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

Saccharin
C7H5NO3S 183.18
1,2-Benzisothiazol-3(2H)-kahi, 1,1-dioxide;
1,2-Benzisothiazolin-3-one 1,1-dioxide [81-07-2].
HOAKAKA
Loaʻa iā Saccharin ka NLT 99.0% a me ka NMT 101.0% o C7H5NO3S, i helu ʻia ma ke kumu maloʻo.
IKE
• Hoʻopili ʻia ka Infrared <197K>
HANA
• Kaʻina hana
Laʻana: 500 mg
Nānā: E hoʻopau i ka Laʻana i 40 mL o ka waiʻona.E hoʻohui i 40 mL o ka wai a me ka phenolphthalein TS.E hoʻokaʻawale me 0.1 N ka sodium hydroxide.E hana i kahi titration blank, inā pono, a hana i ka hoʻoponopono kūpono.ʻO kēlā me kēia mL o 0.1 N sodium hydroxide ua like ia me 18.32 mg o C7H5NO3S.
Nā pae hoʻoholo: 99.0% -101.0% ma ke kumu maloʻo
NA mea haumia
Nā mea haumia ʻole
• Ke koena ma ka ʻā ʻana <281>: NMT 0.2%.ʻO ka mahana wela he 600 ± 50.
• Nā Metala Kaumaha, Hana II <231>: NMT 10 ppm
Nā mea haumia kino
• Ke Kaʻina Hana 1: Ka palena o Toluenesulfonamides
Haʻina maʻamau i loko: 0.25 mg/mL o ka caffeine i loko o ka methylene chloride
Haʻina waiwai maʻamau: 20.0 µg/mL o USP o-Toluenesulfonamide RS a me 20.0 µg/mL o USP p-Toluenesulfonamide RS i ka methylene chloride
Haʻina maʻamau: E hoʻoheheʻe i ka 5.0 mL o ka wai hoʻoheheʻe maʻamau i maloʻo i loko o kahi kahawai o ka nitrogen.E hoʻoheheʻe i ke koena i 1 mL o ka hoʻonā maʻamau Kuloko.
Laʻana hoʻonā: Hoʻokuʻu i 10 g Saccharin i 20 mL o ka wai, a hoʻoheheʻe me ka hoʻohana ʻana i 5-6 mL o 10 N sodium hydroxide.Inā pono, e hoʻoponopono i ka hopena me 1 N sodium hydroxide a i ʻole 1 N hydrochloric acid i kahi pH o 7-8, a hoʻoheheʻe me ka wai i 50 mL.E lulu i ka hoʻonā me ʻehā nui o kēlā me kēia 50 mL o ka methylene chloride.Hoʻohui i nā papa haʻahaʻa, maloʻo ma luna o ka sodium sulfate anhydrous, a kānana.E holoi i ka kānana a me ka sodium sulfate me 10 mL o ka methylene chloride.E hoʻohui i ka hāʻina a me ka holoi ʻana, a e hoʻoheheʻe ʻia i kahi maloʻo i loko o kahi ʻauʻau wai ma kahi mahana ʻaʻole i ʻoi aku ma mua o 40. Me ka hoʻohana ʻana i kahi mea liʻiliʻi o ka methylene chloride, e hoʻololi i ke koena i loko o kahi paipu 10-mL kūpono, e hoʻoheheʻe a maloʻo i loko o kahi kahawai. nitrogen, a hoʻoheheʻe i ke koena i loko o 1.0 mL o ka hoʻonā maʻamau Kuloko.
Haʻina paʻaka: E hoʻoheheʻe i ka 200 mL o ka methylene chloride a maloʻo i loko o ka ʻauʻau wai ma kahi mahana ʻaʻole i ʻoi aku ma mua o 40. E hoʻoheheʻe i ke koena i 1 mL o ka methylene chloride.
Pūnaehana Chromatographic
(E nana Chromatography <621>, Pūnaehana Pono.)
Ke ano: GC
Mea ʻIke: Hoʻopā ahi
kolamu: 0.53-mm × 10-m kolamu silica fused, uhi ʻia me ka pae G3 (ka mānoanoa kiʻiʻoniʻoni 2 µm)
Mahana
Mea hoʻokomo: 250
ʻIke: 250
kolamu: 180
Ke kinoea halihali: Nitrogen
Kahe kahe: 10 mL / min
Ka nui o ka hoʻopio: 1 µL
Māhele māhele: 2:1
Kūpono ʻōnaehana
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Blank
[Note-Ua hoʻoheheʻe ʻia nā mea ma ke ʻano penei: o-toluenesulfonamide, p-toluenesulfonamide, a me ka caffeine.]
Nā koi kūpono: ʻAʻohe piko i nā manawa paʻa no ka maʻamau kūloko, o-toluenesulfonamide, a i ʻole p-toluenesulfonamide;Haʻina hakahaka
Hoʻoholo: NLT 1.5 ma waena o ka o-toluenesulfonamide a me ka p-toluenesulfonamide.
Kānāwai
Nā Laʻana: Haʻina maʻamau a me ka hāʻina Laʻana
Nā pae hoʻoholo: Inā ʻike ʻia kekahi mau piko ma muli o ka o-toluenesulfonamide a me ka p-toluenesulfonamide i ka chromatogram i loaʻa me ka Sample solution, ʻo ka ratio o ko lākou mau wahi i kēlā o ka solution Internal standard ʻo NMT ka ratio like i ka chromatogram i loaʻa me ka solution Standard .
Nā haumia o kēlā me kēia kanaka: E nānā i ka Papa Hoʻomaʻemaʻe 1.
Helu 1
Paʻa inoa ʻae (ppm)
o-Toluenesulfonamide 10
p-Toluenesulfonamide 10
• Ke Kaʻina Hana 2: Ka palena o Benzoate a me Salicylate
Laʻana hoʻonā: 10 mL o kahi hopena wela, saturated o saccharin
Nānā: E hoʻohui i ka ferric chloride TS dropwise i ka hāʻina Laʻana.
Paʻa e ʻae ʻia: ʻAʻole ʻike ʻia ke kala ʻulaʻula a ʻulaʻula paha i ka wai.
NA HOAO KUAI
• Ka Heehee a me ka Mahana 741: 226-230
• Pohō ma ka ho'omalo'o <731>: E ho'omalo'o i kahi la'ana ma 105 no 2 h: nalowale NMT 1.0% o kona kaumaha.
• Ho'āʻo maʻalahi Carbonizable Substances 271
Laʻana hoʻonā: 40 mg/mL i ka sulfuric acid (94.5%-95.5% [w/w] o H2SO4), mālama ʻia ma 48-50 no 10 min
Nā pae ʻae ʻae: ʻAʻole ʻoi aku ka waihoʻoluʻu o ka hāʻina Laʻana ma mua o ka Matching Fluid A, ke nānā ʻia me kahi kāʻei keʻokeʻo.
• Maopopo o ka Haʻina
[Note-E hoʻohālikelike ʻia ka hopena laʻana me ka Reference suspension A a me ka wai i ka lā ākea 5 min ma hope o ka hoʻomākaukau ʻana i ka Reference suspension A.]
Diluent: 200-g/L solution o ka sodium acetate
ʻO ka hopena Hydrazine: 10.0 mg / mL o ka hydrazine sulfate.[Meta-E ʻae e kū no 4-6 h.]
ʻO ka hopena Methenamine: E hoʻololi i 2.5 g o ka methenamine i loko o kahi pahu aniani 100-mL, hoʻohui i 25.0 mL o ka wai, hoʻokomo i ka pahu aniani, a hui a hoʻoheheʻe.
Hoʻokuʻu ʻia ka opalescent mua: E hoʻololi i 25.0 mL o ka solution Hydrazine i ka solution Methenamine i loko o ka pahu aniani pani ʻia he 100-mL.E hui, a e ku no 24 h.[Note-Ua paʻa kēia hoʻokuʻu ʻia no 2 mau mahina, inā mālama ʻia ia i loko o kahi pahu aniani me ka ʻole o nā pōʻino.ʻAʻole pono ka hoʻokuʻu ʻana i ke aniani a pono e hui maikaʻi ʻia ma mua o ka hoʻohana ʻana.E ʻae i ka hoʻokuʻu ʻia e kū no 24 mau hola.]
Opalescence maʻamau: Dilute 15.0 mL o ka Primary opalescent hoʻokuʻu me ka wai i 1000 mL.[Note-ʻAʻole pono e hoʻohana ʻia kēia hoʻokuʻu ʻia ma mua o 24 mau hola ma hope o ka hoʻomākaukau ʻana.]
Hoʻokuʻu ʻia A: Opalescence maʻamau a me ka wai (1 i 20)
Hoʻokuʻu ʻia B: Opalescence maʻamau a me ka wai (1 i ka 10)
Laʻana hoʻonā: 200 mg/mL i ka Diluent
Kānāwai
Nā Laʻana: Diluent, Reference suspension A, Reference suspension B, Sample solution, a me ka wai
E hoʻololi i kahi ʻāpana kūpono o ka hopena laʻana i kahi paipu hoʻāʻo o ke aniani ʻeleʻele, aniani, kū ʻole me ke kumu pālahalaha a me ke anawaena o loko o 15-25 mm e loaʻa ai ka hohonu o 40 mm.E hoʻololi like i nā ʻāpana o ka Reference suspension A, Reference suspension B, ka wai, a me ka Diluent e hoʻokaʻawale i nā paipu hōʻike like.E hoʻohālikelike i nā hoʻonā i ka lā ākea, e nānā pono ana i kahi ʻeleʻele ʻeleʻele (e nānā i ka Spectrophotometry a me Light-Scattering 851, Visual Comparison).[E hoʻomaopopo—Pono ka hoʻopuehu ʻana o ka mālamalama i hiki ke hoʻokaʻawale ʻia ka Reference Suspension A me ka wai, a ʻo ka Reference Suspension B e hiki ke hoʻokaʻawale ʻia mai ka Reference Suspension A. ]
Paʻa e ʻae ai: Hōʻike ka ʻaha Laʻana i ka māmā like me ka wai, a i ʻole Diluent, a i ʻole kona opalescence ʻo NMT ka mea o ka Reference suspension A.
• Ke kala o ka Haʻina
Diluent A: 200-g/L solution o ka sodium acetate
Diluent B: 10-g/L solution o ka waikawa hydrochloric
Haʻina waiwai maʻamau: Ferric chloride CS, cobaltous chloride CS, cupric sulfate CS, a me ka Diluent B (3.0:3.0:2.4:1.6)
Haʻina maʻamau: Haʻina waihona maʻamau a me ka Diluent B (1 i ka 100).[E hoʻomaopopo-E hoʻomākaukau i ka hopena maʻamau ma mua o ka hoʻohana ʻana.]
Haʻina Laʻana: E hoʻohana i ka hāʻina Laʻana mai ka hoʻāʻo no ka Clarity of Solution.
Kānāwai
Nā Laʻana: Diluent A, Haʻina maʻamau, Haʻina hāʻina, a me ka wai
E hoʻololi i kahi ʻāpana kūpono o ka hopena laʻana i kahi paipu hoʻāʻo o ke aniani ʻeleʻele, aniani, kū ʻole me ke kumu pālahalaha a me ke anawaena o loko o 15-25 mm e loaʻa ai ka hohonu o 40 mm.E hoʻololi like i nā ʻāpana o ka solution Standard, Diluent A, a me ka wai e hoʻokaʻawale i nā paipu hoʻāʻo like.E hoʻohālikelike i nā hoʻonā i ka lā ākea, e nānā pono ana i kahi kāʻei keʻokeʻo (e nānā i ka Spectrophotometry a me Light-Scattering 851, Visual Comparison).
Nā pae hoʻohālikelike: He ʻano wai a i ʻole Diluent A ke ʻano o ka hāpana laʻana, a ʻaʻole ʻoi aku ka ʻoi aku o ke kala ma mua o ka hopena maʻamau.
NA KOI HOU
• Hoʻopili a me ka waiho ʻana: mālama i loko o nā pahu paʻa maikaʻi.E mālama i ka lumi wela.
• Nā Kūlana Kūlana USP <11>
USP Saccharin RS Kaomi no ka nānā ʻana i ke ʻano
USP o-Toluenesulfonamide RS
USP p-Toluenesulfonamide RS