1. Tikanga tautuhi o te hydroxypropyl methylcellulose
(1) Tangohia te 1.0g o te tauira, whakamahanahia te 100mL wai (80~90 ℃), whakaoho tonu, ka whakamatao i roto i te pati tio kia huri ra ano he wai pokarekare; hoatu te 2mL o te wai ki roto i te ipuipu, ka ata taapirihia te 1mL o te 0.035% waikawa pungatara anthrone ki te wairewa pakitara ngongo ka waiho mo te 5 meneti. Ka puta he mowhiti matomato i te atanga i waenganui i nga wai e rua.
(2) Tangohia te rahinga tika o te hūpē i whakamahia hei tohu ki te (I) i runga ake ka riringi ki runga i te pereti karaihe. Ka mimiti te wai, ka puta he kiriata ngongo.
2. Te whakarite i te otinga paerewa tātari hydroxypropyl methylcellulose
(1) Te otinga paerewa konutai thiosulfate (0.1mol/L, te wa mana: 1 marama)
Te Whakaritenga: Kohuatia te 1500mL wai matutu, whakamatao ka waiho ki te taha. Paunatia te 25g konutai thiosulfate (ko tona taumaha irapoi ko te 248.17, ngana kia rite ki te 24.817g ina paunatia) 16g ranei te konutai thiosulfate anhydrous, memeha ki te 200mL o te wai whakamatao i runga ake nei, waimeha ki te 1L, hoatu ki roto i te pounamu parauri. ka waiho Whakatokia ki tetahi wahi pouri, tātarihia ka wehea i muri i nga wiki e rua.
Whakatauritenga: Paunatia te 0.15g o te tohutoro pāhare pāporo dichromate ka tunu ki te taumaha tonu, tika ki te 0.0002g. Tāpirihia te 2g pāhare pāporo iodide me te 20mL waikawa pungatara (1+9), ruru pai, ka waiho ki te pouri mo te 10 meneti. Tāpirihia te wai 150mL me te 3ml 0.5% wairewa tohu māngaro, ka titrate ki te 0.1mol/L te wairewa konutai thiosulfate. Ka huri te otinga mai i te kahurangi ki te kahurangi. Ka huri kakariki kanapa ki te pito mutunga. Karekau he konupora chromate i taapirihia ki te whakamatautau kore. Ko te tukanga whakatikatika ka tukuna kia 2 ki te 3 nga wa ka tangohia te uara toharite.
Ko te kukū molar C (mol/L) o te otinga paerewa konutai thiosulfate ka tatauhia i runga i te tauira e whai ake nei:
I roto i te tātai, ko M te papatipu o te pāhare pāporo dichromate; Ko V1 te rōrahi o te konutai thiosulfate i pau, mL; Ko V2 te rōrahi o te konutai thiosulfate i pau i te whakamātautau pātea, mL; Ko te 49.03 te dichromium e rite ana ki te 1 mol o te konutai thiosulfate. Te papatipu o te waikawa pāhare pāporo, g.
I muri i te whakatikatika, taapirihia he iti o te Na2CO3 hei aukati i te pirau moroiti.
(2) NaOH otinga paerewa (0.1mol/L, wa mana: 1 marama)
Te Whakaritenga: Kia paunatia te 4.0 karamu o te NaOH parakore hei tātari ki roto i te ipurau, ka tapirihia te 100mL o te wai makuku kia memeha, katahi ka whakawhitia ki te ipu 1L, tapirihia te wai maturu ki te tohu, ka waiho mo te 7-10 ra kia whakatikahia.
Whakariteritea: Whakanohoia te 0.6~0.8g o te parakore pāhare pāporo hauwai phthalate (tika ki te 0.0001g) ka whakamarokehia ki te 120°C ki roto i te ipu Erlenmeyer 250mL, tāpirihia te 75mL o te wai māturu kia memeha, katahi ka tapirihia te 2~3 pata o te tohu phenolphthalein 1%. Whakatairitetia ki te titant. Whakakorikorihia te wairewa konutai waihā kua oti te whakarite ki runga kia paku whero, ka kore te tae e memeha i roto i te 30 hēkona hei pito mutunga. Tuhia te rōrahi o te konutai waihā. Ko te tukanga whakatikatika ka tukuna kia 2 ki te 3 nga wa ka tangohia te uara toharite. A ka mahi i tetahi whakamatautau kore.
Ko te kukū o te wairewa konutai waihā ka tātaihia e whai ake nei:
I roto i te tātai, ko C te kukū o te wairewa konutai waihā, mol/L; Ko te M te papatipu o te pāhare pāporo hauwai phthalate, G; V1 – te rōrahi o te konutai waihā kua pau, mL; Ko te V2 te tohu i te konutai waihā i pau i te whakamātautau pātea Rōrahi, mL; Ko te 204.2 te papatipu molar o te pāhare pāporo hauwai phthalate, g/mol.
(3) Waikawa sulfuric acid (1+9) (wa mana: 1 marama)
I te wa e korikori ana, me ata tapirihia te 100 mL o te waikawa pungatara puri ki te 900 mL o te wai maturu, ka ata tapiri i te wa e korikori ana.
(4) Waikawa sulfuric acid (1+16.5) (wa mana: 2 marama)
I te wa e whakakorikori ana, me ata tapirihia te 100 mL o te waikawa pungatara puri ki te 1650 mL o te wai maturu ka ata tapiri. Oho i a koe e haere ana.
(5) Tohu māngaro (1%, wā whaimana: 30 rā)
Paunatia te 1.0g o te māngaro wairewa, tāpirihia te 10mL o te wai, whakaohokia ka ringihia ki te 100mL o te wai kohua, kohuatia mo te 2 meneti, ka tu, ka tango i te supernatant hei whakamahi i muri mai.
(6) Tohu māngaro
Tangohia te 5 mL o te wairewa tohu maaka 1% kua oti te whakarite ka waimeha ki te wai ki te 10 mL kia whiwhi ai te tohu maaka 0.5%.
(7) 30% otinga chromium trioxide (wa whai mana: 1 marama)
Paunatia te 60 karamu o te chromium trioxide ka rewa ki te 140mL o te wai-kore-wao.
(8) Te otinga konupora acetate (100g/L, whai mana mo te 2 marama)
Whakarewahia te 10 g o te konupora konupora acetate granules i roto i te 100 mL o te otinga o te 90 mL o te waikawa acetate hukapapa me te 10 mL o te anhydride ahetiki.
(9) 25% otinga konutai acetate (220g/L, wa whaimana: 2 marama)
Whakarewahia te 220g konutai konutai acetate ki roto i te wai ka waimeha ki te 1000mL.
(10) Waikawa pūmāota (1:1, wā whaimana: 2 marama)
Whakaranuhia te waikawa pūmāota me te wai i roto i te ōwehenga rōrahi 1:1.
(11) Acetate buffer (pH=3.5, wa mana: 2 marama)
Whakarewahia te 60mL o te waikawa ahetiki ki roto i te 500mL o te wai, katahi ka tapirihia te 100mL o te haukinia waikawa ka waimeha ki te 1000mL.
(12) Te wairewa whakareri pakawa mata
Whakarewahia te 159.8 mg pākawa mata i roto i te 100 mL wai kei roto 1 mL waikawa nitric (kiato 1.42 g/cm3), waimeha ki te 1000 mL wai, ka uru pai. Ka pai te whakatika. Me whakarite te otinga me te rongoa i roto i te karaihe mata-kore.
(13) Arataki otinga paerewa (wa whai mana: 2 marama)
Me tika te ine i te 10mL o te wairewa whakareri pakawa mata me te taapiri i te wai kia waimeha ki te 100mL.
(14) 2% wairewa hydroxylamine hydrochloride (wa whai mana: 1 marama)
Whakarewahia te 2g o te hydroxylamine hydrochloride ki te 98mL o te wai.
(15) Ammonia (5mol/L, whai mana mo te 2 marama)
Whakarewahia te 175.25g wai haukini ka waimeha ki te 1000mL.
(16) Wai whakaranu (mana: 2 marama)
Whakaranuhia te 100mL o te glycerol, te 75mL o te otinga NaOH (1mol/L) me te 25mL o te wai.
(17) Te otinga Thioacetamide (4%, whai mana mo te 2 marama)
Whakarewahia te 4g o te tioacetamide ki te 96 karae o te wai.
(18) Phenanthroline (0.1%, wa whaimana: 1 marama)
Whakarewahia te 0.1g o te phenanthroline ki te 100mL wai.
(19) pūhaumāota pūhaumāota waikawa (wā whai mana: 1 marama)
Whakarewahia te 20 karamu o te pūhaumāota pūhaumāota ki te 50mL o te waikawa pūhaumāota.
(20) Te wairewa parepare paerewa konupora hydrogen phthalate (pH 4.0, wa whaimana: 2 marama)
Me pauna tika te 10.12g o te pāhare pāporo hauwai phthalate (KHC8H4O4) ka whakamaroke ki te (115±5) ℃ mo te 2 ki te 3 haora. Waimeha ki te 1000mL ki te wai.
(21) Te otinga parepare paerewa Phosphate (pH 6.8, wa whaimana: 2 marama)
Kia tika te pauna 3.533g anhydrous disodium hydrogen phosphate me te 3.387g pāhare pāporo dihydrogen phosphate kua whakamarokehia i te (115±5)°C mo te 2~3 haora, ka waimeha ki te 1000mL ki te wai.
3. Te whakatau i te ihirangi roopu hydroxypropylmethylcellulose
(1) Te whakatau i te ihirangi methoxyl
Ko te whakatau i te ihirangi o te roopu methoxy i runga i te whakamatautau kei roto nga roopu methoxy. Ka pirau te waikawa waiiodic i runga i te whakamahana ki te whakaputa i te methyl iodide (kohua 42.5°C). Ko te Methyl iodide i whakamarohia ki te hauota i roto i te otinga tauhohenga whaiaro. I muri i te horoinga ki te tango i nga matū pokanoa (HI, I2 me H2S), ka ngohia te kohu methyl iodide e te wairewa waikawa acetate o te konupora konupora kei roto Br2 hei hanga IBr, ka waikurahia ki te waikawa iodic. I muri i te whakamaaramatanga, ka tukuna nga ihirangi o te kaiwhiwhi ki te pounamu iodine me te waimeha ki te wai. Whai muri i te taapiri i te waikawa puka hei tango i te taikaha o te Br2, ka taapirihia te KI me te H2SO4. Ka taea te tatau te ihirangi methoxyl ma te titrating 12 ki te otinga Na2S2O3. Ka taea te whakaatu i te whārite tauhohenga e whai ake nei.
Ko te taputapu ine ihirangi methoxyl e whakaatuhia ana i te Whakaahua 7-6.
I roto i te 7-6(a), he ipu a tawhio noa 50mL e hono ana ki te catheter. He ngongo hau totika E kua whakanoho poutū ki te kaki pounamu, tata ki te 25cm te roa me te 9mm te diameter o roto. Ko te pito o runga o te ngongo ka piko ki roto i te ngongo kapi karāhe e 2 mm te diameter o roto me te putanga anga whakararo. Ko te ahua 7-6(b) e whakaatu ana i te taputapu kua pai ake. Ko te Whakaahua 1 e whakaatu ana i te ipu tauhohenga, he ipu porowhita-raro 50mL, me te ngongo hauota kei te taha maui. Ko te 2 te ngongo condenser poutū; Ko te 3 te kirikiri, he wai horoi kei roto; Ko te 4 te ngongo ngongo. Ko te rereketanga nui i waenga i tenei taputapu me te tikanga Pharmacopoeia ko te whakakotahi i nga kaihoroi e rua o te tikanga Pharmacopoeia ki te kotahi, ka taea te whakaiti i te ngaronga o te wai whakauru whakamutunga. I tua atu, he rereke ano te wai horoi i roto i te kirikiri i te tikanga pharmacopoeia. He wai makuku, i te mea ko te taputapu kua pai ake ko te ranunga o te otinga cadmium sulfate me te otinga konutai thiosulfate, he maamaa ake te tango i nga poke i roto i te hau.
Pipeto taputapu: 5mL (5 pihi), 10mL (1 pihi); Puta: 50mL; Te pounamu rōrahi Iodine: 250mL; Taurite tātari.
Reagent phenol (na te mea he totoka, ka rewa i mua i te whangai); hauota hauota ranei; waikawa hauwai (45%); kōeke tātari; otinga pāhare pāporo acetate (100g/L); bromine: kōeke tātari; waikawa formic: kōeke tātari; 25% Te otinga konutai acetate (220g/L); KI: kōeke tātari; waimeha waikawa pungatara (1+9); konutai thiosulfate otinga paerewa (0.1mol/L); tohu phenolphthalein; 1% wairewa waihā; tohu māngaro: 0.5% Wairewa wai māngaro; waimeha waikawa pungatara (1+16.5); 30% chromium trioxide otinga; wai-kore-wao: taapirihia te 10mL o te waikawa pungatara waimeha (1+16.5) ki te 100mL o te wai, whakamahana ki te koropupu, me te tapiri 0.1ml o te 0.02mol/L waikawa permanganic Titer konupora, kohuatia mo te 10 meneti, me noho mawhero; 0.02mol/L konutai konutai titrant: Whakatairitea te 0.1mol/L konutai waikawa titrant kia rite ki te tikanga Hainamana Pharmacopoeia Appendix, me te waimeha tika ki te 0.02mol ki te wai kohuatia, ka whakamataohia te wai maturu /L.
Tāpirihia te 10mL o te wai horoi ki roto i te ngongo horoi, tāpirihia te 31mL o te wai whakauru hou ki roto i te ngongo whakauru, whakauruhia te taputapu, paunatia te 0.05g o te tauira maroke kua whakamarokehia ki te taumaha tonu i te 105°C (tika ki te 0.0001). g), tāpirihia te tauhohenga i te ℃ I roto i te pounamu, tāpirihia te 5 mL o te hydroiodide. Hohoro te hono i te pounamu tauhohenga ki te kaitahuri whakaora (makuku te tauranga huri ki te waikawa hydriodic), ka pupuhi hauota ki roto i te tank i te tere o te 1 ki te 2 mirumiru ia hekona.
Wā tuku: Feb-01-2024