1. Ke ala ʻike o ka hydroxypropyl methylcellulose
(1) E lawe i 1.0g o ka laʻana, e wela 100mL o ka wai (80 ~ 90 ℃), e hoʻoulu mau, a hoʻomaha i loko o ka hau hau a lilo i wai viscous; e hoʻokomo i 2mL o ka wai i loko o kahi paipu hoʻāʻo, a hoʻohui mālie i 1mL o 0.035% anthrone sulfuric acid ma ka hopena o ka paia paipu a waiho no 5 mau minuke. Hōʻike ʻia kahi apo ʻōmaʻomaʻo ma ke kikowaena ma waena o nā wai ʻelua.
(2) E lawe i ka nui kūpono o ka mucus i hoʻohana ʻia no ka ʻike ma (I) ma luna a ninini ma luna o ka pā aniani. Ke hoʻoheheʻe ʻia ka wai, hana ʻia kahi kiʻiʻoniʻoni ductile.
2. Hoʻomākaukau i ka hydroxypropyl methylcellulose analysis solution maʻamau
(1) Sodium thiosulfate solution maʻamau (0.1mol/L, manawa kūpono: 1 mahina)
Hoʻomākaukau: E hoʻolapalapa ma kahi o 1500mL wai i hoʻomaʻamaʻa ʻia, hoʻomaʻalili a waiho ʻia. E kaupaona i 25g sodium thiosulfate (ʻo kona kaumaha mole he 248.17, e ho'āʻo e pololei e like me ka 24.817g i ke kaupaona ʻana) a i ʻole 16g anhydrous sodium thiosulfate, e hoʻoheheʻe i loko o 200mL o ka wai hoʻoluʻu ma luna, e hoʻoheheʻe i 1L, waiho i loko o kahi hue ʻeleʻele. a waiho E kūʻai ma kahi pouli, kānana a waiho ʻia ma hope o ʻelua pule.
Hoʻoponopono: E kaupaona i 0.15g o ka potassium dichromate kuhikuhi a e kālua i ke kaumaha mau, pololei i ka 0.0002g. E hoʻohui i 2g potassium iodide a me 20mL sulfuric acid (1+9), lulu maikaʻi, a waiho i loko o ka pōʻeleʻele no 10 mau minuke. E hoʻohui i 150mL wai a me 3ml 0.5% ka hopena hōʻailona starch, a e titrate me 0.1mol/L sodium thiosulfate solution. Hoʻololi ka hoʻonā mai ka uliuli a i ka uliuli. Huli i ka ʻōmaʻomaʻo ʻōmaʻomaʻo ma ka hopena. ʻAʻole i hoʻohui ʻia ka potassium chromate i ka hoʻokolohua blank. Hoʻopili hou ʻia ke kaʻina hana calibration 2 a 3 mau manawa a lawe ʻia ka waiwai awelika.
Ua helu ʻia ka ʻike molar C (mol/L) o ka solution maʻamau sodium thiosulfate e like me ke ʻano kumu:
I loko o ke kumu hoʻohālike, ʻo M ka nuipaʻa o ka potassium dichromate; ʻO V1 ka nui o ka sodium thiosulfate i hoʻopau ʻia, mL; ʻO V2 ka nui o ka sodium thiosulfate i hoʻopau ʻia i ka hoʻokolohua hakahaka, mL; ʻO 49.03 ka dichromium e like me 1 mol o ka sodium thiosulfate. Ka nui o ka waika potassium, g.
Ma hope o ka calibration, e hoʻohui i kahi mea liʻiliʻi o Na2CO3 e pale i ka microbial decomposition.
(2) NaOH hoʻonā maʻamau (0.1mol/L, manawa kūpono: 1 mahina)
Hoʻomākaukau: E kaupaona ma kahi o 4.0g o ka NaOH maʻemaʻe no ka nānā ʻana i loko o ka beaker, e hoʻohui i 100mL o ka wai i hoʻoheheʻe ʻia e hoʻoheheʻe ʻia, a laila e hoʻoneʻe i kahi pahu volumetric 1L, e hoʻohui i ka wai i hoʻopaʻa ʻia i ka māka, a waiho no 7-10 mau lā a hiki i ka calibration.
Calibration: E kau i ka 0.6 ~ 0.8g o ka potassium hydrogen phthalate maʻemaʻe (pololei i ka 0.0001g) maloʻo ma 120 ° C i loko o kahi pahu Erlenmeyer 250mL, hoʻohui i 75mL o ka wai i hoʻoheheʻe ʻia e hoʻoheheʻe, a laila hoʻohui i 2 ~ 3 kulu o 1% phenolphthalein indicator. Titrate me ka titrant. E ho'āla i ka solution sodium hydroxide i hoʻomākaukau ʻia ma luna a ʻulaʻula iki, a ʻaʻole e mae ke kala i loko o 30 kekona ma ke ʻano he hopena. E kākau i ka nui o ka sodium hydroxide. Hoʻopili hou ʻia ke kaʻina hana calibration 2 a 3 mau manawa a lawe ʻia ka waiwai awelika. A hana i kahi hoʻokolohua hakahaka.
Ua helu ʻia ka ʻike o ka solution sodium hydroxide penei:
I loko o ke kumu hoʻohālike, ʻo C ka manaʻo o ka solution sodium hydroxide, mol/L; Hōʻike ka M i ka nuipaʻa o ka potassium hydrogen phthalate, G; V1 - ka nui o ka sodium hydroxide i hoʻopau ʻia, mL; Hōʻike ka V2 i ka sodium hydroxide i hoʻopau ʻia i ka hoʻokolohua blank Volume, mL; ʻO 204.2 ka nuipaʻa mola o ka potassium hydrogen phthalate, g/mol.
(3) Dilute sulfuric acid (1+9) (manawa mana: 1 mahina)
I ka hoʻoulu ʻana, e hoʻohui pono i ka 100 mL o ka sulfuric acid concentrated i 900 mL o ka wai hoʻoheheʻe a hoʻohui mālie i ka wā e hoʻoulu ai.
(4) E hoʻoheheʻe i ka sulfuric acid (1+16.5) (manawa mana: 2 mahina)
I ka hoʻoulu ʻana, e hoʻohui pono i ka 100 mL o ka sulfuric acid concentrated i 1650 mL o ka wai hoʻoheheʻe a hoʻohui mālie. E hoʻoulu i kou hele ʻana.
(5) Hōʻailona mākū (1%, manawa kūpono: 30 lā)
E kaupaona 1.0g o ka soluble starch, e hoʻohui i 10mL o ka wai, e hoʻoulu a ninini i loko o 100mL o ka wai paila, e hoʻolapalapa no 2 mau minuke, e kū, a lawe i ka supernatant no ka hoʻohana hope.
(6) Hōʻailona mākū
E lawe i 5 mL o ka mea hoʻonā hōʻike starch 1% i hoʻomākaukau ʻia a hoʻoheheʻe ʻia me ka wai i 10 mL e loaʻa ai ka hōʻailona starch 0.5%.
(7) 30% chromium trioxide solution (manawa mana: 1 mahina)
E kaupaona i 60g o ka chromium trioxide a e hoʻoheheʻe ʻia i loko o 140mL o ka wai kūlohelohe.
(8) ʻO ka hopena o ka potassium acetate (100g/L, kūpono no 2 mau mahina)
E hoʻoheheʻe i 10 g o ka anhydrous potassium acetate granules i 100 mL o kahi hopena o 90 mL o ka ʻakika acetic glacial a me 10 mL o ka anhydride acetic.
(9) 25% sodium acetate solution (220g/L, manawa kūpono: 2 mahina)
E hoʻoheheʻe i 220g anhydrous sodium acetate i ka wai a hoʻoheheʻe i 1000mL.
(10) Hydrochloric acid (1:1, manawa kūpono: 2 mahina)
E hoʻohui i ka waika hydrochloric concentrated a me ka wai ma kahi ratio 1:1.
(11) Acetate buffer (pH=3.5, manawa kūpono: 2 mahina)
E hoʻoheheʻe i 60mL o ka acetic acid i 500mL o ka wai, a laila e hoʻohui i 100mL o ka ammonium hydroxide a hoʻoheheʻe i 1000mL.
(12) Hoʻomākaukau hoʻomākaukau ʻana i ka nitrate alakaʻi
E hoʻoheheʻe i 159.8 mg ke kēpau nitrate i 100 mL wai i loaʻa ka 1 mL nitric acid (density 1.42 g/cm3), hoʻoheheʻe i 1000 mL wai, a hui maikaʻi. Paʻa maikaʻi. Pono e hoʻomākaukau a mālama ʻia i loko o ke aniani alakaʻi ʻole.
(13) Ke alakaʻi i ka hopena maʻamau (manawa kūpono: 2 mahina)
E ana pololei i ka 10mL o ka wai hoʻomākaukau hoʻomākaukau kepau nitrate a hoʻohui i ka wai e hoʻoheheʻe i 100mL.
(14) 2% hydroxylamine hydrochloride solution (manawa mana: 1 mahina)
E hoʻoheheʻe i 2g o ka hydroxylamine hydrochloride i 98mL o ka wai.
(15) Ammonia (5mol/L, pono no 2 mahina)
E hoʻoheheʻe i 175.25g wai amonia a hoʻoheheʻe i 1000mL.
(16) Wai huikau (mana: 2 mahina)
Hoʻohui i 100mL o ka glycerol, 75mL o ka solution NaOH (1mol/L) a me 25mL o ka wai.
(17) Thioacetamide solution (4%, pono no 2 mahina)
E hoʻoheheʻe i 4g o thioacetamide i 96g wai.
(18) Phenanthroline (0.1%, manawa kūpono: 1 mahina)
E hoʻoheheʻe i 0.1g o ka phenanthroline i 100mL o ka wai.
(19) Acidic stannous chloride (manawa mana: 1 mahina)
E hoʻoheheʻe i 20g o stannous chloride i 50mL o ka waika hydrochloric concentrated.
(20) Potassium hydrogen phthalate solution buffer maʻamau (pH 4.0, manawa kūpono: 2 mahina)
E kaupaona pololei i 10.12g o ka potassium hydrogen phthalate (KHC8H4O4) a maloʻo ma (115±5) ℃ no 2 a 3 mau hola. E hoʻoheheʻe i ka 1000mL me ka wai.
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Pono ke kaupaona 3.533g anhydrous disodium hydrogen phosphate a me 3.387g potassium dihydrogen phosphate maloʻo ma (115±5) ° C no 2 ~ 3 hola, a hoʻoheheʻe i 1000mL me ka wai.
3. Ka hoʻoholo ʻana i ka ʻike o ka hui hydroxypropylmethylcellulose
(1) Ka hoʻoholo ʻana o ka maʻiʻo methoxyl
Hoʻoholo ʻia ka ʻike o ka hui methoxy ma ka hoʻāʻo i loaʻa nā pūʻulu methoxy. Hiki ke hoʻoheheʻe ʻia ka waiuma Hydroiodic i ka hoʻomehana ʻana e hana i ka methyl iodide (kahi hoʻolapalapa 42.5°C). Hoʻopili ʻia ʻo Methyl iodide me ka nitrogen i loko o ka hoʻonā hoʻonā ponoʻī. Ma hope o ka holoi ʻana no ka wehe ʻana i nā mea hoʻopilikia (HI, I2 a me H2S), hoʻomohu ʻia ka methyl iodide vapor e ka solution acetic acid o ka potassium acetate i loko o ka Br2 e lilo i IBr, a laila hoʻoheheʻe ʻia i ka iodic acid. Ma hope o ka distillation, e hoʻoneʻe ʻia nā mea o ka mea hoʻokipa i kahi hue iodine a hoʻoheheʻe ʻia me ka wai. Ma hope o ka hoʻohui ʻana i ka waika formic e wehe i ka Br2, ua hoʻohui ʻia ʻo KI a me H2SO4. Hiki ke helu ʻia ka maʻiʻo methoxyl ma ka titrating 12 me ka solution Na2S2O3. Hiki ke hōʻike ʻia ka hoʻohālikelike ʻana penei.
Hōʻike ʻia ka mea ana methoxyl ma ke Kiʻi 7-6.
Ma 7-6(a), ʻo A he 50mL poʻe poʻe lalo i hoʻopili ʻia i kahi catheter. Aia kekahi paipu hoʻoheheʻe ea pololei E i hoʻokomo ʻia ma ka ʻōmole, ma kahi o 25cm ka lōʻihi a me 9mm anawaena o loko. Hoʻopiʻi ʻia ka ʻaoʻao o luna o ka paipu i loko o ke aniani capillary tube me ke anawaena o loko o 2 mm a me kahi puka e kū ana i lalo. Hōʻike ka 7-6(b) i ka mea hana i hoʻomaikaʻi ʻia. Hōʻike ka Kiʻi 1 i ka ipu hoʻoheheʻe, ʻo ia ka 50mL poʻe poʻe lalo, me kahi paipu nitrogen ma ka hema. ʻO 2 ka paipu condenser kūpaʻa; ʻO 3 ka mea holoi holoi, kahi wai holoi; ʻO 4 ka paipu hoʻoheheʻe. ʻO ka ʻokoʻa nui loa ma waena o kēia hāmeʻa a me ke ʻano Pharmacopoeia, ʻo ia ka hui ʻana o nā mea hoʻopau ʻelua o ke ʻano Pharmacopoeia i hoʻokahi, hiki ke hōʻemi i ka nalowale o ka wai absorption hope. Eia kekahi, ʻokoʻa ka wai holoi i loko o ka scrubber mai ke ʻano pharmacopoeia. He wai hoʻoheheʻe ʻia, ʻoiai ʻo ka mea i hoʻomaikaʻi ʻia he hui ʻia o ka solution cadmium sulfate a me ka solution sodium thiosulfate, ʻoi aku ka maʻalahi o ka hoʻomoʻa ʻana i nā haumia i loko o ke kinoea distilled.
Pipetta mea kani: 5mL (5 ʻāpana), 10mL (1 ʻāpana); Bureta: 50mL; ʻO ka'ōmole nui o Iodine: 250mL; Kaulike analytical.
Reagent phenol (no ka mea, he paʻa, hehee ia ma mua o ka hānai ʻana); carbon dioxide a i ʻole nitrogen; waikika hydroiodic (45%); papa analytical; ka hopena o ka potassium acetate (100g / L); bromine: analytical grade; formic acid: analytical grade; 25% Sodium acetate solution (220g / L); KI: analytical grade; dilute sulfuric acid (1+9); ka sodium thiosulfate solution maʻamau (0.1mol / L); hōʻailona phenolphthalein; 1% solution ethanol; hōʻailona starch: 0.5% Starch aqueous solution; dilute sulfuric acid (1+16.5); 30% chromium trioxide solution; wai organik-noa: hoʻohui i 10mL o ka sulfuric acid dilute (1 + 16.5) i 100mL o ka wai, wela i ka paila, a hoʻohui i 0.1ml o 0.02mol/L permanganic acid Potassium titer, e hoʻolapalapa no 10 mau minuke, pono e waiho ʻulaʻula; 0.02mol/L sodium hydroxide titrant: E hoʻopololei i ka 0.1mol/L sodium hydroxide titrant e like me ka Chinese Pharmacopoeia Appendix, a e hoʻoheheʻe pololei i ka 0.02mol me ka wai i hoʻolapalapa ʻia a hoʻoluʻu ʻia.
E hoʻohui ma kahi o 10mL o ka wai holoi i loko o ka ipu holoi, e hoʻohui i 31mL o ka wai absorption hou i hoʻomākaukau ʻia i loko o ka pahu absorption, e hoʻokomo i ka mea hana, e kaupaona ma kahi o 0.05g o ka hāpana maloʻo i hoʻomaloʻo ʻia i ke kaumaha mau ma 105 ° C (pololei i 0.0001. g), hoʻohui i ka hopena ma ℃ I loko o ka ʻōmole, hoʻohui i 5 mL o ka hydroiodide. E hoʻopili koke i ka ʻōmole hopena i ka condenser hoʻihoʻi (hoʻomaʻemaʻe i ke awa wili me ka waikawa hydriodic), a e pākī i ka naikokene i loko o ka pahu ma ka wikiwiki o 1 a 2 mau pahu i kēlā me kēia kekona.
Ka manawa hoʻouna: Feb-01-2024