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

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3(2H)-ib, 1,1-dioxide;
1,2-Benzisothiazolin-3-ib 1,1-dioxide [81-07-2].
DEFINITION
Saccharin muaj NLT 99.0% thiab NMT 101.0% ntawm C7H5NO3S, suav ntawm lub hauv paus qhuav.
IDENTIFICATION
• Infrared Absorption <197K>
QHIA
• Cov txheej txheem
Qauv: 500 mg
Kev tsom xam: Dissove cov qauv hauv 40 mL cawv.Ntxiv 40 mL dej thiab phenolphthalein TS.Titrate nrog 0.1 N sodium hydroxide.Ua ib qho titration dawb paug, yog tias tsim nyog, thiab kho qhov tsim nyog.Txhua mL ntawm 0.1 N sodium hydroxide yog sib npaug rau 18.32 mg ntawm C7H5NO3S.
Kev lees txais: 99.0% -101.0% ntawm lub hauv paus qhuav
IMPURITIES
Inorganic impurities
• Residue ntawm Ignition <281>: NMT 0.2%.ignition kub yog 600 ± 50.
• Heavy Metals, Method II <231>: NMT 10 ppm
Organic impurities
• Txheej txheem 1: txwv ntawm Toluenesulfonamides
Cov txheej txheem sab hauv: 0.25 mg / mL ntawm caffeine hauv methylene chloride
Standard Tshuag tov: 20.0 µg/mL ntawm USP o-Toluenesulfonamide RS thiab 20.0 µg/mL ntawm USP p-Toluenesulfonamide RS nyob rau hauv methylene chloride
Standard tov: Evaporate 5.0 mL ntawm Standard Tshuag tov rau dryness nyob rau hauv ib tug kwj ntawm nitrogen.Dissolve qhov seem nyob rau hauv 1 mL ntawm Internal standard tov.
Piv txwv li: Tshem tawm 10 g ntawm Saccharin hauv 20 mL dej, thiab yaj siv 5-6 mL ntawm 10 N sodium hydroxide.Yog tias tsim nyog, kho cov tshuaj nrog 1 N sodium hydroxide lossis 1 N hydrochloric acid rau pH ntawm 7-8, thiab dilute nrog dej mus rau 50 mL.Co cov tshuaj nrog plaub qhov ntau ntawm 50 mL ntawm methylene chloride.Muab cov khaubncaws sab nraud povtseg, qhuav dhau anhydrous sodium sulfate, thiab lim.Ntxuav lub lim thiab sodium sulfate nrog 10 mL ntawm methylene chloride.Muab cov tshuaj tov thiab cov tshuaj ntxuav, thiab evaporate yuav luag kom qhuav nyob rau hauv ib da dej ntawm qhov kub tsis tshaj 40. Siv ib tug me me ntawm methylene chloride, quantitatively hloov cov residue mus rau hauv ib tug haum 10-mL raj, evaporate rau dryness nyob rau hauv ib tug kwj ntawm nitrogen, thiab yaj cov residue hauv 1.0 mL ntawm Internal standard tov.
Cov tshuaj dawb: evaporate 200 mL ntawm methylene chloride kom qhuav nyob rau hauv ib da dej ntawm qhov kub tsis tshaj 40. Dissolve cov residue nyob rau hauv 1 mL ntawm methylene chloride.
Chromatographic system
(Saib Chromatography <621>, System Suitability.)
Qauv: GC
Detector: Nplaim ionization
Kem: 0.53-mm × 10-m fused silica kem, coated nrog G3 theem (zaj duab xis thickness 2 µm)
Kub
Lub cev muaj zog: 250
Detector: 250
Kem: 180
Carrier gas: Nitrogen
Tus nqi ntws: 10 mL / min
Kev txhaj tshuaj loj: 1 µL
Split ratio: 2: 1
Qhov system haum
Cov Qauv: Cov qauv kev daws teeb meem thiab cov tshuaj dawb
[Ceeb toom-Cov tshuaj yog eluted raws li nram no: o-toluenesulfonamide, p-toluenesulfonamide, thiab caffeine.]
Cov kev cai tsim nyog: Tsis muaj qhov siab tshaj ntawm lub sijhawm khaws cia rau tus qauv sab hauv, o-toluenesulfonamide, lossis p-toluenesulfonamide;Kev daws teeb meem
Kev daws teeb meem: NLT 1.5 ntawm o-toluenesulfonamide thiab p-toluenesulfonamide, Standard tov
Kev tsom xam
Qauv: Cov qauv kev daws teeb meem thiab cov qauv kev daws teeb meem
Kev lees txais cov txheej txheem: Yog tias ib qho peaks vim yog o-toluenesulfonamide thiab p-toluenesulfonamide tshwm sim hauv chromatogram tau nrog cov qauv tshuaj, qhov piv ntawm lawv cov cheeb tsam rau qhov kev daws teeb meem sab hauv yog NMT qhov sib piv piv hauv chromatogram tau nrog cov txheej txheem daws teeb meem. .
Ib tug neeg impurities: Saib Impurity Table 1.
Impurity Table 1
Kev lees paub lub npe (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Txheej txheem 2: Kev txwv ntawm Benzoate thiab Salicylate
Piv txwv li: 10 mL ntawm ib tug kub, saturated tov ntawm saccharin
Kev Ntsuam Xyuas: Ntxiv ferric chloride TS dropwise rau cov qauv tshuaj.
Kev lees txais cov qauv: Tsis muaj xim av lossis xim violet tshwm hauv cov kua.
TSEEM CEEB
• Melting Range lossis Kub 741: 226-230
• Poob rau ziab <731>: Qhuav ib qho qauv ntawm 105 rau 2 h: nws poob NMT 1.0% ntawm nws qhov hnyav.
• Npaj Cov Khoom Siv Carbonizable Test 271
Cov qauv tshuaj: 40 mg / mL hauv sulfuric acid (94.5% - 95.5% [w / w] ntawm H2SO4), khaws cia ntawm 48-50 rau 10 min
Kev lees txais cov qauv: Cov qauv kev daws teeb meem tsis muaj xim ntau dua li Matching Fluid A, thaum saib tawm tsam tom qab dawb.
• Clarity of Solution
[Ceeb toom-Cov qauv kev daws teeb meem yog muab piv rau Reference suspension A thiab dej hauv nruab hnub nrig 5 min tom qab kev npaj ntawm Reference suspension A.]
Diluent: 200-g / L daws ntawm sodium acetate
Hydrazine daws: 10.0 mg / mL ntawm hydrazine sulfate.[Ceeb Toom-Thov sawv ntsug li 4-6 teev.]
Cov tshuaj Methenamine: Hloov 2.5 g ntawm methenamine mus rau 100-mL iav-stoppered khob, ntxiv 25.0 mL dej, ntxig rau iav stopper, thiab sib tov kom yaj.
Thawj thawj opalescent ncua: Hloov 25.0 mL ntawm Hydrazine tov rau cov tshuaj Methenamine nyob rau hauv 100-mL iav-stoppered hwj.Sib tov, thiab cia sawv ntsug rau 24 teev.[Ceeb toom-Qhov kev ncua no ruaj khov rau 2 lub hlis, yog tias nws tau muab khaws cia rau hauv lub khob ntim tsis muaj qhov tsis xws luag.Lub ncua kev kawm ntawv yuav tsum tsis txhob ua raws li cov iav thiab yuav tsum tau zoo sib tov ua ntej siv.Cia lub ncua sij hawm sawv ntsug rau 24 teev.]
Cov txheej txheem Opalescence: Dilute 15.0 mL ntawm lub hauv paus opalescent suspension nrog dej mus rau 1000 mL.[Ceeb toom-Qhov kev ncua yuav tsum tsis txhob siv dhau 24 teev tom qab kev npaj.]
Reference suspension A: Opalescence standard thiab dej (1 ntawm 20)
Reference suspension B: Opalescence standard thiab dej (1 ntawm 10)
Sample tov: 200 mg / mL hauv Diluent
Kev tsom xam
Qauv: Diluent, Reference suspension A, Reference suspension B, Sample solution, thiab dej
Hloov ib feem txaus ntawm cov qauv kev daws teeb meem mus rau ib lub raj uas tsis muaj xim, pob tshab, nruab nrab iav nrog lub hauv paus tiaj tus thiab ib txoj kab uas hla ntawm 15-25 hli kom tau qhov tob ntawm 40 hli.Ib yam li lwm qhov kev hloov pauv ntawm Reference suspension A, Reference suspension B, dej, thiab Diluent kom cais cov raj sib txuam.Sib piv cov kev daws teeb meem nyob rau nruab hnub nrig, saib vertically tiv thaiv keeb kwm yav dhau dub (saib Spectrophotometry thiab Light-Scattering 851, Visual Comparison).[Faj seeb—Lub diffusion ntawm lub teeb yuav tsum yog xws li hais tias Reference suspension A tuaj yeem paub qhov txawv ntawm dej, thiab Reference suspension B tuaj yeem paub qhov txawv ntawm Reference suspension A.]
Kev lees txais cov qauv: Cov qauv kev daws teeb meem qhia pom qhov tseeb tib yam li cov dej, lossis Diluent, lossis nws qhov opalescence yog NMT uas ntawm Reference suspension A.
• Xim tshuaj
Diluent A: 200-g / L daws ntawm sodium acetate
Diluent B: 10-g / L daws ntawm hydrochloric acid
Cov txheej txheem kev daws teeb meem: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, thiab Diluent B (3.0: 3.0: 2.4: 1.6)
Standard tov: Standard Tshuag tov thiab Diluent B (1 ntawm 100).[Ceeb Toom- Npaj cov txheej txheem daws tam sim ua ntej siv.]
Sample solution: Siv cov qauv kev daws teeb meem los ntawm kev sim rau Clarity of Solution.
Kev tsom xam
Qauv: Diluent A, Standard tov, Sample tov, thiab dej
Hloov ib feem txaus ntawm cov qauv kev daws teeb meem mus rau ib lub raj uas tsis muaj xim, pob tshab, nruab nrab iav nrog lub hauv paus tiaj tus thiab ib txoj kab uas hla ntawm 15-25 hli kom tau qhov tob ntawm 40 hli.Ib yam li lwm qhov ntawm cov txheej txheem kev daws teeb meem, Diluent A, thiab dej kom sib cais, sib piv cov raj.Sib piv cov kev daws teeb meem nyob rau nruab hnub nrig, saib vertically tiv thaiv cov keeb kwm yav dhau dawb (saib Spectrophotometry thiab Light-Scattering 851, Visual Comparison).
Kev lees txais cov qauv: Cov qauv kev daws teeb meem muaj qhov pom ntawm cov dej los yog Diluent A, lossis tsis muaj xim ntau dua li cov qauv kev daws teeb meem.
TSEEM CEEB
• Ntim thiab Cia: Khaws rau hauv cov thawv kaw kom zoo.Khaws ntawm chav tsev kub.
• USP Reference Standards <11>
USP Saccharin RS Nyem rau Saib Cov Qauv
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS