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

Saccharin
Chithunzi cha C7H5NO3S 183.18
1,2-Benzisothiazol-3 (2H) -imodzi, 1,1-dioxide;
1,2-Benzisothiazolin-3-imodzi 1,1-dioxide [81-07-2].
TANTHAUZO
Saccharin ili ndi NLT 99.0% ndi NMT 101.0% ya C7H5NO3S, yowerengedwa pa zouma.
CHIZINDIKIRO
• Infrared mayamwidwe <197K>
ZOYESA
• Ndondomeko
Chitsanzo: 500 mg
Kusanthula: Sulani Chitsanzo mu 40 ml ya mowa.Onjezerani 40 ml ya madzi ndi phenolphthalein TS.Titrate ndi 0.1 N sodium hydroxide.Chitani mawu opanda kanthu, ngati kuli kofunikira, ndikuwongolera koyenera.ML iliyonse ya 0.1 N sodium hydroxide ndi yofanana ndi 18.32 mg ya C7H5NO3S.
Njira zolandirira: 99.0% -101.0% pazowuma
ZOCHITSA
Zowonongeka Zachilengedwe
• Zotsalira pakuyatsa <281>: NMT 0.2%.Kutentha kwa moto ndi 600 ± 50.
• Zitsulo Zolemera, Njira II <231>: NMT 10 ppm
Zowonongeka Zachilengedwe
• Ndondomeko 1: Malire a Toluenesulfonamides
Njira yothetsera mkati: 0.25 mg/mL ya caffeine mu methylene chloride
Njira yothetsera katundu: 20.0 µg/mL ya USP o-Toluenesulfonamide RS ndi 20.0 µg/mL ya USP p-Toluenesulfonamide RS mu methylene chloride
Yankho lokhazikika: Sungunulani 5.0 mL ya njira yokhazikika ya stock stock kuti iume mumtsinje wa nayitrogeni.Sungunulani zotsalira mu 1 mL ya Internal standard solution.
Yankho lachitsanzo: Imitsani 10 g wa Saccharin mu 20 ml ya madzi, ndikusungunula pogwiritsa ntchito 5-6 mL ya 10 N sodium hydroxide.Ngati ndi kotheka, sinthani yankho ndi 1 N sodium hydroxide kapena 1 N hydrochloric acid kukhala pH ya 7-8, ndikuchepetsa ndi madzi mpaka 50 ml.Gwirani yankho ndi miyeso inayi iliyonse ya 50 mL ya methylene chloride.Phatikizani zigawo zapansi, zouma pa anhydrous sodium sulfate, ndi fyuluta.Tsukani fyuluta ndi sodium sulphate ndi 10 mL ya methylene chloride.Phatikizani yankho ndi kuchapa, ndi nthunzi pafupifupi kuuma mu osamba madzi pa kutentha osapitirira 40. Pogwiritsa ntchito pang'ono methylene kolorayidi, quantitatively kusamutsa zotsalira mu chubu yoyenera 10-mL, nthunzi nthunzi kuuma mu mtsinje wa. nitrogen, ndi kusungunula zotsalira mu 1.0 mL ya Internal standard solution.
Sungunulani 200 mL ya methylene chloride kuti iume mu osamba madzi pa kutentha kosapitirira 40. Sungunulani zotsalira mu 1 mL ya methylene chloride.
Chromatographic system
(Onani Chromatography <621>, Kukwanira Kwadongosolo.)
Njira: GC
Chodziwira: Moto ionization
Mzere: 0.53-mm × 10-m silika wosakanikirana, wokutidwa ndi gawo la G3 (kukhuthala kwa filimu 2 µm)
Kutentha
Injector: 250
Chowunikira: 250
Mzere: 180
Mpweya wonyamula: Nayitrogeni
Kuthamanga: 10 mL / min
Kukula kwa jakisoni: 1 µL
Chiŵerengero chogawanika: 2: 1
Kuyenerera kwadongosolo
Zitsanzo: Njira yokhazikika ndi njira yopanda kanthu
[Zindikirani-Zinthuzi zimachotsedwa motere: o-toluenesulfonamide, p-toluenesulfonamide, ndi caffeine.]
Zofunika Zokwanira: Palibe nsonga pa nthawi yosungiramo muyeso wamkati, o-toluenesulfonamide, kapena p-toluenesulfonamide;Yankho lopanda kanthu
Kusamvana: NLT 1.5 pakati pa o-toluenesulfonamide ndi p-toluenesulfonamide, njira yokhazikika
Kusanthula
Zitsanzo: Yankho lokhazikika ndi yankho lachitsanzo
Njira zolandirira: Ngati nsonga zilizonse chifukwa cha o-toluenesulfonamide ndi p-toluenesulfonamide zikuwonekera mu chromatogram yopezedwa ndi Sample solution, chiŵerengero cha madera awo ndi cha Internal standard solution ndi NMT chiŵerengero chogwirizana mu chromatogram yopezedwa ndi Standard solution. .
Zodetsedwa zapayekha: Onani Table 1.
Table 1
Zoyenera Kulandila Dzina (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Njira 2: Malire a Benzoate ndi Salicylate
Yankho lachitsanzo: 10 ml ya madzi otentha, odzaza saccharin
Kusanthula: Onjezani ferric chloride TS dropwise ku Sample solution.
Njira zolandirira: Palibe mtundu wamadzi kapena mtundu wa violet womwe umapezeka mumadzimadzi.
MAYESO AKE
• Kusungunuka kapena Kutentha 741: 226-230
• Kutaya pakuyanika <731>: Yanikani chitsanzo pa 105 kwa 2 h: imataya NMT 1.0% ya kulemera kwake.
• Kuyesa kwa Zinthu Zowonongeka Kwambiri 271
Njira yothetsera zitsanzo: 40 mg/mL mu sulfuric acid (94.5% -95.5% [w/w] ya H2SO4), yosungidwa pa 48-50 kwa mphindi 10
Njira zolandirira: Yankho lachitsanzo liribenso mtundu kuposa Matching Fluid A, likawonedwa motsutsana ndi maziko oyera.
• Kumveka kwa Yankho
[Zindikirani-Yankho lachitsanzo liyenera kufananizidwa ndi kuyimitsidwa kwa Reference A komanso kuthirira masana masana 5 min pambuyo pokonzekera kuyimitsidwa kwa Reference A.]
Diluent: 200-g/L yankho la sodium acetate
Njira yothetsera hydrazine: 10.0 mg/mL ya hydrazine sulfate.[Zindikirani-Lolani kuyimirira kwa 4-6 h.]
Yankho la Methenamine: Chotsani 2.5 g wa methenamine mu botolo loyimitsa galasi la 100-mL, onjezerani 25.0 mL yamadzi, ikani choyimitsira galasi, ndi kusakaniza kuti musungunuke.
Kuyimitsidwa koyambirira kwa opalescent: Tumizani 25.0 mL ya Hydrazine yankho ku yankho la Methenamine mu botolo loyimitsidwa ndi galasi la 100-mL.Sakanizani, ndipo mulole kuyimirira kwa 24 h.[Zindikirani-Kuyimitsidwaku kumakhala kokhazikika kwa miyezi iwiri, pokhapokha ngati kusungidwa mumtsuko wagalasi wopanda zopindika.Kuyimitsidwa sikuyenera kumamatira ku galasi ndipo kuyenera kusakanikirana bwino musanagwiritse ntchito.Lolani kuyimitsidwa kuyimitsidwa kwa 24 h.]
Muyezo wa Opalescence: Sungunulani 15.0 mL ya kuyimitsidwa kwa Primary opalescent ndi madzi mpaka 1000 mL.[Zindikirani-Kuyimitsa uku sikuyenera kugwiritsidwa ntchito kupitirira maola 24 mutakonzekera.]
Reference kuyimitsidwa A: Opalescence muyezo ndi madzi (1 mu 20)
Reference kuyimitsidwa B: Opalescence muyezo ndi madzi (1 mu 10)
Yankho lachitsanzo: 200 mg/mL mu Diluent
Kusanthula
Zitsanzo: Diluent, Reference kuyimitsidwa A, Reference kuyimitsidwa B, Sample solution, ndi madzi
Tumizani gawo lokwanira la Sample solution ku chubu choyesera cha magalasi opanda mtundu, owonekera, osalowerera ndale okhala ndi maziko athyathyathya ndi mainchesi amkati a 15-25 mm kuti mupeze kuya kwa 40 mm.Mofananamo, sinthani magawo a Reference suspension A, Reference suspension B, madzi, ndi Diluent kuti alekanitse machubu ofananira oyeserera.Yerekezerani zoyankhira masana osakanikirana, kuyang'ana moyimirira kumbuyo kwakuda (onani Spectrophotometry ndi Light-Scattering 851, Visual Comparison).[Zindikirani—Kufalikira kwa kuwala kuyenera kukhala kotero kuti kuyimitsidwa kwa Reference A kungasiyanitsidwe mosavuta ndi madzi, komanso kuti kuyimitsidwa kwa Reference B kungasiyanitsidwe mosavuta ndi Reference suspension A. ]
Njira zolandirira: Yankho lachitsanzo likuwonetsa kumveka kofanana ndi kwamadzi, kapena Diluent, kapena mawonekedwe ake ndi NMT ya Reference suspension A.
• Mtundu wa Njira
Diluent A: 200-g/L yankho la sodium acetate
Diluent B: 10-g/L yankho la hydrochloric acid
Njira yothetsera katundu wokhazikika: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, ndi Diluent B (3.0:3.0:2.4:1.6)
Yankho lokhazikika: Njira yokhazikika yamasheya ndi Diluent B (1 mu 100).[Zindikirani-Konzani yankho la Standard nthawi yomweyo musanagwiritse ntchito.]
Yankho lachitsanzo: Gwiritsani ntchito Chitsanzo cha yankho kuchokera ku mayeso a Clarity of Solution.
Kusanthula
Zitsanzo: Diluent A, njira yokhazikika, njira yothetsera, ndi madzi
Tumizani gawo lokwanira la Sample solution ku chubu choyesera cha magalasi opanda mtundu, owonekera, osalowerera ndale okhala ndi maziko athyathyathya ndi mainchesi amkati a 15-25 mm kuti mupeze kuya kwa 40 mm.Momwemonso sinthani magawo a Standard solution, Diluent A, ndi madzi kuti asiyanitse, machubu oyeserera.Yerekezerani zoyankhira masana osakanikirana, kuyang'ana moyimilira kuseri koyera (onani Spectrophotometry ndi Light-Scattering 851, Visual Comparison).
Njira zolandirira: Yankho lachitsanzo lili ndi mawonekedwe amadzi kapena Diluent A, kapena silikhala lakuda kwambiri kuposa yankho lokhazikika.
ZOWONJEZERA ZOFUNIKA
• Kupaka ndi Kusunga: Sungani m’zotengera zotsekedwa bwino.Sungani kutentha.
• USP Reference Standards <11>
USP Saccharin RS Dinani kuti muwone Kapangidwe
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS