Saccharin anaghị emebi emebi CAS 81-07-2 ịdị ọcha> 99.0% (HPLC)

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3 (2H) -otu, 1,1-dioxide;
1,2-Benzisothiazolin-3-otu 1,1-dioxide [81-07-2].
Nkọwa
Saccharin nwere NLT 99.0% na NMT 101.0% nke C7H5NO3S, gbakọọ na ntọala akpọnwụwo.
Nchọpụta
• Ntinye infrared <197K>
ASSAY
• Usoro
Ihe atụ: 500 mg
Nyocha: Gbasaa ihe nlele ahụ na mmanya 40 ml.Tinye 40 ml mmiri na phenolphthalein TS.Titrate nwere 0.1 N sodium hydroxide.Mee titration oghere, ọ bụrụ na ọ dị mkpa, ma mee mgbazi kwesịrị ekwesị.ML ọ bụla nke 0.1 N sodium hydroxide bụ 18.32 mg nke C7H5NO3S.
Usoro nnabata: 99.0% -101.0% na ntọala akpọnwụwo
IHE adịghị ọcha
Ihe adịghị ọcha
• Ihe fọdụrụ na mgbanye <281>: NMT 0.2%.Igwe ọkụ ọkụ bụ 600 ± 50.
• Ọla dị arọ, Usoro II <231>: NMT 10 ppm
Ihe adịghị ọcha
• Usoro 1: Oke nke Toluenesulfonamides
Ngwọta ọkọlọtọ dị n'ime: 0.25 mg/mL nke caffeine na methylene chloride
Ngwọta ngwaahịa ọkọlọtọ: 20.0 µg/mL nke USP o-Toluenesulfonamide RS na 20.0 μg/mL nke USP p-Toluenesulfonamide RS na methylene chloride
Ngwọta ọkọlọtọ: Wepu 5.0 ml nke ihe ngwọta ọkọlọtọ maka nkụ n'ime iyi nitrogen.Gbanyụọ ihe fọdụrụ na 1 ml nke ihe ngwọta dị n'ime.
Ngwọta nlele: Kwụsị 10 g nke Saccharin na mmiri 20 ml, wee gbarie site na iji 5-6 ml nke 10 N sodium hydroxide.Ọ bụrụ na ọ dị mkpa, dozie ngwọta ya na 1 N sodium hydroxide ma ọ bụ 1 N hydrochloric acid na pH nke 7-8, ma gbanye mmiri na 50 ml.Gwakọta ihe ngwọta ahụ na nha anọ nke ọ bụla n'ime 50 ml nke methylene chloride.Gwakọta ọkwa ndị dị ala, kpoo n'elu sodium sulfate na-ekpo ọkụ, na iyo.Jiri 10 ml nke methylene chloride saa ihe nzacha na sodium sulfate.Gwakọta ihe ngwọta na ịsacha ahụ, na-ekpochapụ ihe fọrọ nke nta ka ọ bụrụ nkụ na mmiri ịsa ahụ na okpomọkụ na-erughị 40. Iji obere methylene chloride, quantitatively nyefee ihe fọdụrụ n'ime tube 10-mL kwesịrị ekwesị, wepụ na nkụ na iyi nke mmiri. nitrogen, ma gbazee ihe fọdụrụ na 1.0 ml nke ihe ngwọta dị n'ime.
Ngwọta oghere: Wepụ 200 ml nke methylene chloride ka nkụ na mmiri ịsa ahụ na okpomọkụ na-agaghị agafe 40. Gbanyụọ ihe fọdụrụ na 1 mL nke methylene chloride.
Sistemụ chromatographic
(Lee Chromatography <621>, Kwesịrị ekwesị Sistemu.)
Ụdị: GC
Ihe nchọpụta: ionization ọkụ
Ogidi: 0.53-mm × 10-m kọlụm silica fused, nke ejiri usoro G3 kpuchie (oke ihe nkiri 2 µm)
Okpomọkụ
Ntinye: 250
Nchọpụta: 250
Ogidi: 180
Ihe na-ebu gas: nitrogen
Ọnụego mmiri: 10 ml / min
Nha igba ogwu: 1µL
Oke nkewa: 2:1
Sistemu kwesịrị ekwesị
Nlereanya: Ngwọta ọkọlọtọ na ngwọta oghere
[Rịba ama- A na-ekekọta ihe ndị ahụ n'usoro a: o-toluenesulfonamide, p-toluenesulfonamide, na caffeine.]
Ihe ndị kwesịrị ekwesị chọrọ: Enweghị ọnụ ọgụgụ kachasị elu n'oge njide maka ọkọlọtọ ime, o-toluenesulfonamide, ma ọ bụ p-toluenesulfonamide;Ihe ngwọta efu
Mkpebi: NLT 1.5 n'etiti o-toluenesulfonamide na p-toluenesulfonamide, Standard ngwọta
Nyocha
Ihe atụ: Ngwọta ọkọlọtọ na ngwọta nlele
Usoro nnabata: Ọ bụrụ na ọnụ ọgụgụ ọ bụla n'ihi o-toluenesulfonamide na p-toluenesulfonamide pụtara na chromatogram enwetara na ngwọta Sample, oke mpaghara ha na nke usoro ọkọlọtọ Internal bụ NMT nha kwekọrọ na chromatogram nwetara na ngwọta Standard. .
Ihe adịghị ọcha n'otu n'otu: Lee Tebụl adịghị ọcha 1.
Tebụl adịghị ọcha 1
Usoro nnabata aha (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Usoro 2: Oke nke Benzoate na Salicylate
Ngwọta nlele: 10 ml nke saccharin dị ọkụ, juputara
Nyocha: Tinye ferric chloride TS dropwise na ngwọta Sample.
Usoro nnabata: Ọ nweghị agba ma ọ bụ violet na-apụta na mmiri mmiri.
Nnwale akọwapụtara
• Oke agbaze ma ọ bụ okpomọkụ 741: 226-230
• Ọnwụ na ihicha <731>: Kpochapụ ihe nlele na 105 maka 2 h: ọ na-efunahụ NMT 1.0% nke ibu ya.
• Nnwale Carbonizable Ngwa ngwa 271
Ihe ngwọta nlele: 40 mg / mL na sulfuric acid (94.5% -95.5% [w / w] nke H2SO4), nọgidere na 48-50 maka 10 min.
Usoro nnabata: Ngwọta nlele enweghị agba karịa Matching Fluid A, mgbe a na-elele ya na nzụlite ọcha.
• Ngwọta doo anya
[Rịba ama-A ga-atụnyere ihe ngwọta nlele ahụ na nkwusioru ntụaka A na mmiri n'ime ìhè ehihie 5 min mgbe nkwadebe nke nkwusioru ntụaka A.]
Ihe mgbaze: 200-g/L ngwọta nke sodium acetate
Ihe ngwọta hydrazine: 10.0 mg / ml nke hydrazine sulfate.[Cheta-Kwe ka ọ kwụrụ maka awa 4-6.]
Ngwọta Methenamine: Nyefee 2.5 g nke methenamine na iko 100-mL, tinye 25.0 ml mmiri, fanye ihe nkwụsị iko, ma gwakọta ka ọ gbazee.
Nkwusioru opalescent nke mbụ: Nyefee 25.0 ml nke ngwọta Hydrazine na ngwọta Methenamine n'ime iko 100-mL kwụsịrị.Gwakọta, ma kwe ka ị kwụrụ maka awa 24.[Rịba ama-Nkwụsịtụ a kwụsiri ike ruo ọnwa 2, ma ọ bụrụhaala na echekwara ya n'ime akpa iko enweghị ntụpọ n'elu.Nkwusioru ahụ ekwesịghị ịrapara na iko a ga-agwakọta nke ọma tupu ejiri ya.Kwe ka nkwusioru ahụ guzoro maka awa 24.]
Ọkọlọtọ opalescence: Jiri mmiri gbanye 15.0 ml nke nkwusioru opalescent nke mbụ ka ọ bụrụ 1000 ml.[Rịba ama-Ekwesighi iji nkwusioru a gafere awa 24 ka emechara nkwadebe.]
Ntụtuaka nkwusioru A: Ọkọlọtọ na-adịghị mma na mmiri (1 n'ime 20)
Ntụgharị aka nkwusioru B: Ọkọlọtọ na-adịghị mma na mmiri (1 n'ime 10)
Ngwọta nlele: 200 mg / ml na diluent
Nyocha
Sample: Diluent, Reference nkwusioru A, Ntụtuaka nkwusioru B, Sample ngwọta, na mmiri
Nyefee akụkụ zuru oke nke ihe ngwọta Sample na tube ule nke enweghị agba, transperent, iko na-anọpụ iche na ntọala dị larịị na dayameta dị n'ime nke 15-25 mm iji nweta omimi nke 40 mm.N'otu aka ahụ nyefe akụkụ nke nkwusioru ntụaka A, nkwusioru nkwusioru B, mmiri na diluent iji kewaa tubes ule dabara adaba.Tulee ihe ngwọta ndị dị n'ìhè ụbọchị gbasasịrị, na-ekiri kwụ ọtọ megide ndabere ojii (lee Spectrophotometry na Light-Scattering 851, Ntụle Anya).[Rịba ama-Mgbasa nke ọkụ ga-abụrịrị na nkwusioru nkwusioru A nwere ike ịmata ngwa ngwa na mmiri, yana nkwusioru ntụaka B nwere ike ịdị iche na nkwusioru ntụaka A.]
Usoro nnabata: Ngwọta Sample na-egosi otu nghọta dị ka nke mmiri, ma ọ bụ Diluent, ma ọ bụ opalescence ya bụ NMT nke nkwusioru ntụaka A.
• Agba nke Ngwọta
Diluent A: 200-g/L ngwọta nke sodium acetate
Diluent B: 10-g/L ngwọta nke hydrochloric acid
Ngwọta ngwaahịa ọkọlọtọ: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, na diluent B (3.0:3.0:2.4:1.6)
Ọkọlọtọ ngwọta: Standard ngwaahịa ngwọta na Diluent B (1 na 100).[Rịba ama- Kwadebe usoro ọkọlọtọ ozugbo tupu ejiri ya.]
Ngwọta nlere: Jiri ihe nlele nlele si n'ule maka Ngwọta doo anya.
Nyocha
Sample: Diluent A, Standard Solution, Sample ngwọta, na mmiri
Nyefee akụkụ zuru oke nke ihe ngwọta Sample na tube ule nke enweghị agba, transperent, iko na-anọpụ iche na ntọala dị larịị na dayameta dị n'ime nke 15-25 mm iji nweta omimi nke 40 mm.N'otu aka ahụ nyefee akụkụ nke Standard solution, Diluent A, na mmiri iji kewaa, tubes ule dabara.Tulee ihe ngwọta ndị dị n'ìhè ụbọchị gbasasịrị, na-ekiri kwụ ọtọ megide ndabere ọcha (lee Spectrophotometry na Light-Scattering 851, Ntụle Anya).
Usoro nnabata: Ngwọta Sample nwere ọdịdị mmiri ma ọ bụ Diluent A, ma ọ bụ enweghị agba agba karịa ọkọlọtọ ọkọlọtọ.
NKWUO GBASARA YA
• Nkwakọ ngwaahịa na Nchekwa: Chekwaa n'ime igbe emechiri nke ọma.Na-echekwa na ụlọ okpomọkụ.
• Ụkpụrụ ntụaka USP <11>
USP Saccharin RS Pịa ka ilele Ọdịdị
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS