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

I-Saccharin
I-C7H5NO3S 183.18
I-1,2-Benzisothiazol-3(2H)-enye, i-1,1-dioxide;
I-1,2-Benzisothiazolin-3-one 1,1-dioxide [81-07-2].
INCAZELO
I-Saccharin iqukethe i-NLT 99.0% kanye ne-NMT 101.0% ye-C7H5NO3S, abalwe ngokomisiwe.
UKUKHOMBA
• I-Infrared Absorption <197K>
ISIVIVINYO
• Inqubo
Isampula: 500 mg
Ukuhlaziya: Susa Isampula ku-40 mL wotshwala.Engeza u-40 mL wamanzi kanye ne-phenolphthalein TS.Titrate nge-0.1 N sodium hydroxide.Yenza i-titration engenalutho, uma kunesidingo, futhi wenze ukulungisa okufanele.I-mL ngayinye ka-0.1 N sodium hydroxide ilingana no-18.32 mg we-C7H5NO3S.
Indlela yokwamukela: 99.0% -101.0% ngokomisiwe
UKUNGCOLA
Ukungcola Okungaphili
• Insalela Ekuthutheni <281>: NMT 0.2%.Izinga lokushisa lomlilo lingama-600 ± 50.
• I-Heavy Metals, Indlela II <231>: NMT 10 ppm
Ukungcola Okuphilayo
• Inqubo 1: Umkhawulo we-Toluenesulfonamides
Isixazululo esijwayelekile sangaphakathi: 0.25 mg/mL we-caffeine ku-methylene chloride
Isixazululo esijwayelekile sesitoko: 20.0 µg/mL we-USP o-Toluenesulfonamide RS kanye no-20.0 µg/mL we-USP p-Toluenesulfonamide RS ku-methylene chloride
Isixazululo esijwayelekile: Junguza u-5.0 mL wesisombululo sesitoko Esijwayelekile endaweni yokoma emgudwini we-nitrogen.Chaza insalela ngo-1 mL wesixazululo esijwayelekile sangaphakathi.
Isixazululo sesampula: Misa u-10 g we-Saccharin ku-20 mL wamanzi, futhi uhlakaze usebenzisa u-5-6 mL we-10 N sodium hydroxide.Uma kunesidingo, lungisa isixazululo nge-1 N sodium hydroxide noma i-1 N hydrochloric acid ibe i-pH engu-7-8, bese uhlanza ngamanzi ku-50 mL.Nyakazisa ikhambi ngamanani amane lilinye lika-50 mL we-methylene chloride.Hlanganisa izingqimba ezingezansi, zome phezu kwe-anhydrous sodium sulfate, nesihlungi.Geza isihlungi kanye ne-sodium sulfate ngo-10 mL we-methylene chloride.Hlanganisa isixazululo nokuwasha, bese uhwamuke ucishe wome emanzini okugeza ngamanzi endaweni yokushisa engeqile ku-40. Usebenzisa inani elincane le-methylene chloride, dlulisa insalela ngobuningi ube yishubhu elifanele elingu-10-mL, uhwamuke uze wome emfudlaneni we. nitrogen, futhi uncibilikise insalela ku-1.0 mL wesixazululo esijwayelekile sangaphakathi.
Isixazululo esingenalutho: Shukumisa u-200 mL we-methylene chloride ukuze wome emanzini okugeza endaweni yokushisa engeqile kuma-40. Chaza insalela ku-1 mL ye-methylene chloride.
Isistimu yeChromatographic
(Bona i-Chromatography <621>, Ukufaneleka Kwesistimu.)
Imodi: GC
Umtshina: I-ionization yomlilo
Ikholomu: 0.53-mm × 10-m ikholomu yesilika ehlanganisiwe, ehlanganiswe nesigaba se-G3 (ugqinsi lwefilimu 2 µm)
Izinga lokushisa
Umjovo: 250
Umtshina: 250
Ikholomu: 180
I-Carrier gas: I-nitrogen
Izinga lokugeleza: 10 mL/min
Usayizi womjovo: 1 µL
Isilinganiso sokuhlukaniswa: 2:1
Ukufaneleka kwesistimu
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esingenalutho
[Qaphela-Izinto zihlukaniswa ngokulandelana okulandelayo: i-o-toluenesulfonamide, i-p-toluenesulfonamide, ne-caffeine.]
Izidingo zokufaneleka: Azikho iziqongo ezikhathini zokugcinwa kwezinga langaphakathi, i-o-toluenesulfonamide, noma i-p-toluenesulfonamide;Isixazululo esingenalutho
Ukulungiswa: I-NLT 1.5 phakathi kwe-o-toluenesulfonamide ne-p-toluenesulfonamide, isixazululo esijwayelekile
Ukuhlaziya
Amasampula: Isixazululo esijwayelekile kanye nesixazululo esiyisampula
Imibandela yokwamukela: Uma noma yiziphi iziqongo ngenxa ye-o-toluenesulfonamide ne-p-toluenesulfonamide zivela ku-chromatogram etholwe ngesixazululo Sesampula, isilinganiso sezindawo zazo naleyo yesixazululo esijwayelekile sangaphakathi yi-NMT isilinganiso esihambisanayo kuchromatogram etholwe nesixazululo Esijwayelekile. .
Ukungcola komuntu ngamunye: Bheka Ithebula Lokungcola 1.
Ithebula Lokungcola 1
Imibandela Yokwamukela Igama (ppm)
I-o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Inqubo 2: Umkhawulo we-Benzoate ne-Salicylate
Isixazululo sesampula: 10 mL wekhambi elishisayo, eligcwele le-saccharin
Ukuhlaziya: Engeza i-ferric chloride TS dropwise kusixazululo Sesampula.
Indlela yokwamukela: Awukho umbala wemvula noma u-violet ovela oketshezini.
IZIVIVINYO EZITHILE
• I-Melting Range noma Izinga Lokushisa 741: 226-230
• Ukulahlekelwa Ekumisweni <731>: Yomisa isampula ku-105 amahora angu-2: ilahlekelwa yi-NMT 1.0% yesisindo sayo.
• Ukuhlolwa kwe-Readily Carbonizable Substances 271
Isixazululo sesampula: 40 mg/mL ku-sulfuric acid (94.5% -95.5% [w/w] ye-H2SO4), egcinwe ku-48-50 imizuzu eyi-10
Imibandela yokwamukela: Isixazululo Sesampula asinawo umbala owedlula I-Fluid A Efanisayo, uma ibhekwa kungemuva elimhlophe.
• Ukucaca Kwesixazululo
[Qaphela-Isixazululo Sesampula kufanele siqhathaniswe Nereferensi yokumiswa A kanye namanzi emini ehlukanisiwe imizuzu emi-5 ngemva kokulungiswa Kwereferensi yokumiswa A.]
I-Diluent: 200-g/L isisombululo se-sodium acetate
Isixazululo se-Hydrazine: 10.0 mg/mL ye-hydrazine sulfate.[Qaphela-Vumela ukuthi ime amahora angu-4-6.]
Isixazululo se-methenamine: Dlulisa u-2.5 g we-methenamine ku-100-mL we-glass-stoppered flask, engeza u-25.0 mL wamanzi, faka isivalo sengilazi, bese uxuba ukuze uncibilike.
Ukumiswa kwe-opalescent okuyisisekelo: Dlulisa u-25.0 mL wesixazululo se-Hydrazine kusixazululo se-Methenamine ku-100-mL yeflask evinjwe ingilazi.Hlanganisa, bese uvumela ukuthi ume amahora angama-24.[Qaphela-Lokhu kumiswa kuzinzile izinyanga ezi-2, inqobo nje uma kugcinwa esitsheni sengilazi esingenasici.Ukumiswa akufanele kuhambisane nengilazi futhi kufanele kuxutshwe kahle ngaphambi kokusetshenziswa.Vumela ukumiswa kume amahora angama-24.]
Izinga le-Opalescence: Nciphisa u-15.0 mL we-Primary opalescent suspension ngamanzi ukuya ku-1000 mL.[Qaphela-Lokhu kumiswa akufanele kusetshenziswe ngemva kwamahora angu-24 ngemva kokulungiswa.]
Ukumiswa kwereferensi A: Izinga le-Opalescence namanzi (1 ku-20)
Ukumiswa kwereferensi B: Izinga le-Opalescence namanzi (1 ku-10)
Isixazululo sesampula: 200 mg/mL ku-Diluent
Ukuhlaziya
Amasampula: I-Diluent, Ukumiswa Kwereferensi A, Ukumiswa Kwereferensi B, Isixazululo sesampula, namanzi
Dlulisa ingxenye eyanele yesisombululo Sesampuli kushubhu yokuhlola yengilazi engenambala, esobala, engathathi hlangothi enesisekelo esiyisicaba kanye nobubanzi bangaphakathi obungu-15-25 mm ukuze uthole ukujula okungama-40 mm.Ngokufanayo dlulisa izingxenye Zokumiswa Kwesithenjwa A, Ukumiswa Kwesithenjwa B, amanzi, kanye ne-Diluent ukuze uhlukanise amashubhu okuhlola afanayo.Qhathanisa izixazululo ekukhanyeni kwasemini okuhlukanisiwe, ukubuka uqonde kungemuva elimnyama (bona i-Spectrophotometry ne-Light-Scattering 851, Visual Comparison).[Qaphela—Ukusatshalaliswa kokukhanya kumelwe kube ngendlela yokuthi ukumiswa Kwereferensi A kukwazi ukuhlukaniswa kalula emanzini, nokuthi ukumiswa Kwereferensi B kungase kuhluke kalula ekumisweni Kwezithenjwa A. ]
Indlela yokwamukela: Isixazululo Sesampula sibonisa ukucaca okufanayo nalokhu kwamanzi, noma i-Diluent, noma i-opalescence yayo yi-NMT yokumiswa kwereferensi A.
• Umbala Wesixazululo
I-Diluent A: 200-g/L isisombululo se-sodium acetate
I-Diluent B: 10-g/L isixazululo se-hydrochloric acid
Isixazululo sesitoko esijwayelekile: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, and Diluent B (3.0:3.0:2.4:1.6)
Isixazululo esijwayelekile: Isixazululo sesitoko esijwayelekile kanye ne-Diluent B (1 ku-100).[Qaphela-Lungisa Isixazululo Esijwayelekile ngokushesha ngaphambi kokusisebenzisa.]
Isixazululo esiyisampula: Sebenzisa Isampula yesixazululo ekuhlolweni kokucaca kwesixazululo.
Ukuhlaziya
Amasampula: I-Diluent A, isixazululo esijwayelekile, isampula yesixazululo, namanzi
Dlulisa ingxenye eyanele yesisombululo Sesampuli kushubhu yokuhlola yengilazi engenambala, esobala, engathathi hlangothi enesisekelo esiyisicaba kanye nobubanzi bangaphakathi obungu-15-25 mm ukuze uthole ukujula okungama-40 mm.Ngokufanayo dlulisa izingxenye zesixazululo Esijwayelekile, i-Diluent A, namanzi ukuze kuhlukaniswe, amashubhu okuhlola afanayo.Qhathanisa izixazululo ekukhanyeni kwasemini okuhlukanisiwe, ukubuka uqonde kungemuva elimhlophe (bheka i-Spectrophotometry ne-Light-Scattering 851, Visual Comparison).
Imibandela yokwamukela: Isixazululo Sesampula sinokubukeka kwamanzi noma i-Diluent A, noma asinawo umbala ogqamile kunesixazululo Esijwayelekile.
IZIDINGO EZENGEZIWE
• Ukupakisha Nokugcina: Londoloza ezitsheni ezivalwe kahle.Gcina ekamelweni lokushisa.
• I-USP Reference Standards <11>
USP Saccharin RS Chofoza ukuze Ubuke Isakhiwo
I-USP o-Toluenesulfonamide RS
I-USP p-Toluenesulfonamide RS