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煤中氮元素分析仪改造及性能验证研究

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为实现使用热导系数与氮气相差较小的、价格更便宜的氩气替换氦气做载气以测定煤中氮元素含量,采取对CHN628元素分析仪进行改造并提升热导池测试灵敏度。改造后的仪器采用氩气做载气并对其设置相关参数,即在基线延迟时间10 s、最短分析时间120 s、比较水平1%、平衡时间30 s、装填压强150 mmHg和氩气流量320 mL/min条件下测定煤样中的氮含量,分析曲线光滑。选择能涵盖日常检测样品氮含量范围的有证煤标准物质标定曲线,曲线的相关系数(r)为0。998,符合线性关系要求;采用空白样品法测得的检出限、定量限分别为0。06%、0。15%,满足方法要求;统计日常工作中采用氩气或氦气做载气的2种方法以测定煤中氮元素含量,同时测定有证煤标准物质GBW 11107p,通过F检验和t检验表明用氩气做载气测定煤中氮元素含量则其期间精密度、短期精密度和准确度均满足国标GB/T 30733-2014要求,因此改造后的元素分析设备可用于测定煤中氮元素含量,且该方法采用的氩气市场供应稳定、价格低,能降低检测成本。
Study on the modification and performance verification of nitrogen element analyzer for coal
To replace helium with cheaper argon,which has a thermal conductivity coefficient close to that of nitro-gen,as the carrier gas for measuring nitrogen content in coal,modifications were made to the CHN628 elemental an-alyzer and its thermal conductivity cell sensitivity was enhanced.The modified instrument employed argon as the carri-er gas with optimized parameters,including a baseline delay time of 10 s,a minimum analysis time of 120 s,a com-parison level of 1%,an equilibrium time of 30 s,a filling pressure of 150 mmHg,and an argon flow rate of 320 mL/min.Under these conditions,the nitrogen content in coal samples was measured with a smooth analytical curve.A certified coal reference material with a nitrogen content range encompassing that of routine test samples was selected to calibrate the curve,yielding a correlation coefficient(r)of 0.998,meeting the requirement for linearity.The limit of detection and limit of quantification were determined to be 0.06%and 0.15%,respective-ly,using the blank sample method,satisfying the method's requirements.A statistical comparison was conducted be-tween the two methods of using argon or helium as the carrier gas to measure nitrogen content in coal,inclu-ding measurements of the certified coal reference material GBW 11107p.F-tests and t-tests indicated that using argon as the carrier gas to measure nitrogen content in coal met the precision and accuracy requirements of the national standard GB/T 30733-2014 for intermediate precision,short-term precision,and accuracy.Therefore,the modi-fied equipment can be used to determine nitrogen content in coal.Furthermore,the adoption of argon in this method,with its stable market supply and low price,can help reduce testing costs.

nitrogen in coalthermal conductivity cellprecisionaccuracylimit of detectioncalibration curveF-testt-test

王建、殷志源、孙天宇、竺浩玮、沈玉双、吴碧海、张晓丹、鲍莉彬

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浙江越华能源检测有限公司,浙江宁波 315211

煤中氮 热导池 精密度 准确度 检出限 标定曲线 F检验 t检验

浙江省能源集团有限公司科技资助项目

ZNKJ-2018-064

2024

煤质技术
煤炭科学研究总院

煤质技术

影响因子:0.393
ISSN:1007-7677
年,卷(期):2024.39(4)