朱姝，吴斌，字雨姝

(核工业230研究所，长沙 410007)

统计方法在微量金分析中的应用

朱姝，吴斌，字雨姝

(核工业230研究所，长沙 410007)

化探金样品前处理过程中消解、富集、解吸等环节控制不严格，往往会导致最后数据处理产生过高的校正系数。为了降低校正系数，用统计学的方法对实验过程进行了详细分析，确定了主要影响因素。将水浴时间延长并保温3 h以上，泡塑大小改为0.2 g，清洗时间不大于15 s，解吸到上机时间间隔小于5 h。方法改进后，检测结果校正系数有了明显改善，从改进前有40%批次的校正系数大于1.2，降到了全部小于1.2，甚至不用校正。方法改进后降低了实验过程的误差，提高了分析测试结果的稳定性。

微量金；校正系数；统计方法

AbstractIn the process of pretreatment of geochemical gold， the control of the process of digestion，enrichment and desorption is not strict，which often leads to excessive correction coef ficient in the final data processing. In order to reduce the correction coef ficient，statistical methods was used to analyse and on firmed the main in fluencing factors in detail. The water bath time was set more than 3 h，foam mass was 0.2 g，cleaning time was not more than 15 s， the time intervals from desorption to detection was less than 5 h. After the method was improved, the correction coef ficient of detection results was improved signi ficantly. The correction coef ficient of the 40% batches before the improvement of the method was more than 1.2，which was reduced to less than 1.2，even without correction. The error of the experimental process was reduced and the stability of the test results was improved .

Keywordstrace Au; correction factor; statistical method

微量金的分析检测主要存在于地质行业，如地球化学普查或者区域地球化学调查中的水系沉积物、土壤、岩石样品等的分析，又称化探金，其金元素含量范围在 0.1×10-9～100×10-9之间，特点是样品数量多，并且要求出具的结果快速、准确。

电感耦合等离子体质谱法(ICP-MS)检测金具有灵敏度高、结果准确的特点，因此被广泛应用于地质样品中微量金的测定［1-2］。ICP-MS 法的关键操作在于样品前处理中金的消解和富集，由于批量样品现场测试的实验数据均含有误差(包括随机误差和过失误差)，累积起来就会使最终分析结果产生偏离，在进行数据处理时经常要对检测结果进行数据校正，又称数据调谐［3］。微量金分析步骤多，实验过程控制不严格往往会导致较大的校正系数。……