氟化物固体缓冲剂-交流电弧直读发射光谱法测定化探样品中易挥发与难挥发微量元素
发布时间：2019-02-25 15:04
【摘要】：应用电弧直读发射光谱法测定化探样品,样品无需消解,采用固体进样的方式可以同时测定多个元素。但目前化探分析中常采用的固体缓冲剂(如焦硫酸钾、氟化钠)的电弧温度较低,只能分析银、硼、锡、铅、钼、铜等易挥发元素,而不能分析铬、锰、钛等沸点较高的难挥发性元素。本文通过碱金属控制较低的电弧温度,并利用难挥发元素能在高温条件下与氟离子发生化学反应降低其激发温度,配制了一种以氟化铝、聚三氟氯乙烯等氟化效率较高的化合物为主要成分的固体缓冲剂,通过优化分析线对的选择、曝光时间、电极形状等分析条件,实现了一次制样可同时分析地球化学样品中14种易挥发和难挥发元素。方法检出限为0.016~46.93μg/g,相对标准偏差为4.1%~12.3%,通过国家标准物质验证了准确度,测定值与标准值相符,各项参数都能满足地球化学普查规范要求。本方法分析效率高,在化探分析中具有一定的实用性。
[Abstract]:The method of direct reading emission spectroscopy is used to determine geochemical samples. The samples do not need to be digested, and many elements can be determined simultaneously by the way of solid-state injection. But at present, the arc temperature of solid buffer (such as potassium pyrosulfate, sodium fluoride), which is commonly used in geochemical analysis, is relatively low. It can only analyze the volatile elements such as silver, boron, tin, lead, molybdenum and copper, but not chromium and manganese. Titanium is a difficult volatile element with high boiling point. In this paper, a kind of aluminum fluoride was prepared by controlling the lower arc temperature by alkali metal and reducing the excitation temperature by chemical reaction of difficult volatile elements with fluorine ion at high temperature. The solid buffer with high fluorination efficiency such as poly (trifluorovinyl chloride) is the main component. By optimizing the selection of analytical line pairs, exposure time, electrode shape and other analytical conditions, the results are as follows: 1. It is realized that 14 volatile and non-volatile elements in geochemical samples can be simultaneously analyzed by one-time sample preparation. The detection limit is 0.016 ~ 46.93 渭 g 路g ~ (- 1) and the relative standard deviation (RSD) is 4.1% ~ 12.3%. The accuracy of the method is verified by the national standard material. The determination value is in accordance with the standard value, and all the parameters can meet the requirements of geochemical survey specification. This method has high analysis efficiency and has some practicability in geochemical exploration analysis.
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本文编号：2430295
[Abstract]:The method of direct reading emission spectroscopy is used to determine geochemical samples. The samples do not need to be digested, and many elements can be determined simultaneously by the way of solid-state injection. But at present, the arc temperature of solid buffer (such as potassium pyrosulfate, sodium fluoride), which is commonly used in geochemical analysis, is relatively low. It can only analyze the volatile elements such as silver, boron, tin, lead, molybdenum and copper, but not chromium and manganese. Titanium is a difficult volatile element with high boiling point. In this paper, a kind of aluminum fluoride was prepared by controlling the lower arc temperature by alkali metal and reducing the excitation temperature by chemical reaction of difficult volatile elements with fluorine ion at high temperature. The solid buffer with high fluorination efficiency such as poly (trifluorovinyl chloride) is the main component. By optimizing the selection of analytical line pairs, exposure time, electrode shape and other analytical conditions, the results are as follows: 1. It is realized that 14 volatile and non-volatile elements in geochemical samples can be simultaneously analyzed by one-time sample preparation. The detection limit is 0.016 ~ 46.93 渭 g 路g ~ (- 1) and the relative standard deviation (RSD) is 4.1% ~ 12.3%. The accuracy of the method is verified by the national standard material. The determination value is in accordance with the standard value, and all the parameters can meet the requirements of geochemical survey specification. This method has high analysis efficiency and has some practicability in geochemical exploration analysis.
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本文编号：2430295
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