X射线荧光光谱法测定高纯石墨中杂质元素

高纯石墨的传统湿法化学测定,需要高温灰化处理样品,程序相对繁琐.试验通过高纯石墨和金属离子溶液配制出有含量梯度的系列高纯石墨定值标样,并经电感耦合等离子体原子发射光谱法(ICP-AES)定值,解决了高纯石墨标准样品缺失的问题.试验对比了不同炭素基体试剂的形貌,确定使用高纯石墨作标准样品的基体试剂,利用ICP-AES方法...

Determination of impurity elements in high purity graphite by X-ray fluorescence spectrometry

During the chemical determination of high purity graphite by traditional wet method, the sample should be treated by high temperature ashing and the procedures are relatively complicated. A series of standard samples for quantification of high purity graphite with content gradient were prepared using high purity graphite and metal ions solution. Then, they were quantified by inductively coupled plasma atomic emission spectrometry (ICP-AES), which solved the problem in lack of high purity graphite standard samples. The morphology of reagents with different carbon matrixes was compared. The high purity graphite was used as the matrix reagent of standard samples. The impurity elements in various binders were determined by ICP-AES. The stearic acid (guarantee reagent) was selected as the binder. The grinding time in experiments was 40 s. The sample was prepared by grinding-pellet method. The contents of vanadium, sodium, calcium, iron, nickel, titanium, aluminum, phosphorus, zinc, manganese,and potassium in high purity graphite materials were determined by X-ray fluorescence spectrometry (XRF). The sample was prepared using 9 g of graphite and 1.5 g of stearic acid as the binder. The precision of sample preparation method was good, and the linearity of working curve was good without correction under above conditions. The trueness of high purity graphite sample was investigated. The determination results were consistent with the theoretical values or those obtained by ICP-AES.