Pub Date : 2001-10-10DOI: 10.1246/NIKKASHI.2001.567
貞信 井上
金属イオンの捕集剤としてN-ベンゾイル-N-フェニルヒドロキシルアミン(以下BPHAと略)を担持したアンバーライトXAD-7樹脂(BPHA/XAD樹脂)を用いて，水溶液中から微量スズを捕集する方法について検討した．0.1–0.4 gのBPHA/XAD樹脂を用い，バッチ法により50–500 cm3の0.25 mol dm−3塩酸酸性溶液中から，微量スズを定量的に捕集できる条件を見いだした．捕集後，スズを吸着した樹脂を，0.5 mol dm−3硫酸-エタノールの混合溶液(1 : 1，v/v)とふりまぜることによりスズを溶離できる．溶離液中のスズは，プレカラム誘導体化試薬として2-(5-ニトロ-2-ピリジルアゾ)-5-[N-プロピル-N-(3-スルホプロピル)アミノ]フェノール(以下Nitro-PAPSと略)を用いたSn-Nitro-PAPS錯体として吸光検出逆相HPLCにより定量する．吸光度フルスケール(AUFS)を0.002に設定した場合，ピーク高さから作成した検量線はスズ(IV)0–8.0 ng cm−3の範囲でよい直線性を示した．検量線の中央値に相当する量のスズ(4.0 ng cm−3)を3回測定したときの相対標準偏差(RSD)は1.8%であった．HPLC法自体(前濃縮を行わない場合)の検出限界(試薬ブランク値の3σ)は0.58 ng cm−3(n = 5)であった．固相抽出とHPLCとの組み合わせによって，試料水500 cm3を用いた場合のスズの検出限界(から試験液の3σ)は0.03 ng cm−3であった．
作为金属离子的捕获剂，采用携带正苯二甲酸二苯基羟基胺(以下简称BPHA)的琥珀光XAD-7树脂(BPHA/XAD树脂)，研究了从水溶液中采集微量锡的方法。采用0.1 - 0.4 g的BPHA/XAD树脂，通过批量法发现了在50 - 500cm3的0.25 mol dm - 3盐酸酸性溶液中定量采集微量锡的条件。捕集后，将吸附锡的树脂与0.5 mol dm - 3硫酸-乙醇的混合溶液(1∶1,v/v)混合，即可溶离锡。溶离液中的锡，用2-(5-硝基-2-吡啶偶氮)-5-[N-丙基-N-(3-磺丙基)氨基]苯酚(以下简称Nitro-PAPS)制成的Sn-Nitro-PAPS配合物通过吸光检测反相HPLC进行定量。当吸光度全标度(AUFS)设定为0.002时，从峰值高度制作的检量线在锡(IV)0 - 8.0 ng cm - 3范围内表现出良好的线性。测量相当于检量线中央值的锡(4.0 ng cm - 3)时的相对标准差(RSD)是1.8%。HPLC法本身(在不进行预浓缩的情况下)的检测极限(试剂消隐值3σ)为0.58 ng cm - 3(n = 5)。通过固相提取与HPLC相结合，使用500cm3样品水时锡的检测极限(从测试液的3σ)为0.03 ng cm - 3。
{"title":"N-ベンゾイル-N-フェニルヒドロキシルアミン担持XAD樹脂を用いた固相抽出濃縮と逆相分配高速液体クロマトグラフィーによる微量スズの定量","authors":"貞信 井上","doi":"10.1246/NIKKASHI.2001.567","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2001.567","url":null,"abstract":"金属イオンの捕集剤としてN-ベンゾイル-N-フェニルヒドロキシルアミン(以下BPHAと略)を担持したアンバーライトXAD-7樹脂(BPHA/XAD樹脂)を用いて，水溶液中から微量スズを捕集する方法について検討した．0.1–0.4 gのBPHA/XAD樹脂を用い，バッチ法により50–500 cm3の0.25 mol dm−3塩酸酸性溶液中から，微量スズを定量的に捕集できる条件を見いだした．捕集後，スズを吸着した樹脂を，0.5 mol dm−3硫酸-エタノールの混合溶液(1 : 1，v/v)とふりまぜることによりスズを溶離できる．溶離液中のスズは，プレカラム誘導体化試薬として2-(5-ニトロ-2-ピリジルアゾ)-5-[N-プロピル-N-(3-スルホプロピル)アミノ]フェノール(以下Nitro-PAPSと略)を用いたSn-Nitro-PAPS錯体として吸光検出逆相HPLCにより定量する．吸光度フルスケール(AUFS)を0.002に設定した場合，ピーク高さから作成した検量線はスズ(IV)0–8.0 ng cm−3の範囲でよい直線性を示した．検量線の中央値に相当する量のスズ(4.0 ng cm−3)を3回測定したときの相対標準偏差(RSD)は1.8%であった．HPLC法自体(前濃縮を行わない場合)の検出限界(試薬ブランク値の3σ)は0.58 ng cm−3(n = 5)であった．固相抽出とHPLCとの組み合わせによって，試料水500 cm3を用いた場合のスズの検出限界(から試験液の3σ)は0.03 ng cm−3であった．","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"30 1","pages":"567-572"},"PeriodicalIF":0.0,"publicationDate":"2001-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76892411","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2001-08-10DOI: 10.1246/NIKKASHI.2001.483
仁 草間, 裕則 荒川
The effect of precursors on CO2 hydrogenation reactivity was observed over Rh–Li/SiO2 and Rh–Fe/SiO2 catalysts prepared by co-impregnation method. The highest CO2 conversions were obtained over the catalysts prepared from Rh acetate and additive nitrate. For the catalysts prepared from chloride precursor, CH4 selectivity was high but CO one low. On the other hand, the catalysts prepared from non-chloride precursors showed high CO selectivity and low CH4 one. The Rh–Li/SiO2 catalyst prepared from Rh nitrate and Li chloride, and the Rh–Fe/SiO2 one prepared from Rh acetate and Fe nitrate showed the highest ethanol selectivity, respectively.
{"title":"シリカ担持ロジウム-リチウム，ロジウム-鉄触媒を用いた二酸化炭素の接触水素化反応に及ぼす触媒前駆物質の影響","authors":"仁 草間, 裕則 荒川","doi":"10.1246/NIKKASHI.2001.483","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2001.483","url":null,"abstract":"The effect of precursors on CO2 hydrogenation reactivity was observed over Rh–Li/SiO2 and Rh–Fe/SiO2 catalysts prepared by co-impregnation method. The highest CO2 conversions were obtained over the catalysts prepared from Rh acetate and additive nitrate. For the catalysts prepared from chloride precursor, CH4 selectivity was high but CO one low. On the other hand, the catalysts prepared from non-chloride precursors showed high CO selectivity and low CH4 one. The Rh–Li/SiO2 catalyst prepared from Rh nitrate and Li chloride, and the Rh–Fe/SiO2 one prepared from Rh acetate and Fe nitrate showed the highest ethanol selectivity, respectively.","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"93 1","pages":"483-485"},"PeriodicalIF":0.0,"publicationDate":"2001-08-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83497531","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2001-07-10DOI: 10.1246/NIKKASHI.2001.433
健一 中林, 博智 江並, 秀秋 束元, 大内 秋比古
The direct photocyclization of four 1,4-diarylcyclohepta-1,3-dienes(1a–d) with different aryl groups (phenyl, 1-naphthyl, and 2-naphthyl groups) by a XeCl excimer laser (308 nm) in hexane gave 1,5-diarylbicyclo[3.2.0]hept-6-enes (2a–c). The efficiency of the photochemical cyclization and fluorescence quantum yield strongly depended upon the aromatic substituents and this is interpreted by the conformation of the molecules.
{"title":"1位あるいは4位にナフチル基を有するジアリールシクロヘプタ-1,3-ジエンの特異的光閉環反応","authors":"健一 中林, 博智 江並, 秀秋 束元, 大内 秋比古","doi":"10.1246/NIKKASHI.2001.433","DOIUrl":"https://doi.org/10.1246/NIKKASHI.2001.433","url":null,"abstract":"The direct photocyclization of four 1,4-diarylcyclohepta-1,3-dienes(1a–d) with different aryl groups (phenyl, 1-naphthyl, and 2-naphthyl groups) by a XeCl excimer laser (308 nm) in hexane gave 1,5-diarylbicyclo[3.2.0]hept-6-enes (2a–c). The efficiency of the photochemical cyclization and fluorescence quantum yield strongly depended upon the aromatic substituents and this is interpreted by the conformation of the molecules.","PeriodicalId":19311,"journal":{"name":"Nippon Kagaku Kaishi","volume":"10 1","pages":"433-435"},"PeriodicalIF":0.0,"publicationDate":"2001-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76321812","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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