1. Habka aqoonsiga ee hydroxypropyl methylcellulose
(1) Qaado 1.0g oo muunad ah, kuleyli 100ml oo biyo ah (80 ~ 90℃), si joogto ah u walaaq, oo ku qabooji qubeyska barafka ilaa ay ka noqoto dareere viscous ah; ku rid 2ml oo dareere ah tuubo tijaabo ah, oo si tartiib ah ugu dar 1mL oo ah 0.035% anthrone sulfuric acid oo weheliya xalka gidaarka tuubada oo u dhaaf 5 daqiiqo. Giraan cagaaran ayaa ka muuqda is dhexgalka u dhexeeya labada dareere.
(2) Qaado xab-xab ku habboon oo loo isticmaalo aqoonsiga gudaha (I) xagga sare oo ku shub saxanka dhalada. Marka ay biyuhu uumi baxaan, filim ductile ah ayaa sameysma.
2. Diyaarinta xalinta falanqaynta hydroxypropyl methylcellulose
(1) Sodium thiosulfate xalka caadiga ah (0.1mol/L, muddada ansaxnimada: 1 bil)
Diyaarinta: karkari ilaa 1500mL biyo nadiif ah, qabow oo meel dhig. Miisaanka 25g sodium thiosulfate (miisaanka kelli waa 248.17, isku day inaad noqoto mid sax ah oo ku saabsan 24.817g markaad miisaanayso) ama 16g anhydrous sodium thiosulfate, ku milmi 200mL ee biyaha qaboojinta ee kor ku xusan, milo 1L, ku rid dhalada brown, oo dhig meel mugdi ah ku kaydi, shaandhayso oo meel dhig laba toddobaad ka dib.
Cabbiridda: Miisaanka 0.15g ee tixraaca potassium dichromate oo dubi miisaan joogto ah, sax ah 0.0002g. Ku dar 2g potassium iodide iyo 20ml sulfuric acid (1+9), si fiican u rux, oo meel mugdi ah ku rid 10 daqiiqo. Ku dar 150mL oo biyo ah iyo 3ml 0.5% xal istaarij ah, oo titrate ku dar 0.1mol/L sodium thiosulfate. Xalku wuxuu isu beddelaa buluug ilaa buluug. Wuxuu noqdaa cagaar dhalaalaya barta ugu dambeysa. Wax chromate potassium ah laguma darin tijaabada bannaan Habka is-habaynta ayaa lagu soo celiyaa 2 ilaa 3 jeer waxaana la qaataa celceliska qiimaha.
Feejignaanta molar C (mol/L) ee sodium thiosulfate xalka caadiga ah waxaa loo xisaabiyaa iyadoo loo eegayo qaacidooyinka soo socda:
Qaaciddada, M waa tirada potassium dichromate; V1 waa mugga sodium thiosulfate la isticmaalo, mL; V2 waa mugga sodium thiosulfate lagu isticmaalo tijaabada bannaan, mL; 49.03 waa dichromium oo u dhiganta 1 mol ee sodium thiosulfate. Cuf of potassium acid, g.
Qalabaynta ka dib, ku dar qadar yar oo Na2CO3 ah si aad uga hortagto burburka microbial.
(2) NaOH heerka caadiga ah (0.1mol/L, muddada ansaxnimada: 1 bil)
Diyaarinta: Miisaan ku saabsan 4.0g oo NaOH saafi ah si aad u falanqeyso milix, ku dar 100mL oo biyo nadiif ah si ay u milaan, ka dibna ku wareeji 1L weel mug leh, ku dar biyo la nadiifiyey calaamadda, oo u daa 7-10 maalmood ilaa la hagaajinayo.
Qalabaynta: Ku rid 0.6 ~ 0.8g of potassium hydrogen phthalate saafi ah (sax ah 0.0001g) la qalajiyey at 120 ° C galay 250mL Erlenmeyer galaas, ku dar 75mL oo biyo nadiifa ah si ay u milaan, ka dibna ku dar 2 ~ 3 dhibcood 1% phenolphthalein. Titrate leh titrant. Ku walaaq xalka sodium hydroxide ee kor lagu diyaariyey ilaa uu ka yara guduudan yahay, midabkuna kuma luminayo 30 ilbiriqsi gudahooda sida barta ugu dambeysa. Qor mugga sodium hydroxide Habka is-habaynta ayaa lagu soo celiyaa 2 ilaa 3 jeer waxaana la qaataa celceliska qiimaha. Oo samee tijaabo maran.
Xalka sodium hydroxide waxaa loo xisaabiyaa sida soo socota:
Qaaciddada, C waa fiirsashada xalka sodium hydroxide, mol / L; M waxay ka dhigan tahay tirada potassium hydrogen phthalate, G; V1 - mugga sodium hydroxide la isticmaalo, mL; V2 waxay ka dhigan tahay sodium hydroxide ee lagu isticmaalo tijaabada bannaan ee mugga, mL; 204.2 waa cufka molar ee potassium hydrogen phthalate, g/mol.
(3) Kala saar sulfuric acid (1+9) (muddada ansaxnimada: 1 bil)
Markaad kareyso, si taxadar leh ugu dar 100 mL oo ah sulfuric acid 900 ml oo biyo ah si tartiib ah ugu dar intaad kareyso.
(4) Ku qas sulfuric acid (1+16.5) (muddada ansaxnimada: 2 bilood)
Markaad walaaqayso, si taxadar leh ugu dar 100 ml oo ah sulfuric acid 1650 ml oo biyo ah oo si tartiib ah ugu dar. Walaaq markaad socoto.
(5) Tilmaamaha istaarijka (1%, muddada ansaxnimada: 30 maalmood)
Miisaanka 1.0g oo istaarij milmaya, ku dar 10mL oo biyo ah, walaaq oo ku shub 100ml oo biyo ah karkaraya, isku kari ilaa 2 daqiiqo, istaag, ka dibna qaado subaga si aad hadhow u isticmaasho.
(6) Tilmaamaha istaarijka
Qaado 5 ml oo ah xalka 1% istaarijka la diyaariyey oo ku mil biyo ilaa 10 mL si aad u hesho 0.5% istaarijka tusaha.
(7) 30% chromium trioxide xal (muddada ansaxnimada: 1 bil)
Miisaanka 60g ee chromium trioxide oo ku mil 140ml oo biyo ah oo aan dabiici ahayn.
(8) Xalka Potassium acetate (100g/L, shaqaynaya 2 bilood)
Ku mil 10 g oo ah granul potassium acetate anhydrous ah 100 ml oo xal ah 90 ml oo ah glacial acetic acid iyo 10 mL oo ah acetic anhydride.
(9) 25% xal sodium acetate (220g/L, muddada ansaxnimada: 2 bilood)
Ku milmi 220g anhydrous sodium acetate biyo ku milmi ilaa 1000ml.
(10) Hydrochloric acid (1:1, muddada ansaxnimada: 2 bilood)
Isku qas aashitada hydrochloric iyo biyaha ee saamiga mugga 1:1.
(11) Acetate buffer (pH=3.5, muddada ansaxnimada: 2 bilood)
Ku mil 60ml oo acetic acid ah 500ml oo biyo ah,kadib ku dar 100ml ammonium hydroxide oo ku milo 1000ml.
(12) Xalka diyaarinta Nitrate-ka rasaasta
Ku milmi 159.8 mg nitrate sunta rasaasta ah 100 ml oo biyo ah oo ka kooban 1 mL nitric acid (cufnaanta 1.42 g/cm3), ku milo 1000 ml oo biyo ah, oo si fiican isku qas. Si fiican ayaa loo hagaajiyay. Xalka waa in la diyaariyaa oo lagu kaydiyaa galaas aan macdanta rasaasta lahayn.
(13) Xalka heerka ledhka (muddada ansaxnimada: 2 bilood)
Si sax ah u cabbir 10ml ee nitrate-ka diyaarinta rasaasta oo ku dar biyo si aad u milmaan 100ml.
(14) 2% hydroxylamine hydrochloride xal (muddada ansaxnimada: 1 bil)
Ku mil 2g oo ah hydroxylamine hydrochloride 98mL oo biyo ah.
(15) Ammonia (5mol/L, shaqaynaysa 2 bilood)
Kala dir 175.25g oo biyo ah ammonia oo ku milo 1000ml.
(16) dareere isku dhafan ( ansax ah: 2 bilood)
Isku qas 100ml oo glycerol ah, 75ml oo xal NaOH ah (1mol/L) iyo 25ml oo biyo ah.
(17) Xalka Thioacetamide (4%, shaqaynaya 2 bilood)
Ku mil 4g of thioacetamide 96g oo biyo ah.
(18) Phenanthroline (0.1%, muddada ansaxnimada: 1 bil)
Ku mil 0.1g oo phenanthroline ah 100ml oo biyo ah.
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Ku mil 20g oo koloriin aad u sarreeya 50ml oo ah hydrochloric acid.
(20) Potassium hydrogen phthalate xalka caadiga ah (pH 4.0, muddada ansaxnimada: 2 bilood)
Si sax ah ugu miisaan 10.12g oo ah potassium hydrogen phthalate (KHC8H4O4) oo ku qalaji (115±5)℃ 2 ilaa 3 saacadood. Ku qas 1000ml oo biyo ah.
(21) Xalka kaydinta heerka fosfate (pH 6.8, muddada ansaxnimada: 2 bilood)
Si sax ah u miisaan 3.533g disodium hydrogen phosphate anhydrous ah iyo 3.387g potassium dihydrogen phosphate la qalajiyey (115 ± 5) ° C 2 ~ 3 saacadood, oo lagu milo ilaa 1000mL biyo.
3. Go'aaminta nuxurka kooxda hydroxypropylmethylcellulose
(1) Go'aaminta maadada methoxyl
Go'aaminta waxa ku jira kooxda methoxy waxay ku salaysan tahay tijaabada ka kooban kooxaha methoxy. Aashitada Hydroiodic waxay burburisaa kuleylka si ay u soo saarto methyl iodide oo kacsan (dhibcaha karkarinta 42.5°C). Methyl iodide waxaa lagu miiray nitrogen ee xalka is-xakamaynta. Ka dib marka la dhaqo si looga saaro walxaha soo dhexgalaya (HI, I2 iyo H2S), uumiga methyl iodide waxaa nuugaya xalka acetic acid ee potassium acetate oo ka kooban Br2 si ay u sameeyaan IBr, kaas oo ka dibna oksidized si iodic acid. Distillation ka dib, waxa ku jira receptor waxaa loo wareejiyaa dhalo iodine ah oo lagu qasi jiray biyo. Ka dib marka lagu daro formic acid si looga saaro xad-dhaafka Br2, KI iyo H2SO4 ayaa lagu daraa. Waxa ku jira methoxyl waxaa lagu xisaabin karaa titrating 12 oo leh xalka Na2S2O3. Isla'egta falcelinta waxaa loo sheegi karaa sidan soo socota.
Qalabka cabbiraadda maadada methoxyl waxa lagu muujiyay sawirka 7-6.
7-6(a), A waa 50mL weel salka hoose ah oo ku xidhan tuubada. Waxa jira tuubo hawo qaboojin oo toosan E oo si toosan loogu rakibay dhuunta dhalada, dhererkeeduna yahay 25cm iyo dhexroorka gudaha 9mm. Cidhifka sare ee tuubada waxa lagu rogmanayaa tuubo koofiyad dhalada ah oo dhexroorkeedu yahay 2 mm iyo meel hoos u sii jeedda. Jaantuska 7-6(b) waxa uu muujinayaa qalabka la hagaajiyay. Jaantuska 1 waxa uu tusinayaa weelka falcelinta, kaas oo ah 50mL caarad hoose oo wareegsan, oo bidix ku leh tuubo nitrogen ah. 2 waa tuubada kondenser-ka tooska ah; 3 waa xoqida, oo ay ku jiraan dareeraha wax lagu dhaqo; 4 waa tuubada nuugista. Farqiga ugu weyn ee u dhexeeya qalabkan iyo habka Pharmacopoeia waa in labada nuuga ee habka Pharmacopoeia la isku daro, taas oo yareyn karta luminta dareeraha nuugista ugu dambeeya. Intaa waxaa dheer, dareeraha wax lagu dhaqo ee xoqida ayaa sidoo kale ka duwan habka farmashiyaha. Waa biyo nadiif ah, halka qalabka la hagaajiyay uu yahay isku-dhafka cadmium sulfate iyo xal sodium thiosulfate, kaas oo si sahlan u nuugaya wasakhda gaaska la miiray.
pipette qalabka: 5ml (5 xabo), 10ml (1 gabal); Burette: 50ml; Dhalada mugga iodine: 250ml; Isku dheelitirnaanta falanqaynta.
Reagent phenol (maxaa yeelay waa mid adag, way dhalaali doontaa ka hor quudinta); carbon dioxide ama nitrogen; hydroiodic acid (45%); darajada gorfaynta; xalalka potassium acetate (100 g / l); bromine: fasalka falanqaynta; formic acid: fasalka falanqaynta; 25% Sodium acetate xal (220g/L); KI: darajada falanqaynta; milo sulfuric acid (1+9); sodium thiosulfate xal caadi ah (0.1mol / L); tilmaame phenolphthalein; 1% ethanol xal; Tilmaamaha istaarijka: 0.5% Xalka aqueous istaarijka; milo sulfuric acid (1+16.5); 30% chromium trioxide xal; Biyo aan dabiici ahayn: ku dar 10ml oo sulfuric acid ah (1+16.5) ilaa 100mL oo biyo ah, kulayl karkarinta, kuna dar 0.1ml oo ah 0.02mol/L permanganic acid titer Potassium, karkari 10 daqiiqo, waa in ay ahaataa casaan; 0.02mol/L sodium hydroxide titrant: Ku qiyaas titrant 0.1mol/L sodium hydroxide sida waafaqsan habka Shiinaha ee Pharmacopoeia Appendix, oo si sax ah ugu milo 0.02mol biyo la karkariyey oo la qaboojiyey/L.
Ku dar qiyaastii 10mL oo dareere dhaqid ah tuubada dhaqida, ku dar 31mL oo dareere nuugista cusub ah oo la diyaariyey gudaha tuubada nuugista, ku rakib qalabka, miisaan qiyaastii 0.05g muunada la qalajiyey ee la qalajiyey ilaa miisaan joogto ah 105°C (sax ah 0.0001) g), ku dar falcelinta ℃ Dhalada dhexdeeda, ku dar 5 mL oo ah hydroidide. Si degdeg ah ugu xidh dhalada falcelinta iyo kondhiyaha soo kabashada (ku qoyso dekedda wax lagu shiidi karo acidhydriodic), oo ku shub nitrogen taangiga heerka 1 ilaa 2 xumbo ilbiriqsikii.
Waqtiga boostada: Febraayo-01-2024