1. Uburyo bwo kumenya hydroxypropyl methylcellulose
. shyira 2mL y'amazi mumiyoboro yipimisha, hanyuma wongereho buhoro buhoro 1mL ya 0,035% acide anthrone sulfurike acide kumurongo wigituba hanyuma ubirekere muminota 5. Impeta y'icyatsi igaragara kuri interineti hagati y'amazi yombi.
(2) Fata ingano ikwiye ya mucus ikoreshwa mukumenyekanisha muri (I) hejuru hanyuma uyisuke ku isahani. Amazi amaze guhinduka, firime ihindagurika.
2. Gutegura hydroxypropyl methylcellulose isesengura risanzwe
(1) Sodium thiosulfate igisubizo gisanzwe (0.1mol / L, igihe cyemewe: ukwezi 1)
Gutegura: Guteka hafi ya 1500mL amazi yatoboye, akonje hanyuma ushire kuruhande. Gupima 25g sodium thiosulfate (uburemere bwa molekuline ni 248.17, gerageza kuba inyangamugayo nka 24.817g mugihe upima) cyangwa 16g anhydrous sodium thiosulfate, uyishongeshe muri 200mL y'amazi akonje yavuzwe haruguru, uyungurura kuri 1L, uyashyire mumacupa yumukara, hanyuma ushire Ububiko ahantu hijimye, kuyungurura hanyuma ushire kuruhande nyuma yibyumweru bibiri.
Calibration: Gupima 0.15g ya potasiyumu dichromate hanyuma utekeshe kuburemere burigihe, neza kuri 0.0002g. Ongeramo 2g potasiyumu iyode na 20mL aside sulfurike (1 + 9), uzunguze neza, hanyuma ushire mu mwijima muminota 10. Ongeramo amazi ya 150mL na 3ml 0.5% yumuti werekana ibisubizo, hanyuma ugabanye umuti wa 0.1mol / L sodium thiosulfate. Igisubizo gihinduka kuva mubururu kugera mubururu. Hindura icyatsi kibisi kumpera yanyuma. Nta potasiyumu chromate yongeyeho mubushakashatsi bwambaye ubusa. Gahunda ya kalibrasi isubirwamo inshuro 2 kugeza kuri 3 kandi impuzandengo irafatwa.
Imyunyungugu ya C (mol / L) ya sodium thiosulfate yumuti usanzwe ibarwa ukurikije formula ikurikira:
Muri formula, M ni misa ya potasiyumu dichromate; V1 nubunini bwa sodium thiosulfate ikoreshwa, mL; V2 nubunini bwa sodiumi thiosulfate ikoreshwa mubushakashatsi bwubusa, mL; 49.03 ni dichromium ihwanye na mol 1 ya sodiumi thiosulfate. Ubwinshi bwa aside ya potasiyumu, g.
Nyuma ya kalibrasi, ongeramo umubare muto wa Na2CO3 kugirango wirinde kwangirika kwa mikorobe.
(2) Igisubizo cya NaOH (0.1mol / L, igihe cyemewe: ukwezi 1)
Gutegura: Gupima hafi 4.0g ya NaOH isukuye kugirango isesengurwe muri beaker, ongeramo 100mL y'amazi yatoboye kugirango ushonge, hanyuma wimure muri flask ya volumetric 1L, ongeramo amazi yatoboye kurikimenyetso, hanyuma ubirekere iminsi 7-10 kugeza kalibrasi.
Calibration: Shyira 0,6 ~ 0.8g ya potasiyumu ya hydrogen phthalate yuzuye (neza na 0.0001g) yumishijwe kuri 120 ° C mumashanyarazi ya 250mL Erlenmeyer, ongeramo 75mL y'amazi yatoboye kugirango ushonga, hanyuma wongereho 2 ~ 3 ibitonyanga bya 1% bya fenolphthalein. Titrate hamwe na titre. Koresha sodium hydroxide yumuti wateguwe hejuru kugeza itukura gato, kandi ibara ntirishira mumasegonda 30 nkibihe byanyuma. Andika ingano ya hydroxide ya sodium. Gahunda ya kalibrasi isubirwamo inshuro 2 kugeza kuri 3 kandi impuzandengo irafatwa. Kandi ukore igeragezwa ryuzuye.
Ubwinshi bwumuti wa sodium hydroxide ubarwa kuburyo bukurikira:
Muri formula, C nubunini bwa sodium hydroxide yumuti, mol / L; M igereranya ubwinshi bwa potasiyumu hydrogen phthalate, G; V1 - ingano ya hydroxide ya sodium yakoreshejwe, mL; V2 yerekana sodium hydroxide ikoreshwa mubigeragezo byubusa Umubumbe, mL; 204.2 ni umubyimba wa potasiyumu hydrogen phthalate, g / mol.
(3) Koresha aside sulfurike (1 + 9) (igihe cyemewe: ukwezi 1)
Mugihe ukurura, ongera witonze 100 mL ya acide sulfurike yibanze kuri 900 mL y'amazi yatoboye hanyuma wongereho buhoro mugihe ukurura.
(4) Koresha aside sulfurike (1 + 16.5) (igihe cyemewe: amezi 2)
Mugihe ukangura, ongera witonze 100 mL ya acide sulfurike yibanze kuri 1650 mL y'amazi yatoboye hanyuma wongereho buhoro. Kangura uko ugenda.
(5) Ikimenyetso cyerekana ibinyamisogwe (1%, igihe cyemewe: iminsi 30)
Gupima 1.0g ya krahisi ishonga, ongeramo 10mL y'amazi, koga hanyuma usuke muri 100mL y'amazi abira, uteke muminota 2, ureke uhagarare, hanyuma ufate supernatant kugirango uyikoreshe nyuma.
(6) Ikimenyetso cyerekana ibinyamisogwe
Fata 5 mL yumuti wateguwe wa 1% ya krahisi hanyuma uyisukemo amazi kugeza kuri mL 10 kugirango ubone ibipimo bya 0.5%.
(7) 30% ya chromium trioxide igisubizo (igihe cyemewe: ukwezi 1)
Gupima 60g ya chromium trioxide hanyuma uyishongeshe muri 140mL y'amazi adafite umubiri.
(8) Potasiyumu acetate yumuti (100g / L, ifite amezi 2)
Kuramo g 10 ya potassium acetate ya anhydrous granules muri mL 100 yumuti wa 90 mL ya acide glacique glacial na mL 10 ya anhydride ya acetike.
(9) 25% sodium acetate yumuti (220g / L, igihe cyemewe: amezi 2)
Kuramo 220g anhydrous sodium acetate mumazi hanyuma ukayungurura 1000mL.
(10) Acide Hydrochloric (1: 1, igihe cyemewe: amezi 2)
Kuvanga aside hydrochloric yibanze hamwe namazi mukigereranyo cya 1: 1.
(11) Buffer ya Acetate (pH = 3.5, igihe cyemewe: amezi 2)
Kuramo 60mL ya acide acetike muri 500mL y'amazi, hanyuma ongeramo 100mL ya hydroxide ya amonium hanyuma uyungurura 1000mL.
(12) Kuyobora igisubizo cyo gutegura nitrate
Kunyunyuza 159.8 mg ya nitrate mu mazi ya mL 100 irimo aside nitrike ya mL 1 (ubucucike bwa 1,42 g / cm3), kuyungurura amazi 1000 mL, hanyuma ukavanga neza. Byakosowe neza. Igisubizo kigomba gutegurwa no kubikwa mubirahuri bidafite isasu.
(13) Kuyobora igisubizo gisanzwe (igihe cyemewe: amezi 2)
Gupima neza 10mL yumuti wa nitrate yo gutegura no kongeramo amazi kugirango ugabanye 100mL.
(14) 2% hydroxylamine hydrochloride igisubizo (igihe cyemewe: ukwezi 1)
Kuramo 2g ya hydroxylamine hydrochloride muri 98mL y'amazi.
(15) Amoniya (5mol / L, ifite amezi 2)
Kuramo amazi ya amoniya 175.25g hanyuma ukayungurura 1000mL.
(16) Amazi avanze (agaciro: amezi 2)
Kuvanga 100mL ya glycerol, 75mL yumuti wa NaOH (1mol / L) na 25mL yamazi.
(17) Umuti wa Thioacetamide (4%, ufite amezi 2)
Kuramo 4g ya thioacetamide muri 96g y'amazi.
(18) Fenanthroline (0.1%, igihe cyemewe: ukwezi 1)
Kuramo 0.1g ya phenanthroline muri 100mL y'amazi.
(19) Acideic stannous chloride (igihe cyemewe: ukwezi 1)
Kuramo 20g ya chloride idasanzwe muri 50mL ya acide hydrochloric yibanze.
(20) Potasiyumu hydrogen phthalate isanzwe ya buffer igisubizo (pH 4.0, igihe cyemewe: amezi 2)
Gupima neza 10.12g ya potasiyumu hydrogen phthalate (KHC8H4O4) hanyuma ukumisha kuri (115 ± 5) ℃ mumasaha 2 kugeza kuri 3. Koresha kugeza kuri 1000mL n'amazi.
(21) Igisubizo cya fosifate gisanzwe (pH 6.8, igihe cyemewe: amezi 2)
Gupima neza 3.533g anhydrous disodium hydrogen fosifate na 3.387g potasiyumu dihydrogen fosifate yumye kuri (115 ± 5) ° C mumasaha 2 ~ 3, hanyuma ukayungurura kugeza kuri 1000mL n'amazi.
3. Kumenya hydroxypropylmethylcellulose yibiri mumatsinda
(1) Kumenya ibirimo mikorobe
Igenamigambi ryibikorwa byitsinda rishingiye ku kizamini kirimo amatsinda mato. Acide Hydroiodic ibora iyo ishyushye kugirango itange methyl iodide ihindagurika (ingingo ibira 42.5 ° C). Methyl iyode yashizwemo na azote mugisubizo cyonyine. Nyuma yo gukaraba kugirango ikureho ibintu bibangamira (HI, I2 na H2S), umwuka wa methyl iodide winjizwa numuti wa acide acetike wa potasiyumu acetate irimo Br2 kugirango ube IBr, hanyuma ugahinduka okiside kuri acide iyode. Nyuma yo kuyungurura, ibiri muri reseptor byimurirwa mu icupa rya iyode hanyuma bigasukwa n'amazi. Nyuma yo kongeramo aside ya formike kugirango ikureho Br2 irenze, KI na H2SO4. Ibirimo metoxyl birashobora kubarwa mugutanga 12 hamwe na Na2S2O3 igisubizo. Ingano ya reaction irashobora kugaragazwa kuburyo bukurikira.
Igikoresho cyo gupima metoxyl cyerekanwe mubishusho 7-6.
Muri 7-6 (a), A ni 50mL izengurutswe-flask ihujwe na catheter. Hano hari umuyoboro ugororotse uhumeka E ushyizwe muburyo butagaragara, uburebure bwa 25cm z'uburebure na 9mm z'imbere. Impera yo hejuru yigituba yunamye mu kirahuri capillary ikirahure gifite diametre y'imbere ya mm 2 hamwe n'isohoka ryerekeza hepfo. Igishushanyo 7-6 (b) cyerekana igikoresho cyateye imbere. Igishushanyo cya 1 cyerekana flask ya reaction, ni flask ya 50mL izengurutswe, hamwe na azote ibumoso. 2 ni umuyoboro uhagaze; 3 ni scrubber, irimo amazi yoza; 4 ni umuyoboro winjira. Itandukaniro rinini hagati yiki gikoresho nuburyo bwa Pharmacopoeia nuko ibyinjira byombi byuburyo bwa Pharmacopoeia byahujwe murimwe, bishobora kugabanya igihombo cyamazi yanyuma. Byongeye kandi, amazi yoza muri scrubber nayo atandukanye nuburyo bwa pharmacopoeia. Ni amazi yatoboye, mugihe igikoresho cyatejwe imbere ni uruvange rwumuti wa kadmium sulfate hamwe nigisubizo cya sodium thiosulfate, cyoroshye kwinjiza imyanda muri gaze yatoboye.
Igikoresho cy'ibikoresho: 5mL (ibice 5), 10mL (igice 1); Burette: 50mL; Icupa ryinshi rya iyode: 250mL; Impirimbanyi zisesenguye.
Reagent phenol (kuko ikomeye, izashonga mbere yo kugaburira); Dioxyde de carbone cyangwa azote; aside hydroiodic (45%); icyiciro cyo gusesengura; potasiyumu acetate yumuti (100g / L); bromine: icyiciro cyo gusesengura; acide formic: icyiciro cyo gusesengura; 25% igisubizo cya Sodium acetate (220g / L); KI: icyiciro cyo gusesengura; kugabanya aside aside (1 + 9); sodium thiosulfate igisubizo gisanzwe (0.1mol / L); icyerekezo cya phenolphthalein; 1% igisubizo cya Ethanol; icyerekezo cya krahisi: 0.5% igisubizo cyamazi yo mumazi; kugabanya aside aside (1 + 16.5); 30% ya chromium trioxide igisubizo; amazi adafite organic: ongeramo 10mL ya acide sulfurike (1 + 16.5) kuri 100mL y'amazi, ubushyuhe bwo guteka, hanyuma ongeramo 0.1ml ya 0.02mol / L acide permanganic aside Potasiyumu, uteke muminota 10, igomba kuguma yijimye; 0.02mol / L sodium hydroxide ya titre: Hindura titre ya 0.1mol / L ya hydroxide ya hydroxide ukurikije uburyo bwa Umugereka wa Pharmacopoeia wubushinwa, hanyuma ugabanye neza kuri 0.02mol ukoresheje amazi yatetse kandi akonje / L.
Ongeramo hafi 10mL yo gukaraba mumazi yo gukaraba, ongeramo 31mL yamazi mashya yateguwe mumashanyarazi, shyiramo igikoresho, upima hafi 0,05g yicyitegererezo cyumye cyumye kugeza kuburemere burigihe kuri 105 ° C (neza na 0.0001 g), ongeramo reaction kuri ℃ Mu icupa, ongeramo 5 mL ya hydroiodide. Huza vuba icupa rya reaction na kondenseri yo kugarura (koresha icyuma gisya hamwe na aside hydriodic), hanyuma usukemo azote mu kigega ku gipimo cya 1 kugeza kuri 2 ku isegonda.
Igihe cyo kohereza: Gashyantare-01-2024