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

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3 (2H) -ngoe, 1,1-dioxide;
1,2-Benzisothiazolin-3-one 1,1-dioxide [81-07-2].
TLHALOSO
Saccharin e na le NLT 99.0% le NMT 101.0% ea C7H5NO3S, e baloang ka mokhoa o omisitsoeng.
TS'ELISO TS'OANE
• Infrared Absorption <197K>
TLHOKOMELO
• Tsamaiso
Mohlala: 500 mg
Tlhahlobo: Qolla Mohlala ho 40 ml ea joala.Kenya 40 ml ea metsi le phenolphthalein TS.Titrate ka 0.1 N sodium hydroxide.Etsa lengolo le se nang letho, haeba ho hlokahala, 'me u etse tokiso e nepahetseng.ML e 'ngoe le e' ngoe ea 0.1 N sodium hydroxide e lekana le 18.32 mg ea C7H5NO3S.
Mekhoa ea ho amohela: 99.0% -101.0% motheong o omisitsoeng
LITŠILA
Tšilafalo ea Inorganic
• Masalla a ho Ignition <281>: NMT 0.2%.Mocheso oa mocheso ke 600 ± 50.
• Heavy Metals, Mokhoa oa II <231>: NMT 10 ppm
Litšila tsa Organic
• Mokhoa oa 1: Moeli oa Toluenesulfonamides
Tharollo e tloaelehileng ea ka hare: 0.25 mg / mL ea caffeine ka methylene chloride
Tharollo e tloaelehileng ea setoko: 20.0 µg/mL ea USP o-Toluenesulfonamide RS le 20.0 µg/mL ea USP p-Toluenesulfonamide RS ho methylene chloride
Tharollo e tlwaelehileng: Moyafafatsa 5.0 mL ya tharollo ya setoko se Tlwaelehileng hore e omelle mokgweng wa naetrojene.Qhala masalla ka 1 mL ea tharollo e tloaelehileng ea ka Hare.
Mohlala oa tharollo: Emisa 10 g ea Saccharin ka 20 ml ea metsi, 'me u qhale ka 5-6 mL ea 10 N sodium hydroxide.Haeba ho hlokahala, fetola tharollo ka 1 N sodium hydroxide kapa 1 N hydrochloric acid ho pH ea 7-8, 'me u hlapolle ka metsi ho 50 ml.Hlohlelletsa tharollo ka litekanyo tse 'ne ho e' ngoe le e 'ngoe ea 50 ml ea methylene chloride.Kopanya likarolo tse ka tlase, omisa holim'a anhydrous sodium sulfate, le sefa.Hlatsoa sefe le sodium sulfate ka 10 mL ea methylene chloride.Kopanya tharollo le ho hlatsoa, ​​'me u fetohe mouoane hoo e ka bang ho omella ka bateng ea metsi ka mocheso o sa feteng 40. U sebelisa tekanyo e nyenyane ea methylene chloride, ka bongata fetisetsa masalla ka har'a tube e loketseng ea 10-mL, e fetoha mouoane ho omella ka molapo oa naetrojene, le ho qhala masalla ka 1.0 mL ea tharollo e tloaelehileng ea ka Hare.
Tharollo e se nang letho: Fafatsa 200 mL ea methylene chloride ho omella ka bateng ea metsi ka mocheso o sa feteng 40. Qhala masalla ka 1 mL ea methylene chloride.
Sistimi ea chromatographic
(Sheba Chromatography <621>, Ho Hlokahala Sistimi.)
Mokhoa: GC
Mohloli: Ionization ea mollo
Kholomo: 0.53-mm × 10-m kholomo ea silica e kopantsoeng, e koahetsoeng ka karolo ea G3 (botenya ba filimi 2 µm)
Mocheso
Ente: 250
Mosireletsi: 250
Lebala: 180
Khase e tsamaisang thepa: Nitrogen
Sekhahla sa phallo: 10 mL / min
Boholo ba ente: 1 µL
Arohane karo-karolelano: 2:1
Ho nepahala ha sistimi
Mehlala: Tharollo e tloaelehileng le tharollo e se nang letho
[Tlhokomeliso-Lintho li hlahisoa ka tatellano e latelang: o-toluenesulfonamide, p-toluenesulfonamide, le caffeine.]
Litlhoko tsa ho tšoaneleha: Ha ho litlhōrō ka nako ea ho boloka maemo a ka hare, o-toluenesulfonamide, kapa p-toluenesulfonamide;Tharollo e se nang letho
Qeto: NLT 1.5 pakeng tsa o-toluenesulfonamide le p-toluenesulfonamide, tharollo e tloaelehileng
Tlhahlobo
Mehlala: Tharollo e tloaelehileng le Tharollo ea Mohlala
Mekhoa ea ho amohela: Haeba litlhōrō leha e le life ka lebaka la o-toluenesulfonamide le p-toluenesulfonamide li hlaha ka har'a chromatogram e fumanoeng ka Tharollo ea Mohlala, karo-karolelano ea libaka tsa bona ho ea tharollo ea ka hare ea ka hare ke NMT tekanyo e lumellanang le chromatogram e fumanoang ka tharollo e tloaelehileng. .
Litšila tsa motho ka mong: Sheba Lethathamo la 1 la Tšilafalo.
Lethathamo la 1 la Tšilafalo
Melao ea Kamohelo ea Lebitso (ppm)
O-Toluenesulfonamide 10
P-Toluenesulfonamide 10
• Mokhoa oa 2: Moeli oa Benzoate le Salicylate
Tharollo ea mohlala: 10 ml ea tharollo e chesang, e tletseng saccharin
Tlhahlobo: Eketsa ferric chloride TS dropwise ho Sample solution.
Mekhoa ea ho amohela: Ha ho na 'mala oa pula kapa violet o hlahang ka har'a mokelikeli.
LITEKO TSEKO
• Melting Range kapa Mocheso 741: 226-230
• Tahlehelo ha o Omisa <731>: Omisa sampole ka 105 bakeng sa 2 h: e lahleheloa ke NMT 1.0% ea boima ba eona.
• Teko ea Lisebelisuoa tse Ka Bonolo 271
Tharollo ea mohlala: 40 mg/mL ka sulfuric acid (94.5% -95.5% [w/w] ea H2SO4), e bolokiloe ho 48-50 bakeng sa metsotso ea 10
Mekhoa ea ho amohela: Tharollo ea Mohlala ha e na mebala e fetang Matching Fluid A, ha e talingoa khahlano le bokamorao bo bosoeu.
• Ho hlaka ha Tharollo
[Tlhokomeliso-Mohlala oa Tharollo e lokela ho bapisoa le Reference suspension A le ho nosetsa motšehare ka metsotso e 5 ka mor'a ho lokisa Reference suspension A.]
Diluent: 200-g/L tharollo ea sodium acetate
Tharollo ea Hydrazine: 10.0 mg/mL ea hydrazine sulfate.[Tlhokomeliso-Lumella ho ema bakeng sa 4-6 h.]
Tharollo ea Methenamine: Fetisetsa 2.5 g ea methenamine ho 100-mL e emisitsoeng ka khalase, eketsa 25.0 mL ea metsi, kenya sekoahelo sa khalase, 'me u kopanye ho qhibiliha.
Ho emisoa ha opalescent ea mantlha: Fetisetsa 25.0 mL ea tharollo ea Hydrazine ho tharollo ea Methenamine ka botlolong e emisitsoeng ka khalase ea 100-mL.Kopanya, 'me u lumelle ho ema bakeng sa 24 h.[Tlhokomeliso-Tlhahiso ena e tsitsitse bakeng sa likhoeli tse 2, ha feela e bolokoa ka har'a sets'oants'o sa khalase ntle le likoli.Ho emisoa ha hoa lokela ho khomarela khalase 'me ho tlameha ho tsoakana hantle pele ho sebelisoa.Lumella ho emisoa ho ema bakeng sa 24 h.]
Tekanyetso ea Opalescence: Hlakola 15.0 mL ea ho emisoa ha Primary opalescent ka metsi ho isa ho 1000 mL.[Tlhokomeliso-Ho emisoa hona ha hoa lokela ho sebelisoa ho feta lihora tse 24 ka mor'a tokisetso.]
Reference suspension A: Opalescence standard le metsi (1 ho 20)
Reference suspension B: Opalescence standard le metsi (1 ho 10)
Tharollo ea mohlala: 200 mg/mL ho Diluent
Tlhahlobo
Mehlala: Diluent, Reference suspension A, Reference suspension B, Sample solution, le metsi
Fetisetsa karolo e lekaneng ea Tharollo ea Mohlala ho tube ea teko ea khalase e se nang mebala, e bonaletsang, e sa nke lehlakore e nang le setsi se bataletseng le bophara ba ka hare ba 15-25 mm ho fumana botebo ba 40 mm.Ka mokhoa o ts'oanang fetisetsa likarolo tsa Reference suspension A, Reference suspension B, metsi, le Diluent ho arola li-tubes tsa teko tse nyallanang.Bapisa litharollo motšehare o pharalletseng, o shebelletse o otlolohile khahlano le bokapele bo botšo (sheba Spectrophotometry le Light-Scattering 851, Visual Comparison).[Hlokomela—Karohano ea leseli e tlameha ho ba ea hore Reference suspension A e ka khetholleha habonolo ho metsi, le hore Reference suspension B e ka khetholloa habonolo ho Reference suspension A. ]
Maemo a kamohelo: Tharollo ea Mohlala e bontša ho hlaka joalo ka ha metsi, kapa Diluent, kapa opalescence ea eona ke NMT ea Reference suspension A.
• Mmala oa Tharollo
Diluent A: 200-g/L tharollo ea sodium acetate
Diluent B: 10-g/L tharollo ea hydrochloric acid
Tharollo e tloaelehileng ea setoko: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, le Diluent B (3.0:3.0:2.4:1.6)
Tharollo e tloaelehileng: Tharollo e tloaelehileng ea setoko le Diluent B (1 ho 100).[Hlokomela-Lokisetsa tharollo ea Maemo hang hang pele o sebelisoa.]
Tharollo ea mohlala: Sebelisa Mohlala oa tharollo ho tsoa tekong ea Clarity of Solution.
Tlhahlobo
Mehlala: Diluent A, Tharollo e tloaelehileng, Mehlala ea tharollo, le metsi
Fetisetsa karolo e lekaneng ea Tharollo ea Mohlala ho tube ea teko ea khalase e se nang mebala, e bonaletsang, e sa nke lehlakore e nang le setsi se bataletseng le bophara ba ka hare ba 15-25 mm ho fumana botebo ba 40 mm.Ka mokhoa o ts'oanang, fetisetsa likarolo tsa tharollo e tloaelehileng, Diluent A, le metsi ho arola li-tubes tsa liteko.Bapisa litharollo motšehare o pharalletseng, u shebeletse u otlolohile khahlano le bokapele bo bosoeu (sheba Spectrophotometry and Light-Scattering 851, Visual Comparison).
Mokhoa oa ho amohela: Tharollo ea Mohlala e na le chebahalo ea metsi kapa Diluent A, kapa ha e na 'mala o matla ho feta tharollo e tloaelehileng.
KEKELETSO LIHLOKO
• Ho Paka le ho Boloka: Boloka ka lijaneng tse koetsoeng hantle.Boloka mocheso oa kamore.
• USP Reference Standards <11>
USP Saccharin RS Tobetsa ho Sheba Sebopeho
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS