1. Mokhoa oa ho khetholla hydroxypropyl methylcellulose
(1) Nka 1.0g ea sampole, futhumatsa 100mL ea metsi (80 ~ 90 ℃), tsosa ka ho tsoelang pele, 'me u pholile ka bateng ea leqhoa ho fihlela e fetoha mokelikeli oa viscous; kenya 2mL ea mokelikeli ka har'a tube ea teko, 'me butle-butle eketsa 1mL ea 0.035% anthrone sulfuric acid hammoho le tharollo ea lebota la tube ebe u e tlohela metsotso e 5. Reng e tala e hlaha sehokelo pakeng tsa maro a mabeli.
(2) Nka tekanyo e loketseng ea mucus e sebelisetsoang ho khetholla ho (I) ka holimo 'me ue tšollele holim'a poleiti ea khalase. Ha metsi a fetoha mouoane, filimi ea ductile e thehoa.
2. Ho lokisetsa tharollo e tloaelehileng ea tlhahlobo ea hydroxypropyl methylcellulose
(1) Sodium thiosulfate tharollo e tloaelehileng (0.1mol/L, nako ea ho sebetsa: khoeli e le 'ngoe)
Litokisetso: Pheha metsi a ka bang 1500mL, a pholile 'me u behelle ka thōko. Beha 25g sodium thiosulfate (boima ba eona ba molek'hule ke 248.17, leka ho nepahala joalo ka 24.817g ha u le boima) kapa 16g anhydrous sodium thiosulfate, e qhibilihe ka 200mL ea metsi a pholileng a ka holimo, hlapolla ho 1L, e behe ka har'a botlolo e sootho. 'me u behe Boloka sebakeng se lefifi, sesefa 'me u behelle ka thōko ka mor'a libeke tse peli.
Tekanyetso: Boima ba 0.15g ea potassium dichromate 'me u bake ho boima bo sa feleng, bo nepahetseng ho isa ho 0.0002g. Kenya 2g potassium iodide le 20mL sulfuric acid (1+9), sisinya hantle, 'me u behe lefifing metsotso e 10. Kenya metsi a 150mL le 3ml 0.5% ea tharollo ea starch, le titrate ka 0.1mol/L sodium thiosulfate solution. Tharollo e fetoha ho tloha boputsoa ho ea ho boputsoa. E fetoha botala bo khanyang qetellong. Ha ho na chromate ea potassium e kentsoeng tekong e se nang letho. Ts'ebetso ea ho lekanya e phetoa ka makhetlo a 2 ho isa ho a 3 'me boleng ba karolelano bo nkoa.
Molar concentration C (mol/L) ea sodium thiosulfate standard solution e baloa ho latela foromo e latelang:
Ka foromo, M ke boima ba potassium dichromate; V1 ke molumo oa sodium thiosulfate e jeoang, mL; V2 ke molumo oa sodium thiosulfate e sebelisitsoeng tekong e se nang letho, mL; 49.03 ke dichromium e lekanang le 1 mol ea sodium thiosulfate. Boima ba asiti ea potassium, g.
Kamora ho lekanya, eketsa palo e nyane ea Na2CO3 ho thibela ho bola ha likokoana-hloko.
(2) Tharollo e tloaelehileng ea NaOH (0.1mol/L, nako ea ho sebetsa: khoeli e le 'ngoe)
Boitokisetso: Nka boima ba 4.0g ea NaOH e hloekileng bakeng sa tlhahlobo ka beaker, eketsa 100mL ea metsi a qhibilihisitsoeng ho qhibiliha, ebe u fetisetsa ho 1L ea volumetric flask, eketsa metsi a hloekisitsoeng ho letšoao, 'me ue tlohele matsatsi a 7-10 ho fihlela ho lekanngoa.
Calibration: Beha 0.6 ~ 0.8g ea potassium hydrogen phthalate e hloekileng (e nepahetseng ho 0.0001g) e omisitsoeng ka 120 ° C ka har'a 250mL Erlenmeyer botlolo, eketsa 75mL ea metsi a hloekisitsoeng ho qhibiliha, ebe u eketsa marotholi a 2 ~ 3 a 1% ea phenolph. Titrate e nang le titrant. Hlohlelletsa tharollo ea sodium hydroxide e lokiselitsoeng ka holimo ho fihlela e le khubelu hanyenyane, 'me' mala ha o fele ka metsotsoana e 30 e le ntlha ea ho qetela. Ngola bophahamo ba sodium hydroxide. Ts'ebetso ea ho lekanya e phetoa ka makhetlo a 2 ho isa ho a 3 'me boleng ba karolelano bo nkoa. 'Me u etse teko e se nang letho.
Khatello ea tharollo ea sodium hydroxide e baloa ka tsela e latelang:
Ka foromo, C ke motsoako oa sodium hydroxide solution, mol / L; M e emetse boima ba potassium hydrogen phthalate, G; V1 - molumo oa sodium hydroxide e jeoang, mL; V2 e emela sodium hydroxide e sebelisitsoeng tekong e se nang letho Volume, mL; 204.2 ke boima ba 'mele oa potasiamo hydrogen phthalate, g/mol.
(3) Hlakola sulfuric acid (1+9) (nako ea ho sebetsa: khoeli e le 'ngoe)
Ha u ntse u hlohlelletsa, ka hloko eketsa 100 mL ea concentrated sulfuric acid ho 900 ml ea metsi a hloekisitsoeng 'me u kenye butle ha u ntse u hlohlelletsa.
(4) Hlakola sulfuric acid (1+16.5) (nako ea ho sebetsa: likhoeli tse 2)
Ha u ntse u hlohlelletsa, ka hloko eketsa 100 mL ea concentrated sulfuric acid ho 1650 ml ea metsi a hloekisitsoeng 'me u kenye butle. Hlohlelletsa ha u ntse u tsamaea.
(5) Letšoao la starch (1%, nako ea ho sebetsa: matsatsi a 30)
Beha boima ba 1.0g ea starch e qhibilihang, eketsa 10mL ea metsi, hlohlelletsa 'me u tšele ka 100mL ea metsi a belang, pheha metsotso e 2, e eme, 'me u nke matla a phahametseng ho sebelisoa hamorao.
(6) Letšoao la starch
Nka 5 ml ea tharollo e lokiselitsoeng ea 1% ea starch 'me u e hlapolle ka metsi ho 10 ml ho fumana 0.5% ea starch.
(7) 30% tharollo ea chromium trioxide (nako ea ho sebetsa: khoeli e le 'ngoe)
Beha 60g ya chromium trioxide mme o e qhale ka 140mL ya metsi a se nang organic.
(8) Tharollo ea Potassium acetate (100g/L, e sebetsa bakeng sa likhoeli tse 2)
Qhala ligrama tse 10 tsa anhydrous potassium acetate granules ka 100 ml ea tharollo ea 90 ml ea glacial acetic acid le 10 ml ea acetic anhydride.
(9) 25% tharollo ea sodium ea acetate (220g/L, nako e nepahetseng: likhoeli tse 2)
Qhala 220g anhydrous sodium acetate ka metsing 'me u hlapolle ho 1000mL.
(10) Hydrochloric acid (1:1, nako ea ho sebetsa: likhoeli tse 2)
Kopanya concentrated hydrochloric acid le metsi ka karolelano ea 1: 1.
(11) Acetate buffer (pH=3.5, nako ea ho sebetsa: likhoeli tse 2)
Qhala 60mL ea acetic acid ka 500mL ea metsi, ebe u eketsa 100mL ea ammonium hydroxide ebe o hlapolla ho 1000mL.
(12) Tharollo ea ho lokisetsa nitrate pele
Hlakola 159.8 mg lead nitrate metsing a 100 ml a nang le 1 mL nitric acid (tekanyo ea 1.42 g/cm3), hlapolla ho 1000 mL ea metsi, 'me u kopanye hantle. E lokisitsoe hantle. Tharollo e lokela ho lokisoa le ho bolokoa ka khalase e se nang loto.
(13) Tharollo e tloaelehileng ea ketapele (nako ea ho sebetsa: likhoeli tse 2)
Lekanya 10mL ea tharollo ea lead nitrate ka nepo ebe u eketsa metsi ho hlapolla ho 100mL.
(14) 2% tharollo ea hydroxylamine hydrochloride (nako ea ho sebetsa: khoeli e le 'ngoe)
Qhala 2g ea hydroxylamine hydrochloride ka 98mL ea metsi.
(15) Ammonia (5mol/L, e sebetsa bakeng sa likhoeli tse peli)
Hlakola 175.25g ea metsi a ammonia 'me u hlapolle ho 1000mL.
(16) Mokelikeli o tsoakiloeng (ho sebetsa: likhoeli tse 2)
Kopanya 100mL ea glycerol, 75mL ea tharollo ea NaOH (1mol/L) le 25mL ea metsi.
(17) Tharollo ea Thioacetamide (4%, e sebetsang bakeng sa likhoeli tse 2)
Qhala 4g ea thioacetamide ka 96g ea metsi.
(18) Phenanthroline (0.1%, nako e nepahetseng: khoeli e le 'ngoe)
Qhala 0.1g ea phenanthropine ka 100mL ea metsi.
(19) Acid stannous chloride (nako ea ho sebetsa: khoeli e le 'ngoe)
Qhala 20g ea stannous chloride ka 50mL ea concentrated hydrochloric acid.
(20) Potassium hydrogen phthalate standard buffer solution (pH 4.0, nako ea ho sebetsa: likhoeli tse 2)
Ka nepo, bekha 10.12g ea potassium hydrogen phthalate (KHC8H4O4) 'me u e omise ho (115±5)℃ bakeng sa lihora tse 2 ho isa ho tse 3. Hlatsoa ho 1000mL ka metsi.
(21) Phosphate standard buffer solution (pH 6.8, nako ea ho sebetsa: likhoeli tse 2)
Eka ka nepo 3.533g anhydrous disodium hydrogen phosphate le 3.387g potassium dihydrogen phosphate omisitsoeng ho (115±5)°C bakeng sa lihora tse 2~3, ebe o hlapolla ho 1000mL ka metsi.
3. Boikemisetso ba litaba tsa sehlopha sa hydroxypropylmethylcellulose
(1) Boikemisetso ba methoxyl content
Boikemisetso ba litaba tsa sehlopha sa methoxy bo thehiloe tekong e nang le lihlopha tsa methoxy. Hydroiodic acid e bola ha e futhumala ho hlahisa methyl iodide e sa tsitsang (sebaka se belang 42.5°C). Methyl iodide e ile ea tšeloa ka naetrojene ka tharollo e ikemetseng. Ka mor'a ho hlatsoa ho tlosa lintho tse sitisang (HI, I2 le H2S), mouoane oa methyl iodide o kenngoa ke motsoako oa acetic acid ea potassium acetate e nang le Br2 ho etsa IBr, ebe oxidized ho iodic acid. Kamora 'distillation, likahare tsa receptor li fetisetsoa botlolong ea iodine ebe e hlapolotsoe ka metsi. Ka mor'a ho eketsa formic acid ho tlosa Br2 e feteletseng, KI le H2SO4 li kenngoa. Likahare tsa methoxyl li ka baloa ka ho etsa titrating 12 ka tharollo ea Na2S2O3. The reaction equation e ka hlalosoa ka tsela e latelang.
Sesebediswa sa ho lekanya dikahare tsa methoxyl se bontshwa ho Setšoantšo sa 7-6.
Ho 7-6(a), A ke botlolo e chitja e tlase ea 50mL e hokahaneng le catheter. Ho na le tube ea condensation ea moea e otlolohileng ea E e kentsoeng ka holimo lebotleng la botlolo, e ka bang bolelele ba 25cm le bophara ba 9mm kahare. Karolo e ka holimo ea tube e kobetsoe ka har'a tube ea capillary ea khalase e bophara ba 2 mm le phallo e shebileng tlase. Setšoantšo sa 7-6 (b) se bontša sesebelisoa se ntlafalitsoeng. Setšoantšo sa 1 se bontša botlolo ea ho arabela, e leng botlolo ea 50mL e pota-potileng, e nang le tube ea nitrogen ka ho le letšehali. 2 ke tube ea condenser e otlolohileng; 3 ke scrubber, e nang le mokelikeli oa ho hlatsoa; 4 ke tube ea ho monya. Phapang e kholo ka ho fetisisa pakeng tsa sesebelisoa sena le mokhoa oa Pharmacopoeia ke hore li-absorber tse peli tsa mokhoa oa Pharmacopoeia li kopantsoe ho ba le le leng, tse ka fokotsang tahlehelo ea mokelikeli oa ho qetela oa ho monya. Ho phaella moo, mokelikeli oa ho hlatsoa ka scrubber o boetse o fapane le mokhoa oa pharmacopoeia. Ke metsi a hloekisitsoeng, ha sesebelisoa se ntlafetseng e le motsoako oa cadmium sulfate solution le sodium thiosulfate solution, eo ho leng bonolo ho monya litšila ka khase e hloekisitsoeng.
Pipette ea lisebelisoa: 5mL (likotoana tse 5), 10mL (sekotoana se le seng); Borette: 50mL; Botlolo ea molumo oa iodine: 250mL; Ho leka-lekanya ho leka-lekanya.
Reagent phenol (hobane e tiile, e tla qhibiliha pele e fepa); carbon dioxide kapa naetrojene; hydroiodic acid (45%); sehlopha sa analytical; tharollo ea potassium acetate (100g/L); bromine: sehlopha sa ho hlahloba; asiti ea formic: sehlopha sa tlhahlobo; 25% ea tharollo ea sodium acetate (220g / L); KI: sehlopha sa tlhahlobo; hlapolla sulfuric acid (1+9); sodium thiosulfate tharollo e tloaelehileng (0.1mol/L); phenolphthalein pontshi; 1% tharollo ea ethanol; sesupo sa starch: 0.5% Tharollo ea metsi a starch; hlapolla sulfuric acid (1 + 16.5); 30% tharollo ea chromium trioxide; metsi a se nang organic: eketsa 10mL ea dilute sulfuric acid (1+16.5) ho 100mL ea metsi, mocheso ho bela, 'me u kenye 0.1ml ea 0.02mol/L permanganic titer Potassium titer, pheha metsotso e 10, e tlameha ho lula e le pinki; 0.02mol/L sodium hydroxide titrant: Lekanya 0.1mol/L sodium hydroxide titrant ho latela mokhoa oa Sehlomathiso sa Pharmacopoeia oa China, 'me ka nepo o hlapolle ho 0.02mol ka metsi a phehiloeng le a pholileng a qhibilihisitsoeng / L.
Eketsa hoo e ka bang 10mL ea metsi a hlatsoang ka har'a tube ea ho hlatsoa, eketsa 31mL ea mokelikeli o sa tsoa lokisoa ka har'a tube ea ho monya, kenya sesebelisoa, boima ba 0.05g ea sampole e omisitsoeng e omisitsoeng ho boima bo sa feleng ho 105 ° C (e nepahetseng ho 0.0001). g), eketsa karabelo ho ℃ ka botlolong, eketsa 5 mL ea hydroiodide. Hokela ka potlako botlolo ea karabelo ho condenser ea ho hlaphoheloa (moisten boema-kepe ba ho sila ka hydriodic acid), 'me u pompe naetrojene ka tanka ka sekhahla sa 1 ho isa ho tse 2 ka motsotsoana.
Nako ea poso: Feb-01-2024