1. Usoro njirimara nke hydroxypropyl methylcellulose
(1) Were 1.0g nke ihe atụ, kpoo 100mL mmiri (80 ~ 90 ℃), nwuo na-aga n'ihu, ma dị jụụ na ice bat ruo mgbe ọ ghọrọ mmiri mmiri viscous; tinye 2mL nke mmiri mmiri n'ime tube ule, ma jiri nwayọọ nwayọọ tinye 1mL nke 0.035% anthrone sulfuric acid n'akụkụ ngwọta tube mgbidi wee hapụ ya maka nkeji ise. Mgbanaka akwụkwọ ndụ akwụkwọ ndụ na-egosi na ihu n'etiti mmiri mmiri abụọ ahụ.
(2) Were ọnụ ọgụgụ kwesịrị ekwesị nke imi eji eme nchọpụta na (I) n'elu ma wụsa ya na efere iko. Ka mmiri na-ekupụ, ihe nkiri ductile na-etolite.
2. Nkwadebe nke hydroxypropyl methylcellulose analysis ọkọlọtọ ngwọta
(1) Sodium thiosulfate ọkọlọtọ ngwọta (0.1mol/L, nkwado oge: 1 ọnwa)
Nkwadebe: sie ihe dị ka 1500ml mmiri distilled, dị jụụ ma wepụ ya. Na-atụ 25g sodium thiosulfate (ihe dị arọ ya bụ 248.17, gbalịa ka ọ bụrụ ihe ziri ezi dị ka 24.817g mgbe ị na-atụ aro) ma ọ bụ 16g sodium thiosulfate anhydrous, gbazee ya na 200ml nke mmiri jụrụ oyi n'elu, gbanye na 1L, tinye ya na karama aja aja, na dobe Chekwaa n'ebe gbara ọchịchịrị, yochaa ma wepụta ya mgbe izu abụọ gachara.
Nhazi: tụọ 0.15g nke ntụnyere potassium dichromate na akpọọ nkụ na ịdị arọ mgbe niile, ziri ezi na 0.0002g. Tinye 2g potassium iodide na 20ml sulfuric acid (1+9), maa jijiji nke ọma, tinyekwa n'ọchịchịrị maka nkeji 10. Tinye 150mL mmiri na 3ml 0.5% starch egosi ngwọta, na titrate na 0.1mol/L sodium thiosulfate ngwọta. Ihe ngwọta na-agbanwe site na-acha anụnụ anụnụ gaa na-acha anụnụ anụnụ. Na-atụgharị akwụkwọ ndụ akwụkwọ ndụ na-egbuke egbuke na njedebe njedebe. Enweghị chromate potassium agbakwunyere na nnwale efu. A na-emeghachi usoro nhazi ahụ ugboro 2 ruo 3 ma were nkezi uru.
A na-agbakọ mkpokọta molar C (mol / L) nke sodium thiosulfate ọkọlọtọ ngwọta dị ka usoro a:
Na usoro, M bụ oke nke potassium dichromate; V1 bụ olu sodium thiosulfate eri, mL; V2 bụ olu sodium thiosulfate riri na nnwale efu, mL; 49.03 bụ dichromium dakọtara na 1 mol nke sodium thiosulfate. Ngwunye potassium acid, g.
Mgbe nhazichara, tinye obere ego nke Na2CO3 iji gbochie ire ere microbial.
(2) Ngwọta ọkọlọtọ NaOH (0.1mol/L, oge nkwado: 1 ọnwa)
Nkwadebe: tụọ ihe dị ka 4.0g nke NaOH dị ọcha maka nyocha n'ime beaker, gbakwunye 100mL nke mmiri mmiri na-agbaze ka ọ gbazee, wee nyefee ya na 1L volumetric flask, tinye mmiri na-ekpo ọkụ na akara ahụ, ma hapụ ya maka ụbọchị 7-10 ruo mgbe nhazi.
Nhazi: Ebe 0.6 ~ 0.8g nke potassium hydrogen phthalate dị ọcha (zie ezie na 0.0001g) nke a mịrị amị na 120 ° C n'ime 250mL Erlenmeyer flask, tinye 75mL nke mmiri distilled ka ọ gbazee, wee tinye 2 ~ 3 tụlee nke 1% phenolphthalein. Titrate na titrant. Kpoo ngwọta sodium hydroxide nke a kwadebere n'elu ruo mgbe ọ dị ntakịrị na-acha uhie uhie, na agba anaghị ada n'ime 30 sekọnd dị ka njedebe. Dee olu sodium hydroxide. A na-emeghachi usoro nhazi ahụ ugboro 2 ruo 3 ma were nkezi uru. Ma mee nnwale efu.
A na-agbakọ mkpokọta sodium hydroxide ngwọta dị ka ndị a:
N'ime usoro ahụ, C bụ ntinye nke ngwọta sodium hydroxide, mol / L; M na-anọchi anya oke potassium hydrogen phthalate, G; V1 - olu sodium hydroxide riri, ml; V2 na-anọchi anya sodium hydroxide riri na nnwale efu, ML; 204.2 bụ molar mass nke potassium hydrogen phthalate, g/mol.
(3) Ghichaa sulfuric acid (1+9) (oge ọ dị irè: otu ọnwa)
Mgbe ị na-akpali akpali, jiri nlezianya tinye 100 ml nke sulfuric acid na-etinye uche na 900 ml nke mmiri distilled ma tinye nwayọọ nwayọọ ka ị na-akpali.
(4) Ghichaa sulfuric acid (1 + 16.5) (oge nkwado: ọnwa 2)
Mgbe ị na-akpali akpali, jiri nlezianya tinye 100 ml nke sulfuric acid gbadoro ụkwụ na 1650 ml nke mmiri distilled wee gbakwunye nwayọọ nwayọọ. Kwuo ka ị na-aga.
(5) Ihe ngosi starch (1%, oge nkwado: ụbọchị 30)
Were 1.0g nke starch soluble, tinye 10ml mmiri, kpalie ma wụsa n'ime 100ml nke mmiri esi, sie maka nkeji 2, hapụ ya ka ọ guzoro, were supernatant were mee ya.
(6) Ihe ngosi starch
Were 5 ml nke ihe ngosi 1% starch a kwadebere ma gbanye ya na mmiri ruo 10 ml iji nweta 0.5% starch egosi.
(7) 30% chromium trioxide ngwọta (oge nkwado: 1 ọnwa)
Were 60g nke chromium trioxide wee gbarie ya na 140ml nke mmiri na-enweghị organic.
(8) Potassium acetate ngwọta (100g / L, dị irè maka ọnwa 2)
Igbari 10 g nke anhydrous potassium acetate granules na 100 ml nke ngwọta nke 90 ml nke glacial acetic acid na 10 ml nke acetic anhydride.
(9) 25% sodium acetate ngwọta (220g/L, oge nkwado: ọnwa 2)
Gbari 220g anhydrous sodium acetate n'ime mmiri wee tụgharịa ruo 1000ml.
(10) Hydrochloric acid (1:1, oge nkwado: ọnwa 2)
Gwakọta hydrochloric acid na mmiri na oke 1: 1.
(11) Acetate buffer (pH=3.5, oge nkwado: ọnwa 2)
Gbarie 60ml nke acetic acid n'ime 500ml mmiri wee gbakwunye 100ml nke ammonium hydroxide wee gbasaa na 1000ml.
(12) Ngwọta nkwadebe nitrate ndu
Gbarie 159.8 mg nitrate lead na 100 ml mmiri nwere 1 ml nitric acid (njupụta 1.42 g/cm3), gbanye na mmiri 1000 ml, wee gwakọta nke ọma. Idozi nke ọma. Ekwesịrị ịkwadebe ngwọta ma chekwaa ya na iko na-enweghị ndu.
(13) Ngwọta ọkọlọtọ ndu (oge nkwado: ọnwa 2)
Gwakọta 10 ml nke ngwọta nitrate ntụ ntụ ma gbakwunye mmiri ka ọ gbasaa na 100ml.
(14) 2% hydroxylamine hydrochloride ngwọta (oge nkwado: 1 ọnwa)
Gbarie 2g hydroxylamine hydrochloride na 98ml mmiri.
(15) Amonia (5mol/L, dị irè maka ọnwa 2)
Igbari 175.25g amonia mmiri na itughari ka 1000ml.
(16) Mmiri mmiri agwakọta (nke ọma: ọnwa 2)
Gwakọta 100ml nke glycerol, 75mL nke NaOH ngwọta (1mol/L) na 25ml mmiri.
(17) Ihe ngwọta Thioacetamide (4%, dị irè maka ọnwa 2)
Gbarie 4g nke thioacetamide na 96g mmiri.
(18) Phenanthroline (0.1%, oge nkwado: 1 ọnwa)
Igbari 0.1g nke phenanthroline na 100ml mmiri.
(19) Acidic chloride stannous (oge dị irè: 1 ọnwa)
Igbari 20g nke stannous chloride na 50mL nke concentrated hydrochloric acid.
(20) Potassium hydrogen phthalate ọkọlọtọ ọkọlọtọ ngwọta (pH 4.0, nkwado oge: 2 ọnwa)
Were nha nke ọma 10.12g nke potassium hydrogen phthalate (KHC8H4O4) wee kpoo ya na (115±5)℃ maka awa 2 ruo 3. Wunye 1000 ml na mmiri.
(21) Ngwọta nchekwa ọkọlọtọ phosphate (pH 6.8, oge nkwado: ọnwa 2)
Were nha nke ọma 3.533g disodium anhydrous disodium hydrogen phosphate na 3.387g potassium dihydrogen phosphate akpọnwụwo na (115±5) Celsius C maka awa 2 ~ 3, wee jiri mmiri gbanye 1000mL.
3. Mkpebi nke ọdịnaya otu hydroxypropylmethylcellulose
(1) Mkpebi nke ọdịnaya metoxyl
Mkpebi nke ọdịnaya otu methoxy dabere na ule nwere otu methoxy. Hydroiodic acid na-emebi ma kpo oku wee mepụta methyl iodide na-agbanwe agbanwe (ebe isi 42.5°C). Methyl iodide gbajiri na nitrogen na ngwọta nke na-emeghachi onwe ya. Mgbe ịsachara iji wepụ ihe ndị na-etinye aka (HI, I2 na H2S), vapor methyl iodide na-etinye uche na ngwọta acetic acid nke potassium acetate nke nwere Br2 iji mepụta IBr, bụ nke a na-emezi oxidized na iodic acid. Mgbe distillation gasịrị, a na-ebufe ọdịnaya nke onye na-anabata ya na karama ayodiin ma gbanye ya na mmiri. Ka ịgbakwunye formic acid iji wepụ ngafe Br2, KI na H2SO4 na-agbakwunye. Enwere ike gbakọọ ọdịnaya methoxyl site na titrating 12 na ngwọta Na2S2O3. Enwere ike igosipụta nha mmeghachi omume dịka ndị a.
Egosiri ngwaọrụ elele ọdịnaya methoxyl na eserese 7-6.
Na 7-6 (a), A bụ flask 50mL gbara gburugburu jikọtara ya na catheter. Enwere tube condensation kwụ ọtọ E etinyere n'okirikiri, ihe dịka 25cm n'ogologo na dayameta dị n'ime 9mm. A na-ehulata nsọtụ elu nke tube n'ime iko capillary tube nke nwere dayameta dị n'ime nke 2 mm na ntinye chere ihu ala. Ọgụgụ 7-6(b) na-egosi ngwaọrụ emelitere. Ọgụgụ 1 na-egosi flask mmeghachi omume, nke bụ flask 50mL gbara gburugburu, nwere tube nitrogen n'aka ekpe. 2 bụ tube condenser kwụ ọtọ; 3 bụ scrubber, nwere mmiri ịsacha; 4 bụ tube absorption. Nnukwu ihe dị iche n'etiti ngwaọrụ a na usoro Pharmacopoeia bụ na a na-ejikọta ihe abụọ nke usoro Pharmacopoeia n'ime otu, nke nwere ike ibelata nkwụsị nke mmiri mmiri mmiri ikpeazụ. Tụkwasị na nke ahụ, mmiri mmiri ịsacha na scrubber dịkwa iche na usoro pharmacopoeia. Ọ bụ mmiri na-ekpo ọkụ, ebe ngwaọrụ a na-emeziwanye bụ ngwakọta nke cadmium sulfate solution na sodium thiosulfate ngwọta, nke dị mfe ịnweta adịghị ọcha na gas distilled.
Pipette ngwá ọrụ: 5ml (5 iberibe), 10ml (1 ibe); mmiri ara ehi: 50ml; Kalama olu ayodiin: 250ml; Ntụle nyocha.
Reagent phenol (n'ihi na ọ bụ ihe siri ike, ọ ga-agbaze tupu nri); nitrogen ma ọ bụ carbon dioxide; hydroiodic acid (45%); akara nyocha; potassium acetate ngwọta (100 g / l); bromine: ọkwa nyocha; formic acid: ọkwa nyocha; 25% sodium acetate ngwọta (220g / L); KI: ọkwa nyocha; itughari sulfuric acid (1 + 9); sodium thiosulfate ọkọlọtọ ngwọta (0.1mol / L); ihe ngosi phenolphthalein; 1% ethanol ngwọta; starch egosi: 0,5% Starch aqueous ngwọta; itughari sulfuric acid (1 + 16.5); 30% chromium trioxide ngwọta; mmiri na-adịghị organic: tinye 10mL nke itughari sulfuric acid (1+16.5) na 100ml mmiri, okpomọkụ ka esi, na tinye 0.1ml nke 0.02mol/L permanganic acid Potassium titer, obụpde maka nkeji 10, ga-anọgide na-acha odo odo; 0.02mol/L sodium hydroxide titrant: Gbakọọ 0.1mol/L sodium hydroxide titrant dị ka Chinese Pharmacopoeia Appendix usoro, ma gbarie nke ọma na 0.02mol na sie na mma distilled mmiri / L.
Tinye ihe dị ka 10mL nke mmiri ịsa ahụ n'ime tube ịsa ahụ, tinye 31mL nke mmiri mmiri a kwadebere ọhụrụ n'ime tube absorption, wụnye ngwa ahụ, tụọ ihe dị ka 0.05g nke ihe nlele a mịrị amị nke akpọnwụwo na ịdị arọ mgbe niile na 105 ° C (nke ziri ezi na 0.0001). g), gbakwunye mmeghachi omume na ℃ Na karama, tinye 5 ml nke hydroiodide. Ngwa ngwa jikọọ karama mmeghachi omume na condenser mgbake (mee ka mmiri mmiri na-egweri na mmiri mmiri na-egweri), ma gbanye nitrogen n'ime tank ahụ na ọnụego 1 ruo 2 afụ kwa nkeji.
Oge nzipu: Feb-01-2024