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

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3 (2H) -daya, 1,1-dioxide;
1,2-Benzisothiazolin-3-daya 1,1-dioxide [81-07-2].
BAYANI
Saccharin ya ƙunshi NLT 99.0% da NMT 101.0% na C7H5NO3S, ƙididdiga akan busasshen tushe.
GANO
• Shakar Infrared <197K>
ASSAY
• Tsari
Misali: 500 MG
Analysis: Narke Samfurin a cikin 40 ml na barasa.Ƙara 40 ml na ruwa da phenolphthalein TS.Titrate tare da 0.1 N sodium hydroxide.Yi titration mara kyau, idan ya cancanta, kuma a yi gyaran da ya dace.Kowane ml na 0.1 N sodium hydroxide yayi daidai da 18.32 MG na C7H5NO3S.
Sharuɗɗan karɓa: 99.0% -101.0% akan busasshen tushe
RASHIN ZUCIYA
Najasa Na Inorganic
• Ragowa akan ƙonewa <281>: NMT 0.2%.Matsakaicin zafin wuta shine 600 ± 50.
• Karfe masu nauyi, Hanyar II <231>: NMT 10 ppm
Najasa Na Halitta
Hanyar 1: Iyakar Toluenesulfonamides
Maganin daidaitaccen ciki: 0.25 mg/mL na maganin kafeyin a cikin methylene chloride
Daidaitaccen bayani na hannun jari: 20.0 μg/ml na USP o-Toluenesulfonamide RS da 20.0 μg/ml na USP p-Toluenesulfonamide RS a cikin methylene chloride
Daidaitaccen Magani: Haɓaka 5.0 ml na daidaitaccen maganin haja zuwa bushewa a cikin rafi na nitrogen.Narkar da ragowar a cikin 1 ml na daidaitaccen bayani na Ciki.
Maganin samfurin: Dakatar da 10 g na Saccharin a cikin 20 ml na ruwa, kuma narke ta amfani da 5-6 ml na 10 N sodium hydroxide.Idan ya cancanta, daidaita maganin tare da 1 N sodium hydroxide ko 1 N hydrochloric acid zuwa pH na 7-8, kuma tsarma da ruwa zuwa 50 ml.Girgiza maganin tare da adadi huɗu kowanne na 50 ml na methylene chloride.Haɗa ƙananan yadudduka, bushe a kan sodium sulfate mara ruwa, da tace.A wanke tacewa da sodium sulfate tare da 10 ml na methylene chloride.Haɗa maganin da wankewa, da kuma ƙafe kusan bushewa a cikin wanka na ruwa a zafin jiki wanda bai wuce 40 ba. Yin amfani da ƙaramin adadin methylene chloride, ƙididdige yawan canja wurin saura a cikin bututun 10-mL mai dacewa, ƙafe zuwa bushewa a cikin rafi na nitrogen, da kuma narkar da ragowar a cikin 1.0 ml na daidaitaccen bayani na ciki.
Maganin Blank: Kashe 200 ml na methylene chloride zuwa bushewa a cikin wanka na ruwa a zafin jiki wanda bai wuce 40 ba. Narke ragowar a cikin 1 ml na methylene chloride.
Tsarin chromatographic
(Duba Chromatography <621>, Dacewar Tsarin.)
Yanayin: GC
Mai ganowa: ionization na harshen wuta
Tushen: 0.53-mm × 10-m Fused silica ginshiƙi, mai rufi da G3 lokaci (fim kauri 2 µm)
Zazzabi
Inji: 250
Mai ganowa: 250
Shafin: 180
Mai ɗaukar iskar gas: Nitrogen
Yawan kwarara: 10 ml/min
Girman allura: 1 µL
Raba rabo: 2:1
Dacewar tsarin
Samfurori: Daidaitaccen Magani da Maganin Blank
[Lura-Abubuwan da aka lalata su a cikin tsari mai zuwa: o-toluenesulfonamide, p-toluenesulfonamide, da maganin kafeyin.]
Abubuwan da suka dace: Babu kololuwa a lokutan riƙewa don daidaitattun ciki, o-toluenesulfonamide, ko p-toluenesulfonamide;Magani mara kyau
Resolution: NLT 1.5 tsakanin o-toluenesulfonamide da p-toluenesulfonamide, Standard bayani
Bincike
Samfurori: Daidaitaccen bayani da Samfurin bayani
Sharuɗɗan karɓa: Idan kowane kololuwa saboda o-toluenesulfonamide da p-toluenesulfonamide sun bayyana a cikin chromatogram da aka samu tare da Maganin Samfurin, rabon yankunansu zuwa na daidaitaccen daidaitaccen bayani na ciki shine NMT daidaitaccen rabo a cikin chromatogram da aka samu tare da daidaitaccen bayani. .
Najasa ɗaya: Dubi Shafukan Najasa 1.
Tebur Najasa 1
Sharuɗɗan Karɓar Suna (ppm)
o-Toluenesulfonamide 10
P-Toluenesulfonamide 10
Hanyar 2: Iyakar Benzoate da Salicylate
Samfurin bayani: 10 ml na zafi, cikakken bayani na saccharin
Analysis: Ƙara ferric chloride TS dropwise zuwa Samfurin bayani.
Sharuɗɗan karɓa: Babu hazo ko launin ruwan violet da ke bayyana a cikin ruwa.
MAKAMMAN JARRABAWA
• Rage Narkewa ko Zazzabi 741: 226-230
• Asara akan bushewa <731>: Busa samfurin a 105 don 2 h: yana rasa NMT 1.0% na nauyinsa.
• Gwajin Kayayyakin Kayayyakin Gaggawa 271
Maganin samfurin: 40 mg / mL a cikin sulfuric acid (94.5% -95.5% [w / w] na H2SO4), kiyayewa a 48-50 don 10 min
Sharuɗɗan karɓa: Maganin samfurin ba shi da launi fiye da Matching Fluid A, lokacin da aka duba shi da farin bango.
• Bayyanar Magani
[Lura-Mafilar samfurin shine za a kwatanta shi da dakatarwar Reference A da ruwa a cikin hasken rana 5 mins bayan shirye-shiryen dakatarwar Reference A.]
Diluent: 200-g/L bayani na sodium acetate
Maganin Hydrazine: 10.0 mg/mL na hydrazine sulfate.[Lura-Ba da izinin tsayawa na awa 4-6.]
Maganin Methenamine: Canja wurin 2.5 g na methenamine zuwa gilashin gilashin 100-mL, ƙara 25.0 ml na ruwa, saka gilashin gilashin, da haɗuwa don narke.
Dakatarwar opalescent na farko: Canja wurin 25.0 ml na maganin Hydrazine zuwa maganin Methenamine a cikin faifan gilashin 100-mL.Mix, kuma ba da izinin tsayawa na awa 24.[Lura-Wannan dakatarwar ta tsaya tsayin daka na tsawon watanni 2, muddin an adana ta a cikin kwandon gilashin da ba ta da lahani.Dakatarwar kada ta manne da gilashin kuma dole ne a hade sosai kafin amfani.Bada izinin dakatarwar ta tsaya na awa 24.]
Matsakaicin kyawawa: Tsarma 15.0 ml na Babban dakatarwar opalescent na Farko da ruwa zuwa 1000 ml.[Lura-Kada a yi amfani da wannan dakatarwar fiye da sa'o'i 24 bayan shiri.]
Dakatar da Magana A: Ma'auni mara kyau da ruwa (1 cikin 20)
Dakatar da Magana B: Ma'aunin haske da ruwa (1 cikin 10)
Maganin samfurin: 200 mg / ml a cikin Diluent
Bincike
Samfura: Diluent, Reference Reference A, Reference Reference B, Samfurin Magani, da ruwa
Canja wurin isasshen yanki na Maganin Samfurin zuwa bututun gwaji mara launi, m, gilashin tsaka tsaki tare da tushe mai lebur da diamita na ciki na 15-25 mm don samun zurfin 40 mm.Hakazalika canja wurin ɓangarorin dakatarwar Reference A, Reference Reference B, ruwa, da Diluent don raba bututun gwaji masu dacewa.Kwatanta mafita a cikin hasken rana mai bazuwa, kallo a tsaye kusa da bangon baƙar fata (duba Spectrophotometry da Haske-Watsawa 851, Kwatancen Kayayyakin gani).[Lura-Bayanin haske dole ne ya zama irin wannan dakatarwar Reference A za a iya bambanta da sauri daga ruwa, kuma za a iya bambanta dakatarwar Reference B daga dakatarwar Magana A.]
Sharuɗɗan karɓa: Maganin Samfurin yana nuna tsabta iri ɗaya da na ruwa, ko Diluent, ko ƙarancinsa shine NMT na dakatarwar Reference A.
• Launi na Magani
Diluent A: 200-g/L bayani na sodium acetate
Diluent B: 10-g/L bayani na hydrochloric acid
Daidaitaccen bayani na jari: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, da Diluent B (3.0:3.0:2.4:1.6)
Daidaitaccen Magani: Daidaitaccen bayani na hannun jari da Diluent B (1 cikin 100).[Lura-Shirya Daidaitaccen bayani nan da nan kafin amfani.]
Maganin samfurin: Yi amfani da samfurin samfurin daga gwajin don Bayyanar Magani.
Bincike
Samfurori: Diluent A, Daidaitaccen Magani, Maganin Samfurin, da ruwa
Canja wurin isasshen yanki na Maganin Samfurin zuwa bututun gwaji mara launi, m, gilashin tsaka tsaki tare da tushe mai lebur da diamita na ciki na 15-25 mm don samun zurfin 40 mm.Hakazalika canja wurin sassan daidaitaccen bayani, Diluent A, da ruwa don ware, bututun gwaji masu dacewa.Kwatanta mafita a cikin hasken rana da ke bazuwa, kallo a tsaye da farar bango (duba Spectrophotometry da Haske-Watsawa 851, Kwatancen Kayayyakin gani).
Sharuɗɗan karɓa: Maganin Samfurin yana da bayyanar ruwa ko Diluent A, ko kuma ba shi da tsananin launi fiye da daidaitaccen bayani.
KARIN BUKATA
• Marufi da Ajiya: Ajiye a cikin kwantena da aka rufe sosai.Ajiye a zafin jiki.
• Matsayin Magana na USP <11>
USP Saccharin RS Danna don Duba Tsarin
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS