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气量法与差减法测定岩石中碳酸盐含量的对比研究

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为探讨气量法与差减法对于岩石中碳酸盐含量(以碳酸钙计)测定的差异性,从实验条件、方法检出限、准确度、精密度和显著性检验方面进行对比分析.结果表明:气量法对于测试环境的温度-压力要求较为严格,环境温度每变化1℃,样品中碳酸盐含量的测定结果会有0.34%的差异;大气压力每变化100 Pa,碳酸盐含量的测定结果会有0.10%的差异,所以气量法需要在温度-压力恒定的条件下进行.而温度-压力的变化对差减法的测定结果基本无影响.气量法的检出限为0.02%低于差减法的检出限0.04%,2种方法分别平行测定碳酸盐含量低、中、高的岩石样品6次,重复测定的相对标准偏差RSD均小于5%,两种方法的精密度良好.对不同类型的岩石成分分析标准物质进行测量,气量法与差减法测定碳酸盐含量的结果均落在参考值的不确定度范围之内,表明2种方法的准确度满足要求.采用t检验进行不同方法的显著性检验分析,2种方法计算出的t值均小于t检验临界值2.228,表明在置信度为95%的条件下,气量法与差减法对于岩石中碳酸盐含量的测量结果不存在显著性差异.气量法对于岩石样品的称样量较大,为0.5~10 g,远高于差减法的称样量0.2 g.为此,提出2种测定方法均可准确精密地测定岩石中的碳酸盐含量,在实际的检测工作中,少量零散的样品优先选择气量法进行测量,大批量样品检测选择差减法更有优势.
Comparative study on the determination of carbonate content in rocks between gasometric method and subtraction method
A comparative study was conducted in the aspects of experimental condition method detection limit,accuracy,precision,significant test to determine the difference between gasometric method and subtraction method in the carbonate content analysis for rock samples.The results showed that the gasometric method has strict requirements for the environment temperature and atmospheric pressure.For every 1℃change in environmental temperature,there will be a 0.34%difference in the determination results of carbonate content;for every 100 Pa change in atmospheric pressure,there will be a 0.10%difference in the measurement results of carbonate content.Therefore,the gasometric method should be carried out under a constant temperature and pressure condition.In contrast,changes in temperature and pressure have almost no effect on the measured results of subtraction method.the detection limit of gasometric method was 0.02%,which was less than the detection limit of subtraction method 0.04%.The repeatability testing,which measured rock samples with low,medium and high carbonate content for 6 times respectively,was conducted between these two methods to determine the relative standard deviation(RSD)of the samples,which was less than 5%.The precision results of both methods were good.Different kinds of rock certified reference material were tested to check accuracy and the results were all with the range of uncertainty for both methods,indicating that the accuracy of both methods met the requirements.According to significant test analysis,the t-values calculated by both methods were less than 2.228 in the light of the t-test critical table,suggesting that there was no significant difference in the measurement results of carbonates content in rocks between the gasometric method and the subtraction method under a confidence level of 95%.The gasometric method requires a large amount of 0.5~10 g rock samples,which is much higher than the subtraction method,which requires 0.2 g.Gasometric method and subtraction method both can accurately and precisely determine carbonate in rock samples.In actual testing work,gasometric method is preferred for measuring samples with small quantities,and subtraction method has advantages in the efficiency of analyzing large batches of samples.

gasometric methodsubtraction methodcarbonate contentcomparative study

李博文、刘高辉、袁健、孙进

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核工业北京地质研究院,北京 100029

气量法 差减法 碳酸盐 方法对比

2024

世界核地质科学
核工业北京地质研究院

世界核地质科学

CSTPCD
影响因子:0.463
ISSN:1672-0636
年,卷(期):2024.41(1)
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