1, idanimọ ti ọna hydroxypropyl methyl cellulose
(1) Mu 1.0g ti apẹẹrẹ, omi kikan (80 ~ 90 ℃) 100mL, aruwo nigbagbogbo, ki o tutu sinu omi viscous ninu iwẹ yinyin; Fi 2mL ti omi sinu tube idanwo, fi sii laiyara 1mL sulfuric acid ojutu ti 0.035% anthrone lẹgbẹẹ ogiri tube, ki o fi silẹ fun iṣẹju 5. Iwọn alawọ ewe han ni wiwo laarin awọn olomi meji.
(2) Mu iye ti o yẹ ti slime ti a mẹnuba loke ti a lo ninu idanimọ (ⅰ) ki o si tú u sori awo gilasi naa. Lẹhin ti omi yọ kuro, fiimu ductile kan ti ṣẹda.
2, hydroxypropyl methyl cellulose onínọmbà ti awọn boṣewa ojutu igbaradi
(1) Sodium thiosulfate ojutu boṣewa (0.1mol/L, wulo: oṣu kan)
Igbaradi: Sise nipa 1500mL distilled omi ati ki o dara titi ti o setan lati lo. Ṣe iwọn 25g sodium thiosulfate (iwuwọn molikula rẹ jẹ 248.17, ati gbiyanju lati jẹ deede si iwọn 24.817g nigbati o ba ṣe iwọn) tabi 16g sodium thiosulfate anhydrous, tu ni 200mL ti omi itutu loke, dilute rẹ si 1L, ki o si gbe sinu brown brown. igo, fi igo naa sinu okunkun, ki o si ṣe àlẹmọ fun lilo lẹhin ọsẹ meji.
Isọdiwọn: Ṣe iwọn 0.15g ti itọkasi potasiomu dichromate ti a yan si iwuwo igbagbogbo, deede si 0.0002g. Fi 2g potasiomu iodide kun ati 20mL sulfuric acid (1+9), gbọn daradara, gbe sinu okunkun fun iṣẹju 10, ṣafikun omi 150mL ati 3ml 0.5% itọka itọka sitashi, titrate pẹlu 0.1mol/L sodium thiosulfate ojutu, ojutu naa yipada lati buluu. si alawọ ewe didan ni aaye ipari. Potasiomu chromate ko ṣe afikun si idanwo òfo. Ilana isọdiwọn tun jẹ awọn akoko 2 ~ 3 ati pe a mu iye apapọ.
Ifojusi molar C (mol/L) ti ojutu boṣewa iṣuu soda thiosulfate ni iṣiro bi atẹle:
Nibo, M jẹ iwọn ti potasiomu dichromate; V1 jẹ iwọn didun ti iṣuu soda thiosulfate ti a jẹ, mL; V2 jẹ iwọn didun ti iṣuu soda thiosulfate ti o jẹ ni idanwo òfo, mL; 49.03 jẹ ọpọ ti potasiomu dichromate deede si 1mol ti iṣuu soda thiosulfate, g.
Lẹhin isọdiwọn, ṣafikun Na2CO3 diẹ lati ṣe idiwọ ibajẹ microbial.
(2) Ojutu boṣewa NaOH (0.1mol/L, iwulo: oṣu kan)
Igbaradi: Nipa 4.0g ti NaOH mimọ fun itupalẹ ni a ṣe iwọn sinu beaker, ati 100mL omi ti a fi omi ṣan ni a fi kun lati tu, lẹhinna gbe lọ si 1L volumetric flask, ati omi ti a fi omi ṣan ti a fi sinu iwọn, ati gbe fun awọn ọjọ 7-10 titi di ọjọ 7-10. isọdiwọn.
Isọdiwọn: Fi 0.6 ~ 0.8g ti potasiomu hydrogen phthalate mimọ ti o gbẹ ni 120 ℃ (deede si 0.0001g) sinu ọpọn conical 250mL, ṣafikun omi distilled 75mL lati tu, lẹhinna ṣafikun 2 ~ 3 silė ti 1% phenolphthalein pẹlu itọkasi, tit. ojutu iṣuu soda hydroxide ti o wa loke ti a pese silẹ titi o fi jẹ pupa diẹ, ati pe aaye ipari ni pe awọ ko dinku laarin 30S. Kọ si isalẹ awọn iwọn didun ti soda hydroxide. Ilana isọdiwọn tun jẹ awọn akoko 2 ~ 3 ati pe a mu iye apapọ. Ki o si ṣe kan òfo ṣàdánwò.
Ifojusi ti ojutu iṣuu soda hydroxide ni iṣiro bi atẹle:
Nibo, C jẹ ifọkansi ti iṣuu soda hydroxide, mol / L; M duro fun iwọn ti potasiomu hydrogen phthalate, G; V1 jẹ iwọn didun ti iṣuu soda hydroxide run, mL; V2 duro fun iwọn didun ti iṣuu soda hydroxide ti o jẹ ni idanwo òfo, mL; 204.2 jẹ iwuwo molar ti potasiomu hydrogen phthalate, g fun mole.
(3) Dilute sulfuric acid (1+9) (Iwulo: oṣu kan)
Labẹ gbigbe, farabalẹ ṣafikun 100mL sulfuric ogidi si omi distilled 900mL, ṣafikun laiyara, lakoko gbigbe.
(4) Dilute sulfuric acid (1+16.5) (Iwulo: osu meji)
Labẹ igbiyanju, farabalẹ fi 100mL ti sulfuric acid ti o ni idojukọ si 1650mL ti omi distilled, fifi kun laiyara. Aruwo bi o ti lọ.
(5) Atọka sitashi (1%, iwulo: awọn ọjọ 30)
Ṣe iwọn sitashi 1.0g ti o le yo, fi omi 10mL kun, dapọ ki o si wọn sinu omi gbigbona 100ml, sise diẹ fun iṣẹju 2, gbe e, ki o si mu supernatant fun lilo.
(6) Atọka sitashi
Atọka sitashi 0.5% ni a gba nipasẹ gbigbe 5mL ti ojutu itọka itọka sitashi 1% ti a pese silẹ ati diluting rẹ si 10mL pẹlu omi.
(7) Ojutu 30% chromium trioxide (ifọwọsi: oṣu kan)
Ṣe iwọn 60g ti chromium trioxide ki o tu ni 140mL ti omi laisi ohun elo Organic.
(8) ojutu acetate potasiomu (100g/L, iwulo: awọn oṣu 2)
10g ti awọn oka acetate potasiomu anhydrous ni a tuka ni ojutu 100mL ti 90mL glacial acetic acid ati 10mL acetic anhydride.
(9) 25% ojutu iṣuu soda acetate (220g/L, iwulo: awọn oṣu 2)
Tu 220g ti iṣuu soda acetate anhydrous ninu omi ati dilute si 1000ml.
(10) Hydrochloric acid (1:1, ìwúlò: oṣù 2)
Illa hydrochloric acid ti o ni idojukọ pẹlu omi ni ipin iwọn didun 1:1.
(11) Ojutu ifipamọ acetate (pH = 3.5, iwulo: awọn oṣu 2)
Tu 60mL acetic acid sinu omi 500mL, lẹhinna fi 100mL ammonium hydroxide kun ati dilute si 1000ml.
(12) Ojutu igbaradi iyọrisi asiwaju
159.8mg ti iyọ asiwaju ni tituka ninu omi 100mL ti o ni 1mL ti acid nitric (iwuwo 1.42g/cm3), ti fomi si 1000mL ti omi ati adalu daradara. Igbaradi ati ibi ipamọ ti ojutu yii yoo ṣee ṣe ni gilasi laisi asiwaju.
(13) Ojutu asiwaju boṣewa (Iwulo: awọn oṣu 2)
Iwọn wiwọn deede ti 10mL ti ojutu igbaradi iyọ iyọ asiwaju ti fomi po pẹlu omi si 100mL.
(14) Ojutu hydroxylamine hydrochloride 2% (akoko afọwọsi: oṣu kan)
Tu 2g ti hydroxylamine hydrochloride sinu 98mL ti omi.
(15) Amonia (5mol/L, wulo: oṣu meji)
175.25g ti amonia ti tu sinu omi ati ti fomi si 1000ml.
(16) Omi ti o dapọ (akoko ifọwọsi: awọn oṣu 2)
Illa 100mL glycerol, ojutu 75mLNaOH (1mol/L), ati omi 25mL.
(17) Ojutu Thioacetamide (4%, iwulo: awọn oṣu 2)
4g thioacetamide ti tuka ni omi 96g.
(18) Phhenanthroline (0.1%, ifọwọsi: oṣu kan)
Tu 0.1g o-phenanthroline sinu omi 100mL.
(19) kiloraidi stannous acid (ifọwọsi: oṣu kan)
Tu 20g stannous kiloraidi ni 50mL ogidi hydrochloric acid.
(20) Potasiomu hydrogen phthalate ojuutu imuduro boṣewa (pH 4.0, ifọwọsi: oṣu 2)
10.12g ti potasiomu hydrogen phthalate (KHC8H4O4) ti ni iwọn deede ati gbigbe ni (115± 5) ℃ fun 2 ~ 3h. Dinku si 1000 milimita pẹlu omi.
(21) Ojútùú dídíjú phosphate (pH 6.8, ìwúlò: oṣù 2)
3.533g ti disodium hydrogen fosifeti anhydrous ati 3.387g ti potasiomu dihydrogen fosifeti ti o gbẹ ni (115 ± 5) ℃ fun 2 ~ 3h ni wọn ṣe deede ati ti fomi si 1000mL pẹlu omi.
3, hydroxypropyl methyl cellulose ẹgbẹ ipinnu akoonu
(1) Ipinnu ti methoxy akoonu
Ipinnu akoonu methoxy da lori jijẹ hydroiodate acid nipasẹ alapapo pẹlu idanwo ti o ni methoxy lati ṣe agbejade methane iodide iyipada (ojuami farabale 42.5 ° C). Methane iodide jẹ distilled pẹlu nitrogen ni ojutu autoreaction. Lẹhin fifọ lati yọ awọn nkan ti o ni idiwọ kuro (HI, I2 ati H2S), iyọ methane iodine ti gba nipasẹ potasiomu acetate acetic acid ojutu ti o ni Br2 lati dagba IBr ati lẹhinna oxidized si iodic acid. Lẹhin distillation, awọn nkan ti o wa ninu olugba ni a gbe lọ si awọn igo iodine ati ti fomi po pẹlu omi. Lẹhin fifi formic acid kun lati yọkuro Br2 pupọ, KI ati H2SO4 ti wa ni afikun. Awọn akoonu methoxy le ṣe iṣiro nipasẹ titrating 12 pẹlu ojutu ti Na2S2O3. Idogba ifaseyin le ṣe afihan bi atẹle.
Ẹrọ fun wiwọn akoonu methoxy han ni Nọmba 7-6.
Ni 7-6 (a), A jẹ 50mL igo isalẹ-isalẹ ti o ni asopọ pẹlu catheter kan. Ọrun igo naa ti ni inaro pẹlu tube itọka afẹfẹ ti o tọ, nipa 25cm ni ipari ati 9mm ni iwọn ila opin inu. Ipari oke ti tube naa ti tẹ sinu tube capillary gilasi kan pẹlu iṣan sisale ati 2mm ni iwọn ila opin inu. olusin 7-6 (b) fihan awọn dara ẹrọ. 1 jẹ flask ifasilẹ, eyiti o jẹ 50mL igo isalẹ-isalẹ, ati paipu nitrogen wa ni apa osi. 2 ni inaro condensing paipu; 3 jẹ scrubber, ti o ni omi fifọ; 4 jẹ tube gbigba. Iyatọ ti o tobi julọ laarin ẹrọ ati ọna pharmacopoeia ni pe awọn olugba meji ti ọna pharmacopoeia ti wa ni idapo sinu ọkan, eyi ti o le dinku isonu ti ojutu gbigba ikẹhin. Ni afikun, omi fifọ ni scrubber tun yatọ si ọna pharmacopoeia, eyiti o jẹ omi distilled, ati ẹrọ ti o ni ilọsiwaju jẹ adalu cadmium sulfate ojutu ati iṣuu soda thiosulfate, eyiti o le ni irọrun adsorb awọn impurities ninu gaasi distilled.
Pipette irinse: 5mL (5), 10ml (1); Burette: 50ml; Igo wiwọn iodine: 250ml; Ṣe itupalẹ iwọntunwọnsi.
Reagent phenol (nitori pe o jẹ to lagbara, nitorinaa yoo dapọ ṣaaju ifunni); Erogba oloro tabi nitrogen; Hydroiodate acid (45%); Onínọmbà ti funfun; Potasiomu acetate ojutu (100g/L); Bromine: atupalẹ mimọ; Formic acid: atupalẹ mimọ; 25% iṣuu soda acetate ojutu (220g / L); KI: atupalẹ ti nw; Dilute sulfuric acid (1+9); Iṣuu soda thiosulfate boṣewa ojutu (0.1mol/L); Atọka Phenolphthalein; 1% ethanol ojutu; Atọka sitashi: 0.5% sitashi ninu omi; Dilute sulfuric acid (1+16.5); 30% ojutu trioxide chromium; Omi ti ko ni Organic: ṣafikun 10mL dilute sulfuric acid (1 + 16.5) si omi 100mL, ooru si farabale, fi kun 0.1ml0.02mol /L potasiomu permanganate titer, sise fun 10min, gbọdọ jẹ Pink; 0.02mol/L sodium hydroxide titration ojutu: Ni ibamu si awọn Chinese Pharmacopoeia appendix ọna, 0.1mol/L sodium hydroxide ojutu ti a calibrated ati ki o deede ti fomi si 0.02mol/L pẹlu boiled ati ki o tutu distilled omi.
Fi nipa 10mL ti ojutu fifọ sinu tube fifọ, ṣafikun 31mL ti ojutu gbigba tuntun ti a pese silẹ sinu tube gbigba, fi ẹrọ naa sori ẹrọ, ṣe iwọn nipa 0.05g (deede si 0.0001g) ti apẹẹrẹ ti o gbẹ ti o ti gbẹ si iwuwo igbagbogbo ni 105 ℃ sinu ọpọn ifaseyin, ki o si fi 5mL hydroiodate kun. Igo ifasilẹ ti wa ni asopọ ni kiakia si condenser imularada (ẹnu lilọ ti wa ni tutu pẹlu hydroiodate), ati nitrogen ti wa ni fifa sinu ojò ni iwọn 1 ~ 2 nyoju fun iṣẹju-aaya. Awọn iwọn otutu ti wa ni iṣakoso laiyara ki nya ti omi farabale ba ga soke si idaji giga ti condenser. Akoko ifaseyin da lori iru ayẹwo, laarin 45min ati 3h. Yọ tube ti o ngba kuro ki o si farabalẹ gbe ojutu ifunmọ sinu igo iodine 500mL ti o ni 10ml ti 25% iṣuu soda acetate ojutu titi ti iwọn didun lapapọ yoo de nipa 125mL.
Labẹ gbigbọn igbagbogbo, laiyara ṣafikun formic acid ju silẹ titi ti ofeefee yoo fi parẹ. Ṣafikun itọka pupa 0.1% methyl, ati pe awọ pupa ko parẹ fun iṣẹju 5. Lẹhinna fi awọn silė mẹta ti formic acid. Jẹ ki o joko fun igba diẹ, lẹhinna fi 1g ti potasiomu iodide ati 5mL ti dilute sulfuric acid (1+9). Ojutu ti wa ni titrated pẹlu 0.1mol/L sodium thiosulfate boṣewa ojutu, ati 3 ~ 4 silė ti 0.5% sitashi Atọka ni won fi kun sunmọ awọn aaye ipari, ati awọn titration ti a tesiwaju titi ti bulu awọ parẹ.
Ni ipo kanna, a ṣe idanwo òfo.
Iṣiro akoonu methoxide lapapọ:
Nibo, V1 ṣe aṣoju iwọn didun (mL) ti iṣuu soda thiosulfate boṣewa ojutu ti o jẹ nipasẹ awọn ayẹwo titration; V2 jẹ iwọn didun ti iṣuu soda thiosulfate boṣewa ojutu ti o jẹ ni idanwo òfo, mL; C jẹ ifọkansi ti iṣuu soda thiosulfate boṣewa ojutu, mol/L; M n tọka si ibi-ti o ti gbẹ ayẹwo, g; 0.00517 jẹ 0.1mol/L sodium thiosulfate fun 1 milimita deede si 0.00517g ti methoxy.
Apapọ akoonu methoxy duro fun apapọ methoxy ati iye hydroxyproxy ti iṣiro methoxy, nitorinaa apapọ alkoxy gbọdọ jẹ atunṣe nipasẹ akoonu hydroxyproxy ti o yọrisi lati gba akoonu methoxy gangan. Akoonu HYDROXYPROPOXY KI A ṢE TUNTUN FUN AWỌN NIPA TI AWỌN NIPA TI AWỌN NIPA HI PẸLU HYDROXYPROPYL PẸLU AWỌN ỌJỌ K=0.93 (Itumọ ti NOMBA NLA TI AWỌN NIPA TI AWỌN NIPA TI AWỌN NIPA). Nitorina:
Àkóónú methoxy tí a ṣàtúnṣe = àkóónú methoxy lápapọ̀ – (àkóónú hydroxypropoxy ×0.93×31/75)
Nibiti awọn nọmba 31 ati 75 jẹ ọpọ eniyan molar ti methoxy ati awọn ẹgbẹ hydroxypropoxy, lẹsẹsẹ.
(2) Ipinnu ti akoonu hydroxypropoxy
Ẹgbẹ hydropropoxy ti o wa ninu ayẹwo ṣe atunṣe pẹlu chromium trioxide lati ṣe agbejade acetic acid. Lẹhin ti o ti sọ distilled lati ojutu autoreaction, akoonu ti chromic acid jẹ ipinnu nipasẹ titration pẹlu ojutu NaOH. Nitoripe iye kekere ti chromic acid yoo mu jade ni ilana distillation, ojutu NaOH yoo tun jẹ, nitorina akoonu ti chromic acid yii yẹ ki o jẹ ipinnu siwaju sii nipasẹ iodimetry ati yọkuro lati inu iṣiro naa. Idogba esi ni:
Awọn ohun elo ati awọn reagents A ṣeto awọn ohun elo pipe fun ipinnu awọn ẹgbẹ hydroxypropoxy; Igo iwọn didun: 1L, 500ml; Silinda wiwọn: 50ml; Pipette: 10ml; Igo wiwọn iodine: 250ml. Burette ipilẹ: 10ml; Iṣuu soda thiosulfate boṣewa ojutu (0.1mol/L); Dilute sulfuric acid (1+16.5); Dilute sulfuric acid (1+9); Atọka sitashi (0.5%).
7-7 jẹ ẹrọ kan fun ipinnu ti akoonu hydroxypropoxy.
Ni 7-7 (a), D jẹ 25mL ni ilopo-ọrun distilling flask, B jẹ a 25mm × 150mm nya monomono tube, C ni a sisan asopọ tube, A jẹ ẹya ina alapapo epo iwẹ, E ni a shunt iwe, G jẹ ọpọn conical kan pẹlu plug gilasi kan, opin opin inu jẹ 0.25-1.25mm, ti a fi sii sinu ọpọn distilling; F jẹ tube isọdọkan ti a ti sopọ si E. Ninu ẹrọ imudara ti o han ni FIG. 7-7 (b), 1 ni riakito, eyi ti o jẹ 50mL distillation flask; 2 jẹ ori distillation; 3 jẹ funnel gilasi 50mL lati ṣakoso iyara ti ṣiṣan omi Organic; 4 jẹ paipu nitrogen; 5 ni paipu condensing. Iyatọ ti o ṣe pataki julọ laarin ẹrọ ti a ṣe atunṣe ati ọna pharmacopoeia jẹ afikun ti funnel gilasi kan lati ṣakoso iwọn sisan omi, ki oṣuwọn ti distillation le ni iṣakoso ni rọọrun.
Awọn ọna idanwo ni apẹẹrẹ ti 105 ℃ gbigbẹ si iwuwo igbagbogbo jẹ nipa 0.1 g (0.0002 g), deede wi ni igo distillation, ṣafikun 10 milimita ti 30% ojutu trioxide chromium, iyẹfun distillation sinu ago iwẹ epo, ipele omi iwẹ epo ni ibamu pẹlu chromium trioxide omi dada, ohun elo ti a fi sori ẹrọ, omi itutu ìmọ, nitrogen, ti ile-iṣẹ wa lati ṣakoso oṣuwọn nitrogen nipa ọkan o ti nkuta fun iṣẹju-aaya. Laarin 30min, iwẹ epo naa ti gbona si 155 ℃ ati ṣetọju ni iwọn otutu yii titi ti ojutu ti a gbajọ ti de 50mL. Awọn distillation ti a duro lati yọ awọn epo wẹ.
Wẹ odi inu ti olutọju pẹlu omi ti a fi omi ṣan, darapọ omi fifọ ati distillate ni igo iodine 500mL, fi 2 silė ti 1% phenolphthalide itọkasi, titrate pẹlu 0.02mol / L sodium hydroxide ojutu si pH iye ti 6.9 ~ 7.1 , ati kọ nọmba lapapọ ti iṣuu soda hydroxide ti o jẹ.
Fi 0.5g iṣuu soda bicarbonate ati 10mL dilute sulfuric acid (1+16.5) sinu igo iodine ki o jẹ ki o duro titi ti ko si erogba oloro ti a ṣejade. Lẹhinna fi 1.0g potasiomu iodide kun, pulọọgi ni wiwọ, gbọn daradara ki o fi sinu okunkun fun iṣẹju 5. Lẹhinna ṣafikun atọka sitashi 1mL 0.5% ki o si titrate rẹ pẹlu 0.02mol/L sodium thiosulfate si aaye ipari. Kọ silẹ iwọn didun ti iṣuu soda thiosulfate ti o jẹ.
Ninu idanwo òfo miiran, awọn nọmba iwọn didun ti iṣuu soda hydroxide ati iṣuu soda thiosulfate titrators ti jẹ ni a gbasilẹ ni atele.
Iṣiro akoonu hydroxypropoxy:
Nibo, K jẹ aworan onisọdipupo atunṣe ti adanwo òfo: V1 jẹ iwọn didun ti iṣuu soda hydroxide titration ti o jẹ nipasẹ apẹẹrẹ, mL. C1 jẹ ifọkansi ti iṣuu soda hydroxide boṣewa ojutu, mol / L; V2 jẹ iwọn didun ti iṣuu soda thiosulfate titration ti o jẹ nipasẹ ayẹwo, mL; C2 jẹ ifọkansi ti iṣuu soda thiosulfate boṣewa ojutu, mol / L; M jẹ iwọn ayẹwo, g; Va jẹ iwọn didun ti iṣuu soda hydroxide titration ti o jẹ ni idanwo òfo, mL; Vb jẹ iwọn didun ti iṣuu soda thiosulfate titration ti o jẹ ninu idanwo òfo, mL.
4. Ipinnu ti ọrinrin
Iwontunwonsi atupale ohun elo (deede si 0.1mg); Igo wiwọn: iwọn ila opin 60mm, iga 30mm; adiro gbigbe.
Ọna idanwo naa ṣe iwọn ayẹwo ni deede 2 ~ 4G (
Akoko ifiweranṣẹ: Oṣu Kẹsan-08-2022