1. Njira yodziwika ya hydroxypropyl methylcellulose
(1) Tengani 1.0g ya chitsanzo, kutentha 100mL madzi (80 ~ 90 ℃), kusonkhezera mosalekeza, ndi kuziziritsa mu ayezi kusamba mpaka kukhala viscous madzi; ikani 2mL yamadzimadzi mu chubu choyesera, ndipo pang'onopang'ono onjezerani 1mL ya 0.035% athrone sulfuric acid pamodzi ndi yankho la khoma la chubu ndikusiya kwa mphindi zisanu. Mphete yobiriwira imawonekera pamawonekedwe apakati pazamadzimadzi awiriwa.
(2) Tengani ntchofu yoyenerera yomwe imagwiritsidwa ntchito pozindikiritsa (I) pamwambapa ndikutsanulira pa mbale yagalasi. Madzi akamasungunuka, filimu ya ductile imapanga.
2. Kukonzekera kwa hydroxypropyl methylcellulose kusanthula njira yothetsera
(1) Sodium thiosulfate muyezo yankho (0.1mol/L, nthawi yovomerezeka: 1 mwezi)
Kukonzekera: Wiritsani pafupifupi 1500mL madzi osungunuka, ozizira ndi kuika pambali. Yesani 25g sodium thiosulfate (kulemera kwake kwa maselo ndi 248.17, yesetsani kukhala olondola monga 24.817g pamene mukulemera) kapena 16g anhydrous sodium thiosulfate, sungunulani mu 200mL wa madzi ozizira pamwambawa, sungunulani ku 1L, ikani mu botolo la bulauni. ndikuyika Sungani pamalo amdima, sefa ndikuyika pambali pakadutsa milungu iwiri.
Kuwerengera: Yezani 0.15g ya potaziyamu dichromate ndikuphika kuti mukhale wolemera nthawi zonse, molondola mpaka 0.0002g. Onjezerani 2g potaziyamu iodide ndi 20mL sulfuric acid (1+9), gwedezani bwino, ndikuyika mumdima kwa mphindi khumi. Onjezani madzi 150mL ndi 3ml 0.5% yankho la wowuma, ndi titrate ndi 0.1mol/L sodium thiosulfate solution. Yankho lake limasintha kuchokera ku buluu kupita ku buluu. Amatembenuza wobiriwira wowala kumapeto. Palibe potassium chromate yomwe idawonjezedwa pakuyesa kopanda kanthu. Njira yoyeserera imabwerezedwa 2 mpaka 3 ndipo mtengo wapakati umatengedwa.
Mlingo wa molar C (mol/L) wa sodium thiosulfate muyezo wa yankho umawerengedwa motsatira njira iyi:
Mu chilinganizo, M ndi kuchuluka kwa potaziyamu dichromate; V1 ndi kuchuluka kwa sodium thiosulfate yomwe imadyedwa, mL; V2 ndi kuchuluka kwa sodium thiosulfate yomwe imagwiritsidwa ntchito pakuyesa kopanda kanthu, mL; 49.03 ndi dichromium yofanana ndi 1 mol ya sodium thiosulfate. Kuchuluka kwa potaziyamu acid, g.
Pambuyo poyesa, onjezerani Na2CO3 pang'ono kuti mupewe kuwonongeka kwa tizilombo.
(2) NaOH muyezo yankho (0.1mol/L, nthawi yovomerezeka: 1 mwezi)
Kukonzekera: Yesani pafupifupi 4.0g ya NaOH yoyera kuti muwunike mu beaker, onjezerani 100mL ya madzi osungunuka kuti asungunuke, kenaka tumizani ku botolo la volumetric 1L, onjezerani madzi osungunuka pa chizindikirocho, ndikusiya kwa masiku 7-10 mpaka makonzedwe.
Calibration: Place 0.6 ~ 0.8g koyera potaziyamu phthalate wa hydrogen (zolondola 0.0001g) zouma pa 120 ° C mu 250mL Erlenmeyer botolo, kuwonjezera 75mL madzi osungunuka kupasuka, ndiyeno onjezerani 2 ~ 3 madontho a 1% mu phenolph. Titrate ndi titrant. Limbikitsani yankho la sodium hydroxide lomwe lakonzedwa pamwambapa mpaka litakhala lofiira pang'ono, ndipo mtunduwo suzimiririka mkati mwa masekondi 30 ngati pomaliza. Lembani voliyumu ya sodium hydroxide. Njira yoyeserera imabwerezedwa 2 mpaka 3 ndipo mtengo wapakati umatengedwa. Ndipo yeserani kanthu.
Kuchuluka kwa sodium hydroxide solution kumawerengedwa motere:
Mu chilinganizo, C ndi ndende ya sodium hydroxide solution, mol/L; M imayimira kuchuluka kwa potaziyamu hydrogen phthalate, G; V1 - kuchuluka kwa sodium hydroxide kudyedwa, ml; V2 imayimira sodium hydroxide yomwe imadyedwa muyeso yopanda kanthu Volume, mL; 204.2 ndi mchere wa potaziyamu hydrogen phthalate, g/mol.
(3) Dilute sulfuric acid (1+9) (nthawi yovomerezeka: mwezi umodzi)
Pamene mukuyambitsa, onjezerani mosamala 100 ml ya concentrated sulfuric acid ku 900 ml ya madzi osungunuka ndikuwonjezera pang'onopang'ono pamene mukuyambitsa.
(4) Dilute sulfuric acid (1+16.5) (nthawi yovomerezeka: miyezi iwiri)
Pamene mukuyambitsa, onjezerani mosamala 100 ml ya concentrated sulfuric acid ku 1650 ml ya madzi osungunuka ndikuwonjezera pang'onopang'ono. Limbikitsani pamene mukupita.
(5) Chizindikiro cha wowuma (1%, nthawi yovomerezeka: masiku 30)
Yesani 1.0g ya wowuma wosungunuka, onjezerani 10mL ya madzi, gwedezani ndi kutsanulira mu 100mL ya madzi otentha, wiritsani kwa mphindi ziwiri, muyime, ndi kutenga supernatant kuti mugwiritse ntchito mtsogolo.
(6) Chizindikiro cha wowuma
Tengani 5 ml ya yankho lokonzekera 1% la wowuma ndikulitsitsa ndi madzi mpaka 10 ml kuti mupeze chizindikiro cha 0.5%.
(7) 30% yankho la chromium trioxide (nthawi yovomerezeka: mwezi umodzi)
Yesani 60g ya chromium trioxide ndikusungunula mu 140mL yamadzi opanda organic.
(8) Potaziyamu acetate solution (100g/L, yovomerezeka kwa miyezi iwiri)
Sungunulani 10 g wa anhydrous potassium acetate granules mu 100 ml ya yankho la 90 ml ya glacial acetic acid ndi 10 mL acetic anhydride.
(9) 25% sodium acetate solution (220g/L, nthawi yovomerezeka: miyezi iwiri)
Sungunulani 220g anhydrous sodium acetate m'madzi ndikuchepetsa mpaka 1000mL.
(10) Hydrochloric acid (1:1, nthawi yovomerezeka: miyezi iwiri)
Sakanizani hydrochloric acid ndi madzi mu chiŵerengero cha 1: 1.
(11) Acetate buffer (pH=3.5, nthawi yovomerezeka: miyezi iwiri)
Sungunulani 60mL ya asidi acetic mu 500mL yamadzi, kenaka onjezerani 100mL ya ammonium hydroxide ndi kuchepetsa ku 1000mL.
(12) Kukonzekera njira yothetsera nitrate
Sungunulani 159.8 mg lead nitrate mu 100 mL madzi okhala ndi 1 mL nitric acid (kachulukidwe 1.42 g/cm3), sungunulani mpaka 1000 mL madzi, ndipo sakanizani bwino. Zokonzedwa bwino. Njira yothetsera vutoli iyenera kukonzedwa ndikusungidwa mu galasi lopanda kutsogolera.
(13) Njira yoyendetsera (nthawi yovomerezeka: miyezi 2)
Yesani bwino 10mL ya lead nitrate yokonzekera yankho ndikuwonjezera madzi kuti asungunuke mpaka 100mL.
(14) 2% hydroxylamine hydrochloride solution (nthawi yovomerezeka: mwezi umodzi)
Sungunulani 2g ya hydroxylamine hydrochloride mu 98mL yamadzi.
(15) Ammonia (5mol/L, yovomerezeka kwa miyezi iwiri)
Sungunulani 175.25g ammonia madzi ndi kuchepetsa 1000mL.
(16) Zosakaniza zamadzimadzi (zovomerezeka: miyezi iwiri)
Sakanizani 100mL ya glycerol, 75mL ya NaOH solution (1mol/L) ndi 25mL yamadzi.
(17) Thioacetamide solution (4%, yovomerezeka kwa miyezi iwiri)
Sungunulani 4g wa thioacetamide mu 96g madzi.
(18) Phenanthroline (0.1%, nthawi yovomerezeka: mwezi umodzi)
Sungunulani 0.1g ya phenanthroline mu 100mL madzi.
(19) Acid stannous chloride (nthawi yovomerezeka: mwezi umodzi)
Sungunulani 20 g wa stannous chloride mu 50mL wa hydrochloric acid wokhazikika.
(20) Potaziyamu hydrogen phthalate muyezo wa buffer solution (pH 4.0, nthawi yovomerezeka: miyezi iwiri)
Yeretsani bwino 10.12g ya potaziyamu hydrogen phthalate (KHC8H4O4) ndikuyimitsa pa (115±5) ℃ kwa maola awiri mpaka atatu. Sungunulani mpaka 1000mL ndi madzi.
(21) Phosphate standard buffer solution (pH 6.8, nthawi yovomerezeka: miyezi iwiri)
Yesani bwino 3.533g anhydrous disodium hydrogen phosphate ndi 3.387g potaziyamu dihydrogen phosphate zouma pa (115±5)°C kwa maola 2~3, ndi kuchepetsa mpaka 1000mL ndi madzi.
3. Kutsimikiza kwa gulu la hydroxypropylmethylcellulose
(1) Kutsimikiza kwa methoxyl
Kutsimikiza kwa gulu la methoxy kumatengera mayeso omwe ali ndi magulu a methoxy. Hydroiodic acid imawola ikatenthedwa kuti ipangitse methyl iodide yosakhazikika (kuwira kwa 42.5°C). Methyl iodide idasungunuka ndi nayitrogeni mu njira yodzichitira yokha. Pambuyo kutsuka kuchotsa zinthu zosokoneza (HI, I2 ndi H2S), nthunzi ya methyl iodide imatengedwa ndi acetic acid solution ya potaziyamu acetate yomwe ili ndi Br2 kupanga IBr, yomwe imasinthidwa kukhala iodic acid. Pambuyo pa distillation, zomwe zili mu cholandirira zimasamutsidwa ku botolo la ayodini ndikuchepetsedwa ndi madzi. Pambuyo powonjezera formic acid kuchotsa Br2 owonjezera, KI ndi H2SO4 amawonjezedwa. Zomwe zili methoxyl zitha kuwerengedwa polemba 12 ndi yankho la Na2S2O3. The reaction equation ikhoza kufotokozedwa motere.
Chipangizo choyezera zinthu za methoxyl chikuwonetsedwa mu Chithunzi 7-6.
Mu 7-6 (a), A ndi botolo la 50mL lozungulira-pansi lolumikizidwa ndi catheter. Pali chubu chowongoka cha mpweya E choyikidwa molunjika pa botolo, pafupifupi 25cm kutalika ndi 9mm mkati mwake. Kumtunda kwa chubu kumapindika mu chubu chagalasi cha capillary chokhala ndi mainchesi 2 mm ndipo chotuluka chimayang'ana pansi. Chithunzi 7-6(b) chikuwonetsa chipangizo chowongoleredwa. Chithunzi 1 chikuwonetsa botolo lamadzi, lomwe ndi botolo lozungulira la 50mL, ndi chubu cha nayitrogeni kumanzere. 2 ndi vertical condenser chubu; 3 ndi scrubber, muli kutsuka madzi; 4 ndi chubu choyamwitsa. Kusiyana kwakukulu pakati pa chipangizochi ndi njira ya Pharmacopoeia ndikuti zotsekemera ziwiri za njira ya Pharmacopoeia zimaphatikizidwa kukhala imodzi, zomwe zingachepetse kutaya kwa madzi omaliza. Kuphatikiza apo, madzi ochapira mu scrubber amasiyananso ndi njira ya pharmacopoeia. Ndi madzi osungunula, pamene chipangizo chowongolera ndi chosakaniza cha cadmium sulfate solution ndi sodium thiosulfate solution, chomwe chimakhala chosavuta kutenga zonyansa mu gasi wosungunuka.
Chida pipette: 5mL (5 zidutswa), 10mL (1 chidutswa); Kuchuluka: 50mL; Botolo la ayodini: 250mL; Kuwerengera bwino.
Reagent phenol (chifukwa ndi yolimba, idzasungunuka musanadye); carbon dioxide kapena nayitrogeni; asidi hydroiodic (45%); kalasi yowunikira; potaziyamu acetate solution (100g/L); bromine: kalasi yowunikira; asidi formic: kusanthula kalasi; 25% Sodium acetate solution (220g/L); KI: kalasi yowunikira; kuchepetsa sulfuric acid (1+9); sodium thiosulfate muyezo njira (0.1mol/L); phenolphthalein chizindikiro; 1% ethanol solution; wowuma chizindikiro: 0,5% Wowuma amadzimadzi njira; kuchepetsa sulfuric acid (1 + 16.5); 30% chromium trioxide solution; madzi opanda organic: onjezerani 10mL ya sulfuric acid (1+16.5) ku 100mL ya madzi, kutentha mpaka kuwira, ndipo onjezerani 0.1ml wa 0.02mol permanganic acid titer ya Potaziyamu, wiritsani kwa mphindi khumi, iyenera kukhala pinki; 0.02mol/L sodium hydroxide titrant: Sinthani 0.1mol/L sodium hydroxide titrant molingana ndi njira yaku China Pharmacopoeia appendix, ndikuchepetsa molondola mpaka 0.02mol ndi madzi owiritsa ndi utakhazikika osungunuka / L.
Onjezani pafupifupi 10mL yamadzi ochapira mu chubu chochapira, onjezerani 31mL wamadzimadzi omwe angokonzedwa kumene mu chubu choyamwitsa, ikani chidacho, kulemera pafupifupi 0.05g ya zouma zouma zomwe zawumitsidwa mpaka kulemera kosalekeza pa 105 ° C (zolondola mpaka 0.0001) g), onjezani zomwe zimachitika ℃ Mu botolo, onjezerani 5 mL wa hydroiodide. Lumikizani mwachangu botolo la zomwe zimachitikira ku condenser yobwezeretsa (nyowetsani doko logaya ndi hydriodic acid), ndikupopera nayitrogeni mu thanki pamlingo wa 1 mpaka 2 thovu pamphindikati.
Nthawi yotumiza: Feb-01-2024