混合けい光体による無機イオンの定性分析

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The mixed fluorescent material technique developed by Tamura {Z. Tamura : Talanta, 19, 573 (1972)} as a qualitative analysis of ultraviolet-absorbing compounds was applied to detection of inorganic ions. Sample solutions of cations were generally prepared by dissolving the nitrates in water, although some of them by dissolving the nitrates or chlorides in dilute HNO3 or HCl. Sample solutions of anions were prepared by dissolving the sodium or potassium salts in 5% Na2CO3. One μl of the sample solution was applied on a Toyo filter paper No. 51A with the aid of Microcaps (Drummond Scientific Co., USA), air-dried and developed about 25 cm with a suitable solvent system. The air-dried paper was placed on a light source (Pan UV Lamp, PUV-1 type, Tokyo Kogaku Kikai) emitting a continuous ultraviolet rays at 250400 nm, covered with a fluorescent screen of 80 μm thickness made of Sr2P2O7/Sn, Zn2SiO4/Mn and YVO4/Eu (20 : 5 : 0.2) and the chromatogram was observed in the dark. About half of ions tested were detected in quantities of below 50 μg. In particular, several transition metal ions were detected with high sensitivity (Table I) in chromatography with 2N HNO3, 2N HCl and n-butanol (2 : 1 : 6, v/v; upper phase, I). The limits of detection and the colors of detectable cations other than those in Table I were Tl+ (0.01 μg, red), Sn 2+ (4 μg, red), ZrO2+ (40 μg, red), Ce3+ (0.1 μg, red), UO22+ (0.1μg, red) and Hg22+ (0.3 μg, reddish brown). On the other hand, Li+, Na+, K+, NH4+, Ca2+, Ba2+, Sr2+, Mg2+, Zn2+, Cd2+, As3+, Al3+, Y3+, La3+, Th4+ and As5+ were not detected in quantities of 50 μg. A simultaneous analysis of 10 cations was achieved by comparing the colors and the Rf values after chromatographic separation with I (Fig. 1) and another solvent system (acetone, 35% HC1 and water, 20 : 2 : 1, v/v; II). The limits of detection of anions were generally order of μg (Table II). Each 50 μg of Cl-, Br-, F-, ClO3-, BrO3-, CN-, ClO-, CO32-, SO42-, SO32-, BO22-, SiO32-, AsO43- and PO43- was negative. Nine anions were simultaneously identified by paper chromato-graphy with n-butanol, methanol and water (1 : 3 : 1, v/v; III) and acetone and water (10 : 1, v/v; IV). Thin layer chromatography of inorganic anions was also studied with silica gel added with 10% of the mixed fluorescent material (Wakogel FM Plate, Wako Pure Chemical Industries, Ltd.). The results obtained were similar to those in paper chromatography (Table III).
社団法人日本分析化学会の論文

混合けい光体による無機イオンの定性分析

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