1, kuzivikanwa kwehydroxypropyl methyl cellulose nzira
(1) Tora 1.0g yemuenzaniso, mvura inopisa (80 ~ 90 ℃) 100mL, simbisa nguva dzose, uye inotonhorera mumvura ye viscous mubhati rechando; Isa 2mL yemvura muchubhu yekuedza, zvishoma nezvishoma wedzera 1mL sulfuric acid solution ye 0.035% anthrone pamadziro echubhu, uye siya kwe5min. Mhete yegirini inoonekwa pane chinongedzo pakati pezvinwiwa zviviri izvi.
(2) Tora huwandu hwakakodzera hweiyo yataurwa pamusoro apa inoshandiswa mukuzivikanwa kwe (ⅰ) uye uidururire pandiro yegirazi. Mushure mokunge mvura inoputika, firimu ye ductile inoumbwa.
2, hydroxypropyl methyl cellulose kuongororwa kweyakajairwa mhinduro kugadzirisa
(1) Sodium thiosulfate yakajairwa mhinduro (0.1mol/L, chokwadi: mwedzi mumwe)
Kugadzirira: Fashaidza anenge 1500mL mvura yakasvibiswa uye inotonhorera kusvika yagadzirira kushandisa. Weresa 25g sodium thiosulfate (huremu hwayo hwemamolecular 248.17, uye edza kuita chokwadi kusvika 24.817g paunenge uchiyera) kana 16g anhydrous sodium thiosulfate, inyunguduse mu200mL yemvura inotonhorera iri pamusoro, inyungurudze kusvika pa1L, woiisa mubrown. bhodhoro, isa bhodhoro murima, worisefa kuti rishandise mushure memavhiki maviri.
Calibration: Were 0.15g yereferensi potassium dichromate yakabikwa kuti irambe ichirema, yakarurama kusvika 0.0002g. Wedzera 2g potassium iodide uye 20mL sulfuric acid (1+9), zunza zvakanaka, isa murima kwe10min, wedzera 150mL mvura uye 3ml 0.5% starch indicator solution, titrate ne 0.1mol/L sodium thiosulfate solution, mhinduro inoshanduka kubva mubhuruu. kusvika kune yakasvibira yakasvibira kumagumo. Potassium chromate haina kuwedzerwa kune isina chinhu kuyedza. Maitiro ekugadzirisa akadzokororwa 2 ~ 3 nguva uye avhareji kukosha kwakatorwa.
Iyo molar concentration C (mol / L) ye sodium thiosulfate yakajairwa mhinduro yakaverengerwa seizvi:
Iko, M ndiko kuwanda kwe potassium dichromate; V1 ihuwandu hwe sodium thiosulfate inopedzwa, mL; V2 ndiyo vhoriyamu yesodium thiosulfate inopedzwa mukuedza kusina chinhu, mL; 49.03 ndiyo yakawanda ye potassium dichromate yakaenzana ne1mol ye sodium thiosulfate, g.
Mushure mekugadzirisa, wedzera zvishoma Na2CO3 kudzivirira kuparara kwehutachiona.
(2) NaOH yakajairwa mhinduro (0.1mol/L, chokwadi: mwedzi mumwe)
Kugadzirira: Inenge 4.0g yeNaOH yakachena yekuongorora yakayerwa mubeaker, uye 100mL mvura yakasvibiswa yakawedzerwa kuti inyunguduke, yozoendeswa kune 1L volumetric flask, uye mvura yakasvibiswa yakawedzerwa pachiyero, uye yakaiswa kwemazuva 7-10 kusvika. calibration.
Calibration: Isa 0.6 ~ 0.8g ye pure potassium hydrogen phthalate yakaomeswa pa 120 ℃ (yakarurama kusvika 0.0001g) mu 250mL conical flask, wedzera 75mL mvura yakasvibiswa kuti inyunguduse, wobva wawedzera 2 ~ 3 madonhwe e1% phenolphthalein. iyo iri pamusoro yakagadzirira sodium hydroxide solution kusvikira yatsvuka zvishoma, uye kuguma kwekuti ruvara haruna kupera mukati me30S. Nyora pasi huwandu hwe sodium hydroxide. Maitiro ekugadzirisa akadzokororwa 2 ~ 3 nguva uye avhareji kukosha kwakatorwa. Uye ita bvunzo isina chinhu.
Iko kusanganiswa kwesodium hydroxide solution yakaverengerwa seizvi:
Iko, C ndiko kusanganiswa kwesodium hydroxide solution, mol/L; M inomiririra huwandu hwe potassium hydrogen phthalate, G; V1 ihuwandu hwe sodium hydroxide inopedzwa, mL; V2 inomiririra vhoriyamu yesodium hydroxide inopedzwa mukuedza kusina chinhu, mL; 204.2 ndiyo molar mass ye potassium hydrogen phthalate, g pa mole.
(3) Dilute sulfuric acid (1+9) (Kushanda: 1 mwedzi)
Pasi pekusimudzira, nyatsowedzera 100mL yakagadziriswa sulfuric acid kusvika 900mL mvura yakasvibiswa, kuwedzera zvishoma nezvishoma, uchikurudzira.
(4) Dilute sulfuric acid (1+16.5) (Kushanda: mwedzi miviri)
Pasi pekusimudzira, nyatsowedzera 100mL ye concentrated sulfuric acid kusvika 1650mL yemvura yakasvibiswa, kuwedzera zvishoma nezvishoma. Kurudzira sezvaunoenda.
(5) Starch chiratidzo (1%, chokwadi: 30 mazuva)
Weresa 1.0g soluble starch, woisa 10mL mvura, kurunga nekuipinza mu100mL mvura iri kufashaira, bika zvishoma for 2min, woiisa, wotora supernatant kuti ushandise.
(6) Starch chiratidzo
0.5% starch chiratidzo chakawanikwa nekutora 5mL yeyakagadzirirwa 1% starch chiratidzo chemhinduro uye kuidzikisa kusvika ku10mL nemvura.
(7) 30% chromium trioxide solution (kutendeseka: 1 mwedzi)
Weresa 60g yechromium trioxide woinyungudutsa mu140mL yemvura isina organic matter.
(8) Potassium acetate solution (100g/L, kushanda: mwedzi miviri)
10g yeanhydrous potassium acetate zviyo zvakanyungudutswa mune 100mL mhinduro ye90mL glacial acetic acid uye 10mL acetic anhydride.
(9) 25% sodium acetate solution (220g/L, chokwadi: mwedzi miviri)
Dissolve 220g yeanhydrous sodium acetate mumvura uye wedzera kusvika ku1000mL.
(10) Hydrochloric acid (1:1, kushanda: mwedzi miviri)
Sanganisa concentrated hydrochloric acid nemvura pachiyero che1: 1.
(11) Acetate buffer solution (pH=3.5, kushanda: mwedzi miviri)
Dissolve 60mL acetic acid mumvura 500mL, wobva wawedzera 100mL ammonium hydroxide uye dilute kusvika 1000mL.
(12) Lead nitrate kugadzirira mhinduro
159.8mg ye lead nitrate yakanyungudutswa mu 100mL mvura ine 1mL ye nitric acid (density 1.42g/cm3), yakanyungudutswa ku1000mL yemvura uye yakasanganiswa zvakanaka. Kugadzirira uye kuchengetwa kwemhinduro iyi kuchaitwa mugirazi isina-lead.
(13) Yakajairwa inotungamira mhinduro (kutendeseka: 2 mwedzi)
Chiyero chakarurama che10mL yelead nitrate yekugadzirisa mhinduro yakanyungudutswa nemvura kusvika ku100mL.
(14) 2% hydroxylamine hydrochloride mhinduro (nguva yechokwadi: 1 mwedzi)
Dissolve 2g yehydroxylamine hydrochloride mu98mL yemvura.
(15) Ammonia (5mol/L, kushanda: mwedzi miviri)
175.25g yeammonia yakanyungudutswa mumvura uye yakaderedzwa kusvika ku1000mL.
(16) Mvura yakasanganiswa (nguva yekushanda: mwedzi miviri)
Sanganisa 100mL glycerol, 75mLNaOH mhinduro (1mol/L), uye 25mL mvura.
(17) Thioacetamide mhinduro (4%, chokwadi: mwedzi miviri)
4g thioacetamide yakanyungudika mumvura 96g.
(18) Phenanthroline (0.1%, chokwadi: mwedzi 1)
Dissolve 0.1g o-phenanthroline mumvura 100mL.
(19) Acid stannous chloride (kushanda: mwedzi 1)
Dissolve 20g stannous chloride mu 50mL concentrated hydrochloric acid.
(20) Potassium hydrogen phthalate standard buffer solution (pH 4.0, kushanda: mwedzi miviri)
10.12g ye potassium hydrogen phthalate (KHC8H4O4) yakayerwa nemazvo uye yakaomeswa pa (115±5) ℃ ye2 ~ 3h. Dilute kusvika 1000mL nemvura.
(21) Phosphate standard buffer solution (pH 6.8, kushanda: mwedzi miviri)
3.533g yeanhydrous disodium hydrogen phosphate uye 3.387g ye potassium dihydrogen phosphate yakaomeswa pa (115±5) ℃ kwe2 ~ 3h yakayerwa nemazvo uye yakaderedzwa kusvika 1000mL nemvura.
3, hydroxypropyl methyl cellulose boka zvemukati kutsunga
(1) Kutsunga kwemethoxy yemukati
Kutemerwa kwemethoxy content kunobva pakuparara kwehydroiodate acid nekudziisa nebvunzo ine methoxy kuti ibudise volatile methane iodide (boiling point 42.5 ° C). Methane iodide yakasvibiswa nenitrogen mune autoreaction solution. Mushure mekugeza kubvisa zvinhu zvinokanganisa (HI, I2 neH2S), iyo iodine methane vapor inotorwa ne potassium acetate acetic acid solution ine Br2 kuumba IBr uye oxidized kune iodic acid. Mushure mekuita distillation, zvinhu zviri mugadhi zvinotamirwa kumabhodhoro ayodhine uye zvakanatswa nemvura. Mushure mekuwedzera formic acid kubvisa yakawandisa Br2, KI uye H2SO4 inowedzerwa. Iyo methoxy yemukati inogona kuverengerwa nekuita 12 ine mhinduro yeNa2S2O3. Iyo reaction equation inogona kuratidzwa nenzira inotevera.
Mudziyo wekuyera methoxy content inoratidzwa muFigure 7-6.
Mu7-6 (a), A i50mL yakatenderera-pasi flask yakabatana necatheter. Iyo bhodhoro yakashongedzerwa yakatwasuka yakashongedzwa nemhepo yakatwasuka chubhu E, inenge 25cm kureba uye 9mm mukati dhayamita. Kumucheto kwepamusoro kwechubhu kwakakotama kuita girazi capillary chubhu ine kubuda yakadzika uye 2mm mukati dhayamita. Mufananidzo 7-6 (b) inoratidza mudziyo wakavandudzwa. 1 ndiyo reaction flask, inova 50mL yakatenderera-pasi flask, uye pombi yenitrogen iri kuruboshwe. 2 ndiyo vertical condensing pombi; 3 ndiyo scrubber, ine mvura yekuwachisa; 4 ndiyo chubhu inopinza. Musiyano mukuru pakati pechigadziro uye nzira ye pharmacopoeia ndeyokuti zviputi zviviri zve pharmacopoeia nzira inosanganiswa mune imwe chete, iyo inogona kuderedza kurasikirwa kwekugadzirisa kwekupedzisira. Mukuwedzera, mvura yekugezesa muscrubber yakasiyanawo neyo pharmacopoeia nzira, iyo yakasvibiswa mvura, uye yakagadziridzwa mudziyo musanganiswa we cadmium sulfate solution uye sodium thiosulfate solution, iyo inogona kupinza nyore nyore tsvina mugasi rakasvibiswa.
Chiridzwa pipette: 5mL (5), 10mL (1); Burette: 50mL; Iodine yekuyeresa bhodhoro: 250mL; Ongorora chiyero.
Reagent phenol (nokuti yakasimba, saka ichasanganiswa isati yadyisa); Carbon dioxide kana nitrogen; Hydroiodate acid (45%); Kuongorora kwezvakachena; Potassium acetate solution (100g/L); Bromine: analytically yakachena; Formic acid: analytically yakachena; 25% sodium acetate solution (220g / L); KI: analytical kuchena; Dilute sulfuric acid (1+9); Sodium thiosulfate yakajairika mhinduro (0.1mol/L); Phenolphthalein chiratidzo; 1% ethanol mhinduro; Starch chiratidzo: 0.5% starch mumvura; Dilute sulfuric acid (1 + 16.5); 30% chromium trioxide mhinduro; Mvura isina organic: wedzera 10mL dilute sulfuric acid (1+16.5) kusvika 100mL mvura, kupisa kusvika kufashaira, uye wedzera 0.1ml0.02mol /L potassium permanganate titer, bika kwe10min, inofanira kuchengeta pink; 0.02mol/L sodium hydroxide titration solution: Zvinoenderana neChinese Pharmacopoeia appendix nzira, 0.1mol/L sodium hydroxide titration solution yakarukwa uye yakaderedzwa nemazvo kusvika 0.02mol/L nemvura yakabikwa uye yakatonhodzwa yakadirwa.
Wedzera nezve 10mL yekugezesa mhinduro muchubhu yekuwachisa, wedzera 31mL yezvichangobva kugadzirwa yekunyura muchubhu yekunyudza, isa chiridzwa, uremu hunosvika 0.05g (chaiyo kusvika 0.0001g) yemuenzaniso wakaomeswa wakaomeswa kuti urambe uchirema pa105. ℃ mubhokisi rekuita, uye wedzera 5mL hydroiodate. Bhodhoro rekuita rinokurumidza kubatanidzwa kune yekudzoreredza condenser (muromo wekukuya wakanyoroveswa nehydroiodate), uye nitrogen inoputirwa mutangi pamwero we1 ~ 2 mabhuru pasekondi. Kupisa kunodzorwa zvishoma nezvishoma kuitira kuti utsi hwemvura iri kufashaira hukwire kusvika pahafu yehurefu hwemukonyeri. Nguva yekuita zvinoenderana nemhando yemuenzaniso, pakati pe45min ne3h. Bvisa chubhu inonyudza uye nyatso fambisa mushonga wemushonga mu500mL ayodini flask ine 10ml ye25% sodium acetate solution kusvika huwandu hwese hwasvika 125mL.
Pasi pekugara uchizununguka, zvishoma nezvishoma wedzera formic acid inodonha nekudonha kusvika iyo yero yanyangarika. Wedzera donhwe re 0.1% methyl tsvuku chiratidzo, uye ruvara rutsvuku harunyangarike kwemaminitsi mashanu. Wobva wawedzera madonhwe matatu efomic acid. Rega igare kwechinguva, wobva wawedzera 1g ye potassium iodide uye 5mL ye dilute sulfuric acid (1+9). Mhinduro yacho yakaitwa ne 0.1mol / L sodium thiosulfate standard solution, uye 3 ~ 4 madonhwe e0.5% starch chiratidzo akawedzerwa pedyo nekuguma, uye titration yakaenderera mberi kusvikira ruvara rwebhuruu rwanyangarika.
Mumamiriro ezvinhu akafanana, kuedza kusina chinhu kwakaitwa.
Kuverengera kweyese methoxide yemukati:
Iko, V1 inomiririra vhoriyamu (mL) yesodium thiosulfate yakajairwa mhinduro inopedzwa netitration samples; V2 ndiyo vhoriyamu yesodium thiosulfate yakajairwa mhinduro inopedzwa mukuyedzwa kusina chinhu, mL; C ndiko kusangana kwe sodium thiosulfate yakajairwa mhinduro, mol/L; M inoreva kuwanda kwemuenzaniso wakaomeswa, g; 0.00517 ndeye 0.1mol / L sodium thiosulfate pa 1ml yakaenzana ne0.00517g yemethoxy.
Iyo yakazara methoxy yemukati inomiririra iyo yakazara methoxy uye iyo hydroxyproxy kukosha kwemethoxy kuverenga, saka iyo yakazara alkoxy inofanirwa kugadziriswa neinoguma hydroxyproxy content kuti iwane chaiyo methoxy content. Iyo HYDROXYPROPOXY ZVIRI MUKATI ZVINOFANIRA KUTANGA KURENGERERWA KUTI PROPENE AKABUDZWA NEKUITWA KWAHI NEHYDROXYPROPYL NEA CONSTANT K=0.93 (ZVINOREVA ZVIKURU ZVIMWE ZVIMWE ZVIMWE ZVIMWE ZVIMWE ZVIMWE ZVINOTAURWA NEMOrgan NZIRA). Naizvozvo:
Yakagadziriswa methoxy yemukati = yakazara methoxy yemukati - (hydroxypropoxy zvemukati × 0.93 × 31/75)
Iko kune nhamba 31 uye 75 ndiyo molar mass ye methoxy uye hydroxypropoxy mapoka, zvichiteerana.
(2) Kutsunga kweiyo hydroxypropoxy yemukati
Boka rehydropropoxy mumuenzaniso rinosangana nechromium trioxide kugadzira acetic acid. Mushure mekunyungudutswa kubva kune autoreaction mhinduro, zvirimo zvechromic acid zvinotemerwa netitration neNaOH mhinduro. Nemhaka yekuti chidimbu chiduku che chromic acid chichabudiswa kunze kwekuita distillation, mhinduro yeNaOH ichadyiwawo, saka zviri mukati meiyi chromic acid zvinofanira kuwedzererwa ne iodimetry uye kubviswa kubva pakuverenga. Mhinduro equation ndeiyi:
Zviridzwa uye reagents Seti yakakwana yezviridzwa zvekutsunga kwemapoka ehydroxypropoxy; Volumetric bhodhoro: 1L, 500mL; Kuyera silinda: 50mL; Pipette: 10mL; Iodine yekuyeresa bhodhoro: 250mL. Basic burette: 10mL; Sodium thiosulfate yakajairika mhinduro (0.1mol/L); Dilute sulfuric acid (1 + 16.5); Dilute sulfuric acid (1+9); Starrch chiratidzo (0.5%).
7-7 chishandiso chekugadzirisa hydroxypropoxy yemukati.
Mu7-7 (a), D ine 25mL ine mitsipa miviri, B ichubhu ye 25mm×150mm steam jenareta, C ichubhu yekubatanidza inoyerera, A igetsi rekudziisa mafuta ekugezesa, E imbiru, G. iyo conical flask ine girazi plug, iyo yekupedzisira dhayamita yemukati ndeye 0.25-1.25mm, inopinzwa mudistilling flask; F is a condensing chubhu yakabatana neE. Muchigadzirwa chakavandudzwa chinoratidzwa muFIG. 7-7 (b), 1 ndiyo reactor, iri 50mL distillation flask; 2 ndiye musoro wezviyo; 3 i50mL yegirazi funnel yekudzora kumhanya kwekuyerera kwemvura yeorganic; 4 i nitrogen pombi; 5 ndiyo pombi inosunga. Musiyano unonyanya kukosha pakati pechigadzirwa chakagadziridzwa uye nzira ye pharmacopoeia ndeyekuwedzerwa kwegirasi girasi kudzora chiyero chekuyerera kwemvura, kuitira kuti chiyero che distillation chive nyore kudzorwa.
Nzira dzekuyedza mumuenzaniso we105 ℃ kuomeswa kusvika kuhuremu hunoramba huchingoita 0.1 g (0.0002 g), dzakanyatsotaurwa mubhodhoro redistillation, wedzera 10 ml ye30% chromium trioxide solution, the distillation flask mukapu yekugezera mafuta, mafuta ekugezesa fluid level. inoenderana nechromium trioxide liquid surface, midziyo yakaiswa, yakavhurika mvura yekutonhodza, nitrogen, yefekitari yedu kudzora mwero wenitrogen inenge bubble rimwe pasekondi. Mukati me30min, iyo yekugezesa yemafuta yakadziya kusvika 155 ℃ uye yakachengetedzwa panguva iyi tembiricha kusvika mhinduro yakaunganidzwa yasvika 50mL. Distillation yakamiswa kubvisa mafuta ekugezera.
Geza madziro emukati meinotonhorera nemvura yakasvibiswa, sanganisa mvura yekugeza uye distillate mu500mL iodine bhodhoro, wedzera madonhwe maviri e1% phenolphthalide indicator, titrate ne 0.02mol/L sodium hydroxide solution kune pH kukosha kwe6.9 ~ 7.1 , uye nyora pasi nhamba yose yesodium hydroxide inodyiwa.
Wedzera 0.5g sodium bicarbonate uye 10mL dilute sulfuric acid (1+16.5) mubhodhoro reiodine wosiya ikamira kusvika pasisina carbon dioxide yagadzirwa. Zvadaro wobva wawedzera 1.0g potassium iodide, sunga zvakasimba, zunza zvakanaka uye uisiye murima kwemaminitsi mashanu. Wobva wawedzera 1mL 0.5% starch chiratidzo uye titrate ne 0.02mol/L sodium thiosulfate kusvika kumagumo. Nyora pasi huwandu hwesodium thiosulfate inopedzwa.
Mune kumwe kuedza kusina chinhu, huwandu hwehuwandu hwe sodium hydroxide uye sodium thiosulfate titrators dzakadyiwa dzakarekodhwa zvakateerana.
Kuverengera kweiyo hydroxypropoxy yemukati:
Iko, K ndiyo inogadzirisa coefficient pikicha yeyedzo isina chinhu: V1 ndiyo vhoriyamu yesodium hydroxide titration inopedzwa nemuenzaniso, mL. C1 ndiyo chiyero che sodium hydroxide standard solution, mol/L; V2 ndiyo vhoriyamu ye sodium thiosulfate titration inopedzwa nemuenzaniso, mL; C2 ndiyo chiyero che sodium thiosulfate yakajairwa mhinduro, mol/L; M ndiye muenzaniso wehuwandu, g; Va ndiyo vhoriyamu yesodium hydroxide titration inopedzwa mukuedza kusina chinhu, mL; Vb ndiyo vhoriyamu yesodium thiosulfate titration inopedzwa muyedzo isina chinhu, mL.
4. Kutsunga unyoro
Instrumental analytical balance (yakarurama kusvika ku0.1mg); Kuyeresa bhodhoro: dhayamita 60mm, kureba 30mm; Kuomesa ovheni.
Nzira yekuedza inoyera nenzira kwayo sampuli 2 ~ 4G (
Nguva yekutumira: Sep-08-2022