Showing papers in "Bunseki Kagaku in 1983"

Post-column fluorometric detection of reducing sugars in high performance liquid chromatography using arginine

Abstract: Arginine was found to react with reducing sugars after being heated in boric acid solution at neutral pH; highly fluorescent derivatives were produced. This reaction was applied to a postcolumn reaction system for high performance liquid chromatography and found to be useful for highly sensitive determination of reducing sugars.

Color Reaction Between Pyrogallol Red - Molybdenum(VI) Complex and Protein

Abstract: A color reaction between pyrogallol red(PR) -molybdenum(VI) complex and protein was investigated. A spectrophotometric method using the PR-molybdenum(VI) complex could be used in the concentration range of 0 - 400 μg/10 ml of albumin, where the Sandell sensitivity was calculated to be 0.0048 μg/cm2 for albumin at 600 nm. A detection test of protein on a spot plate was also studied. The proposed method was applied to the determination of urinary protein; analytical results were satisfactory.

Determination of the standard free energies of transfer of alkylammonium ions from nitrobenzene to water using polarographic methods with immiscible electrolyte solution interface

Abstract: The standard Gibbs free energies of transfer of fifteen kinds of alkylammonium ions from nitrobenzene to water, ΔGΘ, N→Wtr, j, were determined by means of cyclic voltammetry and potential-step chronoamperometry. The ΔGΘ, N→Wtr, j of the alkylammonium ions has an additive-constitutive property.

4-(2-ピリジルアゾ)レソルシノールを用いる白金(ii)及びパラジウム(ii)の吸光検出逆相イオン対分配高速液体クロマトグラフィー

Abstract: 白金(II)及びパラジウム(II)は,塩化物イオン共存下2-プロパノール-水混合溶媒中で4-(2-ピリジルアゾ)レソルシノール(PAR,H2par)と反応して,金属イオン:塩化物イオン:PAR;1:1:1の三元錯体を形成する.1価の陰イオン種[PtCl(par)-]及び[PdCl(par)-]は,テトラブチルアンモニウムイオンを対陽イオンとして,逆相イオン対分配高速液体クロマトグラフィーによる分離が可能である.これを利用して,PARによる白金(II)及びパラジウム(II)の同時定量法を確立した.本法により1×10-6moldm-3の白金(II)及び5×10-7moldm-3のパラジウム(II)が定量できた.1×10-5moldm-3の目的成分に対し,10-4moldm-3の鉄(II),コバルト(II),ニッケル(II),銅(II),亜鉛(II),アルミニウム(III),クロム(III)及びロジウム(III)の共存は許容された.

Study on wet digestion method for determination of total arsenic in marine organisms by continuous flow arsine generation and atomic absorption spectrometry using some model compounds

Abstract: A wet digestion method to determine total arsenic in marine organisms by continuous flow arsine generation and atomic absorption spectrometry was studied using some model compounds. Conditions for the generation of arsine were also studied for inorganic arsenite and arsenate, methylarsonic acid, dimethylarsinic acid, and phenylarsonic acid. The methylated arsenic species, phenylarsonic acid and arsenobetaine were completely decomposed to inorganic arsenate by the wet oxidation with nitric acid-perchloric acid-sulfuric acid system; an addition of nickel ion in the digestion process was not needed. Perchloric acid was essential to the complete decomposition of arsenobetaine when digestion was carried out on a hot plate.

Crown ether-based extraction photometric reagents for calcium

Abstract: New, highly sensitive extraction photometric reagents for calcium were derived from cryptand-21 and -22 by introducing mono-protonic chromophoric groups, 2-hydroxy-5-X-benzyls (X = 4-nitrophenylazo, 2, 4-dinitrophenylazo), on the amino nitrogens. The reagents (H2L) extracted alkaline earth metal ions (M2+) into 1, 2-dichloroethane by forming ML type complexes. The selectivity followed the order, Ca2+>Sr2+>Ba2+>>Mg2+, for both types of the reagents, and the extractability with cryptand-22 reagents surpassed that of cryptand-21 reagents. The interferences and the masking of transition metals in the determination of calcium were studied.

α,β,γ,δ-テトラキス(4-ヒドロキシフェニル)ポルフィンを用いる微量銅(II)及び亜鉛(II)の高速液体クロマトグラフィー

Abstract: α,β,γ,δ-テトラキス(4-ヒドロキシフェニル)ポルフィン (THPP)の高速液体クロマトグラフィー(HPLC)用分析試薬としての性能を調べた. THPPは,アルコール類に非常に良く溶解し,エタノール-水混合溶媒{(40～50)v/v%}中で同時錯形成反応が行えること,化学結合型充てん剤(オクタデシルシラン)と溶離液(エタノール:水=75:25 v/v%)を用いた逆相分配系HPLCによる金属錯体の分離が可能であること,又検出波長(420nm)における銅錯体及び亜鉛錯体のモル吸光係数はそれぞれ3.2×105cm-1mol-1dm3であることを明らかとした.定量操作によって得られたクロマトグラムのピーク高さによる検量線は各々,0～2×10-6mol dm-3の範囲で直線であり,検量線中央値における5回繰り返し測定の変動係数は,銅(II)(2.1%), 亜鉛(II)(3.4%)であった.

Separation mechanism of anion chromatography on silica gel coated with polyamide crown resin and its application

Abstract: A new packing material of silica gel coated with polyamide crown resin was useful to separate anions but did not separate cations with water as eluent. It was shown by photoacoustic spectroscopy that the selectivity for cations was diminished because of hydrogen bond between silanol group on the silica gel surface and the crown ether of the polyamide crown resin. The elution volume of anion was dependent on the Gibbs free energy of hydration and the salt of a strongly hydrated anion eluted earlier than the salt of a weakly hydrated anion. The silica gel coated with the resin can be applied to chromatograph anions in environmental sample solutions and amino acids.

Fluorescence reaction of common epoxides with nicotinamide and acetophenone

Abstract: A spectrofluorometric method for determination of common epoxides based on a fluorescence reaction of the epoxy group with nicotinamide and acetophenone is described. By the method, as little as 10ng order of five aliphatic epoxides could be determined with a coefficient of variation of ca. 3 to 5%.The analysis of the reaction product showed that the fluorophore had a 2, 7-naphthyridine structure.

Distribution coefficients of alkaline earth metal ions and their possible applications on crystalline hydrous titanium dioxide fibers

Abstract: The distribution coefficients of alkaline earth metal ions were measured on crystalline hydrous titanium dioxide fibers at 298K. The adsorption behavior of these ions was well explained by their ion-exchange reaction with hydrogen-ions in the fibers. The distribution coefficients of alkaline earth metals were determined as a function of pH. Separation of strontium(II) from barium(II) was achieved by using a column of this ion-exchanger with hydrochloric acid solutions as an eluent.

Adsorption behavior of tungsten(vi) onto activated carbon

Abstract: The adsorption behavior of tungsten(VI) onto activated carbon was studied by using a column method. The result was compared with those of molybdenum(VI), chromium(VI) and other ions. The adsorption of tungsten(VI) shows remarkable pH-dependency, like that of molybdenum(VI) and chromium(VI). The adsorption-pH curves shift toward the higher pH in the following order: HClO4

マレオニトリルジチオールを用いるパラジウム(ii)及び白金(ii)の吸光検出逆相イオン対クロマトグラフィー

Abstract: マレオニトリルジチオール(MNT, H2L)を用いて,パラジウム(II)及び白金(II)を吸光検出高速液体クロマトグラフィーにより分離定量する方法を開発した.錯形成反応は, pH=5 (0.01 mol dm-3酢酸緩衝液), 10-3mol dm-3エチレンジアミン四酢酸二ナトリウム(EDTA), 4×10-4mol dm-3MNTの溶液中で,80℃, 40分間の加熱で定量的に進行した.充てん剤としてODS-シリカを用い,溶離液として0.2wt%の臭化テトラブチルアンモニウム,0.1wt%の酢酸-酢酸ナトジウム,及び0.02wt%のEDTAを含む42 wt%テトラヒドロフラン-水混合溶媒が適当であった.検出波長320nmにおける検量線は,パラジウム(II): (2×10-8～10-5)mol dm-3,白金(II): (5×10-8～10-5)mol dm-3の範囲で直線となった.本法は,既存の吸光分析法に比べて最も高感度な分析法である.

Digestion method of marine organisms for determination of total arsenic by atomic absorption spectrometry

Abstract: A wet digestion method adding nickel ion for the determination of total arsenic in marine organisms was evaluated from the characteristics of arsenic in graphite furnace atomic absorption spectrometry. The necessity of an addition of nickel ion in a wet digestion process could not be confirmed in any case examined. The concentrations of arsenic in marine organisms determined by graphite furnace and arsine generation atomic absorption spectrometry after digested with nitric acid, perchloric acid and sulfuric acid were in good agreement with each other. The accuracy of each method was studied by analyzing NBS SRM 1566 oyster tissue.

マラカイトグリーン-過ヨウ素酸カリウム触媒酸化反応の誘導期測定による極微量マンガン(ii)の吸光光度定量

Abstract: 高濃度のマラカイトグリーン(MG)溶液を用い,水に対し吸光度約1.8を示す吸収板を対照液の代わりに用いて,約0.2以下の吸光度変化を測定すると,過ヨウ素酸によるMGの酸化反応はマンガン(II)の存在量に逆比例する誘導期を示し,誘導期後,反応は擬零次反応で近似できた.従って,一次反応として速度定数を求める既報のように,吸光度の経時変化を対数プロットする必要もなく,記録紙上の吸光度の経時変化から,直接,簡便に誘導期が求められた.吸光度変化の測定時間は既報の半分以下の25分以内で済み,更に簡便に(5～200)ngのマンガン(II)が定量できた.又,共存イオンの影響も既報より少なく,特に,鉄(III)はマンガン(II)の104倍量まで共存しても差し支えなかった.

Generation of trace amount of acrolein standard gas using reaction gas chromatography

Abstract: A new method for the generation of acrolein standard gas has been described. It is based on the dehydration of glycerol by using potassium hydrogen sulfate as the catalyst. Comparing the results with formerly reported allyl alcohol oxidation method, the present method provides easier and much reproducible means for the preparation in the nanogram range.

Determination of trace low molecular weight aliphatic carbonyl compounds in auto exhaust by gas chromatography with a glass capillary column

Abstract: ガラスキャピラリーカラムを使用したガスクロマトグラフィーによる微量低級カルボニル化合物の定量法について検討した.自動車排気ガス中のカルボニル化合物を2,4-ジニトロフェニルヒドラジン(DNPH)と反応させ誘導体化した後,ガラスキャピラリーカラム(液相OV-17,内径0.27mm,長さ30m)を装着したガスクロマトグラフにより分析した結果,プロピオンアルデヒド,アセトン及びアクロレインの炭素数3から成る低級カルボニル化合物は,完全に分離され個別に定量が可能となり,ホルムアルデヒドやアセトアルデヒドなどと同時分析ができた.本法によるカルボニル化合物の定量限界濃度は,排気ガス10lを採取した場合,ホルムアルデヒド,アセトアルデヒド,及びアクロレインでは,それぞれ,85ppb,140ppb,及び190ppbであった.

薄層クロマトグラフィー及びガスクロマトグラフィーを用いたヒト血しょう,血小板,赤血球膜の脂質画分の高級脂肪酸の定量法

Abstract: 生体試料中の種々の脂質中の高級多価不飽和脂肪酸を精度よく分離定量する目的でヒト血しょう,血小板,赤血球膜ゴーストから総脂質を抽出した後薄層クロマトグラフィーによりリン脂質,中性脂肪,コレステロールエステル及び遊離脂肪酸を分離し三フッ化ホウ素メタノールによりメチルエステル化しガスクロマトグラフィーで分離定量した.抽出操作中の脂肪酸の酸化を防止する目的で0.2%のブチルヒドロキシトルエンを添加し薄層クロマトグラフィー上の試料の検出に蛍光物質を用いたところ回収率,再現性ともに良好な結果が得られた。更に高度に精製されたエイコサペンタエン酸エチルエステル摂取後の健常人において,血しょう,血小板,及び赤血球膜ゴーストのいずれのリン脂質画分においても有意のエイコサペンタエン酸の増加を認めた.本法は種々の生体試料中の脂質画分での高級脂肪酸の定量法の一つとして有用と考えられる.

Flow injection analysis using immobilized enzyme reagent

Abstract: A flow injection analytical method (f.i.a.) with a glass capillary open tubular reactor is proposed, on the inner wall of which an enzyme is immobilized by covalent attachment. A procedure is discussed for designing the f.i.a. system in which a given pair of the sampling rate and the reaction time should be achieved. This method allows to determine the inner diameter and the length of the reactor, flow rate of the carrier stream and the operational pressure. As an example, the design of reactor and the optimization of operational parameters in determination of ethanol by alcohol dehydrogenase are shown.