采用氧弹燃烧-离子色谱法测定煤中硫及氯含量的研究
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摘要
简要介绍应用氧弹燃烧-离子色谱法测定煤中全硫和氯含量时所采用的仪器与试剂、煤样预处理方法,通过对氧弹燃烧和离子色谱的实验条件进行优化以确定最佳的试验条件。煤中硫、氯燃烧后其气体被氧弹中的碱性溶液所吸收,过滤后整合定容,采用离子色谱外标法测定溶液中Cl~-、SO_4~(2-)的浓度,最后计算出煤中硫、氯含量。结合对样品及氧弹内吸收液的选择、洗涤方式及气体过滤方式对含量测定的影响探讨,通过试验比对可知:以氧弹燃烧法处理样品,用Na_2CO_3-NaHCO_3-H_2O_2混合溶液10mL或用蒸馏水10mL做吸收液对发热量测定影响不大,均满足GB/T 213要求的重复性限。因此可在进行煤炭发热量测定的同时,采用1.8mmol/L Na_2CO_3与1.7mmol/L NaHCO3混合液为离子色谱淋洗液,实现煤中全硫和氯含量的离子色谱法快速测定,即采用离子色谱法同时测定煤中硫及氯含量具有较好的准确性和重复性。
The equipment,reagents and pre-treatment method of coal sample in determination of total sulfur and chlorine in coal by oxygen bomb combustion-ion chromatography method were briefly introduced,through optimizing the experimental conditions of oxygen bomb combustion and ion chromatography,the best experimental condition could be determined.After combustion,the gas of sulfur and chlorine was absorbed by alkaline solution in oxygen bomb,after filtration,the integration and volume determination were done,ion chromatography external calibration method was used to determine the concentration of Cl-,SO24-in solution,finally,the sulfur and chlorine contents in coal were calculated.How the selection of samples and absorbing liquid in oxygen bomb,washing way and gas filtration mode affected the content determination was discussed,through experimental comparison we can see that:the oxygen bomb combustion was used to treat the sample,if 10 ml ofNa2 CO3-NaHCO3-H2 O mixture or 10 ml distilled water were used as the absorbing liquid,the calorific value determination would not be affected obviously,the repeatability limit of GB/T 213 could be required.Therefore,while the coal calorific value determination was carried out,mixture of 1.8 mmol/L Na2 CO3 and 1.7 mmol/L NaHCO3 could be used as the ion chromatography eluent,so that the rapid determination of total sulfur and chlorine content in coal by ion chromatography could be realized,which meant that using the ion chromatography to determine the sulfur and chlorine in coal at the same time had good accuracy and repeatability.
The equipment,reagents and pre-treatment method of coal sample in determination of total sulfur and chlorine in coal by oxygen bomb combustion-ion chromatography method were briefly introduced,through optimizing the experimental conditions of oxygen bomb combustion and ion chromatography,the best experimental condition could be determined.After combustion,the gas of sulfur and chlorine was absorbed by alkaline solution in oxygen bomb,after filtration,the integration and volume determination were done,ion chromatography external calibration method was used to determine the concentration of Cl-,SO24-in solution,finally,the sulfur and chlorine contents in coal were calculated.How the selection of samples and absorbing liquid in oxygen bomb,washing way and gas filtration mode affected the content determination was discussed,through experimental comparison we can see that:the oxygen bomb combustion was used to treat the sample,if 10 ml ofNa2 CO3-NaHCO3-H2 O mixture or 10 ml distilled water were used as the absorbing liquid,the calorific value determination would not be affected obviously,the repeatability limit of GB/T 213 could be required.Therefore,while the coal calorific value determination was carried out,mixture of 1.8 mmol/L Na2 CO3 and 1.7 mmol/L NaHCO3 could be used as the ion chromatography eluent,so that the rapid determination of total sulfur and chlorine content in coal by ion chromatography could be realized,which meant that using the ion chromatography to determine the sulfur and chlorine in coal at the same time had good accuracy and repeatability.
引文
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[9]王昌钊,吴双民,张遴.氧弹燃烧-原子荧光光谱法测定煤中汞含量[J].化学分析计量,2017,26(2):70-72.
[10]娄丽,郭雨时,郝陶光.离子色谱法同时测定煤炭中氟及氯含量[J].煤炭与化工,2017,40(4):80-84.
[11]冯媛媛,徐志斌.对离子色谱法测定煤炭中氟和氯量中样品处理方法的比较[J].理化检验(化学分册),2017,53(5):598-602.
[12]苏征,叶佳宇,宋卫得,等.微波激发氧弹燃烧-离子色谱法检测煤炭中氟和氯[J].冶金分析,2017,37(7):45-50.
[2]全国煤炭标准化技术委员会.煤中全硫的测定方法:GB/T 214-2007[S].北京:中国标准出版社,2008:06.
[3]全国煤炭标准化技术委员会.煤中氯的测定方法:GB/T 3558-2014[S].北京:中国标准出版社,2014:10.
[4]孙贤祥.煤中硫化物硫的间接火焰原子吸收法测定[J].光谱学与光谱分析,1998,18(6):707-710.
[5]薛程.艾士卡-离子色谱法测定煤中全硫[J].洁净煤技术,2015,21(3):11-17.
[6]李东,孙家义.氧弹分解-高效液相色谱法测定煤中氯[J].分析实验室,2001,20(5):76-77.
[7]刘东艳,张园力.等离子发射光谱法测定煤中总硫的方法研究[J].光谱学与光谱分析,2002,22(1):89-91.
[8]宋义,郭芬,谷松海.X射线荧光光谱法同时测定煤中砷硫磷氯[J].岩矿测试,2006,25(3):285-287.
[9]王昌钊,吴双民,张遴.氧弹燃烧-原子荧光光谱法测定煤中汞含量[J].化学分析计量,2017,26(2):70-72.
[10]娄丽,郭雨时,郝陶光.离子色谱法同时测定煤炭中氟及氯含量[J].煤炭与化工,2017,40(4):80-84.
[11]冯媛媛,徐志斌.对离子色谱法测定煤炭中氟和氯量中样品处理方法的比较[J].理化检验(化学分册),2017,53(5):598-602.
[12]苏征,叶佳宇,宋卫得,等.微波激发氧弹燃烧-离子色谱法检测煤炭中氟和氯[J].冶金分析,2017,37(7):45-50.