1, gano hanyar hydroxypropyl methyl cellulose
(1) Ɗauki 1.0g na samfurin, ruwa mai zafi (80 ~ 90 ℃) 100mL, motsawa akai-akai, kuma sanyaya cikin ruwa mai danko a cikin wanka na kankara; Saka 2mL na ruwa a cikin bututun gwaji, a hankali ƙara 1mL sulfuric acid bayani na 0.035% anthrone tare da bangon bututu, sa'annan ku bar minti 5. Koren zobe yana bayyana a mahaɗin tsakanin ruwaye biyu.
(2) Ɗauki daidai adadin da aka ambata a sama wanda aka yi amfani da shi wajen tantance (ⅰ) a zuba a kan farantin gilashin. Bayan ruwan ya ƙafe, an kafa fim ɗin ductile.
2, hydroxypropyl methyl cellulose bincike na daidaitattun shirye-shiryen bayani
(1) Sodium thiosulfate misali bayani (0.1mol/L, inganci: wata daya)
Shiri: tafasa game da 1500mL distilled ruwa da sanyi har sai an shirya don amfani. Auna nauyin 25g sodium thiosulfate (nauyin kwayoyinsa 248.17, kuma kuyi ƙoƙarin zama daidai zuwa kimanin 24.817g lokacin yin awo) ko 16g sodium thiosulfate anhydrous, narke shi a cikin 200mL na ruwan sanyi na sama, tsarma shi zuwa 1L, sa'annan a sanya shi a cikin launin ruwan kasa. kwalaba, sanya kwalbar a cikin duhu, sannan a tace ta don amfani bayan makonni biyu.
Calibration: Auna 0.15g na tunani potassium dichromate gasa zuwa kullum nauyi, daidai zuwa 0.0002g. Ƙara 2g potassium iodide da 20mL sulfuric acid (1+9), girgiza da kyau, sanya a cikin duhu don 10min, ƙara 150ml ruwa da 3ml 0.5% sitaci bayani bayani, titrate tare da 0.1mol/L sodium thiosulfate bayani, maganin ya juya daga blue. zuwa haske kore a ƙarshen batu. Potassium chromate ba a saka shi cikin gwaji mara kyau ba. An maimaita tsarin daidaitawa sau 2 ~ 3 kuma an ɗauki matsakaicin ƙimar.
An ƙididdige ma'auni na molar C (mol / L) na daidaitaccen bayani na sodium thiosulfate kamar haka:
Inda, 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 adadin potassium dichromate daidai da 1mol na sodium thiosulfate, g.
Bayan daidaitawa, ƙara ɗan Na2CO3 don hana bazuwar ƙwayoyin cuta.
(2) NaOH daidaitaccen bayani (0.1mol/L, inganci: wata ɗaya)
Shiri: Kimanin 4.0g na NaOH mai tsabta don bincike an auna shi a cikin beaker, kuma an zuba ruwa mai laushi 100mL don narke, sa'an nan kuma a tura shi zuwa kwalban 1L mai girma, kuma an zuba ruwa mai tsabta a cikin ma'auni, kuma an sanya shi don kwanaki 7-10 har sai daidaitawa.
Calibration: Saka 0.6 ~ 0.8g na pure potassium hydrogen phthalate dried a 120 ℃ (daidai zuwa 0.0001g) a cikin wani 250mL conical flask, ƙara 75mL distilled ruwa don narkar da shi, sa'an nan ƙara 2 ~ 3 saukad da 1% phenolphthalein tare da nuna alama, tit. Maganin sodium hydroxide da aka shirya a sama har sai ya ɗan ja, kuma ƙarshen ƙarshen shine cewa launi ba ya shuɗe a cikin 30S. Rubuta ƙarar sodium hydroxide. An maimaita tsarin daidaitawa sau 2 ~ 3 kuma an ɗauki matsakaicin ƙimar. Kuma ku yi gwaji mara kyau.
An ƙididdige ƙaddamarwar maganin sodium hydroxide kamar haka:
Inda, C shine ƙaddamar da maganin sodium hydroxide, mol / L; M yana wakiltar adadin potassium hydrogen phthalate, G; V1 shine ƙarar sodium hydroxide cinyewa, mL; V2 yana wakiltar ƙarar sodium hydroxide da aka cinye a cikin gwaji mara kyau, mL; 204.2 shine ma'aunin ƙwanƙwasa na potassium hydrogen phthalate, g kowace tawadar Allah.
(3) Narke sulfuric acid (1+9) (Ingantacciyar: wata 1)
Karkashin motsawa, a hankali ƙara 100mL sulfuric acid mai hankali zuwa ruwa mai narkewa 900mL, ƙara sannu a hankali, yayin motsawa.
(4) Narke sulfuric acid (1+16.5) (Ingantacciyar: watanni 2)
Karkashin motsawa, a hankali ƙara 100ml na sulfuric acid mai mahimmanci zuwa 1650ml na ruwa mai narkewa, ƙara sannu a hankali. Dama yayin da kuke tafiya.
(5) Alamar sitaci (1%, inganci: kwanaki 30)
Za a yi awo 1.0g mai soluble, a zuba ruwa 10mL, a jujjuya a zuba a cikin ruwan tafasasshen ruwa 100mL, a tafasa kadan na 2min, sai a sanya shi, sannan a dauki supernatant don amfani.
(6) Alamar sitaci
0.5% sitaci nuna alama aka samu ta hanyar shan 5mL na shirya 1% sitaci bayani bayani da kuma diluting shi zuwa 10mL da ruwa.
(7) 30% chromium trioxide bayani (inganci: wata 1)
Auna 60g na chromium trioxide kuma a narkar da shi a cikin 140ml na ruwa ba tare da kwayoyin halitta ba.
(8) Maganin acetate na potassium (100g/L, inganci: watanni 2)
10g na anhydrous potassium acetate hatsi an narkar da a cikin wani 100ml bayani na 90ml glacial acetic acid da 10ml acetic anhydride.
(9) 25% sodium acetate bayani (220g/L, inganci: watanni 2)
Narkar da 220g na anhydrous sodium acetate a cikin ruwa da kuma tsarma zuwa 1000ml.
(10) Hydrochloric acid (1:1, inganci: watanni 2)
Mix hydrochloric acid da aka tattara tare da ruwa a rabo na 1: 1.
(11) Maganin buffer acetate (pH = 3.5, inganci: watanni 2)
Narkar da 60ml acetic acid a cikin ruwa 500ml, sa'an nan kuma ƙara 100ml ammonium hydroxide da dilute zuwa 1000ml.
(12) Maganin shiri na gubar nitrate
An narkar da 159.8mg na nitrate gubar a cikin ruwa 100mL mai dauke da 1mL na nitric acid (yawan 1.42g/cm3), an diluted zuwa 1000mL na ruwa kuma an gauraya da kyau. Shirye-shiryen da adana wannan bayani za a yi a cikin gilashin da ba shi da gubar.
(13) Daidaitaccen maganin gubar (ingantattun: watanni 2)
Daidaitaccen ma'auni na 10ml na maganin shirye-shiryen nitrate na gubar an diluted da ruwa 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, inganci: watanni 2)
An narkar da 175.25g na ammonia a cikin ruwa kuma an diluted zuwa 1000ml.
(16) Ruwa mai gauraya (lokacin inganci: watanni 2)
Mix 100ml glycerol, 75mLNaOH bayani (1mol/L), da ruwa 25mL.
(17) Maganin Thioacetamide (4%, inganci: watanni 2)
An narkar da 4g thioacetamide a cikin ruwa 96g.
(18) Phenanthroline (0.1%, inganci: wata 1)
Narke 0.1g o-phenanthroline a cikin ruwa 100ml.
(19) Acid chloride stannous (daidaituwa: wata 1)
Narkar da 20g stannous chloride a cikin 50mL maida hankali hydrochloric acid.
(20) Potassium hydrogen phthalate daidaitaccen maganin buffer (pH 4.0, inganci: watanni 2)
10.12g na potassium hydrogen phthalate (KHC8H4O4) an auna daidai kuma a bushe a (115±5) ℃ na 2 ~ 3h. Tsarma zuwa 1000 ml da ruwa.
(21) Maganin buffer daidaitaccen phosphate (pH 6.8, inganci: watanni 2)
3.533g na anhydrous disodium hydrogen phosphate da 3.387g na potassium dihydrogen phosphate dried a (115±5) ℃ for 2 ~ 3h aka daidai auna da diluted zuwa 1000ml da ruwa.
3, hydroxypropyl methyl cellulose ƙungiyar ƙaddara abun ciki
(1) Ƙayyade abun ciki na methoxy
Ƙaddamar da abun ciki na methoxy ya dogara ne akan bazuwar acid hydroiodate ta hanyar dumama tare da gwajin da ke ɗauke da methoxy don samar da methane iodide maras tabbas (madaidaicin tafasa 42.5 ° C). Methane iodide yana distilled tare da nitrogen a cikin maganin autoreaction. Bayan wankewa don cire abubuwa masu shiga tsakani (HI, I2 da H2S), tururin methane na iodine yana shafe ta hanyar potassium acetate acetic acid bayani mai dauke da Br2 don samar da IBr sannan kuma ya zama oxidized zuwa iodic acid. Bayan distillation, abubuwan da ke cikin mai karɓa suna canjawa wuri zuwa kwalabe na 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 methoxy ta titrating 12 tare da bayani na Na2S2O3. Ana iya bayyana ma'aunin amsa kamar haka.
Ana nuna na'urar don auna abun ciki methoxy a cikin hoto 7-6.
A cikin 7-6 (a), A shine faifan zagaye-kasa na 50ml wanda aka haɗa da catheter. Kwancen kwalbar yana tsaye a tsaye tare da madaidaiciyar bututun kwantar da iska mai kusan 25cm a tsayi da 9mm a diamita na ciki. Ƙarshen ƙarshen bututun yana lanƙwasa a cikin bututun capillary na gilashi tare da fitarwa zuwa ƙasa da 2mm a diamita na ciki. Hoto na 7-6 (b) yana nuna ingantaccen na'urar. 1 shine flask ɗin amsawa, wanda shine 50mL flask zagaye-kasa, kuma bututun nitrogen yana gefen hagu. 2 shi ne bututu mai ɗaukar nauyi a tsaye; 3 shine mai gogewa, mai dauke da ruwan wanka; 4 shine bututun sha. Babban bambanci tsakanin na'urar da hanyar pharmacopoeia shine cewa ana haɗa nau'i biyu na hanyar pharmacopoeia zuwa ɗaya, wanda zai iya rage asarar mafita ta ƙarshe. Bugu da kari, ruwan wankan da ke cikin goge shi ma ya sha bamban da hanyar pharmacopoeia, wanda aka gurbata ruwa, kuma ingantacciyar na’urar ita ce cakudewar maganin cadmium sulfate da maganin sodium thiosulfate, wanda zai iya fi dacewa da lalata dattin da ke cikin distilled gas.
Kayan aiki pipette: 5ml (5), 10ml (1); Ruwa: 50ml; Iodine gwangwani kwalban: 250ml; Yi nazarin ma'auni.
Reagent phenol (saboda yana da ƙarfi, don haka za a haɗa shi kafin ciyarwa); nitrogen ko carbon dioxide; Hydroiodate acid (45%); Binciken tsarki; Potassium acetate bayani (100g / L); Bromine: tsantsar nazari; Formic acid: analytically tsarki; 25% sodium acetate bayani (220g / L); KI: tsarkin nazari; Tsarma sulfuric acid (1 + 9); Sodium thiosulfate daidaitaccen bayani (0.1mol / L); Phenolphthalein nuna alama; 1% maganin ethanol; Alamar sitaci: 0.5% sitaci a cikin ruwa; Tsarma sulfuric acid (1 + 16.5); 30% chromium trioxide bayani; Ruwa mara kyau: ƙara 10mL dilute sulfuric acid (1+16.5) zuwa ruwa 100mL, zafi zuwa tafasa, kuma ƙara 0.1ml0.02mol /L potassium permanganate titer, tafasa don 10min, dole ne a kiyaye ruwan hoda; 0.02mol/L sodium hydroxide titration bayani: A cewar hanyar Pharmacopoeia appendix na kasar Sin, 0.1mol/L sodium hydroxide titration bayani an calibrated da daidai diluted zuwa 0.02mol/L tare da tafasasshen ruwa da kuma sanyaya distilled ruwa.
Ƙara kimanin 10mL na maganin wankewa a cikin bututun wankewa, ƙara 31mL na sabon maganin sha a cikin bututun sha, shigar da kayan aiki, auna kimanin 0.05g (daidai zuwa 0.0001g) na busassun samfurin da aka bushe don nauyin nauyi a 105. ℃ a cikin flask dauki, kuma ƙara 5mL hydroiodate. Ana haɗa kwalban amsawa da sauri zuwa na'urar na'urar dawowa (baki mai niƙa yana da ruwa da hydroiodate), kuma ana zubar da nitrogen a cikin tanki a ƙimar kumfa 1 ~ 2 a sakan daya. Ana sarrafa zafin jiki a hankali don tururi na tafasar ruwa ya tashi zuwa rabin tsayin na'urar. Lokacin amsawa ya dogara da yanayin samfurin, tsakanin 45min da 3h. Cire bututun abin sha kuma a hankali canja wurin maganin abin sha a cikin gilashin iodine na 500mL mai dauke da 10ml na 25% sodium acetate bayani har sai jimlar girma ya kai kimanin 125mL.
Ƙarƙashin girgiza akai-akai, a hankali ƙara digon formic acid ta digo har sai launin rawaya ya ɓace. Ƙara digo na 0.1% methyl ja mai nuna alama, kuma launin ja baya ɓacewa na mintuna 5. Sannan a zuba digo uku na formic acid. Bari ya zauna na ɗan lokaci, sannan a ƙara 1 g na potassium iodide da 5 ml na sulfuric acid (1+9). An ƙaddamar da maganin tare da 0.1mol / L sodium thiosulfate daidaitaccen bayani, kuma an ƙara 3 ~ 4 saukad da 0.5% alamar sitaci kusa da ƙarshen ƙarshen, kuma an ci gaba da titration har sai launin shudi ya ɓace.
A cikin irin wannan yanayi, an yi gwaji mara kyau.
Lissafin jimlar abun ciki methoxide:
Inda, V1 yana wakiltar ƙarar (mL) na daidaitaccen maganin sodium thiosulfate wanda aka cinye ta samfuran titration; V2 shine ƙarar sodium thiosulfate daidaitaccen bayani wanda aka cinye a cikin gwaji mara kyau, mL; C shine maida hankali na sodium thiosulfate daidaitaccen bayani, mol / L; M yana nufin adadin busasshen samfurin, g; 0.00517 shine 0.1mol/L sodium thiosulfate a kowace 1ml daidai da 0.00517g na methoxy.
Jimlar abun ciki na methoxy yana wakiltar jimillar methoxy da ƙimar hydroxyproxy na lissafin methoxy, don haka jimlar alkoxy dole ne a gyara ta hanyar abin da ke haifar da hydroxyproxy don samun ainihin abun cikin methoxy. YA KAMATA A FARKO A GYARA ABUBUWAN HYDROXYPROPOXY DOMIN KYAUTA TA HANYAR RASHIN HIDROXYPROPYL TARE DA DOMIN K=0.93 (MA'ANAR MANYAN LAMBA NA SAMUN SAMUN SAMUN SAUKI). Saboda haka:
Ingantattun abun ciki na methoxy = jimlar abun ciki na methoxy - (abincin hydroxypropoxy ×0.93×31/75)
Inda lambobi 31 da 75 su ne molar talakawan methoxy da hydroxypropoxy, bi da bi.
(2) Ƙaddamar da abun ciki na hydroxypropoxy
Ƙungiyar hydropropoxy a cikin samfurin tana amsawa tare da chromium trioxide don samar da acetic acid. Bayan an cire shi daga maganin autoreaction, abun ciki na chromic acid ana ƙaddara ta titration tare da maganin NaOH. Domin za a fitar da ɗan ƙaramin chromic acid a cikin tsarin distillation, kuma za a sha maganin NaOH, don haka abin da ke cikin wannan chromic acid ya kamata a ƙara ƙaddara ta hanyar iodimetry kuma a cire shi daga lissafin. Ma'aunin martani shine:
Instruments da reagents Cikakken saitin kayan aikin don tantance ƙungiyoyin hydroxypropoxy; kwalban ƙarami: 1L, 500ml; Silinda mai aunawa: 50ml; Pipette: 10ml; Iodine gwangwani kwalban: 250ml. Tushen asali: 10ml; Sodium thiosulfate daidaitaccen bayani (0.1mol / L); Tsarma sulfuric acid (1 + 16.5); Tsarma sulfuric acid (1 + 9); Alamar sitaci (0.5%).
7-7 na'ura ce don tantance abun ciki na hydroxypropoxy.
A 7-7 (a), D ne 25mL biyu-wuyan distilling flask, B ne 25mm × 150mm tururi janareta tube, C ne kwarara dangane tube, A ne lantarki dumama mai wanka, E ne shunt shafi, G flask ne na conical tare da filogi na gilashi, ƙarshen ciki diamita shine 0.25-1.25mm, an saka shi a cikin filashin distilling; F bututu ne mai haɗawa da E. A cikin ingantaccen na'urar da aka nuna a FIG. 7-7 (b), 1 shine reactor, wanda shine gilashin distillation na 50ml; 2 shine shugaban distillation; 3 shine mazugi na gilashin 50mL don sarrafa saurin kwararar ruwa; 4 shine bututun nitrogen; 5 shi ne bututun da ke ɗaukar nauyi. Bambanci mafi mahimmanci tsakanin na'urar da aka gyara da hanyar pharmacopoeia shine ƙari na mazugi na gilashi don sarrafa adadin ruwa, ta yadda za'a iya sarrafa adadin distillation cikin sauƙi.
Hanyoyin gwaji a cikin samfurin 105 ℃ bushewa zuwa nauyin nauyi shine game da 0.1 g (0.0002 g), daidai ya ce a cikin kwalban distillation, ƙara 10 ml na 30% chromium trioxide bayani, da distillation flask a cikin man wanka kofin, mai wanka ruwa matakin. daidai da chromium trioxide ruwa surface, shigar kayan aiki, bude sanyaya ruwa, nitrogen, mu masana'anta don sarrafa kudi na nitrogen game da kumfa daya a sakan daya. A cikin minti 30, an yi zafi da wanka mai mai zuwa 155 ℃ kuma ana kiyaye shi a wannan zafin jiki har sai maganin da aka tattara ya kai 50mL. An dakatar da distillation don cire bahon mai.
A wanke bangon ciki na mai sanyaya tare da ruwa mai narkewa, hada ruwan wanka da distillate a cikin kwalban iodine na 500mL, ƙara 2 saukad da na 1% phenolphthalide nuna alama, titrate tare da 0.02mol / L sodium hydroxide bayani zuwa pH darajar 6.9 ~ 7.1. , kuma rubuta jimlar adadin sodium hydroxide da aka cinye.
Ƙara 0.5g sodium bicarbonate da 10mL dilute sulfuric acid (1+16.5) a cikin kwalban aidin kuma bar shi ya tsaya har sai an samar da carbon dioxide. Sannan a zuba 1.0g na potassium iodide, a toshe shi sosai, a girgiza shi da kyau a bar shi a cikin duhu na 5min. Sa'an nan ƙara 1ml 0.5% sitaci nuna alama kuma titrate shi da 0.02mol/L sodium thiosulfate zuwa karshen batu. Rubuta adadin sodium thiosulfate da aka cinye.
A wani gwajin mara komai, an yi rikodin ƙarar lambobi na sodium hydroxide da sodium thiosulfate titrator da aka cinye.
Lissafin abun ciki na hydroxypropoxy:
Inda, K shine hoto mai daidaitawa na gwaji mara kyau: V1 shine ƙarar titration sodium hydroxide wanda samfurin ya cinye, mL. C1 shine ƙaddamar da daidaitaccen bayani na sodium hydroxide, mol / L; V2 shine ƙarar sodium thiosulfate titration wanda samfurin ya cinye, mL; C2 shine maida hankali na sodium thiosulfate daidaitaccen bayani, mol / L; M shine yawan samfurin, g; Va shine ƙarar titration sodium hydroxide da ake cinyewa a cikin gwaji mara kyau, mL; Vb shine ƙarar sodium thiosulfate titration da ake cinyewa a cikin gwaji mara kyau, mL.
4. Ƙaddamar da danshi
Ma'aunin nazari na kayan aiki (daidai zuwa 0.1mg); kwalban aunawa: diamita 60mm, tsayi 30mm; Bushewar tanda.
Hanyar gwajin daidai tana auna samfurin 2 ~ 4G (
Lokacin aikawa: Satumba-08-2022