煤中氟测定方法解析及改进
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摘要
介绍氟离子选择电极法检测煤中氟离子的原理及其方法,就国标中ΔE的范围部分进行论证实验并提出改进方案,即采用国标GB/T 4633—2014的标准加入法测试煤中氟含量,固定斜率下加入250μg/mL氟化钠标准溶液进行15次重复测定或加入100μg/mL氟化钠标准溶液进行30次重复测定,动态斜率下加入500μg/mL氟化钠标准溶液进行30次重复测定,并对实验数据进行统计分析,分别计算干基氟含量(Fd)的算术平均值和相对标准偏差。由统计分析可知,ΔE的范围对Fd测定值的精密度和准确度无必要的相关性,在实验过程中严格控制试验条件即可保证测定结果的准确性。
This paper introduced the principles and method of using fluoride ion selective electrode method to determine the fluorine in coal,the range ofΔE was demonstrated by experiment,and the improving plan was proposed,that was to say,the standard addition method in GB/T 4633—2014 to determine the fluorine in coal was adopted,under the fixed slope,250μg/mL sodium fluoride standard solution was added to proceed 15 times of repeated tests,or 100μg/mL sodium fluoride standard solution was added to proceed 30 times of repeated tests,under dynamic slope,500μg/mL sodium fluoride standard solution was added to proceed 30 times of repeated tests,the experimental data was analyzed,the arithmetic mean and relative standard deviation of dry fluorine content(Fd)were calculated respectively.From statistical analysis we can see that,range ofΔEhas no necessary relation with precision and accuracy of Fd,in the experimental process,strict control of experimental conditions could ensure the accuracy of testing results.
This paper introduced the principles and method of using fluoride ion selective electrode method to determine the fluorine in coal,the range ofΔE was demonstrated by experiment,and the improving plan was proposed,that was to say,the standard addition method in GB/T 4633—2014 to determine the fluorine in coal was adopted,under the fixed slope,250μg/mL sodium fluoride standard solution was added to proceed 15 times of repeated tests,or 100μg/mL sodium fluoride standard solution was added to proceed 30 times of repeated tests,under dynamic slope,500μg/mL sodium fluoride standard solution was added to proceed 30 times of repeated tests,the experimental data was analyzed,the arithmetic mean and relative standard deviation of dry fluorine content(Fd)were calculated respectively.From statistical analysis we can see that,range ofΔEhas no necessary relation with precision and accuracy of Fd,in the experimental process,strict control of experimental conditions could ensure the accuracy of testing results.
引文
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[12]李映日,邓双,王红梅,等.高温燃烧水解-淋洗液在线发生离子色谱法同时测定煤中氟和氯[J].环境工程,2011,29(5):130-134.
[13]全国煤炭标准化技术委员会.煤中氟的测定方法:GB/T 4633-2014[S].北京:中国标准出版社,2014:10.
[2]郭丽.离子色谱法测定饮用水中氟化物的含量[J].科技创新与生产力,2013(1):105-107.
[3]刘丽娜.浅谈影响煤中氟测定的几个因素[J].内蒙古煤炭经济,2016(21):109-110.
[4]李晓洪,官学贵.煤中氟含量测定可替代方法研究[J].西北煤炭,2007,5(3):38-39.
[5]张珍,魏宁,李侃社,等.离子选择性电极法测定煤中氟含量的影响因素分析[J].煤质技术,2014(5):16-20.
[6]郭沛,赵秀宏,王明星,等.高温燃烧水解-T70自动电位滴定仪测定煤中氟[J].煤质技术,2017(1):42-46.
[7]乔柱,姜郁,王恒,等.高温燃烧水解-离子色谱法同时测定煤中氟和氯[J].煤质技术,2015(1):6-9.
[8]马爱花.浅析煤中氟的测定[J].西部探矿工程,2015(8):143-144.
[9]周晓平.浅议基于电位分析法的煤中氟氯含量测定算法[J].中国仪器仪表,2008(10):81-83.
[10]齐庆杰,刘建忠,周俊虎,等.煤中微量元素氟测定方法的研究进展[J].煤炭转化,2000,23(2):7-11.
[11]齐庆杰,刘剑,刘建忠,等.煤中氟高温燃烧水解法测定影响因素实验研究[J].辽宁工程技术大学学报,2002,21(4):401-404.
[12]李映日,邓双,王红梅,等.高温燃烧水解-淋洗液在线发生离子色谱法同时测定煤中氟和氯[J].环境工程,2011,29(5):130-134.
[13]全国煤炭标准化技术委员会.煤中氟的测定方法:GB/T 4633-2014[S].北京:中国标准出版社,2014:10.