Saccharin Insoluble CAS 81-07-2 Kuchena > 99.0% (HPLC)

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3(2H)-imwe, 1,1-dioxide;
1,2-Benzisothiazolin-3-imwe 1,1-dioxide [81-07-2].
DEFINITION
Saccharin ine NLT 99.0% uye NMT 101.0% yeC7H5NO3S, yakaverengerwa payakaomeswa.
KUZIVA
• Infrared Absorption <197K>
ASSAY
• Maitiro
Muenzaniso: 500 mg
Kuongorora: Dissove Sample mu40 mL yedoro.Wedzera 40 mL yemvura uye phenolphthalein TS.Titrate ine 0.1 N sodium hydroxide.Ita titration isina chinhu, kana zvichidikanwa, uye ita gadziriso yakakodzera.Imwe mL ye0.1 N sodium hydroxide yakaenzana ne18.32 mg yeC7H5NO3S.
Maitiro ekugamuchira: 99.0% -101.0% pane yakaomeswa hwaro
KUSIRIRA
Inorganic Impurities
• Zvakasara paKubatidza <281>: NMT 0.2%.Iyo tembiricha yekudzima i600 ± 50.
• Heavy Metals, Method II <231>: NMT 10 ppm
Organic Kusachena
• Nzira 1: Muganhu weToluenesulfonamides
Internal standard solution: 0.25 mg/mL ye caffeine mu methylene chloride
Standard stock solution: 20.0 µg/mL yeUSP o-Toluenesulfonamide RS uye 20.0 µg/mL yeUSP p-Toluenesulfonamide RS mumethylene chloride
Mushonga wakajairwa: Evaporate 5.0 mL yeStandard stock solution pakuoma murukova rwenitrogen.Dissolve zvakasara mu 1 mL yeInternal standard solution.
Sample solution: Misa 10 g yeSaccharin mu20 mL yemvura, uye nyungudusa uchishandisa 5-6 mL ye10 N sodium hydroxide.Kana zvichidiwa, gadzirisa mhinduro ne 1 N sodium hydroxide kana 1 N hydrochloric acid kusvika pH ye7-8, uye dilue nemvura kusvika ku50 mL.Zunza mushonga nezvikamu zvina chimwe nechimwe che50 mL yemethylene chloride.Sanganisa zvidimbu zvezasi, zviome pamusoro peanhydrous sodium sulfate, uye sefa.Geza sefa uye sodium sulfate ne10 mL yemethylene chloride.Sanganisa mhinduro uye washings, uye kuputika kunenge kuoma mumvura yekugeza pane tembiricha isingapfuuri 40. Uchishandisa chidimbu chidiki che methylene chloride, quantitatively endesa zvakasara muakakodzera 10-mL chubhu, evaporate kuoma murukova rwe. nitrogen, uye nyungudutsa zvakasara mu1.0 mL yeInternal standard solution.
Blank solution: Evaporate 200 mL yemethylene chloride kusvika pakuoma mumvura yekugeza patembiricha isingadariki 40. Nyura zvakasara mu1 mL yemethylene chloride.
Chromatographic system
(Ona Chromatography <621>, System Suitability.)
Modhi: GC
Detector: Moto ionization
Column: 0.53-mm × 10-m yakasanganiswa silica column, yakaputirwa neG3 chikamu (firimu ukobvu 2 µm)
Tembiricha
Injector: 250
Detector: 250
Chikamu: 180
Mutakuri gasi: Nitrogen
Kuyerera: 10 mL / min
Jekiseni saizi: 1 µL
Kupatsanura ratio: 2:1
Kukodzera kwehurongwa
Samples: Standard solution uye Blank solution
[Cherechedza-Zvinhu izvi zvakaburitswa nenzira inotevera: o-toluenesulfonamide, p-toluenesulfonamide, uye caffeine.]
Zvinodiwa zvekukodzera: Hapana nhongonya panguva dzekuchengetedza kwemukati mwero, o-toluenesulfonamide, kana p-toluenesulfonamide;Blank solution
Chisarudzo: NLT 1.5 pakati pe o-toluenesulfonamide uye p-toluenesulfonamide, Standard solution
Analysis
Samples: Yakajairwa mhinduro uye Sample mhinduro
Mamiriro ekugamuchira: Kana paine mapikisi epamusoro nekuda kwe o-toluenesulfonamide uye p-toluenesulfonamide akaonekwa muchromatogram yakawanikwa neSample solution, reshiyo yenzvimbo dzadzo neiyo yeInternal standard solution iNMT chiyero chinoenderana muchromatogram yakawanikwa neStandard solution. .
Kusachena kwemunhu: Ona Kusachena Tafura 1.
Kusachena Tafura 1
Maitiro ekugamuchira zita (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Nzira 2: Muganhu weBenzoate uye Salicylate
Sample solution: 10 mL yemushonga unopisa, wakazara saccharin
Ongororo: Wedzera ferric chloride TS inodonha kune Sample solution.
Maitiro ekugamuchira: Hapana mvura inonaya kana yeviolet ruvara inoonekwa mumvura.
ZVIYEDZO ZVAKANAKA
• Melting Range kana Tembiricha 741: 226-230
• Kurasikirwa paKuomesa <731>: Pukuta sampuli pa105 kwe2 h: inorasikirwa neNMT 1.0% yehuremu hwayo.
• Zviri nyore Carbonizable Substances Test 271
Sample solution: 40 mg/mL mu sulfuric acid (94.5% -95.5% [w/w] yeH2SO4), yakachengetedzwa pa48-50 ye10 min.
Maitiro ekugamuchira: Sample solution haina rumwe ruvara kupfuura Matching Fluid A, kana ichionekwa pakatarisana nechena kumashure.
• Kujeka Kwemhinduro
[Cherechedza-Mushonga weSample unofananidzwa neReference suspension A uye kumvura mumasikati machena maminetsi mashanu mushure mekugadzirira Reference kumiswa A.]
Diluent: 200-g/L mhinduro ye sodium acetate
Hydrazine solution: 10.0 mg/mL ye hydrazine sulfate.[Cherechedza-Bvumira kumira kwe4-6 h.]
Methenamine solution: Kuendesa 2.5 g yemethenamine kune 100-mL glass-stoppered flask, wedzera 25.0 mL yemvura, isa chivharo chegirazi, uye sanganisa kuti unyunguduke.
Primary opalescent suspension: Kuendesa 25.0 mL yeHydrazine solution kune Methenamine solution mu100-mL glass-stoppered flask.Sanganisa, uye bvumira kumira kwe24 h.[Cherechedza-Kuturika uku kwakagadzikana kwemwedzi miviri, kunze kwekunge yachengetwa mugaba regirazi risina kuremara.Iyo yekumisa haifanire kuomerera kune girazi uye inofanira kunge yakanyatso kusanganiswa isati yashandiswa.Bvumira kumisa kumira kwe24 h.]
Opalescence standard: Dilute 15.0 mL yePrimary opalescent kuturika nemvura kusvika ku1000 mL.[Cherechedza-Uku kuturika hakufanirwe kushandiswa kupfuura 24 h mushure mekugadzirira.]
Reference kumiswa A: Opalescence chiyero uye mvura (1 mu20)
Reference kumiswa B: Opalescence chiyero uye mvura (1 mu10)
Sample solution: 200 mg/mL mu Diluent
Analysis
Samples: Diluent, Reference suspension A, Reference suspension B, Sample solution, uye mvura.
Tumira chikamu chakakwana cheSample solution kune test tube yegirazi isina ruvara, yakajeka, isina kwayakarerekera ine chigadziko chakafuratira uye dhayamita yemukati ye15-25 mm kuti uwane kudzika kwe40 mm.Saizvozvo fambisa zvikamu zveReference suspension A, Reference suspension B, mvura, uye Diluent kuti iparadzanise machubhu ekuyedza anoenderana.Enzanisa zvigadziriso muchiedza chemasikati chakapararira, uchiona wakamira uchitarisana nemashure matema (ona Spectrophotometry uye Chiedza-Kuparadzira 851, Visual Comparison).[Cherechedza—Kupararira kwechiedza kunofanira kunge kwakaita kuti Reference suspension A igone kusiyaniswa kubva mumvura, uye kuti Reference kuturika B inogona kusiyaniswa zviri nyore kubva kune Reference suspension A. ]
Maitiro ekugamuchira: Mushonga weSample unoratidza kujeka kwakafanana nekwemvura, kana Diluent, kana kuti opalescence yayo iNMT iya yeReference suspension A.
• Ruvara rweKugadzirisa
Diluent A: 200-g/L mhinduro ye sodium acetate
Diluent B: 10-g/L mhinduro yehydrochloric acid
Standard stock solution: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, uye Diluent B (3.0:3.0:2.4:1.6)
Yakajairwa mhinduro: Yakajairika stock solution uye Diluent B (1 mu100).[Cherechedza-Gadzirira mhinduro yeStandard pakarepo usati washandisa.]
Sample solution: Shandisa Sample solution kubva muyedzo yeClarity of Solution.
Analysis
Samples: Diluent A, Standard solution, Sample solution, uye mvura
Tumira chikamu chakakwana cheSample solution kune test tube yegirazi isina ruvara, yakajeka, isina kwayakarerekera ine chigadziko chakafuratira uye dhayamita yemukati ye15-25 mm kuti uwane kudzika kwe40 mm.Saizvozvo fambisa zvikamu zveiyo Standard mhinduro, Diluent A, uye mvura kuti iparadzanise, inoenderana nebvunzo machubhu.Enzanisa zvigadziriso muchiedza chemasikati chakapararira, uchitarisa wakamira uchitarisana neshure chena (ona Spectrophotometry uye Chiedza-Kuparadzira 851, Visual Comparison).
Maitiro ekugamuchira: Sample solution ine chitarisiko chemvura kana Diluent A, kana kuti haina kunyanya kupenya kupfuura iyo Standard solution.
ZVIMWE ZVINODIWA
• Kurongedza uye Kuchengeta: Chengetedza mumidziyo yakavharwa zvakanaka.Chengetedza pane tembiricha yekamuri.
• USP Reference Standards <11>
USP Saccharin RS Dzvanya kuti uone Chimiro
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS