摘要
为了对饱和溶解法测定天然气中元素硫溶解度的精密度开展系统研究,组织国内12家实验室分别对同一批次的20个样品进行了重复测试,按照国际标准ISO 4259-1《石油及相关产品测量方法与结果精密度第1部分:试验方法精密度数据的确定》进行了元素硫溶解度的精密度体系研究。该体系首先综合使用GESD方法预筛选、Cochran与Hawkins方法检验、库克距离分析数据异常值;然后运用统计学模型和自动化数据处理方法进行重复性和再现性评估;最后采用精细化分段浓度区间研究精密度的浓度依赖性特征。研究结果表明:①所有的实验数据均能够通过异常值检验;②重复性自由度和再现性自由度均满足统计分析要求;③在重复性/再现性条件下,在95%的置信区间里,所获得的两次独立测试结果的差值都没有超过相应浓度范围内的重复性限/再现性限。结论认为,所建立的元素硫溶解度精密度研究体系能够准确评价测试数据的一致性和可靠性;重复性限和再现性限的确定为ISO国际标准《饱和溶解法测定元素硫溶解度》的制订和现行行业标准的修订完善提供了技术支撑。
To systematically investigate the precision of elemental sulfur solubility measurement in natural gas by saturated dissolution method,20 samples from the same batch underwent repeated testing across 12 domestic laboratories.A precision systematic analysis for elemental sulfur solubility was conducted in accordance with the ISO 4259-1 Precision of measurement methods and results—Part 1:Determination of precision data in relation to methods of test.Firstly,GESD method,Cochran and Hawkins method,and Cook distance were utilized for pre-screening,testing,and analyzing data outlier,respectively.Then,statistical models and automated data processing approaches were used for repeatability and reproducibility evaluations.Finally,the concentration-dependent precision characteristics were clarified through refined segmented concentration intervals.Results indicated that(1)all experimental data can pass the outlier test;(2)degrees of freedom of both repeatability and reproducibility meet the requirements of statistical analysis;and(3)under repeatability/reproducibility conditions,within a 95%confidence interval,the difference between two independent results obtained does not exceed the repeatability/reproducibility limit within the corresponding concentration range.The established precision analysis system can accurately evaluate the consistency and reliability of test data.The determination of repeatability and reproducibility limits provides critical technical support for developing the ISO standard Determination of elemental sulfur solubility by saturated dissolution method as well as the revision and improvement of current industry standards.
作者
赵丹
王丽
万莹
尹庆
杨艳
唐志娟
ZHAO Dan;WANG Li;WAN Ying;YIN Qing;YANG Yan;TANG Zhijuan(Exploration and Development Research Institute,PetroChina Southwest Oil&Gasfield Company,Chengdu,Sichuan 610041,China;School of Artificial Intelligence,Chengdu University of Information Technology,Chengdu,Sichuan 610225,China)
出处
《天然气勘探与开发》
2025年第4期107-115,共9页
Natural Gas Exploration and Development
基金
中国石油西南油气田公司科研项目“天然气饱和溶解法测定元素硫溶解度等三项国际标准研究”(编号:2024D110-02-01)。
关键词
天然气
元素硫溶解度
饱和溶解法
精密度研究体系
异常值检验
重复性
再现性
ISO标准
Natural gas
Elemental sulfur solubility
Saturated dissolution method
Precision analysis
Outlier test
Repeatability
Reproducibility
ISO standard
