电感耦合等离子体发射光谱法测定铝土矿中镓——酸溶和碱熔预处理方法比较

文加波; 商丹; 宋婉虹; 彭国萍

电感耦合等离子体发射光谱法测定铝土矿中镓——酸溶和碱熔预处理方法比较

1.
贵州省地质矿产勘查开发局一○六地质大队, 贵州遵义 563000
2.
上海大学材料科学与工程学院, 上海 200072
3.
贵州省地质矿产勘查开发局一○六地质大队, 贵州遵义 563000
4.
贵州省地质矿产勘查开发局一○六地质大队, 贵州遵义 563000

基金项目:

贵州省地质勘查基金(周转金)矿产项目(TK2009-006)

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- 收稿日期: 2010-08-20
- 修回日期: 2010-12-19

Quantification of Gallium in Bauxites by Inductively Coupled Plasma-Atomic Emission Spectrometry-Comparison of Sample Pretreatment Methods between Alkali Fusion and Acid Dissolution

1.
106 Geological Party, Guizhou Bureau of Geology and Mineral Exploration & Development, Zunyi 563000, China
2.
School of Materials Science and Engineering, Shanghai University, Shanghai 200072, China
3.
106 Geological Party, Guizhou Bureau of Geology and Mineral Exploration & Development, Zunyi 563000, China
4.
106 Geological Party, Guizhou Bureau of Geology and Mineral Exploration & Development, Zunyi 563000, China

摘要

摘要: 研究了盐酸-硝酸-氢氟酸-高氯酸酸溶和氢氧化钠碱熔两种测定铝土矿石样品中镓的前处理方法,利用电感耦合等离子体发射光谱法(ICP-AES)进行测定。对熔矿试剂及条件、分析谱线的选择和元素的干扰进行了讨论,采用不同含量的铝土矿石国家标准物质样品进行了条件实验。分析结果表明:采用盐酸-硝酸-氢氟酸-高氯酸溶解样品,会导致铝土矿石样品溶解不完全,得到的数据失真;而采用氢氧化钠碱熔法处理铝土矿石样品后,用ICP-AES法测定,镓的测定值准确度高,方法检出限为0.15 μg/g,相对标准偏差(RSD,n=11)为2.51%~5.97%,回收率为94.8%~108.2%。该方法灵敏度高,精密度好,分析时间短,易于流程操作。方法经国家一级标准物质分析验证,测定结果与标准值相符,特别适用于铝土矿石样品中镓的测定。
- 关键词: /
- 镓 /
- 铝土矿 /
- 电感耦合等离子体发射光谱法 /
- 酸溶 /
- 氢氧化钠碱熔
Abstract: Two different sample pretreatment methods-NaOH alkali fusion method and HCl-HNO₃-HF-HClO₄ acid dissolution method were compared in order to quantify Ga in bauxite ore samples by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The loaded reagents, chemical procedure, selection of analysis spectral lines and interferences are discussed in this paper. National Standard Reference bauxite ore samples with different Ga contents were analyzed by using both sample pretreatment methods. The analytical results indicate that the bauxite ore samples were incompletely dissolved by using HCl-HNO₃-HF-HClO₄ acids, which provided an incorrect result. Meanwhile, the pretreatment for bauxite ore samples with sodium hydroxide by alkali fusion provided higher accuracy and precision, giving a range of 2.51%-5.97% (RSD, n=11) and a detection limit for Ga of 0.15 μg/g with recoveries of the method ranging from 94.8% to 108.2%. The reliability of the alkali fusion method has been tested by quantification of Ga in National Standard Reference materials and the results were in agreement with the certified values. This method has advantages of rapid analysis, simple operation and more efficient measurement of Ga in bauxite ore samples.
- gallium /
- bauxite /
- ore /
- inductively /
- coupled /
- plasma-atomic

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参考文献(25)

曾惠芳,戢朝玉,鲁锦英.感耦等离子体质谱法同时测定岩石中痕量元素的研究[J].岩矿测试,1995,14(3):173-178.

张军,汉春利,徐益谦,顾中铸.煤中次要元素的赋存方式[J].煤炭转化,1999,22(2):6-11.

殷宁万,阙松娇,戢朝玉,袁玄辉.化探样品的等离子体直读光谱分析[J].岩矿测试,1984,3(1):65-72.

王蕾,何红蓼,李冰.碱熔沉淀-等离子体质谱法测定样品中的多元素[J].岩矿测试,2003,22(2):86-92.

叶家瑜,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:225-230.

刘春晓,刘英,臧幕文.电感耦合等离子原子发射光谱法中悬浮液直接进样技术的研究与应用的进展[J].理化检验:化学分册,2007,35(2):164-167.

龚迎莉,汪双清,沈斌.电感耦合等离子体原子发射光谱法同时测定沉积岩中15个元素[J].岩矿测试,2007,26(3):230-232.

李国榕,王亚平,孙元方,董天姿,王海鹰.电感耦合等离子体质谱法测定地质样品中稀散镓铟碲铊[J].岩矿测试,2010,29(3):255-258.

韩江伟,熊小林,朱照宇,吴金花.等离子体质谱法测定玄武岩中微量元素三种预处理方法的比较[J].岩矿测试,2008,27(5):325-328.

周天泽,邹洪.原子光谱样品处理技术[M].北京:化学工业出版社,2006:21-38.

刘颖,刘海臣,李献华.用ICP-MS准确测定岩石样品中的40种微量元素[J].地球化学,1996,25(6):552-558.

何红蓼,李冰,韩丽萍,孙德忠,王淑贤,李松.封闭压力酸溶-ICP-MS法测定地质样品中47个元素的评价[J].分析试验室,2002,21(5):8-12.

倪文山,张萍,姚明星,孟亚兰,李贤珍.萃取富集-电感耦合等离子体原子发射光谱法测定矿石中镓[J].冶金分析,2010,30(4):14-17.

田晓娅,陈超子.应用ICP-AES法同时测定土壤中27种元素的方法研究[J].土壤通报,1993,24(4):188-190.

郭鹏.电感耦合等离子体质谱法测定高纯氧化钽中28种痕量杂质元素[J].分析试验室,2008,27(3):106-109.

解原,李承湘,朱为民.ICP-OES法同时测定含铟渣料中的多元素[J].湖南有色金属,2007,23(5):49-51.

刘华,李健,杜东平,谢灵芝.ICP-OES法测定煤中镓、钡、钍、磷[J] .煤质技术,2010,25(1):19-21.

何晋浙.ICP-AES法在元素分析测试中的应用技术[J].浙江工业大学学报,2006,34(1):539-541.

叶家瑜,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:29-45.

龚思维,楚民生,沈泽敏,蒋海宁.ICP-AES法测定铝中铁、硅、铜、镓、镁、锌、锰和钛[J].分析试验室,2004,23(1):40-42.

沈恒培.深海沉积物及多金属结核中微量元素的光谱测定[J].岩矿测试,1997,16(2):91-97.

韩美,胡净宇,陈玉红,王海舟.集合式屑状标准物质校正-激光烧蚀电感耦合等离子体质谱法分析镍基高温合金中痕量元素[J].冶金分析,2010,30(3):1-6.

吕振生,赵庆令,李清彩,葛童.电感耦合等离子体发射光谱法测定钨矿石中8种成分[J].冶金分析,2010,30(9):47-50.

侯广顺,张丽娜.ICP-AES法测定铜、铅、锌精粉中的七种伴生元素[J].冶金分析,2010,30(10):47-50.

袁玄辉,阙松娇,伍新宇,殷宁万.等离子体直读光谱法同时测定岩石中15个痕量稀土元素[J].岩矿测试,1983,2(2):127-129.

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电感耦合等离子体发射光谱法测定铝土矿中镓——酸溶和碱熔预处理方法比较

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Quantification of Gallium in Bauxites by Inductively Coupled Plasma-Atomic Emission Spectrometry-Comparison of Sample Pretreatment Methods between Alkali Fusion and Acid Dissolution

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