1. Hanyar ganewa na hydroxypropyl methylcellulose
(1) Ɗauki 1.0g na samfurin, zafi 100mL na ruwa (80 ~ 90 ℃), motsawa akai-akai, kuma sanyaya a cikin wanka na kankara har sai ya zama ruwa mai danko;saka 2mL na ruwa a cikin bututun gwaji, sannan a hankali ƙara 1ml na 0.035% anthrone sulfuric acid tare da maganin bangon bututu sannan a bar shi na mintuna 5.Koren zobe yana bayyana a mahaɗin tsakanin ruwayoyin biyu.
(2) Ɗauki adadin da ya dace na ƙoƙon da aka yi amfani da shi don ganewa a cikin (I) a sama kuma a zuba a kan farantin gilashi.Yayin da ruwa ya ƙafe, fim ɗin ductile yana samuwa.
2. Shiri na hydroxypropyl methylcellulose bincike daidaitaccen bayani
(1) Sodium thiosulfate daidaitaccen bayani (0.1mol/L, lokacin inganci: wata 1)
Shiri: tafasa kamar 1500mL distilled ruwa, sanyi kuma ajiye.Auna nauyin 25g sodium thiosulfate (nauyin kwayoyinsa 248.17, gwada daidai kamar 24.817g lokacin yin awo) ko 16g anhydrous sodium thiosulfate, narkar da shi a cikin 200mL na ruwan sanyi na sama, tsarma zuwa 1L, sanya shi a cikin kwalban ruwan kasa, sannan a ajiye a wuri mai duhu, tace sannan a ajiye bayan sati biyu.
Calibration: Auna 0.15g na tunani potassium dichromate da gasa zuwa kullum nauyi, daidai zuwa 0.0002g.Ƙara 2g potassium iodide da 20ml sulfuric acid (1+9), girgiza da kyau, kuma sanya a cikin duhu na minti 10.Ƙara 150mL ruwa da 3ml 0.5% sitaci bayani bayani, da kuma titrate tare da 0.1mol/L sodium thiosulfate bayani.Maganin yana canzawa daga shuɗi zuwa shuɗi.Yana juya kore mai haske a ƙarshen ƙarshen.Ba a ƙara chromate na potassium a cikin gwajin da ba komai ba.Ana maimaita tsarin daidaitawa sau 2 zuwa 3 kuma ana ɗaukar matsakaicin ƙimar.
Ana ƙididdige ma'auni na molar C (mol / L) na daidaitaccen bayani na sodium thiosulfate bisa ga dabara mai zuwa:
A cikin tsari, M shine adadin potassium dichromate;V1 shine ƙarar sodium thiosulfate cinyewa, mL;V2 shine ƙarar sodium thiosulfate da aka cinye a cikin gwaji mara kyau, mL;49.03 shine dichromium daidai da 1 mol na sodium thiosulfate.Matsakaicin adadin potassium, g.
Bayan daidaitawa, ƙara ƙaramin adadin Na2CO3 don hana bazuwar ƙwayoyin cuta.
(2) NaOH daidaitaccen bayani (0.1mol/L, lokacin inganci: wata 1)
Shiri: Auna kimanin 4.0g na NaOH mai tsabta don bincike a cikin beaker, ƙara 100mL na ruwa mai narkewa don narke, sa'an nan kuma canjawa wuri zuwa 1L volumetric flask, ƙara distilled ruwa zuwa alamar, kuma bar shi tsawon kwanaki 7-10 har sai an daidaita shi.
Calibration: Sanya 0.6 ~ 0.8g na tsantsa potassium hydrogen phthalate (daidai zuwa 0.0001g) bushe a 120 ° C cikin 250mL Erlenmeyer flask, ƙara 75mL na distilled ruwa don narkewa, sa'an nan kuma ƙara 2 ~ 3 saukad da na 1% phenolphthalein nuna alama.Titrate tare da titrant.Sanya maganin sodium hydroxide da aka shirya a sama har sai ya ɗan yi ja, kuma launi ba ya ɓacewa cikin daƙiƙa 30 a matsayin ƙarshen ƙarshen.Rubuta ƙarar sodium hydroxide.Ana maimaita tsarin daidaitawa sau 2 zuwa 3 kuma ana ɗaukar matsakaicin ƙimar.Kuma ku yi gwaji mara kyau.
Ana ƙididdige yawan adadin maganin sodium hydroxide kamar haka:
A cikin dabarar, C shine ƙaddamar da maganin sodium hydroxide, mol / L;M yana wakiltar adadin potassium hydrogen phthalate, G;V1 - ƙarar sodium hydroxide cinyewa, mL;V2 yana wakiltar sodium hydroxide da ake cinyewa a cikin gwaji mara kyau Ƙarar, mL;204.2 shine ma'aunin ƙwanƙwasa na potassium hydrogen phthalate, g/mol.
(3) Narke sulfuric acid (1+9) (lokacin inganci: wata 1)
Yayin motsawa, a hankali ƙara 100 ml na sulfuric acid mai mahimmanci zuwa 900 ml na ruwa mai narkewa kuma ƙara sannu a hankali yayin motsawa.
(4) Narke sulfuric acid (1+16.5) (lokacin inganci: watanni 2)
Yayin motsawa, a hankali ƙara 100 ml na sulfuric acid mai mahimmanci zuwa 1650 ml na ruwa mai narkewa kuma ƙara sannu a hankali.Dama yayin da kuke tafiya.
(5) Alamar sitaci (1%, lokacin aiki: kwanaki 30)
Za a yi awo 1.0g na sitaci mai narkewa, a zuba 10ml na ruwa, a jujjuya a zuba a cikin ruwan tafasasshen 100mL, a tafasa na minti 2, sai a tsaya, sai a dauko supernatant a yi amfani da shi.
(6) Alamar sitaci
Ɗauki 5 ml na maganin sitaci na 1% da aka shirya kuma a tsoma shi da ruwa zuwa 10 ml don samun alamar sitaci 0.5%.
(7) 30% chromium trioxide bayani (lokacin inganci: wata 1)
Auna 60g na chromium trioxide kuma narkar da shi a cikin 140ml na ruwa maras lafiya.
(8) Maganin potassium acetate (100g/L, yana aiki na watanni 2)
Narke 10 g na anhydrous potassium acetate granules a cikin 100 ml na maganin 90 ml na glacial acetic acid da 10 ml na acetic anhydride.
(9) 25% sodium acetate bayani (220g/L, lokacin inganci: watanni 2)
Narkar da 220g anhydrous sodium acetate a cikin ruwa da kuma tsarma zuwa 1000ml.
(10) Hydrochloric acid (1: 1, lokacin aiki: watanni 2)
Mix hydrochloric acid da aka tattara da ruwa a cikin rabo na 1:1.
(11) Acetate buffer (pH = 3.5, lokacin inganci: watanni 2)
Narkar da 60ml na acetic acid a cikin 500ml na ruwa, sa'an nan kuma ƙara 100ml na ammonium hydroxide da dilute zuwa 1000ml.
(12) Maganin shiri na gubar nitrate
Narkar da 159.8 MG gubar nitrate a cikin 100 ml ruwa dauke da 1 ml nitric acid (yawanci 1.42 g/cm3), tsarma zuwa 1000 ml ruwa, da kuma Mix da kyau.Da kyau gyarawa.Ya kamata a shirya maganin kuma a adana shi a cikin gilashin da ba shi da gubar.
(13) Madaidaicin jagorar jagora (lokacin inganci: watanni 2)
Daidai auna 10ml na maganin nitrate na gubar kuma ƙara ruwa don tsarma zuwa 100ml.
(14) 2% hydroxylamine hydrochloride bayani (lokacin inganci: wata 1)
Narkar da 2g na hydroxylamine hydrochloride a cikin 98mL na ruwa.
(15) Ammoniya (5mol/L, yana aiki har tsawon watanni 2)
Narkar da 175.25g ammonia ruwa da kuma tsarma zuwa 1000ml.
(16) Ruwa mai gauraya (mai inganci: watanni 2)
Mix 100ml na glycerol, 75mL na maganin NaOH (1mol/L) da 25ml na ruwa.
(17) Maganin Thioacetamide (4%, yana aiki na watanni 2)
Narke 4g na thioacetamide a cikin 96g na ruwa.
(18) Phenanthroline (0.1%, lokacin aiki: wata 1)
Narke 0.1g na phenanthroline a cikin 100ml na ruwa.
(19) chloride mai acidic (lokacin inganci: wata 1)
Narkar da 20g na chloride mai ban sha'awa a cikin 50mL na hydrochloric acid mai maida hankali.
(20) Potassium hydrogen phthalate daidaitaccen maganin buffer (pH 4.0, lokacin inganci: watanni 2)
Daidai auna 10.12g na potassium hydrogen phthalate (KHC8H4O4) kuma bushe shi a (115± 5) 2 zuwa 3 hours.Tsarma zuwa 1000 ml da ruwa.
(21) Maganin buffer daidaitaccen phosphate (pH 6.8, lokacin inganci: watanni 2)
Daidai auna 3.533g disodium anhydrous disodium hydrogen phosphate da 3.387g potassium dihydrogen phosphate bushe a (115±5) ° C na 2 ~ 3 hours, da kuma tsarma zuwa 1000ml da ruwa.
3. Ƙaddamar da abun ciki na ƙungiyar hydroxypropylmethylcellulose
(1) Ƙayyade abun ciki na methoxyl
Ƙaddamar da abun cikin ƙungiyar methoxy ya dogara ne akan gwajin da ke ɗauke da ƙungiyoyin methoxy.Hydroiodic acid yana rushewa akan dumama don samar da methyl iodide maras tabbas (tafafi 42.5°C).Methyl iodide an distilled tare da nitrogen a cikin maganin mai da kansa.Bayan wankewa don cire abubuwa masu shiga tsakani (HI, I2 da H2S), tururin methyl iodide yana shayar da shi ta hanyar maganin acetic acid na potassium acetate mai dauke da Br2 don samar da IBr, wanda aka sanya shi zuwa acid iodic.Bayan distillation, abubuwan da ke cikin mai karɓa suna canjawa wuri zuwa kwalban iodine kuma an diluted da ruwa.Bayan ƙara formic acid don cire wuce haddi Br2, KI da H2SO4 an kara.Ana iya ƙididdige abun ciki na methoxyl ta hanyar titrating 12 tare da maganin Na2S2O3.Ana iya bayyana ma'aunin amsa kamar haka.
Ana nuna na'urar auna abun ciki methoxyl a hoto na 7-6.
A cikin 7-6(a), A shine filashin zagaye na 50mL wanda aka haɗa da catheter.Akwai madaidaiciyar bututun iska mai sanyaya E a tsaye a wuyan kwalbar, tsayin kusan 25cm da diamita na ciki 9mm.Ƙarshen ƙarshen bututun yana lanƙwasa cikin bututun capillary na gilashi tare da diamita na ciki na 2 mm da mashigin yana fuskantar ƙasa.Hoto na 7-6(b) yana nuna ingantaccen na'urar.Hoto na 1 yana nuna flask ɗin amsawa, wanda shine filako mai zagaye na 50mL, tare da bututun nitrogen a hagu.2 shine bututun na'urar kwandon shara a tsaye;3 shine mai gogewa, mai dauke da ruwan wanka;4 shine bututun sha.Babban bambanci tsakanin wannan na'urar da hanyar Pharmacopoeia shi ne cewa masu sha biyu na hanyar Pharmacopoeia an haɗa su zuwa ɗaya, wanda zai iya rage asarar ruwa na ƙarshe.Bugu da kari, ruwan wankewa a cikin goge shima ya bambanta da hanyar pharmacopoeia.Yana da ruwa mai tsabta, yayin da ingantaccen na'urar shine cakuda maganin cadmium sulfate da sodium thiosulfate bayani, wanda ya fi sauƙi don shayar da ƙazanta a cikin iskar gas.
pipette kayan aiki: 5ml (5 guda), 10ml (1 yanki);Ruwa: 50ml;Iodine ƙarar kwalban: 250ml;Ma'aunin nazari.
Reagent phenol (saboda yana da ƙarfi, zai narke kafin ciyarwa);nitrogen ko carbon dioxide;hydroiodic acid (45%);darajar nazari;potassium acetate bayani (100 g / l);bromine: darajar nazari;formic acid: darajar nazari;25% Sodium acetate bayani (220g / L);KI: darajar nazari;tsarma sulfuric acid (1 + 9);sodium thiosulfate daidaitaccen bayani (0.1mol / L);phenolphthalein nuna alama;1% maganin ethanol;sitaci nuna alama: 0.5% Sitaci ruwa bayani;tsarma sulfuric acid (1 + 16.5);30% chromium trioxide bayani;Ruwan da ba shi da kwayoyin halitta: ƙara 10mL na dilute sulfuric acid (1+16.5) zuwa 100ml na ruwa, zafi zuwa tafasa, kuma ƙara 0.1ml na 0.02mol/L permanganic acid Potassium titer, tafasa don minti 10, dole ne ya kasance ruwan hoda;0.02mol/L sodium hydroxide titrant: Daidaita 0.1mol/L sodium hydroxide titrant bisa ga Hanyar Pharmacopoeia na Sinanci, kuma a tsarma daidai 0.02mol tare da tafasasshen ruwa mai sanyaya / L.
Ƙara kimanin 10mL na ruwan wankewa a cikin bututun wankewa, ƙara 31mL na sabon ruwan sha da aka shirya a cikin bututun sha, shigar da kayan aiki, auna kimanin 0.05g na busasshen samfurin da aka bushe zuwa nauyi akai-akai a 105 ° C (daidai zuwa 0.0001). g), ƙara dauki a ℃ A cikin kwalban, ƙara 5 ml na hydroiodide.Haɗa kwalaben amsa da sauri zuwa na'urar dawo da kayan aiki (danka tashar niƙa tare da acidhydriodic), sannan a zub da nitrogen cikin tanki a ƙimar kumfa 1 zuwa 2 a sakan daya.
Lokacin aikawa: Fabrairu-01-2024