燃烧炉-离子色谱联用法测定氧化锌富集物中卤素
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摘要
建立了燃烧炉-离子色谱联用法测定氧化锌富集物中卤素含量的方法。样品在燃烧炉内加热、燃烧、分解,逸出含卤气体被吸收液吸收后进入离子色谱进行定量分析。实验对进样方式、称样量、燃烧温度、保持时间进行了讨论和优化。结果表明:在2～10 mg称样量、1050℃燃烧、保持200 s条件下,不使用助熔剂即可实现样品的充分燃烧分解。分析采用A5-150分离柱,淋洗液为1.0 mM NaHCO3+3.2 mM Na_2CO_3,流速为0.7 mL/min,30℃条件下进行分离。氟、氯、溴的方法检出限分别为45.25μg/kg、21.55μg/kg、61.53μg/kg,精密度RSD(11)≤9.6%,实际样品测定结果与现有方法吻合,可氟、氯、溴同步测定,满足进口氧化锌富集物的快速检验需求。
In this work, a method for the determination of halogen content in zinc oxide rich compounds by combustion furnace ion chromatography was established. The sample is heated, burned, and decomposed in the combustion furnace. The halogen gas is escaped and absorbed by the absorbent and pumped into the ion chromatography for quantitative analysis. The experiment discusses and optimizes the sampling method, sample quantity, combustion temperature and holding time. The results show that the sample can be fully burned and decomposed without flux under the conditions of 2 mg ～ 10 mg sample, 1050 ℃ combustion and 200 s maintenance. The analysis used A5-150 separation column, eluent 1.0 mM NaHCO3 + 3.2 mM Na2 CO3, flow rate 0.7 mL/min, 30 ℃ conditions for separation. The detection limits of fluorine, chlorine, and bromine were 45.25 μg/kg, 21.55 μg/kg, 61.53 μg/kg, and the precision RSD(11) ≤ 9.6 %. The actual sample determination results were consistent with the existing methods. Fluorine, chlorine and bromine can be measured synchronously to meet the needs of rapid inspection of imported zinc oxide concentrate products.
In this work, a method for the determination of halogen content in zinc oxide rich compounds by combustion furnace ion chromatography was established. The sample is heated, burned, and decomposed in the combustion furnace. The halogen gas is escaped and absorbed by the absorbent and pumped into the ion chromatography for quantitative analysis. The experiment discusses and optimizes the sampling method, sample quantity, combustion temperature and holding time. The results show that the sample can be fully burned and decomposed without flux under the conditions of 2 mg ～ 10 mg sample, 1050 ℃ combustion and 200 s maintenance. The analysis used A5-150 separation column, eluent 1.0 mM NaHCO3 + 3.2 mM Na2 CO3, flow rate 0.7 mL/min, 30 ℃ conditions for separation. The detection limits of fluorine, chlorine, and bromine were 45.25 μg/kg, 21.55 μg/kg, 61.53 μg/kg, and the precision RSD(11) ≤ 9.6 %. The actual sample determination results were consistent with the existing methods. Fluorine, chlorine and bromine can be measured synchronously to meet the needs of rapid inspection of imported zinc oxide concentrate products.
引文
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[3]冯均利,于泓锦,唐蒙奇,等.进口含锌物料的表征和鉴别[J].化工环保,2018,38(06):738-743.
[4]冯均利,于泓锦,刘冬,等.ICP-AES测定粗制氧化锌中Pb、Cd、Cr和As的含量[J].福建分析测试,2018,(06):6-9.
[5]吴景武,于泓锦,冯均利,等.粗制氧化锌的X射线衍射全谱图拟合定量相分析探讨[J].冶金分析,2018,38(9):14-19.
[6]黄沁怡,衷明华.氧弹燃烧-离子色谱法测定假连翘中氟、氯、氮、硫的含量[J].广东化工,2017,44(13):14-19.
[7]李婷,任丽萍,闵红,等.燃烧炉-离子色谱联用法测定铁矿石中氯[J].冶金分析,2018,38(7):51-56.
[8]王碗,刘肖,蔡亚岐,等.自动快速燃烧炉-离子色谱联用技术检测水泥等建材中的氯[J].分析试验室,2007,26(12):10-13.
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