Abstract：After the sample was dissolved by hydrochloric acid and nitric acid, the nitric acid was dried by distillation and the hydrochloric acid in the extract solution was controlled at around 1.0 mol/L. With 5-mercapto-3-phenyl-1,3,4-thiadiazole-2(3H)-thione potassium salt (bismuth reagent Ⅱ) as complex agent and octyl phenoxy poly ethoxy (Triton X-100) as extraction agent, gold was extracted with cloud point extraction in boiling water bath. Thus, a method for determination of gold in geological sample was established by inductively coupled plasma mass spectrometry(ICP-MS). The optimal conditions for cloud point extraction were as follows: 0.5 mL of bismuth reagent Ⅱ, 2.5 mL of Triton X-100 solution was added in the diluted sample solution, the colorimetric tube was heated in water bath at 100 ℃ for 30 min and the organic phase was diluted to 5 mL with 10% (volume fraction) diluted aqua regia. The matrix effect of bismuth reagent Ⅱ and signal drift of instrument could be effectively corrected with 20 μg/L 185Re as inner standard. The enrichment ratio of cloud point extraction was 4.75. The detection limit was 1.3 μg/L. GBW07405 yellow-red soil certified reference material, GBW07300 gold component analysis certified reference material for gold ores, S1 and S2 actual rock samples were determined by this method, whose results were consistent with the certified values or those obtained by foam adsorption-graphite furnace atomic absorption spectrometry. The relative standard deviation (RSD, n=6) was 1.2%-3.6%.
余滔,邵坤,李可及. 浊点萃取-电感耦合等离子体质谱法测定地质样品中金[J]. 冶金分析, 2015, 35(3): 32-36.
YU Tao,SHAO Kun,LI Ke-ji. Determination of gold in geological sample by inductively coupled plasma mass spectrometry with cloud point extraction. , 2015, 35(3): 32-36.
LIAN Y P,ZHEN W,TAI Z G , et al. Cloud point extraction and flame atomic absorption spectrometry analysis of palladium,platinum,and gold ions frome industrial polluted soil [J]. Rare Metals,2012,31(5):512-516.
[6]
DENG J, HUANG K H, AN L, et al.Cloud point extraction and simultaneous spectrophotometric determination of Ⅴ, Co and Cu ions in water samples by 5-Br-PADAP using partial least squares regression[J].Journal of Radioanalytical and Nuclear Chemistry, 2014, 300(2):835-842.
[7]
Sylvester P J, Eggins S M. Analysis of Re, Au, Pd, Pt and Rh in NIST glass certified reference materials and natural basalt glasses by laser ablation ICP-MS[J]. Geostandards Newsletter, 1997, 21(2):215-229.
陈建波,刘伟,崔艳梅,等.浊点萃取-高效液相色谱法测定草莓汁中的多种农药残留[J].分析化学(Chinese Journal of Analytical Chemistry),2008,36(3):401-404.
[10]
Md Saleh N, Muggundha R, Sharifah M, et al.Extraction of parabens from water samples using cloud point extraction with a non-ionic surfactant with β-cyclodextrin as modifier[J].Journal of Surfactants and Detergents,2014,17(4):747-758.
[11]
Sardar N, Ali M S,Kamil M, et al.Phase behavior of nonionic polymer hydroxypropylmethyl cellulose: Effect of gemini and single-chain surfactants on the energetics at the cloud point [J].Journal of Chemical and Engineering Data, 2010, 55 (11): 4990-4994.
