1. Kuzivikanwa nzira yehydroxypropyl methylcellulose
(1) Tora 1.0g yemuenzaniso, kupisa 100mL yemvura (80 ~ 90 ℃), fambisa nguva dzose, uye utonhore mubhati rechando kusvikira yava mvura inopenya; isa 2mL yemvura muchubhu yekuyedza, wobva wawedzera zvishoma nezvishoma 1mL ye0.035% anthrone sulfuric acid padivi pechubhu madziro mhinduro woisiya kwemaminitsi mashanu. Mhete yegirini inoonekwa pakusangana pakati pezvinwiwa zviviri izvi.
(2) Tora huwandu hwakakodzera hwemukosi unoshandiswa pakuzivikanwa mu (I) pamusoro uye uidururire pandiro yegirazi. Sezvo mvura inoputika, firimu re ductile rinoita.
2. Kugadzirira kwehydroxypropyl methylcellulose yekuongorora yakajairwa mhinduro
(1) Sodium thiosulfate yakajairwa mhinduro (0.1mol/L, nguva yechokwadi: 1 mwedzi)
Kugadzirira: Birai anenge 1500mL mvura yakasvibiswa, inotonhorera uye isa parutivi. Weresa 25g sodium thiosulfate (huremu hwayo hwemamolecular 248.17, edza kuve yakarurama senge 24.817g kana uchiyera) kana 16g anhydrous sodium thiosulfate, inyunguduse mu200mL yemvura inotonhorera iri pamusoro, dilute kusvika pa1L, isa mubhodhoro rebrown. woisa Chengeta munzvimbo ine rima, sefa uye woisa parutivi mushure memavhiki maviri.
Calibration: Weresa 0.15g yereferensi potassium dichromate uye bika kune huremu hunoramba huripo, hwakakwana kusvika 0.0002g. Wedzera 2g potassium iodide uye 20mL sulfuric acid (1+9), zunza zvakanaka, woisa murima kwemaminitsi gumi. Wedzera 150mL mvura uye 3ml 0.5% starch indicator solution, uye titrate ne 0.1mol/L sodium thiosulfate solution. Mhinduro inoshanduka kubva pabhuruu kuenda kubhuruu. Inoshandura girini yakajeka pamagumo. Hapana potassium chromate yakawedzerwa mukuedza kusina chinhu. Nzira yekuenzanisa inodzokororwa 2 kusvika ku3 nguva uye chiyero chepakati chinotorwa.
Iyo molar concentration C (mol / L) yesodium thiosulfate yakajairwa mhinduro inoverengerwa zvinoenderana neinotevera fomula:
Mune fomula, M ndiyo uwandu hwe potassium dichromate; V1 ihuwandu hwe sodium thiosulfate inopedzwa, mL; V2 ndiyo vhoriyamu yesodium thiosulfate inopedzwa muyedzo isina chinhu, mL; 49.03 ndiyo dichromium yakaenzana ne1 mol ye sodium thiosulfate. Kuwanda kweasidhi ye potassium, g.
Mushure mekugadzirisa, wedzera zvishoma zveNa2CO3 kudzivirira kuparara kwehutachiona.
(2) NaOH yakajairwa mhinduro (0.1mol/L, nguva yechokwadi: 1 mwedzi)
Kugadzirira: Weresa inenge 4.0g yeNaOH yakachena yekuongorora mubeaker, wedzera 100mL yemvura yakasvibiswa kuti inyunguduke, wozoendesa kune 1L volumetric flask, wedzera mvura yakasvibiswa kune mucherechedzo, uye uisiye kwemazuva 7-10 kusvika pakugadzirisa.
Calibration: Isa 0.6 ~ 0.8g ye pure potassium hydrogen phthalate (yakarurama kusvika 0.0001g) yakaomeswa pa 120 ° C mu 250mL Erlenmeyer flask, wedzera 75mL yemvura yakasvibiswa kuti inyunguduke, uye wobva wawedzera 2 ~ 3 madonhwe e1% mu phenolph. Titrate ine titrant. Kurudzira iyo sodium hydroxide solution yakagadziridzwa pamusoro kusvika yatsvuka zvishoma, uye ruvara haruna kupera mukati memasekonzi makumi matatu seyekupedzisira. Nyora huwandu hwe sodium hydroxide. Nzira yekuenzanisa inodzokororwa 2 kusvika ku3 nguva uye chiyero chepakati chinotorwa. Uye ita bvunzo isina chinhu.
Iko kusanganiswa kwesodium hydroxide solution inoverengerwa seizvi:
Mune fomula, C ndiko kusangana kwesodium hydroxide solution, mol/L; M inomiririra huwandu hwe potassium hydrogen phthalate, G; V1 - huwandu hwe sodium hydroxide inopedzwa, mL; V2 inomiririra sodium hydroxide inopedzwa muyedzo isina chinhu Vhoriyamu, mL; 204.2 ndiyo molar mass ye potassium hydrogen phthalate, g/mol.
(3) Dilute sulfuric acid (1+9) (nguva yechokwadi: 1 mwedzi)
Paunenge uchikurudzira, nyatsowedzera 100 mL yeconcentrated sulfuric acid kusvika 900 mL yemvura yakasvibiswa uye wedzera zvishoma nezvishoma uchikurudzira.
(4) Dilute sulfuric acid (1+16.5) (nguva yechokwadi: mwedzi miviri)
Paunenge uchikurudzira, nyatsowedzera 100 mL yeconcentrated sulfuric acid kusvika 1650 mL yemvura yakasvibiswa uye wedzera zvishoma nezvishoma. Kurudzira sezvaunoenda.
(5) Starch chiratidzo (1%, nguva yechokwadi: 30 mazuva)
Weresa 1.0g yestarch yakanyunguduka, woisa 10mL yemvura, kurunga wodira mu100mL yemvura iri kufashaira, fashaira kwemaminetsi maviri, rega kumira, wotora mashura wozoshandisa gare gare.
(6) Starch chiratidzo
Tora 5 mL yeyakagadzirirwa 1% starch indicator solution uye uidure nemvura kusvika ku10 mL kuti uwane 0.5% starch chiratidzo.
(7) 30% chromium trioxide solution (nguva yechokwadi: 1 mwedzi)
Weresa 60g yechromium trioxide woinyungudutsa mu140mL yemvura isina organic.
(8) Potassium acetate solution (100g/L, inoshanda kwemwedzi miviri)
Dissolve 10 g yeanhydrous potassium acetate granules mu100 mL yemhinduro ye90 mL yeglacial acetic acid uye 10 mL yeacetic anhydride.
(9) 25% sodium acetate solution (220g/L, nguva yechokwadi: mwedzi miviri)
Dissolve 220g anhydrous sodium acetate mumvura uye wedzera kusvika 1000mL.
(10) Hydrochloric acid (1:1, nguva yechokwadi: mwedzi miviri)
Sanganisa concentrated hydrochloric acid nemvura muchiyero che1: 1.
(11) Acetate buffer (pH=3.5, nguva yechokwadi: mwedzi miviri)
Dissolve 60mL yeacetic acid mu500mL yemvura, wobva wawedzera 100mL yeammonium hydroxide uye wedzera ku1000mL.
(12) Lead nitrate kugadzirira mhinduro
Dissolve 159.8 mg lead nitrate mu100 mL mvura ine 1 mL nitric acid (density 1.42 g/cm3), dilute kusvika 1000 mL mvura, uye sanganisa zvakanaka. Yakanyatsogadziriswa. Mhinduro yacho inofanira kugadzirirwa uye kuchengetwa mugirazi isina-lead.
(13) Lead standard solution (nguva yechokwadi: mwedzi miviri)
Nyatsoyera 10mL yelead nitrate yekugadzirira mhinduro uye wedzera mvura kuti iwedzere kusvika ku100mL.
(14) 2% hydroxylamine hydrochloride mhinduro (nguva yechokwadi: 1 mwedzi)
Dissolve 2g yehydroxylamine hydrochloride mu98mL yemvura.
(15) Ammonia (5mol/L, inoshanda kwemwedzi miviri)
Dissolve 175.25g ammonia mvura uye diluted kusvika 1000mL.
(16) Mvura yakasanganiswa (kushanda: mwedzi miviri)
Sanganisa 100mL yeglycerol, 75mL yeNaOH solution (1mol/L) uye 25mL yemvura.
(17) Thioacetamide mhinduro (4%, inoshanda kwemwedzi miviri)
Dissolve 4g yethioacetamide mu96g yemvura.
(18) Phenanthroline (0.1%, nguva yechokwadi: mwedzi 1)
Dissolve 0.1g ye phenanthroline mu 100mL yemvura.
(19) Acid stannous chloride (nguva yechokwadi: mwedzi 1)
Dissolve 20g yestannous chloride mu50mL yeconcentrated hydrochloric acid.
(20) Potassium hydrogen phthalate standard buffer solution (pH 4.0, nguva yechokwadi: mwedzi miviri)
Nyatsoyera 10.12g ye potassium hydrogen phthalate (KHC8H4O4) woiomesa pa (115±5) ℃ kwemaawa maviri kusvika matatu. Dilute kusvika 1000mL nemvura.
(21) Phosphate standard buffer solution (pH 6.8, nguva yechokwadi: mwedzi miviri)
Huremu chaihwo 3.533g anhydrous disodium hydrogen phosphate uye 3.387g potassium dihydrogen phosphate yakaomeswa pa (115±5)°C kwemaawa 2~3, uye dilute kusvika 1000mL nemvura.
3. Kutsunga kwehuwandu hweboka re hydroxypropylmethylcellulose
(1) Kutemerwa kwemethoxyl yemukati
Kutsunga kwemethoxy group yemukati kunobva pane bvunzo ine methoxy mapoka. Hydroiodic acid inoora painopisa kuti ibudise methyl iodide inoputika (inofashaira 42.5°C). Methyl iodide yakanyungudutswa nenitrogen mune yekuzvigadzirisa mhinduro. Mushure mekugeza kubvisa zvinhu zvinokanganisa (HI, I2 neH2S), methyl iodide vapor inotorwa neacetic acid solution ye potassium acetate ine Br2 kuti iite IBr, iyo inobva yaiswa kune iodic acid. Mushure mekuita distillation, zviri mukati memugamuchiri zvinotamirwa kubhodhoro reiodine uye rinonatswa nemvura. Mushure mekuwedzera formic acid kubvisa yakawandisa Br2, KI uye H2SO4 inowedzerwa. Iyo methoxyl yemukati inogona kuverengerwa nekuita 12 neNa2S2O3 mhinduro. Iyo reaction equation inogona kuratidzwa nenzira inotevera.
Iyo methoxyl yemukati yekuyera mudziyo inoratidzwa muMufananidzo 7-6.
Mu7-6(a), A i50mL yakatenderera-yakadzika flask yakabatana necatheter. Kune yakatwasuka mweya condensation chubhu E yakamira yakamira pabhodhoro, inenge 25cm kureba uye 9mm yemukati dhayamita. Kumucheto kwepamusoro kwechubhu yakakotama mugirazi capillary chubhu ine dhayamita yemukati ye2 mm uye chinobuda chinotarisa pasi. Mufananidzo 7-6(b) unoratidza mudziyo wakavandudzwa. Mufananidzo 1 unoratidza bhodhoro rekuita, inova 50mL yakatenderera-yakadzika flask, ine nitrogen chubhu kuruboshwe. 2 ndiyo vertical condenser chubhu; 3 ndiyo scrubber, ine mvura yekuwachisa; 4 ndiyo chubhu inopinza. Musiyano mukuru pakati pechigadziro ichi uye nzira yePharmacopoeia ndeyokuti zviputi zviviri zveFarmacopoeia nzira inosanganiswa kuva imwe, iyo inogona kuderedza kurasikirwa kwemvura yekupedzisira. Mukuwedzera, mvura yekugeza mu scrubber yakasiyanawo neyo pharmacopoeia nzira. Imvura yakasvibiswa, nepo mudziyo wakagadziridzwa uri musanganiswa wecadmium sulfate solution uye sodium thiosulfate mhinduro, iri nyore kutora tsvina mugasi rakasvibiswa.
Chiridzwa pipette: 5mL (5 zvidimbu), 10mL (1 chidimbu); Burette: 50mL; Iodine vhoriyamu bhodhoro: 250mL; Analytical balance.
Reagent phenol (nokuti yakasimba, inonyunguduka isati yadyisa); carbon dioxide kana nitrogen; hydroiodic acid (45%); analytical giredhi; potassium acetate solution (100g/L); bromine: analytical giredhi; formic acid: analytical giredhi; 25% Sodium acetate solution (220g/L); KI: analytical giredhi; dilute sulfuric acid (1+9); sodium thiosulfate yakajairika mhinduro (0.1mol/L); phenolphthalein chiratidzo; 1% ethanol mhinduro; starch chiratidzo: 0.5% Starch aqueous mhinduro; dilute sulfuric acid (1 + 16.5); 30% chromium trioxide mhinduro; organic-isina mvura: wedzera 10mL ye dilute sulfuric acid (1+16.5) kusvika 100mL yemvura, kupisa kusvika kufashaira, wowedzera 0.1ml ye0.02mol/L permanganic acid Potassium titer, bika kwemaminetsi gumi, inofanira kuramba iri pink; 0.02mol/L sodium hydroxide titrant: Gadzirisa iyo 0.1mol/L sodium hydroxide titrant maererano neChinese Pharmacopoeia Appendix nzira, uye nenzira kwayo dilute kusvika 0.02mol nemvura yakafashaidzwa uye yakatonhodzwa yakadirwa / L.
Wedzera nezve 10mL yemvura yekuwachisa muchubhu yekuwachisa, wedzera 31mL yemvura ichangobva kugadzirwa muchubhu yekunyudza, isa chiridzwa, uremu hunosvika 0.05g yemuenzaniso wakaomeswa wakaomeswa kuti urambe uchirema pa105 ° C (chaizvo kusvika 0.0001 g), wedzera maitiro pa ℃ Mubhodhoro, wedzera 5 mL yehydroiodide. Kurumidza batanidza bhodhoro rekuita kune inogadzirisa condenser (moisten chiteshi chekukuya ne hydriodic acid), uye pombi nitrogen mutangi pamwero we1 kusvika ku2 mabhubhu pasekondi.
Nguva yekutumira: Feb-01-2024