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

Hakaraina
C7H5NO3S 183.18
1,2-Benzisothiazol-3(2H)-kotahi, 1,1-hauora;
1,2-Benzisothiazolin-3-one 1,1-hauhā [81-07-2].
WHAKAMAHI
Kei roto i te Saccharin te NLT 99.0% me te NMT 101.0% o C7H5NO3S, kua tatauhia i runga i te whakamaroke.
WHAKATAUTANGA
• Te Kohanga Infrared <197K>
WHAKAMAHI
• Tikanga
Tauira: 500 mg
Tātaritanga: Wehea te Tauira ki te 40 mL o te waipiro.Tāpirihia he 40 mL wai me te phenolphthalein TS.Whakawetohia ki te 0.1 N te konutai waihā.Me mahi he titration patea, mehemea e tika ana, me te whakatika tika.Ko ia mL o te 0.1 N konutai waihā he rite ki te 18.32 mg o C7H5NO3S.
Paearu whakaae: 99.0% -101.0% i runga i te whakamaroke
NGA POKE
Nga poke parakore
• Te toenga i runga i te mura <281>: NMT 0.2%.Ko 600 ± 50 te pāmahana whakakā.
• Nga Koura Nui, Tikanga II <231>: NMT 10 ppm
Nga poke pararopi
• Tikanga 1: Te Tepe o Toluenesulfonamides
Te otinga paerewa o roto: 0.25 mg/mL o te kawhe i roto i te methylene chloride
Te otinga kararehe paerewa: 20.0 µg/mL o USP o-Toluenesulfonamide RS me 20.0 µg/mL o USP p-Toluenesulfonamide RS i roto i te methylene chloride
Wairewa Paerewa: Whakaeto 5.0 mL o te wairewa rakau Paerewa kia maroke i roto i te awa hauota.Whakarewahia te toenga ki te 1 mL o te otinga paerewa o roto.
Tauira otinga: Whakatarewahia te 10 g o Saccharin ki te 20 mL wai, ka memeha ma te whakamahi i te 5-6 mL o te 10 N konutai waikawa.Mena e tika ana, whakatikahia te otinga ki te 1 N te konutai waikawa me te 1 N te waikawa pūhaumāota ki te pH o 7-8, ka waimeha ki te wai ki te 50 mL.Ruperupea te wairewa kia wha nga rahinga mo ia 50 mL o te methylene chloride.Whakakotahitia nga papa o raro, whakamaroke ki runga i te konutai konutai pūkawa, me te tātari.Horoia te tātari me te konutai pūkawa ngāwha ki te 10 mL o te methylene pūhaumāota.Whakakotahitia te wairewa me nga horoinga, ka whakaeto kia maroke i roto i te kaukau wai i te pāmahana kaua e neke ake i te 40. Ma te whakamahi i te iti o te methylene chloride, whakawhiti ine te toenga ki roto i te ngongo 10-mL pai, ka mimiti ki te maroke i roto i te awa. hauota, ka whakakore i te toenga ki te 1.0 mL o te otinga paerewa o roto.
Wairewa patea: Whakaeto te 200 mL o te methylene chloride ki te maroke i roto i te pati wai i te pāmahana kaua e neke atu i te 40. Whakarewahia te toenga ki te 1 mL o te methylene chloride.
Pūnaha Chromatographic
(Tirohia te Chromatography <621>, Whakaritenga Pūnaha.)
Aratau: GC
Kaipupuri: Te katote mura
Tīwae: 0.53-mm × 10-m te tīwae silica whakakotahi, pania ki te wahanga G3 (te matotoru kiriata 2 µm)
Te pāmahana
Injector: 250
Kaitirotiro: 250
Tīwae: 180
hau kawe: hauota
Rere rere: 10 mL/min
Rahi werohanga: 1 µL
Ritua ōwehenga: 2:1
Te pai o te punaha
Tauira: Wairewa Paerewa me te otinga Patea
[Tuhipoka-Ko nga matū ka whakahekehia i roto i te raupapa e whai ake nei: o-toluenesulfonamide, p-toluenesulfonamide, me te kawhe.]
Nga whakaritenga e tika ana: Kaore he tihi i nga wa pupuri mo te paerewa o roto, o-toluenesulfonamide, p-toluenesulfonamide ranei;Te otinga parakore
Whakatau: NLT 1.5 i waenganui i te o-toluenesulfonamide me te p-toluenesulfonamide, Wairewa Paerewa
Tātaritanga
Tauira: otinga Paerewa me te otinga Tauira
Paearu Whakaaetanga: Mena ka puta etahi tihi na te o-toluenesulfonamide me te p-toluenesulfonamide i roto i te chromatogram i whiwhi me te Tauira otinga, ko te ōwehenga o o raatau waahi ki tera o te otinga paerewa o roto ko te NMT te ōwehenga e rite ana ki te chromatogram i whiwhi me te otinga Paerewa. .
Nga poke takitahi: Tirohia te Ripanga poke 1.
Ripanga poke 1
Paearu Whakaaetanga Ingoa (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Tikanga 2: Te Tepe o te Benzoate me te Salicylate
Tauira otinga: 10 mL o te wairewa wera, kukū o te saccharin
Tātaritanga: Tāpirihia te ferric chloride TS dropwise ki te otinga Tauira.
Paearu whakaae: Karekau he rerenga, he tae puru ranei i roto i te wai.
NGA WHAKAMATAUTANGA
• Te Awhe Whakarewa, Te Pahana 741: 226-230
• Ngaronga i te whakamaroke <731>: Me whakamaroke he tauira ki te 105 mo te 2 haora: ka ngaro te NMT 1.0% o tona taumaha.
• Whakamātautau matū kawa 271
Tauira otinga: 40 mg/mL i roto i te waikawa pungatara (94.5%-95.5% [w/w] o H2SO4), ka mau ki te 48-50 mo te 10 meneti
Paearu whakaae: Ko te otinga Tauira kaore he tae nui atu i te Whakaorite ki te Wai A, ina tirohia ki te papamuri ma.
• Maramatanga o te Otinga
[Tuhipoka-Me whakatauritea te tauira otinga ki te whakatārewatanga Tohutoro A me te wai i te awatea marara 5 meneti i muri i te takahanga o te whakatārewatanga Tohutoro A.]
Waiwai: 200-g/L otinga o te konutai acetate
Wairewa Hydrazine: 10.0 mg/mL o te hydrazine sulfate.[Tuhipoka-Tua mo te 4-6 haora.]
Te wairewa Methenamine: Whakawhitihia te 2.5 g o te methenamine ki te 100-mL ipuipu kaata, ka tapirihia te 25.0 mL o te wai, ka kuhu i te kaarai, ka uru kia memeha.
Te whakatārewatanga opalescent tuatahi: Whakawhitihia te 25.0 mL o te wairewa Hydrazine ki te wairewa Methenamine i roto i te 100-mL ipu karaihe-tihi.Whakaranuhia, ka waiho kia tu mo te 24 haora.[Tuhipoka-Ka noho pumau tenei whakatārewatanga mo te 2 marama, mena ka penapena ki roto i te ipu karaihe kaore he koha o te mata.Ko te whakatārewatanga me kaua e piri ki te karaihe, me uru pai i mua i te whakamahi.Tukua te whakatārewatanga kia tu mo te 24 haora.]
Paerewa Opalescence: Ringihia te 15.0 mL o te whakatārewatanga opalescent tuatahi ki te wai ki te 1000 mL.[Tuhipoka-Kaua e whakamahia tenei whakatārewatanga i tua atu i te 24 haora i muri i te whakaritenga.]
Te whakatārewatanga tohutoro A: Paerewa Opalescence me te wai (1 i roto i te 20)
Te whakatārewatanga tohutoro B: Paerewa Opalescence me te wai (1 i roto i te 10)
Tauira otinga: 200 mg/mL i te Diluent
Tātaritanga
Tauira: Diluent, Tohutoro whakatārewatanga A, Tohutoro whakatārewatanga B, Tauira otinga, me te wai
Whakawhitia he wahi rawaka o te Tauira otinga ki te ipuipu whakamatautau he karaehe taekore, maramara, koretake me te turanga papatahi me te diameter o roto o te 15-25 mm kia 40 mm te hohonu.Me whakawhiti ano etahi wahanga o te whakatārewatanga Tohutoro A, te whakatārewatanga Tohutoro B, te wai, me te Diluent ki te wehe i nga ipuipu whakamatautau rite.Whakatauritehia nga otinga i roto i te awatea marara, ma te titiro poutū ki te papamuri pango (tirohia te Spectrophotometry me te Marara-Marama 851, Whakataurite Ataata).[Tuhipoka—Ko te whakamaaramatanga o te marama me tino mohio te whakatārewatanga Tohutoro A i te wai, me te whakatārewatanga Tohutoro B ka taea te wehewehe mai i te whakatārewatanga Tohutoro A. ]
Paearu whakaae: Ko te tauira otinga e whakaatu ana he rite te marama ki to te wai, te Diluent ranei, ko tona opalescence ranei ko te NMT o te whakatārewatanga Tohutoro A.
• Te Tae o te Otinga
Diluent A: 200-g/L otinga o te konutai acetate
Waiwai B: 10-g/L wairewa o te waikawa pūhaumāota
Te otinga kararehe paerewa: Ferric chloride CS, cobaltous chloride CS, kapuriki sulfate CS, me te Diluent B (3.0:3.0:2.4:1.6)
Wairewa Paerewa: Wairewa rakau paerewa me te Diluent B (1 i roto i te 100).[Tuhipoka-Whakaritea te otinga Paerewa i mua tonu i te whakamahi.]
Tauira otinga: Whakamahia te Tauira otinga mai i te whakamatautau mo te Maama o te Otinga.
Tātaritanga
Tauira: Diluent A, Wairewa Paerewa, Tauira otinga, me te wai
Whakawhitia he wahi rawaka o te Tauira otinga ki te ipuipu whakamatautau he karaehe taekore, maramara, koretake me te turanga papatahi me te diameter o roto o te 15-25 mm kia 40 mm te hohonu.Waihoki, whakawhitia etahi wahanga o te wairewa Paerewa, Diluent A, me te wai hei wehe, kia rite ki nga ipuipu whakamatautau.Whakatauritea nga otinga i te awatea marara, ma te titiro poutū ki te papamuri ma (tirohia te Spectrophotometry me te Marara-Marama 851, Whakataurite Ataata).
Paearu whakaae: He wai te ahua o te otinga Tauira, he Diluent A ranei, kaore ranei i te kaha ake te tae ki te otinga Paerewa.
HE WHAKAMAHI ATU
• Te Whakapai me te Rokiroki: Whakaorangia ki roto i nga ipu kua kati pai.Rokiroki ki te pāmahana rūma.
• Paerewa Tohutoro USP <11>
USP Saccharin RS Pāwhiri ki te Tiro Hanganga
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS