1, te tautuhi i te tikanga hydroxypropyl methyl cellulose
(1) Tangohia te 1.0g o te tauira, te wai whakamahana (80~90 ℃) 100mL, te whakaoho tonu, ka whakamatao ki roto i te wai kirikiri i roto i te pati hukapapa; Kuhua te 2mL o te wai ki roto i te ipuipu, me ata taapirihia he wairewa waikawa pungatara 1mL o te koroni 0.035% ki te taha o te pakitara ngongo, ka waiho mo te 5 meneti. Ka puta te mowhiti matomato ki te atanga i waenganui i nga wai e rua.
(2) Tangohia te nui e tika ana o te parapara kua whakahuahia ake nei hei tohu mo te (ⅰ) ka riringi ki runga i te pereti karaihe. I muri i te mimiti o te wai, ka hanga he kiriata ngongo.
2, hydroxypropyl methyl cellulose tātaritanga o te whakaritenga otinga paerewa
(1) Te otinga paerewa konutai thiosulfate (0.1mol/L, whaimana: kotahi marama)
Te Whakaritenga: Kohuatia te 1500mL wai matutu ka whakamatao kia rite ki te whakamahi. Paunatia te 25g konutai thiosulfate (ko tona taumaha irapoi ko te 248.17, ka ngana kia tika ki te 24.817g ina paunatia) 16g ranei te konutai thiosulfate anhydrous, memeha ki te 200mL o te wai whakamatao o runga ake nei, waimeha ki te 1L, ka waiho ki te 1L. pounamu, hoatu te pounamu ki te pouri, ka tātarihia kia whakamahia i muri i nga wiki e rua.
Whakatauritenga: Paunatia te 0.15g o te tohutoro pāhare pāporo dichromate i tunua ki te taumaha tonu, tika ki te 0.0002g. Tāpirihia te 2g pāhare pāporo iodide me te 20mL waikawa pungatara (1+9), ruru pai, waiho i roto i te pouri mo te 10min, tāpiri 150mL wai me te 3ml 0.5% wairewa tohu māngaro, titrate ki te otinga konutai thiosulfate 0.1mol/L, ka huri te otinga mai i te puru. ki te kakariki kanapa i te pito mutunga. Karekau te konukawata konukawata i tapirihia ki te whakamatautau kore. Ko te tukanga whakatikatika i tukuna e 2 ~ 3 nga wa ka tangohia te uara toharite.
Ko te kukū molar C (mol/L) o te konutai thiosulfate otinga paerewa i tatauhia penei:
Ko te M ko 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 whakamātau pātea, mL; Ko te 49.03 te papatipu o te pāhare pāporo dichromate e rite ana ki te 1mol o te konutai thiosulfate, g.
Whai muri i te whakatikatika, taapirihia he Na2CO3 iti hei aukati i te pirau moroiti.
(2) NaOH otinga paerewa (0.1mol/L, whaimana: kotahi marama)
Te Whakaritenga: Tata ki te 4.0g o te NaOH parakore mo te wetewete i paunatia ki roto i te ipurau, ka tapirihia te 100mL wai maturu kia memeha, katahi ka whakawhitia ki te ipu 1L volumetric, ka tapirihia te wai maturu ki te pauna, ka waiho mo te 7-10 ra tae noa ki te whakatikatika.
Whakariteritea: Kuhua te 0.6~0.8g o te konupora hauwai phthalate parakore kua whakamarokehia ki te 120 ℃ (tika ki te 0.0001g) ki roto i te ipu koeko 250mL, tāpirihia te 75mL wai māturu kia memeha, katahi ka tapirihia kia 2~3 pata o te 1% phenolphthalein tohu, titrate. ko te wairewa konutai waikawa i runga ake nei kia paku whero, a ko te mutunga ko te tae kaore e memeha i roto i te 30S. Tuhia te rōrahi o te konutai waihā. Ko te tukanga whakatikatika i tukuna e 2 ~ 3 nga wa ka tangohia te uara toharite. A ka mahi i tetahi whakamatautau kore.
Ko te kukū o te wairewa konutai waihā i tātai penei:
Ina, ko C te kukū o te wairewa konutai waihā, mol/L; Ko te M te papatipu o te pāhare pāporo hauwai phthalate, G; Ko V1 te rōrahi o te konutai waihā i pau, mL; Ko te V2 e tohu ana i te rōrahi o te konutai waihā i pau i te whakamātautau pātea, mL; Ko te 204.2 te papatipu molar o te pāhare pāporo hauwai phthalate, g mo ia kamiriona.
(3) Dilute waikawa pungatara (1+9) (Mana: 1 marama)
I raro i te whakakorikoritanga, me ata tapirihia te 100mL waikawa pungatara mau ki te 900mL wai maturu, me ata toha, i te whakaohooho.
(4) Waikawa sulfuric acid (1+16.5) (Whaimana: 2 marama)
I raro i te whakakorikoritanga, me ata tapirihia te 100mL o te waikawa pungatara kawa ki te 1650mL o te wai makuku, me te ata taapiri. Oho i a koe e haere ana.
(5) Tohu māngaro (1%, whaimana: 30 ra)
Paunatia te 1.0g māngaro wairewa, tāpirihia te 10mL wai, whakaohokia ka werohia ki roto ki te 100mL wai kohua, kohuatia paku mo te 2 meneti, tuu, ka tango i te supernatant hei whakamahi.
(6) Tohu māngaro
0.5% te tohu māngaro i whiwhi mā te tango i te 5mL o te wairewa tohu māngaro 1% kua oti te whakarite me te waimeha ki te 10mL ki te wai.
(7) 30% chromium trioxide otinga (mana: 1 marama)
Paunatia te 60 karamu o te chromium trioxide ka rewa ki roto i te 140mL wai karekau he mea pararopi.
(8) Te otinga konupora acetate (100g/L, whaimana: 2 marama)
10 karamu o te pāhare pāhare pāporo acetate karekau i rewa ki te wairewa 100mL o te 90mL waikawa ahetiki hukapapa me te 10mL anhydride acetic.
(9) 25% otinga konutai acetate (220g/L, whaimana: 2 marama)
Whakarewahia te 220g o te konutai konutai acetate ki roto i te wai ka waimeha ki te 1000mL.
(10) Waikawa pūmāota (1:1, whaimana: 2 marama)
Whakaranuhia te waikawa pūhaumāota ki te wai i te ōwehenga rōrahi 1:1.
(11) Ko te otinga parepare acetate (pH=3.5, whaimana: 2 marama)
Whakarewahia te 60mL waikawa ahetiki ki roto i te 500mL wai, katahi ka tapirihia te 100mL haukinia waikawa ka waimeha ki te 1000mL.
(12) Te wairewa whakareri pakawa mata
Ko te 159.8mg o te pākawa mata i whakarewahia ki te 100mL wai kei roto te 1mL o te waikawa nitric (kiato 1.42g/cm3), i whakahiatotia ki te 1000mL wai ka uru pai. Ko te whakarite me te rokiroki o tenei otinga ka mahia i roto i te karaihe mata-kore.
(13) Te otinga arataki paerewa (mana: 2 marama)
Ko te inenga tika o te 10mL o te wairewa takatika pakawa mata i waimeha ki te wai 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) Hamoni (5mol/L, whaimana: 2 marama)
Ko te 175.25 karamu o te haukini i memeha ki te wai, ka waimeha ki te 1000mL.
(16) Wai whakaranu (wa whai mana: 2 marama)
Whakaranuhia te 100mL glycerol, 75mLNaOH wairewa (1mol/L), me te 25mL wai.
(17) Te otinga Thioacetamide (4%, whaimana: 2 marama)
4g thioacetamide i rewa ki te 96g wai.
(18) Phenanthroline (0.1%, whaimana: 1 marama)
Whakarewahia te 0.1g o-phenanthroline ki te 100mL wai.
(19) Acid stannous chloride (mana: 1 marama)
Whakarewahia te 20g pūhaumāota pūhaumāota ki te 50mL waikawa pūhaumāota.
(20) Te wairewa parepare paerewa konupora hydrogen phthalate (pH 4.0, whaimana: 2 marama)
10.12g o te pāhare pāporo hauwai phthalate (KHC8H4O4) i tika te pauna me te whakamaroke ki te (115±5) ℃ mo te 2~3h. Waimeha ki te 1000mL ki te wai.
(21) Te otinga parepare paerewa Phosphate (pH 6.8, whaimana: 2 marama)
Ko te 3.533g o te disodium hydrogen phosphate anhydrous me te 3.387g o te pāhare pāporo dihydrogen phosphate i whakamaroke i te (115±5) ℃ mo te 2~3h i ata paunatia ka diluted ki te 1000mL ki te wai.
3, hydroxypropyl methyl cellulose rōpū whakatau ihirangi
(1) Te whakatau i te ihirangi methoxy
Ko te whakatau o te ihirangi methoxy i ahu mai i te pirau o te waikawa hydroiodate na roto i te whakamahana me te whakamatautau kei roto te methoxy hei whakaputa i te methane iodide (kohuatanga 42.5 ° C). Ko te methane iodide ka maturu ki te hauota i roto i te otinga autoreaction. I muri i te horoinga ki te tango i nga matū pokanoa (HI, I2 me H2S), ka ngongo te kohu mewaro iodine e te wairewa waikawa acetate acetate konupora kei roto te Br2 hei hanga IBr katahi ka waikura ki te waikawa iodic. I muri i te whakamarumaru, ka tukuna nga matū o te kaikawe ki nga ipu iodine ka waimeha ki te wai. Whai muri i te taapiri i te waikawa formic hei tango i te taikaha o te Br2, ka taapirihia te KI me te H2SO4. Ka taea te tatau te ihirangi methoxy ma te titrating 12 me te otinga o Na2S2O3. Ka taea te whakaatu i te whārite tauhohenga e whai ake nei.
Ko te taputapu mo te ine i te ihirangi methoxy e whakaatuhia ana i te Whakaahua 7-6.
I roto i te 7-6 (a), ko te A he ipu porotaka-raro 50mL e hono ana ki te catheter. Ko te kaokao pounamu he mea whakakikoruatia ki te ngongo whakawera hau tika E, tata ki te 25cm te roa me te 9mm te whanui o roto. Ka piko te pito o runga o te ngongo ki roto i te ngongo kapi karāhe me te putanga whakararo me te 2mm te diameter o roto. Ko te ahua 7-6 (b) e whakaatu ana i te taputapu kua pai ake. Ko te 1 te ipu tauhohenga, he ipu porowhita-raro 50mL, kei te taha maui te paipa hauota. Ko te 2 te putorino whakamarumaru poutū; Ko te 3 te kirikiri, he wai horoi kei roto; Ko te 4 te ngongo ngongo. Ko te rereketanga nui i waenga i te 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 mate o te otinga whakaurunga whakamutunga. I tua atu, he rereke ano te wai horoi i roto i te scrubber mai i te tikanga pharmacopoeia, he wai makuku, a, ko te taputapu pai ake ko te ranunga o te otinga cadmium sulfate me te otinga konutai thiosulfate, ka ngawari ake te whakauru i nga poke i roto i te hau.
Pipito taputapu: 5mL (5), 10mL (1); Puta: 50mL; Te pounamu ine iodine: 250mL; Tātarihia te toenga.
Reagent phenol (na te mea he totoka, no reira ka whakakotahi i mua i te whangai); Te hauota hauota ranei; Waikawa waiora (45%); Tātaritanga o parakore; Te otinga konupora acetate (100g/L); Bromine: parakore te tātari; Waikawa Formic: parakore te tātari; 25% otinga konutai acetate (220g/L); KI: purea tātari; Waiwai sulfuric acid (1+9); Wairewa paerewa konutai thiosulfate (0.1mol/L); Tohu Phenolphthalein; 1% wairewa waihā; Tohu māngaro: 0.5% māngaro i roto i te wai; Waimeha waikawa pungatara (1+16.5); 30% chromium trioxide otinga; Te wai-kore-a-waa: taapirihia te 10mL waikawa pungatara (1+16.5) ki te 100mL wai, whakamahana ki te koropupu, me te taapiri i te 0.1ml0.02mol /L konupora permanganate titer, kohuatia mo te 10min, me noho mawhero; 0.02mol/L konutai konutai titration otinga: E ai ki te tikanga apitihanga Pharmacopoeia Hainamana, 0.1mol/L konutai wairewa titration wairewa i whakatikaia, ka diluted tika ki te 0.02mol/L ki te wai māturu kohua me te matao.
Taapirihia te 10mL o te wairewa horoi ki roto i te ngongo horoi, taapirihia te 31mL o te wairewa urunga hou kua rite ki roto i te ngongo whakauru, whakauruhia te taputapu, te taumaha ki te 0.05g (tika ki te 0.0001g) o te tauira maroke kua whakamarokehia ki te taumaha tonu i te 105 ℃ ki roto i te ipu tauhohenga, ka tāpirihia te 5mL hydroiodate. Ka tere te hono o te pounamu tauhohenga ki te condenser whakaora (ka makuku te waha huri ki te hydroiodate), ka panaia te hauota ki roto i te tank i te tere o te 1~2 mirumiru ia rua. Ka āta whakahaeretia te pāmahana kia piki ake te mamaoa o te wē koropupū ki te haurua o te teitei o te condenser. Ko te wa tauhohenga ka whakawhirinaki ki te ahua o te tauira, i waenga i te 45min me te 3h. Tango i te ngongo ngongo ka ata whakawhitia te wairewa ngongo ki roto i te ipu iodine 500mL kei roto te 10ml o te 25% te wairewa konutai acetate tae noa ki te 125mL.
I raro i te wiriwiri tonu, me ata taapirihia te waikawa maatai ia topata kia ngaro ra ano te kowhai. Tāpirihia he maturuturu o te tohu 0.1% methyl red, a kaore te tae whero e ngaro mo te 5 meneti. Kātahi ka tāpirihia kia toru ngā pata o te waikawa formic. Me noho mo te wa poto, katahi ka tapirihia te 1 karamu o te pāhare pāporo iodide me te 5mL o te waikawa pungatara waimeha (1+9). I titrated te otinga ki te 0.1mol/L konutai thiosulfate otinga paerewa, me te 3~4 pata o 0.5% tohu māngaro i tāpirihia tata ki te pito mutunga, a ka haere tonu te titration tae noa ki ngaro te tae kahurangi.
I te ahua ano, i mahia he whakamatautau kore.
Te tatauranga o te ihirangi methoxide katoa:
Ina, ko te V1 te tohu o te rōrahi (mL) o te konutai thiosulfate wairewa paerewa e pau ana e nga tauira titration; Ko V2 te rōrahi o te wairewa paerewa konutai thiosulfate i pau i te whakamātau pātea, mL; Ko C te kukū o te konutai thiosulfate otinga paerewa, mol/L; M e tohu ana ki te papatipu o te tauira maroke, g; Ko te 0.00517 he 0.1mol/L konutai thiosulfate mo ia 1ml e rite ana ki te 0.00517g o te methoxy.
Ko te tapeke o nga ihirangi methoxy e tohu ana i te tapeke methoxy me te uara hydroxyproxy o te tatauranga methoxy, no reira me whakatika te tapeke alkoxy e te ihirangi hydroxyproxy ka puta ki te whiwhi i te ihirangi methoxy tika. KO TE KAUPAPA HYDROXYPROPOXY TUATAHI ME WHAKATIKA MO TE PROPENE I TE WHAKAMAHI A TE HI ME TE HYDROXYPROPYL ME TE KAUPAPA K=0.93 (KO TE TINO O TE TAHI NUI O NGA TAUIRA I WHAKATAURANGA E TE WHAKAMAHI MORGAN). Na reira:
Ko te ihirangi methoxy kua whakatika = te katoa o nga ihirangi methoxy – (hydroxypropoxy content ×0.93×31/75)
Ko nga nama 31 me te 75 ko nga papatipu molar o nga roopu methoxy me te hydroxypropoxy.
(2) Te whakatau i te ihirangi hydroxypropoxy
Ko te roopu hydropropoxy i roto i te tauira ka tauhohe ki te chromium trioxide ki te whakaputa waikawa acetic. Whai muri i te whakamaroketanga mai i te otinga autoreaction, ka whakatauhia te ihirangi o te waikawa chromic ma te titration me te otinga NaOH. No te mea he iti te waikawa chromic ka puta mai i roto i te tukanga whakamarumaru, ka pau ano te otinga NaOH, na reira me whakatau ano te ihirangi o tenei waikawa chromic ma te iodimetry me te tango mai i te tatauranga. Ko te whārite tauhohenga ko:
Nga taputapu me nga reagents He huinga taputapu katoa mo te whakatau i nga roopu hydroxypropoxy; Pounamu Volumetric: 1L, 500mL; Puta ine: 50mL; Pipeto: 10mL; Te pounamu inenga iodine: 250mL. Burette taketake: 10mL; Wairewa paerewa konutai thiosulfate (0.1mol/L); Waimeha waikawa pungatara (1+16.5); Waiwai sulfuric acid (1+9); Tohu māngaro (0.5%).
Ko te 7-7 he taputapu mo te whakatau i te ihirangi hydroxypropoxy.
I roto i te 7-7 (a), D he 25mL rua-kaki maturu ipu, B he 25mm×150mm ngongo hanga mamaoa, C he ngongo hononga rere, A he kaukau hinu whakawera hiko, E he pou shunt, G he ipu koeko me te mono karaihe, ko te pito o roto ko te 0.25-1.25mm te diameter, ka kuhu ki roto i te ipu whakangao; Ko F he ngongo whakamatao e hono ana ki a E. I roto i te taputapu kua pai ake e whakaatuhia ana i te FIG. 7-7 (b), ko te 1 te reactor, he ipu whakamahana 50mL; Ko te 2 te upoko whakamarumaru; Ko te 3 he korokoro karaihe 50mL hei whakahaere i te tere o te rere o te wai pararopi; 4 he paipa hauota; Ko te 5 te putorino whakamaroke. Ko te tino rerekeetanga i waenga i te taputapu whakarereke me te tikanga rongoako ko te taapiri i te kohanga karaihe hei whakahaere i te tere o te rere o te wai, kia ngawari ai te whakahaere i te tere o te whakamaarama.
Ko nga tikanga whakamatautau i roto i te tauira o te whakamaroke 105 ℃ ki te taumaha tonu ko te 0.1 g (0.0002 g), ka kii tika i roto i te pounamu whakakorikori, taapirihia te 10 ml o te 30% chromium trioxide otinga, te pounamu whakamaroke ki te kapu hinu hinu, te hinu kaukau wai taumata. e rite ana ki te mata wai chromium trioxide, nga taputapu kua whakauruhia, te wai whakamatao tuwhera, te hauota, o to maatau wheketere hei whakahaere i te tere o te hauota mo te kotahi mirumiru ia rua. I roto i te 30min, ka whakawerahia te pati hinu ki te 155 ℃, ka mau tonu ki tenei pāmahana tae noa ki te 50mL te otinga kua kohia. I whakamutua te whakamarumaru hei tango i te pati hinu.
Horoihia te pakitara o roto o te whakamatao ki te wai makuku, whakakotahi i te wai horoi me te whakamarumaru ki roto i te pounamu iodine 500mL, taapirihia nga pata 2 o te tohu tohu phenolphthalide 1%, titrate ki te 0.02mol/L konutai wairewa wairewa ki te uara pH o 6.9~7.1 , ka tuhia te tapeke o te konutai waihā i pau.
Tāpirihia te 0.5g konutai bicarbonate me te 10mL waimeha waikawa pungatara (1+16.5) ki te pounamu iodine ka waiho kia kore rawa e puta te hauhā. Kātahi ka tāpirihia te 1.0g pāhare pāporo iodide, ka piri, ka ruru pai, ka waiho ki te pouri mo te 5 meneti. Kātahi ka tāpirihia te 1mL 0.5% te tohu māngaro ka titrate ki te 0.02mol/L konutai thiosulfate ki te pito mutunga. Tuhia te rōrahi o te konutai thiosulfate i pau.
I tetahi atu whakamätautau patea, i tuhia nga nama o te konutai waiwai me te konutai thiosulfate titrators i pau.
Te tatauranga o te ihirangi hydroxypropoxy:
Kei hea, ko K te pikitia whakarea whakatika o te whakamatautau paratea: Ko V1 te rōrahi o te titration konutai konutai i pau i te tauira, mL. Ko te C1 te kukū o te wairewa paerewa konutai, mol/L; Ko V2 te rōrahi o te titration konutai thiosulfate i pau i te tauira, mL; Ko te C2 te kukū o te otinga paerewa konutai thiosulfate, mol/L; Ko M te papatipu tauira, g; Ko te Va te rōrahi o te titration konutai waihā i pau i te whakamātautau pātea, mL; Ko te Vb te rōrahi o te titration konutai thiosulfate i pau i te whakamātautau pātea, mL.
4. Te whakatau i te makuku
Taurite tātari taputapu (tika ki te 0.1mg); Ine pounamu: diameter 60mm, teitei 30mm; Umu whakamaroke.
Ko te tikanga whakamatautau ka pauna tika i te tauira 2~ 4G (
Te wa tuku: Sep-08-2022