磁力搅拌-离子选择电极法测量铜精矿中的水溶性氟
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摘要
建立磁力搅拌–离子选择电极法测定铜精矿中的水溶性氟。采用磁力搅拌法对样品进行前处理,研究了浸取温度、浸取时间、测量温度等因素对氟测定的影响,经试验确定浸取温度为50℃,浸取时间为180 min,测量温度为20℃。氟在0.5～2.5μg/mL范围内其质量浓度的自然对数与电位值呈良好的线性关系,相关系数r2=0.999 8,方法检出限为0.03μg/mL,定量限为0.1μg/mL。铜精矿样品测定结果的相对标准偏差为4.26%(n=6),加标回收率为97.9%～105.0%。该方法重现性好,操作简单,可用于铜精矿中水溶性氟的准确定量分析。
A ion selective electrode method with magnetic stirring mode was established for the determination of water soluble fluorine in copper concentrates. The sample was pretreated with magnetic stirring device. The influencing factors such as leaching temperature,leaching time and measuring temperature on the determination of fluorine was studied. After the experiment,the experimental conditions were determined that the leaching temperature was 50℃,the leaching time was 180 min,and the measure temperature was 20℃. The natural logarithm of fluorine ion mass concentration was in good linearity with the potential value in the range of 0.5–2.5 g/mL,and the linear correlation coefficient(r2) was 0.999 8,the detection limit of fluorine was 0.03 μg/mL, and limit of quantification was 0.1 μg/mL. The relative standard deviation of copper concentrate sample determination results was 4.26%(n=6),and the average recovery of fluorine was 97.9%–105.0%. The method is accurate,reproducible and simple, it can be used for quantitative analysis of water soluble fluorine in copper concentrates.
A ion selective electrode method with magnetic stirring mode was established for the determination of water soluble fluorine in copper concentrates. The sample was pretreated with magnetic stirring device. The influencing factors such as leaching temperature,leaching time and measuring temperature on the determination of fluorine was studied. After the experiment,the experimental conditions were determined that the leaching temperature was 50℃,the leaching time was 180 min,and the measure temperature was 20℃. The natural logarithm of fluorine ion mass concentration was in good linearity with the potential value in the range of 0.5–2.5 g/mL,and the linear correlation coefficient(r2) was 0.999 8,the detection limit of fluorine was 0.03 μg/mL, and limit of quantification was 0.1 μg/mL. The relative standard deviation of copper concentrate sample determination results was 4.26%(n=6),and the average recovery of fluorine was 97.9%–105.0%. The method is accurate,reproducible and simple, it can be used for quantitative analysis of water soluble fluorine in copper concentrates.
引文
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[3]任晓敏,陈敏.牙齿正畸中应用氟保护漆预防牙釉质脱矿疗效观察[J].中国误诊学杂志,2009,9(27):6 615–6 616.
[4]质检总局2017年第106号公告环境保护部商务部关于公布进口铜精矿中有毒有害元素限量[R].
[5] GB/T 20424–2006重金属精矿产品中有害元素的限量范围[S].
[6]魏建军,赵明,卢伟霞,等.郑州市饮水型地方性氟中毒病区改水防制效果评价[J].河南预防医学杂志,2017,28(12):920–921.
[7]张江甲,王三祥,吴赵明,等.山西省饮水型地方性氟中毒监测结果分析[N].疾病预防控制通报,2015,30(1):48–52.
[8]董璐,陈伟,姚培杰,等.西安市氟中毒病区水氟含量与儿童氟斑牙和龋齿的关系[J].中国学校卫生,2018,39(1):101–103.
[9]王烁,李伯灵,谈伟军.饮水型地方性氟中毒健康危险度评价[J].职业与健康,2011,27(9):1 041–1 044.
[10]云中杰,陈培中,边建朝,等.山东省地方性氟中毒病区村水氟检测结果分析[J].中国地方病学杂志,2005,24(5):551–553.
[11] GB/T 3884.5–2012铜精矿化学分析方法氟量的测定[S].
[12]陈士清,施光明,李泉,等.磁力驱动搅拌器的发展和应用[J].化工机械2013.40(4):415–419.
[13]陈静,王烨,王敏捷.离子色谱法测定土壤中的有效氟[J].岩矿测试,2009(2):173–175.
[14]陈锦玲,曹东霞,邝柏杨.离子色谱法测定牙膏中可溶性氟含量[J].化学分析计量,2014,23(12):60–62.
[15]李中贤,赵灿方,刘小培,等.水中氟化物的氟试剂分光光度法测定[J].河南科学,2012,30(1):55–57.
[16]张玉明,石庆.氟试剂分光光度法测定氟化物的方法分析[J].水文,2002.22(6):50–53.
[17]周福林,宋少飞,张稳婵,等.离子选择性电极在氟离子测定中的应用[J].宜春学院学报(自然科学),2007,29(6):81–85.
[18]盛晓风,郭莹莹,尚德荣,等.离子选择电极法测定高氟样品中氟的方法改进[J].食品工业科技,2013(9):285–289.
[19]刘青,贺先进.电位法测定铜精矿中的氟[J].环境科学,2017(10):98–99.