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本文研究了在磷酸介质中用乙基紫显色,以乙酸异戍酯萃取比色测定微量铊的方法。确定在20毫升发色溶液体积中各试剂用量:3毫升磷酸(2∶1)、1毫升25％三氯化铁、1毫升0.2％乙基紫、10毫升乙酸异戊酯。有色络合物稳定48小时,温度在5—31℃没有影响,最大吸收峰在603毫微米处,0—40微克铊/10毫升服从比尔定律,克分子消光系数为1.1×10~5。大量 NH_4~+、K~+、Na~+、UO_2~(2+)、SO_4~(2-)、NO_3~-、BO_3~(3-)、C_2H_3O_(2-)、C_2O_4~(2-)、C_4_H_4O_6~(2-)、C_6H_5O_7~(3-);100毫克Sn~(4+)、Mn~(2+)、Cu~(2+)、Zn~(2+);50毫克Al~(3+);10毫克Mo~(6+)、Zr~(4+)、Si~(4+)、Ca~(2+)、Mg~(2+)、Ba~(2+)、Pb~(2+)、Cd~(2+)、Sb~(3+)、Co~(2+)、Ni~(2+);5毫克La~(3+);4.5毫克F~-;3毫克Th~(4+)、Te~(4+)、Bi~(3+)、As~(3+)、As~(5+);2毫克V~(5+)、In~(3+);1.5毫克Se~(4+);1毫克Ga~(3+);500微克W~(6+);250微克Ag~+;200微克Re~(7+)、Cr~(6+)、Hg~(2+);100微克Sb~(5+);1微克Au~(3+)没有影响,加入0.5克柠檬酸可消除1毫克Cr~(6+)的影响,以二氯化锡还原过滤可消除100微克Au~(6+)、10毫克Hg~(2+)、10毫克Sb~(5+)的干扰。本法选择性好,灵敏度高,操作简便。矿样测定结果表明,方法的准确性和重现性均良好。
In this paper, we studied the method of colorimetric determination of trace amounts of thallium with ethyl violet in phosphoric acid medium and the colorimetric extraction with isoprenyl acetate. Determine the amount of each reagent in a volume of 20 ml of chromogenic solution: 3 ml phosphoric acid (2: 1), 1 ml 25% ferric chloride, 1 ml 0.2% ethyl violet and 10 ml isoamyl acetate. The colored complex is stable for 48 hours, the temperature has no effect at 5-31 ℃, the maximum absorption peak at 603 nm, 0-40 μg thallium / 10 ml obeys Bill’s law, and the molecular extinction coefficient is 1.1 × 10 -5. A large number of NH 4 +, K +, Na +, UO 2 2+, SO 4 2-, NO 3 -, BO 3 3-, C 2 H 3 O 2-, C 2 O 4 2-, , C 4 H 4 O 6 2-, C 6 H 5 O 3-7; 100 mg Sn 4+, Mn 2 +, Cu 2+, Zn 2+ 50 mg Al ~ (2 +), 3 +); 10 mg Mo 6+, Zr 4+, Si 4+, Ca 2+, Mg 2+, Ba 2+, Pb 2+, (2 +), Cd 2+, Sb 3+, Co 2+, Ni 2+; 5 mg La 3+; 4.5 mg F 3 - (4 +), Te ~ (4 +), Bi ~ (3 +), As ~ (3 +) and As ~ (5 + ; 1.5 mg Se ~ (4 +); 1 mg Ga ~ (3 +); 500 μg W ~ (6 +); 250 μg Ag ~ +; 200 μg Re ~ Hg 2 +, 100 μg Sb 5+ and 1 μg Au 3+ did not affect the addition of 0.5 g citric acid to 1 mg Cr 6+, Reduction filtration can eliminate the interference of 100 μg Au ~ (6 +), 10 mg Hg ~ (2 +) and 10 mg Sb ~ (5+). The law of selectivity, sensitivity, easy to operate. The result of ore sample determination shows that the accuracy and reproducibility of the method are good.