不确定度评定在焦磷酸法测定工作场所粉尘游离二氧化硅中的应用
|
摘要
[目的]对焦磷酸法测定工作场所粉尘游离二氧化硅质量分数进行不确定度评定。[方法]依据《测量不确定度评定与表示》(JJF 1059.1-2012)对《工作场所空气中粉尘测定第4部分:游离二氧化硅含量》(GBZ/T 192.4-2007)中焦磷酸法测定带来的不确定度的来源进行识别和评定,并合成不确定度。[结果]该方法测定过程中产生不确定度分量的主要来源为重复性和温度方面。不经氢氟酸处理的重复性方面相对标准不确定度为8.89×10~(-2),经氢氟酸处理后的重复性方面相对标准不确定度为5.90×10~(-2);温度计检定的温度方面相对标准不确定度为0.26×10~(-2),马弗炉校准的温度方面相对标准不确定度为0.12×10~(-2)。不经氢氟酸处理的工作场所粉尘游离二氧化硅质量分数合成标准不确定度为1.35%,扩展标准不确定度为2.70%;经氢氟酸处理后的工作场所粉尘游离二氧化硅质量分数合成标准不确定度为0.57%,扩展标准不确定度为1.14%。工作场所粉尘游离二氧化硅质量分数标准不确定度结果:不经氢氟酸处理为(15.18±2.70)%,经氢氟酸处理后为(9.66±1.14)%。[结论]在保持所使用的称量仪器具有良好的精密性、操作性和重复性基础上,应加强操作培训,熟悉操作处理全过程,以减少操作重复性和温度方面产生的不确定度叠加。
[Objective] To evaluate the uncertainty in determining free silica in dust of workplace by pyrophosphoric acid method. [Methods] According to the Evaluation and Expression of Uncertainty in Measurement(JJF 1059.1-2012) and the Method for Determination of Dust in the Air of Workplace Part 4:Content of Free Silica in Dust(GBZ/T 192.4-2007),the uncertainty of pyrophosphoric acid method was sourced,evaluated and combined. [Results] The repeatability and temperature were the main sources of uncertainty components in the determination process. The relative standard uncertainty of repeatability without treatment by hydrofluoric acid was 8.89 × 10~(-2),and the relative standard uncertainty of repeatability after treatment by hydrofluoric acid was 5.90 × 10~(-2);the relative standard uncertainty of temperature by thermometer calibration was 0.26 × 10~(-2),and the relative standard uncertainty of temperature by muffle furnace calibration was 0.12 × 10~(-2). The combined standard uncertainty of free silica in dust at workplace without treatment by hydrofluoric acid was 1.35%,and the expanded standard uncertainty was 2.70%;the combined standard uncertainty of free silica in dust at workplace after treatment by hydrofluoric acid was 0.57%,and the expanded standard uncertainty was 1.14%. The results of the standard uncertainty of free silica in dust at workplace were(15.18 ± 2.70)% without treatment by hydrofluoric acid and(9.66 ± 1.14)% after treatment by hydrofluoric acid. [Conclusion] Except for maintaining the precision, operability and repeatability of all used weighing instrument,to strengthen the operation training and familiarity with the whole process of operation will reduce the uncertainty.
[Objective] To evaluate the uncertainty in determining free silica in dust of workplace by pyrophosphoric acid method. [Methods] According to the Evaluation and Expression of Uncertainty in Measurement(JJF 1059.1-2012) and the Method for Determination of Dust in the Air of Workplace Part 4:Content of Free Silica in Dust(GBZ/T 192.4-2007),the uncertainty of pyrophosphoric acid method was sourced,evaluated and combined. [Results] The repeatability and temperature were the main sources of uncertainty components in the determination process. The relative standard uncertainty of repeatability without treatment by hydrofluoric acid was 8.89 × 10~(-2),and the relative standard uncertainty of repeatability after treatment by hydrofluoric acid was 5.90 × 10~(-2);the relative standard uncertainty of temperature by thermometer calibration was 0.26 × 10~(-2),and the relative standard uncertainty of temperature by muffle furnace calibration was 0.12 × 10~(-2). The combined standard uncertainty of free silica in dust at workplace without treatment by hydrofluoric acid was 1.35%,and the expanded standard uncertainty was 2.70%;the combined standard uncertainty of free silica in dust at workplace after treatment by hydrofluoric acid was 0.57%,and the expanded standard uncertainty was 1.14%. The results of the standard uncertainty of free silica in dust at workplace were(15.18 ± 2.70)% without treatment by hydrofluoric acid and(9.66 ± 1.14)% after treatment by hydrofluoric acid. [Conclusion] Except for maintaining the precision, operability and repeatability of all used weighing instrument,to strengthen the operation training and familiarity with the whole process of operation will reduce the uncertainty.
引文
[1]中国国家认证认可监督管理委员会.国家认监委关于印发《检验检测机构资质认定评审准则》及释义和《检验检测机构资质认定评审员管理要求》的通知[R/OL].(2016-05-31)[2018-1-30].http://www.cnca.gov.cn/xxgk/gwxx/2016/201606/t20160602_51598.shtml.
[2]姚叶斌,许健健,赵中梅.测量不确定度估算在职业卫生检测中的应用[J].山东工业技术,2015(3):294-295.
[3]中华人民共和国卫生部.工作场所空气中粉尘测定第4部分:游离二氧化硅含量:GBZ/T 192.4-2007[S].北京:人民卫生出版社,2008.
[4]吴健,李小娟,朱宝立,等.焦磷酸法测定粉尘中游离二氧化硅的方法改进[J].中国卫生检验杂志,2015,25(11):1865-1866.
[5]陈晓君,高华,段志欢.磷酸法测定粉尘中游离二氧化硅方法探讨[J].海峡预防医学杂志,2014,20(6):47-48.
[6]崔凯,常继兵,沈凌.工作场所空气中矽尘游离二氧化硅焦磷酸法测定结果的不确定度评定[J].环境与职业医学,2016,33(4):394-397.
[7]全国法制计量管理计量技术委员会.测量不确定度评定与表示:JJF1059.1-2012[S].北京:中国质检出版社,2013.
[8]肖瑞芬.焦磷酸法测定粉尘中游离二氧化硅含量的分析[J].化学工程与装备,2016(5):245-246.
[9]吴文毅,江思顺,邬丽,等.焦磷酸法测定游离二氧化硅含量方法改进[J].微量元素与健康研究,2015,32(2):54-56.
[10]严月,朱晓俊,陈永青.焦磷酸法测定粉尘中游离二氧化硅含量的实验条件研究[J].中国工业医学杂志,2015,28(2):125-126,134.
[2]姚叶斌,许健健,赵中梅.测量不确定度估算在职业卫生检测中的应用[J].山东工业技术,2015(3):294-295.
[3]中华人民共和国卫生部.工作场所空气中粉尘测定第4部分:游离二氧化硅含量:GBZ/T 192.4-2007[S].北京:人民卫生出版社,2008.
[4]吴健,李小娟,朱宝立,等.焦磷酸法测定粉尘中游离二氧化硅的方法改进[J].中国卫生检验杂志,2015,25(11):1865-1866.
[5]陈晓君,高华,段志欢.磷酸法测定粉尘中游离二氧化硅方法探讨[J].海峡预防医学杂志,2014,20(6):47-48.
[6]崔凯,常继兵,沈凌.工作场所空气中矽尘游离二氧化硅焦磷酸法测定结果的不确定度评定[J].环境与职业医学,2016,33(4):394-397.
[7]全国法制计量管理计量技术委员会.测量不确定度评定与表示:JJF1059.1-2012[S].北京:中国质检出版社,2013.
[8]肖瑞芬.焦磷酸法测定粉尘中游离二氧化硅含量的分析[J].化学工程与装备,2016(5):245-246.
[9]吴文毅,江思顺,邬丽,等.焦磷酸法测定游离二氧化硅含量方法改进[J].微量元素与健康研究,2015,32(2):54-56.
[10]严月,朱晓俊,陈永青.焦磷酸法测定粉尘中游离二氧化硅含量的实验条件研究[J].中国工业医学杂志,2015,28(2):125-126,134.