1, aqoonsiga habka hydroxypropyl methyl cellulose
(1) Qaado 1.0g oo muunad ah, biyo kulul (80 ~ 90 ℃) 100ml, walaaq si joogto ah, oo ku qabooji dareeraha viscous ee qubeyska barafka; Ku rid 2ml oo dareere ah tuubada tijaabada, si tartiib ah ugu dar 1mL sulfuric acid xal 0.035% anthrone ah oo weheliya gidaarka tuubada, oo ku dhaaf 5min. Giraaniga cagaarka ah wuxuu ka muuqdaa is dhexgalka u dhexeeya labada dareere.
(2) Qaado xadiga ku habboon ee dhoobada kor lagu soo sheegay ee loo isticmaalay aqoonsiga (ⅰ) oo ku shub saxanka dhalada. Ka dib markii biyuhu uumibaxa, filim ductile ah ayaa la sameeyaa.
2, falanqaynta hydroxypropyl methyl cellulose ee diyaarinta xalka caadiga ah
(1) Sodium thiosulfate xal caadi ah (0.1mol/L, ansax ah: hal bil)
Diyaarinta: Karkari ilaa 1500mL oo biyo nadiif ah oo qabow ilaa inta aad diyaar u tahay in la isticmaalo. Miisaanka 25g sodium thiosulfate (miisaanka kelli waa 248.17, iskuna day inaad sax ahaato qiyaastii 24.817g markaad miisaanayso) ama 16g anhydrous sodium thiosulfate, ku milmi 200mL ee biyaha qaboojinta ee sare, ku qas 1L, oo ku rid brown dhalada, dhalada geli gudcurka, oo sifdi isticmaal laba toddobaad ka dib.
Cabbiridda: Miisaanka 0.15g ee tixraaca potassium dichromate lagu dubay miisaan joogto ah, sax ah 0.0002g. Ku dar 2g potassium iodide iyo 20mL sulfuric acid (1+9), si fiican u rux, ku rid mugdiga 10min, ku dar 150ml biyo ah iyo 3ml 0.5% xal istaarij ah, titrate leh 0.1mol/L sodium thiosulfate, xalku wuxuu ka soo noqdaa buluug cagaar dhalaalaya barta dhamaadka. Potassium chromate laguma darin tijaabada bannaan. Habka is-habaynta ayaa lagu soo celiyay 2 ~ 3 jeer waxaana la qaatay celceliska qiimaha.
Feejignaanta molar C (mol/L) ee sodium thiosulfate xalka caadiga ah ayaa loo xisaabiyay sida soo socota:
Halka, M ay tahay tirada potassium dichromate; V1 waa mugga sodium thiosulfate la isticmaalo, mL; V2 waa mugga sodium thiosulfate ee lagu isticmaalo tijaabada maran, mL; 49.03 waa cufnaanta potassium dichromate oo u dhiganta 1mol of sodium thiosulfate, g.
Qalabaynta ka dib, ku dar wax yar Na2CO3 si aad uga hortagto burburka microbial.
(2) NaOH xalalka caadiga ah (0.1mol/L, ansax ah: hal bil)
Diyaarinta: Qiyaastii 4.0g oo NaOH saafi ah ayaa lagu miisaamay digsi, iyo 100mL biyo nadiif ah ayaa lagu daray si ay u milmaan, ka dibna loo wareejiyo 1L weel mug leh, iyo biyo nadiif ah ayaa lagu daray miisaanka, oo la dhigay 7-10 maalmood ilaa qiyaasid.
Cabbiridda: Ku rid 0.6 ~ 0.8g oo ah potassium hydrogen phthalate saafi ah oo la qalajiyey at 120 ℃ (sax ah ilaa 0.0001g) 250mL weel kooneedka ah, ku dar 75mL biyo nadiif ah si ay u milaan, ka dibna ku dar 2 ~ 3 dhibcood 1% phenolphthalein leh tilmaame, tit. xalalka sodium hydroxide ee kor ku xusan ee la diyaariyey ilaa uu ka yara guduudan yahay, iyo dhammaadka barta waa in midabku uusan ku lumin 30S gudahood. Qor mugga sodium hydroxide Habka is-habaynta ayaa lagu soo celiyay 2 ~ 3 jeer waxaana la qaatay celceliska qiimaha. Oo samee tijaabo maran.
Xalka sodium hydroxide waxaa loo xisaabiyay sida soo socota:
Halkee, C waa fiirsashada xalka sodium hydroxide, mol/L; M waxay ka dhigan tahay tirada potassium hydrogen phthalate, G; V1 waa mugga sodium hydroxide la isticmaalo, mL; V2 waxay ka dhigan tahay mugga sodium hydroxide ee lagu isticmaalo tijaabada bannaan, mL; 204.2 waa cufka molar ee potassium hydrogen phthalate, g halkii mole.
(3) Ku qas aashitada sulfuric (1+9) (Ansax: 1 bil)
Marka la walaaqayo, si taxadar leh ugu dar 100mL sulfuric acid 900mL oo biyo ah, kuna dar si tartiib ah, adigoo walaaqaya.
(4) Kala saar sulfuric acid (1+16.5) (Ansax: 2 bilood)
Marka la walaaqayo, si taxadar leh ugu dar 100mL oo ah sulfuric acid 1650mL oo biyo nadiif ah, si tartiib ah ugu dar. Walaaq markaad socoto.
(5) Tilmaamaha istaarijka (1%, ansax ah: 30 maalmood)
Miisaanka 1.0g istaarijka milmaya, ku dar 10mL biyo, walaaq oo ku dur 100mL biyo karkaraya, wax yar karkari 2min, dhig, ka dibna qaado subaga si aad u isticmaasho.
(6) Tilmaamaha istaarijka
Tilmaamaha istaarijka 0.5% waxaa lagu helay iyadoo la qaatay 5mL oo la diyaariyey 1% istaarijka tusaha oo lagu qaso 10mL biyo.
(7) 30% chromium trioxide xal ( ansax ah: 1 bil)
Miisaanka 60g ee chromium trioxide oo ku mil 140ml oo biyo ah iyada oo aan lahayn walxo dabiici ah.
(8) Xalka Potassium acetate (100g/L, ansax ah: 2 bilood)
10g oo ah badarka potassium acetate anhydrous ayaa lagu milmay 100ml xal 90mL glacial acetic acid iyo 10ml acetic anhydride.
(9) 25% xal sodium acetate (220g/L, ansax ah: 2 bilood)
Ku mil 220g oo sodium acetate anhydrous ah oo biyo ah kuna qas 1000ml.
(10) Hydrochloric acid (1:1, ansax ah: 2 bilood)
Ku qas aashitada hydrochloric ee biyaha leh 1:1 saamiga.
(11) Xalka Acetate (pH=3.5, ansax: 2 bilood)
Ku milmi 60ml acetic acid 500ml oo biyo ah,kadib ku dar 100ml ammonium hydroxide oo ku milo 1000ml.
(12) Xalka diyaarinta Nitrate-ka rasaasta
159.8mg ee nitrate-ka rasaasta ayaa lagu milmay 100ml biyo ah oo ka kooban 1mL oo nitric acid ah (cufnaanta 1.42g/cm3), lagu qasi jiray 1000mL oo biyo ah si fiicanna loo qasay. Diyaarinta iyo kaydinta xalkan waa in lagu fuliyaa muraayadda aan rasaasta lahayn.
(13) Xalka rasaasta caadiga ah ( ansax ah: 2 bilood)
Cabbir sax ah oo ah 10ml ee nitrate-ka diyaarinta rasaasta rasaasta ayaa lagu qasi jiray biyo ilaa 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, ansax ah: 2 bilood)
175.25g oo ammonia ah ayaa lagu milmay biyo waxaana lagu qasi jiray 1000ml.
(16) dareere isku dhafan (muddada ansaxnimada: 2 bilood)
Isku qas 100ml glycerol, 75mLNaOH xal (1mol/L), iyo 25mL oo biyo ah.
(17) Xalka Thioacetamide (4%, ansax ah: 2 bilood)
4g thioacetamide ayaa lagu milmay 96g oo biyo ah.
(18) Phenanthroline (0.1%, ansax ah: 1 bil)
Ku mil 0.1g o-phenanthroline 100ml oo biyo ah.
19
Ku mil 20g koloridhida stannous 50mL hydrochloric acid.
(20) Potassium hydrogen phthalate xal beddesha caadiga ah (pH 4.0, ansax ah: 2 bilood)
10.12g of potassium hydrogen phthalate (KHC8H4O4) ayaa si sax ah loo miisaamay oo la qalajiyey (115±5) ℃ 2 ~ 3h. Ku qas 1000ml oo biyo ah.
(21) Xalka kaydinta heerka fosfate (pH 6.8, ansax ah: 2 bilood)
3.533g of disodium hydrogen phosphate anhydrous iyo 3.387g of potassium dihydrogen phosphate la qalajiyey at (115 ± 5) ℃ 2 ~ 3h ayaa si sax ah loo miisaamay oo lagu qasi jiray 1000mL biyo.
3, hydroxypropyl methyl cellulose kooxda go'aaminta nuxurka
(1) Go'aaminta nuxurka methoxy
Go'aaminta maadada methoxy waxay ku saleysan tahay kala-goynta aashitada hydroiodate iyadoo lagu kululeynayo shaybaar ka kooban methoxy si loo soo saaro methane iodide kacsan (dhibic karkarinta 42.5 ° C). Methane iodide waxaa lagu miiray nitrogen si loo xalliyo falcelinta tooska ah. Ka dib marka la dhaqo si looga saaro walxaha faragelinta leh (HI, I2 iyo H2S), uumiga methane ee iodine waxaa nuugaya potassium acetate acetic acid oo ka kooban Br2 si ay u sameeyaan IBr ka dibna oxidized si aysiidh iodic ah. Ka dib marka la nadiifiyo, walxaha ku jira aqbalaha waxaa loo wareejiyaa dhalooyinka iodine waxaana lagu qasi karaa biyo. Ka dib marka lagu daro formic acid si looga saaro xad-dhaafka Br2, KI iyo H2SO4 ayaa lagu daraa. Waxa ku jira methoxy waxaa lagu xisaabin karaa titrating 12 oo leh xalka Na2S2O3. Isla'egta falcelinta waxaa loo sheegi karaa sidan soo socota.
Qalabka lagu cabbiro nuxurka methoxy waxa lagu muujiyay sawirka 7-6.
7-6 (a), A waa 50mL weel xaga hoose ah oo ku xidhan tuubada. Qoorta dhalada waxay si toosan ugu qalabaysan tahay tuubo hawo qaboojin toos ah oo E, oo ku saabsan 25cm oo dherer ah iyo 9mm dhexroorka gudaha ah. Cidhifka sare ee tuubada waxa lagu xoojiyey tuubo koofiyad dhalada ah oo leh meel hoose iyo dhexroor 2mm ah. Jaantuska 7-6 (b) wuxuu muujinayaa qalabka la hagaajiyay. 1 waa weelka falcelinta, kaas oo ah 50mL weel xaga hoose ah, tuubada nitrogen-ka ayaa dhanka bidix ah. 2 waa tuubada tubada toosan; 3 waa xoqida, oo ay ku jiraan dareeraha wax lagu dhaqo; 4 waa tuubada nuugista. Farqiga ugu weyn ee u dhexeeya qalabka iyo habka pharmacopoeia waa in labada nuuga ee habka pharmacopoeia la isku daro, taas oo yareyn karta luminta xalka ugu dambeeya ee nuugista. Intaa waxaa dheer, dareeraha lagu dhaqo qashinka ee ku jira qashinka ayaa sidoo kale ka duwan habka pharmacopoeia, kaas oo ah biyo nadiif ah, iyo qalabka la hagaajiyay waa isku dhafka cadmium sulfate xal iyo thiosulfate sodium, taas oo si sahlan u xajin karta wasakhda ku jirta gaaska miiray.
pipette qalabka: 5ml (5), 10ml (1); Burette: 50ml; Dhalada qiyaasta iodine: 250ml; Falanqee dheelitirka.
Reagent phenol (maxaa yeelay waa mid adag, sidaas darteed waa la isku dari doonaa ka hor quudinta); Kaarboon dioxide ama nitrogen; Hydroiodate acid (45%); Falanqaynta saafiga ah; Xalka Potassium acetate (100g/L); Bromine: falanqayn ahaan saafi ah; Formic acid: falanqeyn ahaan saafi ah; 25% xal sodium acetate (220g / L); KI: nadiifnimada gorfaynta; Kala saar sulfuric acid (1+9); Sodium thiosulfate xal caadi ah (0.1mol/L); Tilmaamaha Phenolphthalein; 1% ethanol xal; Tilmaamaha istaarijka: 0.5% istaarijka biyaha; Kala saar sulfuric acid (1+16.5); 30% chromium trioxide xal; Biyo aan dabiici ahayn: ku dar 10ml sulfuric acid (1+16.5) ilaa 100ml oo biyo ah, kulayl karkarinta, oo ku dar 0.1ml0.02mol/L potassium permanganate titer, karkari 10min, waa in ay ahaataa casaan; 0.02mol/L titration sodium hydroxide: Marka loo eego habka Pharmacopoeia ee Shiinaha ee lifaaqa, 0.1mol/L titration sodium hydroxide ayaa la cabbiray oo si sax ah loogu milmay 0.02mol/L biyo la karkariyey oo la qaboojiyey.
Ku dar qiyaastii 10mL oo ah xalka dhaqida tuubada dhaqida, ku dar 31mL oo ah xalka nuugista ee cusub ee la diyaariyey gudaha tuubada nuugista, ku rakib qalabka, miisaan qiyaastii 0.05g (sax ah 0.0001g) muunada la qalajiyey ee la qalajiyey ilaa miisaan joogto ah 105 Geli weelka falcelinta, oo ku dar 5mL hydroiodate. Dhalada falcelinta waxay si dhakhso ah ugu xidhan tahay kondhiyaha soo kabashada (afka shiida waxa lagu qooyay hydroiodate), iyo nitrogen waxa lagu shubaa haanta iyada oo qiyaasta 1 ~ 2 goobooyin ilbiriqsikii. Heerkulka si tartiib ah ayaa loo xakameeyaa si uumiga dareeraha karkaraya uu kor ugu kaco ilaa kala badh dhererka kondhiyaha. Waqtiga falcelinta waxay kuxirantahay nooca shaybaarka, inta u dhaxaysa 45min iyo 3h. Ka saar tuubada nuugista oo si taxadir leh ugu wareeji xalka nuugista 500mL oo ku shub 10ml oo ah 25% sodium acetate xal ilaa inta mugga guud uu gaaro 125ml.
Gariir joogta ah hoosteeda, si tartiib ah ugu dar dhibicda aashitada formic by dhibic ilaa jaalaha uu baaba'ayo. Ku dar dhibic 0.1% methyl tusaha cas, midabka casna ma baaba'o 5 daqiiqo. Kadib ku dar saddex dhibcood oo formic acid ah. In yar ha fadhiisto, ka dibna ku dar 1g oo potassium iodide ah iyo 5mL oo ah sulfuric acid (1+9). Xalka waxaa lagu titrateed 0.1mol / L sodium thiosulfate xal heerka, iyo 3 ~ 4 dhibcood 0.5% istaarijka tilmaame ayaa lagu daray meel u dhow barta dhamaadka, iyo titration waa la sii waday ilaa midabka buluugga ah la waayay.
Isla xaaladdaas, tijaabo maran ayaa la sameeyay.
Xisaabinta wadarta guud ee ka kooban methoxide:
Halkee, V1 ka dhigan tahay mugga (mL) ee sodium thiosulfate xal heerka caadiga ah oo lagu isticmaalo muunado titration; V2 waa mugga sodium thiosulfate xalka caadiga ah ee lagu isticmaalo tijaabada maran, mL; C waa fiirsashada sodium thiosulfate xal heerka caadiga ah, mol/L; M waxa loola jeedaa tirada muunada la qalajiyey, g; 0.00517 waa 0.1mol/L sodium thiosulfate halkii 1ml oo u dhiganta 0.00517g ee methoxy.
Isku geynta maadada methoxy waxay ka dhigan tahay wadarta guud ee methoxy iyo qiimaha hydroxyproxy ee xisaabinta methoxy, markaa wadarta alkoxy waa in lagu saxo nuxurka hydroxyproxy ee ka dhashay si loo helo nuxurka methoxy ee saxda ah. NUUXA HYDROXYPROPXY waa in marka hore lagu saxo si sax ah oo ay soo saarto falcelinta HI oo leh HYDROXYPROPYL oo joogto ah K=0.93 Sidaa darteed:
Maadada methoxy ee la saxay = wadarta guud ee maadada methoxy - (ka kooban hydroxypropoxy ×0.93×31/75)
Halka ay tirooyinka 31 iyo 75 ay yihiin cufka molar ee kooxaha methoxy iyo hydroxypropoxy, siday u kala horreeyaan.
(2) Go'aaminta waxa ku jira hydroxypropoxy
Kooxda hydropropoxy ee muunada waxay la falgalaan chromium trioxide si ay u soo saaraan acetic acid. Ka dib marka laga nadiifiyo xalka autoreaction, waxa ku jira chromic acid waxaa lagu go'aamiyaa titration leh xal NaOH. Sababtoo ah qadar yar oo chromic acid ah ayaa lagu soo saari doonaa habka nadiifinta, xalka NaOH sidoo kale waa la cuni doonaa, markaa waxa ku jira chromic acid waa in lagu sii go'aamiyaa iodimetry lagana gooyaa xisaabinta. Isla'egta falcelintu waa:
Qalabka iyo reagents Qalab dhamaystiran oo go'aaminta kooxaha hydroxypropoxy; Dhalada mugga leh: 1L, 500ml; Dhululubada cabbirka: 50ml; Pipette: 10ml; Dhalada cabbirka iodine: 250ml. Burette aasaasiga ah: 10ml; Sodium thiosulfate xal caadi ah (0.1mol/L); Kala saar sulfuric acid (1+16.5); Kala saar sulfuric acid (1+9); Tilmaamaha istaarijka (0.5%).
7-7 waa aalad lagu go'aamiyo nuxurka hydroxypropoxy.
In 7-7 (a), D waa 25mL weel laba-luqun distilling, B waa 25mm × 150mm tuubo dhaliye uumi, C waa tuubada isku xidhka socodka, A waa qubeyska saliid kululaynta koronto, E waa tiir shunt ah, G waa weel toosan oo leh fur galaas ah, dhexroorka gudaha ugu dambeeya waa 0.25-1.25mm, oo la geliyo weelka wax lagu nadiifiyo; F waa tuubo isku ururin ah oo ku xidhan E. Qalabka la hagaajiyay ee lagu muujiyay FIG. 7-7 (b), 1 waa reactor-ka, kaas oo ah weel 50ml ah oo nadiifinta; 2 waa madaxa distillation; 3 waa maro galaas 50mL si loo xakameeyo xawaaraha socodka biyaha dabiiciga ah; 4 waa tuubo nitrogen; 5 waa tuubada isku ururisa. Farqiga ugu weyn ee u dhexeeya qalabka wax laga beddelay iyo habka pharmacopoeia waa ku-darka muraayadda muraayadda si loo xakameeyo heerka socodka biyaha, si heerka qulqulka si fudud loo xakameeyo.
Hababka tijaabada ee muunada 105 ℃ engejinta miisaanka joogtada ah waxay ku saabsan tahay 0.1 g (0.0002 g), sax ah ayaa lagu sheegay dhalada distillation, ku dar 10 ml oo ah 30% xal trioxide chromium, weelka nadiifinta ee koobka qubayska saliidda, heerka dareeraha qubeyska saliidda waafaqsan dusha dareeraha dareeraha ah ee chromium trioxide, qalab rakiban, biyo qaboojin furan, nitrogen, warshadeena si loo xakameeyo heerka nitrogen ee ku saabsan hal xumbo ilbiriqsikii. 30min gudahood, qubeyska saliidda ayaa la kululeeyay ilaa 155 ℃ waxaana lagu hayaa heerkulkan ilaa xalka la ururiyay uu gaadhay 50mL. Distillation ayaa la joojiyay si looga saaro saliidda qubeyska.
Ku dhaq darbiga gudaha ee qaboojiyaha biyo nadiif ah, isku dar biyaha dhaqida iyo distillate ee dhalada 500mL ee iodine, ku dar 2 dhibcood oo ah 1% phenolphthalide tilmaame, titrate leh 0.02mol/L sodium hydroxide xal qiimaha pH ee 6.9 ~ 7.1 , oo qor wadarta tirada sodium hydroxide ee la isticmaalo.
Ku dar 0.5g sodium bicarbonate iyo 10ml sulfuric acid (1+16.5) ku darso dhalada iodineka oo ha istaagto ilaa aan la soo saarin kaarboon laba ogsaydh. Ka dib ku dar 1.0g potassium iodide, si adag u xidh, si fiican u rux oo ku dhaaf mugdi 5 daqiiqo ah. Ka dib ku dar 1ml 0.5% istaarijka tusaha oo ku titrate 0.02mol/L sodium thiosulfate ilaa meesha ugu dambeysa. Qor mugga sodium thiosulfate ee la isticmaalo.
Tijaabo kale oo madhan, tirooyinka mugga sodium hydroxide iyo sodium thiosulfate titrator-ka la isticmaalo ayaa la duubay siday u kala horreeyaan.
Xisaabinta waxa ku jira hydroxypropoxy:
Halkee, K waa sawirka isku-dhafka saxda ah ee tijaabada bannaan: V1 waa mugga titration sodium hydroxide ee ay isticmaasho muunada, mL. C1 waa fiirsashada xalalka heerka sodium hydroxide, mol/L; V2 waa mugga titration sodium thiosulfate ee la isticmaalo muunada, mL; C2 waa fiirsashada sodium thiosulfate xal heerka caadiga ah, mol / L; M waa tirada muunada, g; Va waa mugga titration sodium hydroxide ee lagu isticmaalo tijaabada maran, mL; Vb waa mugga titration sodium thiosulfate lagu isticmaalo tijaabada maran, mL.
4. Go'aaminta qoyaanka
Isku-dheellitirka falanqaynta qalabka (sax ah ilaa 0.1mg); Dhalada cabbirka: dhexroorka 60mm, dhererka 30mm; Foornada qalajinta.
Habka tijaabada ayaa si sax ah u miisaamaya muunada 2 ~ 4G (
Waqtiga boostada: Sebtembar-08-2022