1, kumenya hydroxypropyl methyl selulose uburyo
. Shira 2mL y'amazi mumiyoboro yipimisha, shyiramo buhoro buhoro 1mL acide sulfurike ya 0,035% anthrone kurukuta rwigituba, hanyuma usige 5min. Impeta y'icyatsi igaragara kuri interineti hagati y'amazi yombi.
(2) Fata urugero rukwiye rwa slime yavuzwe haruguru ikoreshwa mukumenyekanisha (ⅰ) hanyuma uyisuke ku isahani. Amazi amaze guhumeka, hakorwa firime ihindagurika.
2, hydroxypropyl methyl selulose isesengura ryibisubizo bisanzwe
(1) Sodium thiosulfate igisubizo gisanzwe (0.1mol / L, agaciro: ukwezi kumwe)
Gutegura: Guteka hafi ya 1500mL y'amazi yatoboye hanyuma ukonje kugeza witeguye gukoresha. Gupima 25g sodium thiosulfate (uburemere bwa molekuline ni 248.17, kandi ugerageze kuba inyangamugayo hafi 24.817g mugihe upima) cyangwa 16g anhydrous sodium thiosulfate, uyishongeshe muri 200mL y'amazi akonje yavuzwe haruguru, uyunguruze kuri 1L, hanyuma uyashyire mubururu. icupa, shyira icupa mu mwijima, hanyuma uyungurure kugirango ukoreshwe nyuma yibyumweru bibiri.
Calibration: Gupima 0.15g ya potasiyumu dichromate yatetse kugeza uburemere buhoraho, neza na 0.0002g. Ongeramo 2g potassium iyode na 20mL acide sulfurike (1 + 9), uzunguze neza, ushire mu mwijima kuminota 10min, ongeramo amazi ya 150mL hamwe na 3ml 0.5% yumuti wibimenyetso, witondere hamwe na 0.1mol / L sodium thiosulfate, igisubizo gihinduka mubururu Kuri Icyatsi kibisi kumpera yanyuma. Chromate ya Potasiyumu ntabwo yongewe mubushakashatsi bwubusa. Gahunda ya kalibrasi yasubiwemo inshuro 2 ~ 3 kandi impuzandengo yafashwe.
Imyunyungugu ya C (mol / L) ya sodium thiosulfate yumuti usanzwe yabazwe kuburyo bukurikira:
Aho, M ni misa ya potasiyumu dichromate; V1 nubunini bwa sodium thiosulfate ikoreshwa, mL; V2 nubunini bwa sodiumi thiosulfate ikoreshwa mubushakashatsi bwuzuye, mL; 49.03 ni misa ya potasiyumu dichromate ihwanye na 1mol ya sodium thiosulfate, g.
Nyuma ya kalibrasi, ongeramo Na2CO3 nkeya kugirango wirinde kwangirika kwa mikorobe.
(2) Igisubizo cya NaOH (0.1mol / L, agaciro: ukwezi kumwe)
Gutegura: Hafi ya 4.0g ya NaOH yuzuye kugirango isesengurwe yapimwe muri beaker, hanyuma amazi ya 100mL yongewemo yongerwaho gushonga, hanyuma yimurirwa muri flask ya 1L, hanyuma amazi yatoboye yongerwaho umunzani, ashyirwa muminsi 7-10 kugeza kalibrasi.
Calibration: Shyira 0,6 ~ 0.8g ya potasiyumu ya hydrogen phthalate yumye yumye kuri 120 ℃ (neza na 0.0001g) mumashanyarazi ya 250mL, shyiramo 75mL amazi yatoboye kugirango uyashonge, hanyuma ushyiremo 2 ~ 3 ibitonyanga bya 1% bya fenolphthalein, titre hamwe na igisubizo cya hydroxide ya sodium yavuzwe haruguru kugeza itukura gato, kandi iherezo ni uko ibara ridacika muri 30S. Andika ingano ya hydroxide ya sodium. Gahunda ya kalibrasi yasubiwemo inshuro 2 ~ 3 kandi impuzandengo yafashwe. Kandi ukore igeragezwa ryuzuye.
Ubwinshi bwumuti wa sodium hydroxide wabazwe kuburyo bukurikira:
Aho, C ni kwibanda kuri sodium hydroxide yumuti, mol / L; M igereranya ubwinshi bwa potasiyumu hydrogen phthalate, G; V1 nubunini bwa hydroxide ya sodium ikoreshwa, mL; V2 yerekana ingano ya hydroxide ya sodium ikoreshwa mubushakashatsi bwuzuye, mL; 204.2 ni umubyimba wa potasiyumu hydrogen phthalate, g kuri mole.
(3) Koresha aside sulfurike (1 + 9) (Agaciro: ukwezi 1)
Mugihe cyo gukurura, shyiramo witonze 100mL yibanze ya acide sulfurike mumazi 900mL yatoboye, wongereho buhoro, mugihe ukurura.
(4) Koresha aside sulfurike (1 + 16.5) (Agaciro: amezi 2)
Mugihe gikurura, ongeramo witonze 100mL ya acide sulfurike yibanze kuri 1650mL y'amazi yatoboye, wongereho buhoro. Kangura uko ugenda.
(5) Ikimenyetso cya krahisi (1%, agaciro: iminsi 30)
Gupima 1.0g ibishishwa byoroshye, ongeramo amazi ya 10mL, koga hanyuma ubishyire mumazi abira 100mL, uteke gato kuri 2min, ubishyire, hanyuma ufate ndengakamere kugirango ubikoreshe.
(6) Ikimenyetso cyerekana ibinyamisogwe
0.5% ibipimo bya krahisi byabonetse ufata 5mL yumuti wateguwe wa 1% ya krahisi hanyuma ukayungurura 10mL namazi.
(7) 30% ya chromium trioxide igisubizo (agaciro: ukwezi 1)
Gupima 60g ya chromium trioxide hanyuma uyishongeshe muri 140mL y'amazi adafite ibinyabuzima.
(8) Potasiyumu acetate yumuti (100g / L, agaciro: amezi 2)
10g ya potasiyumu ya acide ya anhydrous yashonga mumuti 100mL ya acide acetike ya glacial 90mL na 10mL anhydride.
(9) 25% ya sodium acetate yumuti (220g / L, agaciro: amezi 2)
Kuramo 220g ya anhydrous sodium acetate mumazi hanyuma uyungurura 1000mL.
(10) Acide Hydrochloric (1: 1, agaciro: amezi 2)
Kuvanga aside hydrochloric yibanze hamwe namazi ku kigereranyo cya 1: 1.
(11) Acetate buffer igisubizo (pH = 3.5, agaciro: amezi 2)
Kuramo aside 60mL ya acetike mumazi ya 500mL, hanyuma wongeremo 100mL hydroxide ya ammonium hanyuma uyungurura 1000mL.
(12) Kuyobora igisubizo cyo gutegura nitrate
159.8mg ya nitrate ya sisitemu yashongeshejwe mumazi 100mL arimo 1mL ya acide ya nitric (ubucucike 1.42g / cm3), ivangwa na 1000mL y'amazi hanyuma ivangwa neza. Gutegura no kubika iki gisubizo bigomba gukorwa mu kirahure kitarimo isasu.
(13) Igisubizo gisanzwe cyo kuyobora (agaciro: amezi 2)
Igipimo nyacyo cya 10mL ya nitrate yo gutegura igisubizo cya nitrate yavanze n'amazi kugeza 100mL.
(14) 2% hydroxylamine hydrochloride igisubizo (igihe cyemewe: ukwezi 1)
Kuramo 2g ya hydroxylamine hydrochloride muri 98mL y'amazi.
(15) Amoniya (5mol / L, agaciro: amezi 2)
175.25g ya ammonia yashongeshejwe mumazi hanyuma ayungurura 1000mL.
(16) Amazi avanze (igihe cyemewe: amezi 2)
Kuvanga 100mL glycerol, 75mLNaOH igisubizo (1mol / L), namazi 25mL.
(17) Igisubizo cya Thioacetamide (4%, agaciro: amezi 2)
4g thioacetamide yashonga mumazi 96g.
(18) Fenanthroline (0.1%, agaciro: ukwezi 1)
Kuramo 0.1g o-phenanthroline mumazi 100mL.
(19) Acide stannous chloride (ifite agaciro: ukwezi 1)
Kunyunyuza 20g ya chloride ya 50mL ya acide hydrochloric.
(20) Potasiyumu hydrogen phthalate igisubizo gisanzwe (pH 4.0, agaciro: amezi 2)
10.12g ya potasiyumu hydrogen phthalate (KHC8H4O4) yapimwe neza kandi yumishwa kuri (115 ± 5) ℃ kuri 2 ~ 3h. Koresha kugeza kuri 1000mL n'amazi.
(21) Igisubizo cya fosifate gisanzwe (pH 6.8, agaciro: amezi 2)
3.533g ya anhydrous disodium hydrogen fosifate na 3.387g ya potasiyumu dihydrogen fosifate yumye kuri (115 ± 5) ℃ kuri 2 ~ 3h yapimwe neza kandi ivangwa kugeza kuri 1000mL n'amazi.
3, hydroxypropyl methyl selulose igenamigambi ryitsinda
(1) Kumenya ibirimo imikorere
Kugena ibirimo mikorobe bishingiye ku kubora kwa aside hydroiodate ukoresheje ubushyuhe hamwe n'ikizamini kirimo mikorobe yo kubyara metani ihindagurika (ingingo itetse 42.5 ° C). Metode iodide itandukanijwe na azote mugisubizo cya autoreaction. Nyuma yo gukaraba kugirango ukureho ibintu bibangamira (HI, I2 na H2S), imyuka ya metani metani iva mu mavuta ya potasiyumu acetate acetike acide irimo Br2 ikora IBr hanyuma igahinduka okiside kuri acide iyode. Nyuma yo kuyungurura, ibintu mubyemera byimurirwa mumacupa ya iyode hanyuma bigasukurwa namazi. Nyuma yo kongeramo aside ya formike kugirango ikureho Br2 irenze, KI na H2SO4. Ibikoresho bya methoxy birashobora kubarwa mugutanga titre 12 hamwe numuti wa Na2S2O3. Ingano ya reaction irashobora kugaragazwa kuburyo bukurikira.
Igikoresho cyo gupima ibirimo imikorere irerekanwa mu gishushanyo 7-6.
Muri 7-6 (a), A ni 50mL izenguruka-hepfo flask ihujwe na catheter. Icupa ryujuje ibyuma bihagaritse umuyaga uhuza umuyaga E, hafi 25cm z'uburebure na 9mm z'umurambararo w'imbere. Impera yo hejuru yigituba yunamye mumirahuri ya capillary ikirahure gisohoka hepfo na 2mm mumurambararo w'imbere. Igishushanyo 7-6 (b) cyerekana igikoresho cyateye imbere. 1 ni flask ya reaction, ni flask ya 50mL izenguruka-hepfo, naho umuyoboro wa azote uri ibumoso. 2 ni umuyoboro uhagaze; 3 ni scrubber, irimo amazi yoza; 4 ni umuyoboro winjira. Itandukaniro rinini hagati yigikoresho nuburyo bwa pharmacopoeia nuko ibyinjira byombi byuburyo bwa pharmacopoeia bihujwe murimwe, bishobora kugabanya igihombo cyumuti wanyuma. Byongeye kandi, amazi yo gukaraba muri scrubber nayo atandukanye nuburyo bwa pharmacopoeia, aribwo amazi yatoboye, kandi igikoresho cyanonosowe ni uruvange rwumuti wa cadmium sulfate hamwe nigisubizo cya sodium thiosulfate, gishobora kworoha cyane kwanduza umwanda uri muri gaze yamenetse.
Igikoresho cy'ibikoresho: 5mL (5), 10mL (1); Burette: 50mL; Icupa ryo gupima iyode: 250mL; Gerageza gusesengura.
Reagent phenol (kuko irakomeye, bityo izahuzwa mbere yo kugaburira); Dioxyde de Carbone cyangwa azote; Acide Hydroiodate (45%); Isesengura ryera; Potasiyumu acetate yumuti (100g / L); Bromine: isesengura neza; Acide isanzwe: isesengura neza; 25% sodium acetate yumuti (220g / L); KI: ubuziranenge bw'isesengura; Koresha aside sulfurike (1 + 9); Sodium thiosulfate igisubizo gisanzwe (0.1mol / L); Ikimenyetso cya Fenolphthalein; 1% igisubizo cya Ethanol; Ikimenyetso cya krahisi: 0.5% ibinyamisogwe mumazi; Koresha aside sulfurike (1 + 16.5); 30% ya chromium trioxide igisubizo; Amazi adafite umubiri: ongeramo 10mL ya acide sulfurike (1 + 16.5) mumazi 100mL, ubushyuhe bwo guteka, hanyuma wongeremo 0.1ml0.02mol / L potassium permanganate titer, guteka 10min, bigomba gukomeza kuba ibara ryijimye; 0.02mol / L sodium hydroxide yumuti wa titre: Ukurikije uburyo bwumugereka wa Pharmacopoeia wubushinwa, umuti wa hydroxide ya sodium ya 0.1mol / L wahinduwe neza hanyuma uhindurwamo neza kugeza 0.02mol / L hamwe namazi yatetse kandi akonje.
Ongeramo hafi 10mL yumuti wo gukaraba mumashanyarazi, ongeramo 31mL yumuti mushya wateguwe mumashanyarazi, shyiramo igikoresho, upima hafi 0.05g (neza na 0.0001g) yicyitegererezo cyumye cyumye kugeza kuburemere burigihe kuri 105 ℃ muri reaction ya flask, hanyuma wongereho 5mL hydroiodate. Icupa rya reaction rihita rihuzwa na kondenseri yo gukira (umunwa usya uba wuzuye hydroiodate), hanyuma azote ikajugunywa mu kigega ku gipimo cya 1 ~ 2 ku isegonda. Ubushyuhe bugenzurwa gahoro gahoro kuburyo umwuka wamazi abira uzamuka kugera kuri kimwe cya kabiri cyuburebure bwa condenser. Igihe cyo kubyitwaramo gishingiye kumiterere yicyitegererezo, hagati ya 45min na 3h. Kuraho umuyoboro winjiza hanyuma wimure witonze igisubizo cyinjira muri flask ya 500mL iyode irimo 10ml ya 25% ya sodium acetate ya sodium kugeza igihe igiteranyo cyose kigera kuri 125mL.
Mugihe cyo kunyeganyega buri gihe, shyiramo buhoro buhoro aside aside igabanuka kugeza umuhondo ubuze. Ongeraho igitonyanga cya 0.1% methyl itukura, kandi ibara ritukura ntiribura muminota 5. Noneho shyiramo ibitonyanga bitatu bya acide. Reka bicare umwanya muto, hanyuma ushyiremo 1g ya potasiyumu iyode na 5mL ya acide sulfurike (1 + 9). Igisubizo cyiswe titre 0.1mol / L sodium thiosulfate yumuti usanzwe, hanyuma ibitonyanga 3 ~ 4 byerekana 0.5% byerekana krahisi byongeweho hafi yanyuma, kandi titre yarakomeje kugeza ibara ry'ubururu ryabuze.
Mu bihe bimwe, hakozwe igeragezwa ryambaye ubusa.
Kubara ibikubiyemo byose:
Aho, V1 yerekana ingano (mL) ya sodium thiosulfate yumuti usanzwe ukoreshwa nicyitegererezo; V2 nubunini bwa sodium thiosulfate igisubizo gisanzwe gikoreshwa mubushakashatsi bwubusa, mL; C ni intumbero ya sodium thiosulfate igisubizo gisanzwe, mol / L; M bivuga misa yicyitegererezo cyumye, g; 0.00517 ni 0.1mol / L sodium thiosulfate kuri 1ml ihwanye na 0.00517g ya mikorerexy.
Igiteranyo cyuzuye cya mikorerexy cyerekana imikorere yose hamwe na hydroxyproxy yagaciro yo kubara, bityo alkoxy yose igomba gukosorwa nibivamo hydroxyproxy kugirango ibone ibirimo neza. HYDROXYPROPOXY IBIKORWA BIKWIYE GUKORWA BWA MBERE KUBIKORWA BYATANZWE NA REACTION YA HI NA HYDROXYPROPYL HAMWE NA K = 0.93 (BISOBANURO UMUBARE NININI W'INGINGO ZASOBANUWE NA Morgan. Kubwibyo:
Ikosorwa ryibikorwa bikosowe = ibirimo byose - - hydroxypropoxy content × 0.93 × 31/75)
Aho imibare 31 na 75 aribwo bwinshi bwimitsi ya hydroxypropoxy.
(2) Kumenya ibirimo hydroxypropoxy
Itsinda rya hydropropoxy murugero rwakira hamwe na chromium trioxide kugirango ikore aside acike. Nyuma yo kwitandukanya nigisubizo cya autoreaction, ibirimo aside ya chromic bigenwa na titre hamwe na NaOH igisubizo. Kubera ko aside nkeya ya chromic izazanwa mugikorwa cyo kuyitandukanya, igisubizo cya NaOH nacyo kizakoreshwa, bityo ibiri muri iyi aside ya chromic bigomba kurushaho kugenwa na iyode kandi bigakurwa mubarwa. Ikigereranyo cya reaction ni:
Ibikoresho na reagent Igikoresho cyuzuye cyo kugena amatsinda ya hydroxypropoxy; Icupa ryinshi: 1L, 500mL; Gupima silinderi: 50mL; Pipette: 10mL; Icupa ryo gupima iyode: 250mL. Burette y'ibanze: 10mL; Sodium thiosulfate igisubizo gisanzwe (0.1mol / L); Koresha aside sulfurike (1 + 16.5); Koresha aside sulfurike (1 + 9); Ikimenyetso cya krahisi (0.5%).
7-7 ni igikoresho cyo kumenya ibirimo hydroxypropoxy.
Muri 7-7 (a), D ni flask ya 25mL ya kabiri-ijosi, B ni umuyoboro wa moteri ya 25mm × 150mm, C ni umuyoboro uhuza amazi, A ni ubwogero bwamavuta yo gushyushya amashanyarazi, E ni inkingi ya shunt, G ni flask ya conical ifite ikirahuri cyikirahure, diameter yimbere yimbere ni 0.25-1.25mm, yinjijwe mumashanyarazi; F numuyoboro uhuza uhujwe na E. Mubikoresho byanonosowe byerekanwe muri FIG. 7-7 (b), 1 ni reaction, ni flask ya 50mL ya distillation; 2 ni umutwe wa distillation; 3 ni 50mL ikirahure cyo kugenzura umuvuduko wamazi kama; 4 ni umuyoboro wa azote; 5 ni umuyoboro uhuza. Itandukaniro rikomeye hagati yigikoresho cyahinduwe nuburyo bwa pharmacopoeia nukwongeramo ikirahuri cyikirahure kugirango kigenzure umuvuduko wamazi, kugirango igipimo cyo gutobora gishobora kugenzurwa byoroshye.
Uburyo bwo kwipimisha murugero rwa 105 ℃ gukama kugeza kuburemere buhoraho ni nka 0.1 g (0.0002 g), byavuzwe neza mumacupa ya distillation, ongeramo ml 10 yumuti wa chromium trioxide 30%, flask flask mubikombe byogeramo amavuta, amazi yo kwiyuhagira amavuta bihuye na chromium trioxide yubuso bwamazi, ibikoresho byashyizweho, amazi akonje, azote, y'uruganda rwacu kugirango igenzure igipimo cya azote hafi ya bubble imwe kumasegonda. Muri 30min, ubwogero bwamavuta bwashyutswe kugeza kuri 155 ℃ kandi bugumishwa kuri ubu bushyuhe kugeza igisubizo cyegeranijwe kigeze kuri 50mL. Disillation yahagaritswe kugirango ikureho ubwogero bwamavuta.
Koza urukuta rw'imbere rwa cooler n'amazi yatoboye, komatanya amazi yo gukaraba hamwe na distillate mumacupa ya iyode ya 500mL, ongeramo ibitonyanga 2 byerekana 1% ya fenolphthalide, titre hamwe na 0.02mol / L sodium hydroxide yumuti kuri pH agaciro ka 6.9 ~ 7.1 , hanyuma wandike umubare rusange wa sodium hydroxide yakoreshejwe.
Ongeramo 0.5g sodium bicarbonate na 10mL ya acide sulfurike (1 + 16.5) mumacupa ya iyode hanyuma ureke ihagarare kugeza nta dioxyde de carbone ikozwe. Noneho shyiramo 1.0g potasiyumu iyode, uyicomeke neza, uyinyeganyeze neza hanyuma uyisige mu mwijima kuri 5min. Noneho ongeramo 1mL 0.5% yerekana krahisi hanyuma uyitange hamwe na 0.02mol / L sodium thiosulfate kugeza kumpera. Andika ingano ya sodiumi thiosulfate yakoreshejwe.
Mu bundi bushakashatsi bwambaye ubusa, ingano ya sodium hydroxide na sodium thiosulfate titre yakoreshejwe yakoreshejwe byanditswe.
Kubara ibirimo hydroxypropoxy:
Aho, K nigishushanyo mbonera cyo gukosora igeragezwa ryubusa: V1 nubunini bwa sodium hydroxide titre ikoreshwa nicyitegererezo, mL. C1 ni kwibanda kuri sodium hydroxide igisubizo gisanzwe, mol / L; V2 nubunini bwa sodiumi thiosulfate titre ikoreshwa nicyitegererezo, mL; C2 ni intumbero ya sodium thiosulfate igisubizo gisanzwe, mol / L; M nicyitegererezo cya misa, g; Va nubunini bwa sodium hydroxide titre ikoreshwa mubigeragezo byubusa, mL; Vb nubunini bwa titre ya sodium thiosulfate ikoreshwa mubigeragezo byubusa, mL.
4. Kumenya ubushuhe
Igikoresho cyo gusesengura ibikoresho (neza kuri 0.1mg); Gupima icupa: diameter 60mm, uburebure bwa 30mm; Amashyiga yumye.
Uburyo bwikizamini bupima neza icyitegererezo 2 ~ 4G (
Igihe cyo kohereza: Nzeri-08-2022