa ntchito pozindikiritsa (ⅰ) ndikutsanulira pa mbale yagalasi. Madzi akamasungunuka, filimu ya ductile imapangidwa.

2, kusanthula kwa hydroxypropyl methyl cellulose pakukonzekera kwanthawi zonse

(1) Sodium thiosulfate standard solution (0.1mol/L, kutsimikizika: mwezi umodzi)

Kukonzekera: Wiritsani pafupifupi 1500mL madzi osungunuka ndi ozizira mpaka okonzeka kugwiritsa ntchito. Yesani 25g sodium thiosulfate (kulemera kwake kwa molekyulu ndi 248.17, ndipo yesani kulondola kufika pa 24.817g pamene mukulemera) kapena 16g anhydrous sodium thiosulfate, musungunule mu 200mL ya madzi ozizira pamwambawa, sungunulani mpaka 1L, ndi kuika mu bulauni. botolo, ikani botolo mumdima, ndipo sefa kuti mugwiritse ntchito pakatha milungu iwiri.

Kuwerengera: Kulemera kwa 0.15g ya potaziyamu dichromate yophikidwa kuti ikhale yolemera nthawi zonse, yolondola mpaka 0.0002g. Onjezani 2g potassium iodide ndi 20mL sulfuric acid (1+9), gwedezani bwino, ikani mumdima kwa 10min, onjezani madzi 150mL ndi 3ml 0.5% wowuma chizindikiro yankho, titrate ndi 0.1mol/L sodium thiosulfate solution, yankho limasanduka buluu mpaka kubiriwira kowala kumapeto. Potaziyamu chromate sinawonjezedwe pakuyesa kopanda kanthu. Njira yowongolera idabwerezedwa nthawi 2 ~ 3 ndipo mtengo wapakati unatengedwa.

Mlingo wa molar C (mol/L) wa sodium thiosulfate standard solution adawerengedwa motere:

Kumene, M ndi kuchuluka kwa potaziyamu dichromate; V1 ndi kuchuluka kwa sodium thiosulfate yomwe imadyedwa, mL; V2 ndi kuchuluka kwa sodium thiosulfate yomwe imagwiritsidwa ntchito poyesera popanda kanthu, mL; 49.03 ndi unyinji wa potassium dichromate wofanana ndi 1mol wa sodium thiosulfate, g.

Mukakonza, onjezani Na2CO3 pang'ono kuti mupewe kuwonongeka kwa tizilombo.

(2) NaOH standard solution (0.1mol/L, kutsimikizika: mwezi umodzi)

Kukonzekera: Pafupifupi 4.0g ya NaOH yoyera kuti ayesedwe adayezedwa mu beaker, ndipo madzi osungunuka a 100mL anawonjezeredwa kuti asungunuke, kenako amasamutsidwa ku botolo la volumetric 1L, ndipo madzi osungunuka anawonjezeredwa pa sikelo, ndikuyikidwa kwa masiku 7-10 mpaka. kuwongolera.

Calibration: Ikani 0.6 ~ 0.8g wa koyera potaziyamu phthalate wa hydrogen phthalate zouma pa 120 ℃ (zolondola mpaka 0.0001g) mu 250mL conical botolo, onjezerani 75mL madzi osungunuka kuti musungunuke, kenaka yikani 2 ~ 3 madontho a 1% phenolphthalein ndi phenolphthalein. pamwamba okonzeka sodium hydroxide njira mpaka wofiira pang'ono, ndipo mapeto ndi kuti mtundu si kuzimiririka mkati 30S. Lembani kuchuluka kwa sodium hydroxide. Njira yowongolera idabwerezedwa nthawi 2 ~ 3 ndipo mtengo wapakati unatengedwa. Ndipo yeserani kanthu.

Kuchuluka kwa sodium hydroxide solution kunawerengedwa motere:

Kumene, C ndi ndende ya sodium hydroxide solution, mol/L; M imayimira kuchuluka kwa potaziyamu hydrogen phthalate, G; V1 ndi kuchuluka kwa sodium hydroxide yomwe imadyedwa, ml; V2 imayimira kuchuluka kwa sodium hydroxide yomwe imagwiritsidwa ntchito poyesera popanda kanthu, mL; 204.2 ndi kuchuluka kwa potassium hydrogen phthalate, g pa mole.

(3) Dilute sulfuric acid (1+9) (Kutsimikizika: 1 mwezi)

Poyambitsa, onjezerani mosamala 100mL ya sulfuric acid ku 900mL madzi osungunuka, kuwonjezera pang'onopang'ono, ndikuyambitsa.

(4) Dilute sulfuric acid (1+16.5) (Kuvomerezeka: miyezi iwiri)

Poyambitsa, onjezerani mosamala 100mL ya sulfuric acid yokhazikika ku 1650mL yamadzi osungunuka, ndikuwonjezera pang'onopang'ono. Limbikitsani pamene mukupita.

(5) Chizindikiro cha wowuma (1%, kutsimikizika: masiku 30)

Yesani 1.0g wowuma wosungunuka, onjezerani 10mL madzi, gwedezani ndi jekeseni mu 100mL madzi otentha, wiritsani pang'ono kwa 2min, ikani, ndi kutenga supernatant kuti mugwiritse ntchito.

(6) Chizindikiro cha wowuma

Chizindikiro cha 0.5% chowuma chidapezedwa potenga 5mL ya 1% yokonzekera yowuma yowuma ndikuyitsitsa mpaka 10mL ndi madzi.

(7) 30% yankho la chromium trioxide (kuvomerezeka: mwezi umodzi)

Yesani 60g ya chromium trioxide ndikusungunula mu 140mL yamadzi popanda zinthu zamoyo.

(8) Potaziyamu acetate solution (100g/L, kuvomerezeka: miyezi iwiri)

10g ya mbewu za anhydrous potassium acetate zinasungunuka mu 100mL njira ya 90mL glacial acetic acid ndi 10mL acetic anhydride.

(9) 25% sodium acetate solution (220g/L, kuvomerezeka: miyezi iwiri)

Sungunulani 220g ya anhydrous sodium acetate m'madzi ndikuchepetsa mpaka 1000mL.

(10) Hydrochloric acid (1:1, kuvomerezeka: miyezi iwiri)

Sakanizani hydrochloric acid ndi madzi mu chiŵerengero cha 1: 1.

(11) Acetate buffer solution (pH=3.5, kuvomerezeka: miyezi 2)

Sungunulani 60mL acetic acid mu 500mL madzi, kenaka onjezerani 100mL ammonium hydroxide ndi kuchepetsa ku 1000mL.

(12) Kukonzekera njira yothetsera nitrate

159.8mg ya nitrate yotsogolera inasungunuka m'madzi a 100mL omwe ali ndi 1mL ya nitric acid (kachulukidwe 1.42g / cm3), kuchepetsedwa ku 1000mL yamadzi ndikusakaniza bwino. Kukonzekera ndi kusungirako yankholi kudzachitidwa mu galasi lopanda kutsogolera.

(13) Njira yoyendetsera yokhazikika (yovomerezeka: miyezi iwiri)

Muyezo wolondola wa 10mL wa lead nitrate pokonzekera njira unachepetsedwa ndi madzi mpaka 100mL.

(14) 2% hydroxylamine hydrochloride solution (nthawi yovomerezeka: mwezi umodzi)

Sungunulani 2g ya hydroxylamine hydrochloride mu 98mL yamadzi.

(15) Ammonia (5mol/L, kuvomerezeka: miyezi iwiri)

175.25g ya ammonia idasungunuka m'madzi ndikuchepetsedwa mpaka 1000mL.

(16) Madzi osakanikirana (nthawi yovomerezeka: miyezi iwiri)

Sakanizani 100mL glycerol, 75mLNaOH solution (1mol/L), ndi 25mL madzi.

(17) Thioacetamide yankho (4%, kuvomerezeka: miyezi 2)

4g thioacetamide idasungunuka m'madzi 96g.

(18) Phenanthroline (0.1%, kuvomerezeka: mwezi umodzi)

Sungunulani 0.1g o-phenanthroline mu 100mL madzi.

(19) Acid stannous chloride (kuvomerezeka: mwezi umodzi)

Sungunulani 20g stannous chloride mu 50mL yoyikira hydrochloric acid.

(20) Potaziyamu hydrogen phthalate muyeso buffer solution (pH 4.0, kuvomerezeka: miyezi 2)

10.12g ya potaziyamu hydrogen phthalate (KHC8H4O4) idayezedwa bwino ndikuwumitsidwa pa (115±5) ℃ kwa 2 ~ 3h. Sungunulani mpaka 1000mL ndi madzi.

(21) Phosphate standard buffer solution (pH 6.8, kuvomerezeka: miyezi 2)

3.533g ya anhydrous disodium hydrogen phosphate ndi 3.387g ya potaziyamu dihydrogen phosphate zouma pa (115±5) ℃ kwa 2 ~ 3h adayezedwa molondola ndikuchepetsedwa mpaka 1000mL ndi madzi.

3, kutsimikiza kwa gulu la hydroxypropyl methyl cellulose

(1) Kutsimikiza kwa zinthu za methoxy

Kutsimikiza kwa zinthu za methoxy kumatengera kuwonongeka kwa asidi wa hydroiodate potenthetsa ndi mayeso okhala ndi methoxy kuti apange ayodini wa methane (kuwira 42.5 ° C). Methane iodide imathiridwa ndi nayitrogeni mu autoreaction solution. Pambuyo kutsuka kuchotsa zinthu zosokoneza (HI, I2 ndi H2S), mpweya wa ayodini wa methane umatengedwa ndi njira ya potaziyamu acetate acetic acid yomwe ili ndi Br2 kupanga IBr ndiyeno oxidized kukhala iodic acid. Pambuyo pa distillation, zinthu zomwe zimalandiridwa zimasamutsidwa ku mabotolo a ayodini ndikuchepetsedwa ndi madzi. Pambuyo powonjezera formic acid kuchotsa Br2 owonjezera, KI ndi H2SO4 amawonjezedwa. Zomwe zili mu methoxy zitha kuwerengedwa polemba 12 ndi yankho la Na2S2O3. The reaction equation ikhoza kufotokozedwa motere.

Chipangizo choyezera zinthu za methoxy chikuwonetsedwa mu Chithunzi 7-6.

Mu 7-6 (a), A ndi botolo la 50mL lozungulira-pansi lolumikizidwa ndi catheter. Botololi limakhala ndi chubu E chowongoka cha mpweya, pafupifupi 25cm m'litali ndi 9mm mkati mwake. Kumtunda kwa chubu kumapindika mu chubu chagalasi cha capillary chokhala ndi chotulutsira pansi ndi 2mm mkati mwake. Chithunzi 7-6 (b) chikuwonetsa chipangizo chowongoleredwa. 1 ndi botolo la reaction, lomwe ndi botolo la 50mL lozungulira, ndipo chitoliro cha nayitrogeni chili kumanzere. 2 ndi ofukula condensing chitoliro; 3 ndi scrubber, muli kutsuka madzi; 4 ndi chubu choyamwitsa. Kusiyana kwakukulu pakati pa chipangizocho ndi njira ya pharmacopoeia ndikuti zosakaniza ziwiri za njira ya pharmacopoeia zimaphatikizidwa kukhala imodzi, zomwe zingachepetse kutayika kwa njira yomaliza yoyamwa. Kuonjezera apo, madzi ochapira mu scrubber amasiyananso ndi njira ya pharmacopoeia, yomwe imakhala madzi osungunuka, ndipo chipangizo chowongolera ndi chosakaniza cha cadmium sulfate solution ndi sodium thiosulfate solution, chomwe chingathe kusokoneza mosavuta zonyansa mu gasi wosungunuka.

Chida pipette: 5mL (5), 10mL (1); Kuchuluka: 50mL; Botolo loyezera ayodini: 250mL; Ganizirani mofatsa.

Reagent phenol (chifukwa ndi olimba, kotero izo anasakaniza pamaso kudyetsa); Mpweya wa carbon dioxide kapena nayitrogeni; Hydroiodate asidi (45%); Kusanthula koyera; Potaziyamu acetate yankho (100g/L); Bromine: kusanthula koyera; Formic acid: kusanthula koyera; 25% sodium acetate solution (220g/L); KI: chiyero chowunikira; Kuchepetsa sulfuric acid (1 + 9); Sodium thiosulfate muyezo njira (0.1mol/L); Phenolphthalein chizindikiro; 1% ethanol solution; Wowuma chizindikiro: 0,5% wowuma m'madzi; Kuchepetsa sulfuric acid (1 + 16.5); 30% yankho la chromium trioxide; Madzi opanda organic: onjezerani 10mL dilute sulfuric acid (1+16.5) mpaka 100mL madzi, kutentha mpaka kuwira, ndipo onjezerani 0.1ml0.02mol /L potassium permanganate titer, wiritsani kwa mphindi 10, ziyenera kukhala pinki; 0.02mol/L sodium hydroxide titration solution: Malinga ndi njira yaku China ya Pharmacopoeia appendix, 0.1mol/L sodium hydroxide titration solution idasinthidwa ndikusinthidwa molondola mpaka 0.02mol/L ndi madzi owiritsa ndi utakhazikika.

Onjezani za 10mL ya yankho lochapira mu chubu chochapira, onjezerani 31mL ya njira yoyamwitsa yomwe yangokonzedwa kumene mu chubu choyamwitsa, ikani chidacho, cholemera pafupifupi 0.05g (zolondola mpaka 0.0001g) zouma zouma zomwe zawumitsidwa mpaka kulemera kosalekeza pa 105. ℃ mu botolo lamadzi, ndikuwonjezera 5mL hydroiodate. Botolo lomwe limapangidwa limalumikizidwa mwachangu ndi cholumikizira chotsitsimutsa (pakamwa pogaya ndi chonyowa ndi hydroiodate), ndipo nayitrogeni imapopedwa mu thanki pamlingo wa 1 ~ 2 thovu pamphindikati. Kutentha kumayendetsedwa pang'onopang'ono kuti nthunzi yamadzi otentha ikwere mpaka theka la kutalika kwa condenser. Nthawi yochitira zimadalira mtundu wa chitsanzo, pakati pa 45min ndi 3h. Chotsani chubu choyamwitsa ndikusamutsa mosamala madziwo mu botolo la ayodini la 500mL lomwe lili ndi 10ml ya 25% sodium acetate solution mpaka voliyumu yonse ifike pafupifupi 125mL.

Pakugwedezeka kosalekeza, pang'onopang'ono onjezerani formic acid dontho ndi dontho mpaka chikasu chizimiririka. Onjezani dontho la 0.1% chizindikiro chofiira cha methyl, ndipo mtundu wofiira sutha kwa mphindi 5. Kenako onjezerani madontho atatu a formic acid. Siyani kuti ikhale kwakanthawi, kenaka onjezerani 1g ya ayodini wa potaziyamu ndi 5mL ya dilute sulfuric acid (1+9). Njira yothetsera vutoli idasinthidwa ndi 0.1mol / L sodium thiosulfate standard solution, ndipo madontho 3 ~ 4 a 0.5% chizindikiro cha wowuma adawonjezedwa pafupi ndi mapeto, ndipo titration inapitilizidwa mpaka mtundu wa buluu utatha.

Muzochitika zomwezo, kuyesa kopanda kanthu kunachitidwa.

Kuwerengera kuchuluka kwa methoxide:

Kumene, V1 imayimira voliyumu (mL) ya sodium thiosulfate solution yogwiritsidwa ntchito ndi zitsanzo za titration; V2 ndi kuchuluka kwa sodium thiosulfate solution yogwiritsidwa ntchito poyesera zopanda kanthu, mL; C ndi ndende ya sodium thiosulfate muyezo njira, mol/L; M amatanthauza kulemera kwa zitsanzo zouma, g; 0.00517 ndi 0.1mol/L sodium thiosulfate pa 1ml yofanana ndi 0.00517g ya methoxy.

Zomwe zili mu methoxy zimayimira chiwerengero chonse cha methoxy ndi mtengo wa hydroxyproxy wa kuwerengera kwa methoxy, kotero kuti alkoxy yonse iyenera kukonzedwa ndi zotsatira za hydroxyproxy kuti mupeze zenizeni za methoxy. ZOKHALA ZA HYDROXYPROPOXY ZIYENERA KUKONZEDWA ZOYENERA KUKHALA ZOPHUNZITSIDWA NDI ZOMWE HI NDI HYDROXYPROPYL NDI CONSTANT K=0.93 (KUTANTHAUZA KWA ZITSANZO ZAZIKULU ZOCHEDWA NDI NTCHITO YA Morgan). Chifukwa chake:

Zomwe zasinthidwa za methoxy = zonse za methoxy - (hydroxypropoxy content × 0.93×31/75)

Kumene manambala 31 ndi 75 ndi magulu a molar a methoxy ndi hydroxypropoxy magulu, motsatira.

(2) Kudziwitsa za hydroxypropoxy

Gulu la hydropropoxy mu zitsanzo limakumana ndi chromium trioxide kupanga acetic acid. Pambuyo posungunuka kuchokera ku yankho la autoreaction, zomwe zili mu chromic acid zimatsimikiziridwa ndi titration ndi yankho la NaOH. Chifukwa chochepa cha chromic acid chidzatulutsidwa mu ndondomeko ya distillation, yankho la NaOH lidzadyedwanso, kotero zomwe zili mu chromic acid iyi ziyenera kutsimikiziridwa mowonjezereka ndi iodimetry ndikuchotsedwa pa kuwerengera. Reaction equation ndi:

Zida ndi ma reagents Gulu lathunthu la zida zowunikira magulu a hydroxypropoxy; Botolo la volumetric: 1L, 500mL; Silinda yoyezera: 50mL; Kuchuluka: 10mL; Botolo loyezera ayodini: 250mL. Freette yoyamba: 10mL; Sodium thiosulfate muyezo njira (0.1mol/L); Kuchepetsa sulfuric acid (1 + 16.5); Kuchepetsa sulfuric acid (1 + 9); Chizindikiro cha wowuma (0.5%).

7-7 ndi chipangizo chodziwitsa za hydroxypropoxy.

Mu 7-7 (a), D ndi botolo la 25mL la khosi lawiri, B ndi chubu la 25mm×150mm la nthunzi, C ndi chubu cholumikizira, A ndi chosambira chamagetsi chamagetsi, E ndi gawo la shunt, G ndi botolo la conical ndi pulagi ya galasi, mapeto ake amkati ndi 0.25-1.25mm, olowetsedwa mu botolo la distilling; F ndi chubu chokongoletsedwa cholumikizidwa ndi E. Mu chipangizo chowongoleredwa chomwe chikuwonetsedwa mu FIG. 7-7 (b), 1 ndi riyakitala, yomwe ndi 50mL distillation botolo; 2 ndiye mutu wa distillation; 3 ndi 50mL galasi funnel kulamulira liwiro organic madzi otaya; 4 ndi chitoliro cha nayitrogeni; 5 ndiye chitoliro chowongolera. Kusiyanitsa kwakukulu pakati pa chipangizo chosinthidwa ndi njira ya pharmacopoeia ndi kuwonjezera kwa galasi la galasi kuti athetse kuthamanga kwa madzi, kotero kuti mlingo wa distillation ukhoza kuyendetsedwa mosavuta.

Njira zoyesera mu zitsanzo za 105 ℃ kuyanika mpaka kulemera kosalekeza ndi pafupifupi 0.1 g (0.0002 g), zolondola zimanenedwa mu botolo la distillation, onjezerani 10 ml ya 30% chromium trioxide solution, botolo la distillation mu kapu yosambira yamafuta, mafuta osamba amadzimadzi. zogwirizana ndi chromium trioxide madzi pamwamba, zida zoikamo, madzi ozizira otseguka, nayitrogeni, a fakitale yathu kuwongolera kuchuluka kwa nayitrogeni pafupifupi kuwira kumodzi pamphindikati. Mkati mwa 30min, kusamba kwamafuta kunatenthedwa mpaka 155 ℃ ndikusungidwa pa kutentha uku mpaka yankho losonkhanitsidwa lifika 50mL. The distillation anaimitsidwa kuchotsa mafuta kusamba.

Sambani khoma lamkati la ozizira ndi madzi osungunuka, phatikizani madzi osamba ndi distillate mu botolo la ayodini la 500mL, onjezerani madontho awiri a 1% phenolphthalide indicator, titrate ndi 0.02mol / L sodium hydroxide solution ku pH ya 6.9 ~ 7.1 , ndi kulemba chiwerengero chonse cha sodium hydroxide chomwe chadyedwa.

Onjezani 0.5g sodium bicarbonate ndi 10mL dilute sulfuric acid (1+16.5) mu botolo la ayodini ndipo muyime mpaka mpweya woipa usatuluke. Kenaka yikani 1.0g potaziyamu iodide, ikani mwamphamvu, gwedezani bwino ndikusiya mumdima kwa 5min. Kenako onjezerani 1mL 0.5% chizindikiro cha wowuma ndikuchiyika ndi 0.02mol/L sodium thiosulfate mpaka kumapeto. Lembani kuchuluka kwa sodium thiosulfate yomwe yamwa.

Mu kuyesa kwina kopanda kanthu, kuchuluka kwa ma voliyumu a sodium hydroxide ndi sodium thiosulfate titrators omwe amadyedwa adalembedwa motsatana.

Kuwerengera kwa hydroxypropoxy content:

Pomwe, K ndi chithunzi chowongolera choyesera chomwe chilibe kanthu: V1 ndiye kuchuluka kwa sodium hydroxide titration yomwe imadyedwa ndi chitsanzo, mL. C1 ndiye ndende ya sodium hydroxide standard solution, mol/L; V2 ndi kuchuluka kwa sodium thiosulfate titration yomwe imadyedwa ndi chitsanzo, mL; C2 ndi ndende ya sodium thiosulfate muyezo solution, mol/L; M ndiye misa yachitsanzo, g; Va ndi kuchuluka kwa sodium hydroxide titration yomwe imagwiritsidwa ntchito poyesera, mL; Vb ndi kuchuluka kwa sodium thiosulfate titration yomwe imagwiritsidwa ntchito pakuyesa kopanda kanthu, mL.

4. Kutsimikiza kwa chinyezi

Kusanthula kwa zida (zolondola mpaka 0.1mg); Kuyeza botolo: awiri 60mm, kutalika 30mm; Kuyanika uvuni.

Njira yoyesera imalemera bwino chitsanzo 2 ~ 4G (