|
|
|
| The determination of trace tin in water samples by inductively coupled plasma mass spectrometry (ICP-MS) after separation and enrichment using mercapto containing dextran gel |
Bing-Xu XU, Xia XING, Jin-Li XU, Hai-Jie CHEN, Qin ZHANG, Ya-Xuan LIU( ) |
| Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences, Langfang 065000, China |
|
|
|
|
Abstract The content of tin in geochemical water samples is generally low, and there is no standard method which can be used currently. In this investigation, the trace tin in water samples was detected by inductively coupled plasma mass spectrometry (ICP-MS) after separation and enrichment using mercapto containing dextran gel (SDG). The separation conditions of the SDG column were optimized. The separating effect of tin was the best when the acidity of the solution before filtering by the column was 1% (v/v) hydrochloric acid, the ion strength was 0.1mol/L counted by NaAc, the acidity of eluent was 6N hydrochloric acid and the volume of the eluent was 30 mL. When the proposed method was applied to analyzing actual water samples, the detection limit of tin was 0.37μg/L, the precision (RSD%) was less than 10%, and the recovery rate was in the range of 90%~110%, which could satisfy the determination requirement of trace tin in geochemical water samples.
|
|
Received: 13 December 2018
Published: 15 August 2019
|
|
|
|
Corresponding Authors:
Ya-Xuan LIU
E-mail: liuyaxuan@igge.cn
|
|
|
|
| 参数 | 射频功率
/W | 雾化气流量
/(L·min-1) | 辅助气流量
/(L·min-1) | 冷却气流量
/(L·min-1) | 扫描方式 | 扫描次数
/次 | 停留时间
/ms | 采样深度
/step | | 设定值 | 1400 | 0.86 | 0.7 | 14 | 跳峰扫描 | 60 | 10 | 200 |
|
Operating parameters of ICP-MS
|
|
The relationship between adsorption quality of tin and acidity
|
|
The relationship between adsorption quality of tin and ionic strength
|
|
The relationship between elution quality and acidity of eluent
|
|
The relationship between elution quality and volume of eluent
|
| 样品 | 测定值
/(μg·L-1) | 加标量
/(μg·L-1) | 加标后测定值
/(μg·L-1) | 回收量
/(μg·L-1) | 回收率
/% | AFS测定值
/(μg·L-1) | | 水样1 | 1.06 | 2.0 | 2.89 | 1.84 | 91.78 | 1.11 | | 水样2 | 1.08 | 2.0 | 2.93 | 1.85 | 92.49 | 1.13 | | 水样3 | 0.95 | 2.0 | 3.05 | 2.10 | 105.12 | 0.93 | | 水样4 | 0.90 | 2.0 | 3.05 | 2.15 | 107.67 | 0.79 | | 水样5 | 1.36 | 2.0 | 3.47 | 2.11 | 105.69 | 1.25 | | 水样6 | 1.56 | 2.0 | 3.43 | 1.87 | 93.72 | 1.55 | | 水样7 | 0.68 | 2.0 | 2.56 | 1.88 | 94.19 | 0.73 |
|
Determination of tin in water samples
|
| 样品 | ICP-MS | 测定值
/(μg·L-1) | 平均值
/(μg·L-1) | RSD/% | | 水样8 | 2.65
2.65
2.28
2.28
2.12
2.12 | 2.28 | 10.00 | | 水样9 | 5.23
5.23
4.93
4.93
4.12
4.12 | 4.70 | 8.24 | | 水样10 | 6.93
6.93
7.25
7.25
6.78
6.78 | 7.10 | 7.53 | | 样品 | AFS | 测定值
/(μg·L-1) | 平均值
/(μg·L-1) | RSD/% | | 水样8 | 2.05
2.29
1.88
2.69
2.58
1.98 | 2.24 | 14.83 | | 水样9 | 4.39
4.97
5.90
4.42
4.86
4.84 | 4.90 | 11.21 | | 水样10 | 6.95
6.95
6.12
7.22
7.38
8.52 | 7.19 | 10.91 |
|
Precision of the method
|
| 仪器 | ICP-MS | | 测定值/(μg·L-1) | 0.53
0.71
0.86
0.62
0.58
0.67
0.74
0.87
0.89
0.73
0.76
0.89 | | 检出限/(μg·L-1) | 0.37 | | 仪器 | AFS | | 测定值/(μg·L-1) | 0.5110
0.5580
1.2780
1.2575
1.3530
0.9700
0.8910
0.7330
0.5250
0.5815
0.5900
0.5320 | | 检出限/(μg·L-1) | 0.98 |
|
Detection limit of the method
|
| [1] |
杨月欣, 王光亚 . 实用食物营养成分分析手册[M]. 北京: 中国轻工业出版社, 2002.
|
| [1] |
Yang Y X, Wang G Y. Practical food nutrition analysis manual[M]. Beijing: China Light Industry Press, 2002.
|
| [2] |
钟彬扬 . 氢化物发生原子荧光法测定生活饮用水中的痕量锑、锡[J]. 广东微量元素科学, 2015,22(10):11-14.
|
| [2] |
Zhong B Y . Combined determination atomic fluorescence spectrometic was used to analyze trace Sb, Sn in drinking water by hydride generation atomic fluorescence spectrometry[J]. Guangdong Trace Elements Science, 2015,22(10):11-14.
|
| [3] |
GB5749—2006 生活饮用水卫生标准[S]. 2006.
|
| [3] |
GB5749—2006 Standards for drinking water quality[S]. 2006.
|
| [4] |
韩兆祥, 王宝庆 . 改性膨润土对有机锡的吸附动力学研究[J]. 水利渔业, 2008,28(2):19-21.
|
| [4] |
Han Z X, Wang B Q . The study of adsorption kinetics to organotin on modified bentonite[J]. Reservoir Fisheries, 2008,28(2):19-21.
|
| [5] |
Elsheimer H N, Fries T L . Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry[J]. Analytica Chimica Acta, 1990,239:145-149.
|
| [6] |
Leao D J, Junior M M S, Brandao G C , et al. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry[J]. Talanta, 2016,153:45-50.
|
| [7] |
Gurkan R, Altunay N . Determination of total Sn in some canned beverages by FAAS after separation and preconcentration[J]. Food Chemistry, 2015,177:102-110.
|
| [8] |
Huang X R, Zhang W J, Han S H , et al. Determination of tin in canned foods by UV/visible spectrophotometric technique using mixed surfactants[J]. Talanta, 1997,44:817-822.
|
| [9] |
Jiang X J, Gan W E, Wan L Z , et al. Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode[J]. Journal of Hazardous Materials, 2010,184:331-336.
|
| [10] |
Campbell W C, Ottaway J M . Atom-formation processes in carbon-furnace atomizers used in atomic-absorption spectrometry[J]. Talanta, 1974,21(8):837-844.
|
| [11] |
Welsch E R, Chao T T . Determination of trace amounts of tin in geological materials by atomic absorption spectrometry[J]. Analytica Chimica Acta, 1976,82(2):337-342.
|
| [12] |
黄建兵, 吴少尉, 马艳芳 , 等. 富氧空气—乙炔火焰原子吸收光谱法测定地质样品中的微量锡[J]. 分析实验室, 2003,22(3):23-25.
|
| [12] |
Huang J B, Wu S W, Ma Y F , et al. Determination of trace tin in geological samples with oxygen enriched air-acetylene flame in atomic absorption spectrometry[J]. Chinese Journal of Analysis Laboratory, 2003,22(3):23-25.
|
| [13] |
罗宗铭, 陈凯瑞, 杨雪娇 . 锡(Ⅳ)—磺基水杨酸—溴邻苯三酚红—溴化十六烷基三甲基铵胶束混配络合物的显色反应[J]. 光谱实验室, 2001,18(2):155-158.
|
| [13] |
Luo Z M, Chen K R, Yang X J . The colour reaction of micellar mixed ligand complex of tin(Ⅳ)-sulfosalicylic acid-bromopyrogallol red-cetyltrimethylammonium bromide[J]. Chinese Journal of Spectroscopy Laboratory, 2001,18(2):155-158.
|
| [14] |
Farias S, Rodriguez R E, Ledesma A , et al. Assessment of acid media effects on the determination of tin by hydride generation-inductively coupled plasma atomic emission spectrometry[J]. Microchemical Jurmal, 2002,73:79.
|
| [15] |
张雪梅, 张勤 . 发射光谱法测定勘查地球化学样品中银硼锡钼铅[J]. 岩矿测试, 2006,25(4):323-326.
|
| [15] |
Zhang X M, Zhang Q . Determination of silver, boron, tin, molybdenum and lead in geochemical exploration samples by emission spectrometry[J]. Rock and Mineral Analysis, 2006,25(4):323-326.
|
| [16] |
王起超, 汪淑哲 . 巯基葡聚糖凝胶的制备及其对微量重金属离子吸附性能的研究[J]. 化学试剂, 1985,7(3):166-168.
|
| [16] |
Wang Q C, Wang S Z . A study on the preparation of sulfhydryl dextran gel and its adsorbability for heavy metallic ions[J]. Chemical Reagents, 1985,7(3):166-168.
|
| [17] |
王起超, 汪淑哲 . 巯基葡聚糖凝胶的制备及其在分析化学中的应用[J]. 分析化学, 1986,14(8):584-587.
|
| [17] |
Wang Q C, Wang S Z . Preparation of sulfhydryl dextran and its application in analytical chemistry[J]. Chinese Journal of Analytical Chemistry, 1986,14(8):584-587.
|
| [18] |
李慧芝, 张颖 . 巯基葡聚糖凝胶对钯、金、铟、锗离子吸附性能的研究[J]. 分析化学学报, 2005,21(3):337-338.
|
| [18] |
Li H Z, Zhang Y . The study on the adsorption of metal ions of Pd(Ⅱ), Au(Ⅲ), In(Ⅲ) and Ge(Ⅳ) on the sulfhydryl dextran gel[J]. Analytica Chimica Acta, 2005,21(3):337-338.
|
|
|
|
