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作 者:张嘉俊 李波平 陈远鸿 陈少敏 黄伟强 曾广丰 梁浩新 ZHANG Jia-Jun;LI Bo-Ping;CHEN Yuan-Hong;CHEN Shao-Min;HUANG Wei-Qiang;ZENG Guang-Feng;LIANG Hao-Xin(Guangzhou Customs Technology Center,Guangzhou 510623)
机构地区:[1]广州海关技术中心,广州510623
出 处:《中国口岸科学技术》2021年第9期59-63,共5页China Port Science and Technology
摘 要:为了寻找可以替代实验用水可溶性硅检测的铂金皿的蒸发容器,通过国标硅钼蓝法对玻璃烧杯、不锈钢皿、聚四氟乙烯皿进行初步筛选。分别对一级水和二级水进行检测,结果显示:通过玻璃烧杯、不锈钢皿蒸发后的水样可溶性硅含量均高于0.01 mg/mL标准溶液,而且比通过铂金皿蒸发后的水样可溶性硅含量高;而通过聚四氟乙烯皿蒸发后的水样可溶性硅含量低于0.01 mg/mL标准溶液,且与通过铂金皿蒸发后的水样可溶性硅含量一致,表明聚四氟乙烯皿效果与铂金皿效果一致。进一步通过电感耦合等离子体发射光谱法确定分别使用聚四氟乙烯皿、铂金皿蒸发样品检测结果的差异性,以及使用聚四氟乙烯皿检测的回收率,计算得出统计量|t|=1.17<2.23=t_(0.05(10)),故不拒绝假设,即认为两种方法测定结果无显著性差异。化合物在0.04~1.0 mg/L范围内呈良好线性关系,相关系数R^(2)为0.995,在0.005 mg/L、0.015 mg/L、0.020mg/L 3个添加水平下,平均回收率为92.0%~103.3%,相对标准偏差为2.69%~3.52%。通过上述实验验证,使用聚四氟乙烯皿可以替代铂金皿蒸发实验用水不影响实验结果,从而大大降低检测成本。In order to find an evaporating vessel that can replace the platinum dish in the determination of soluble silicon in laboratory water,the glass beaker,stainless steel dish and polytetrafluoroethylene dish were studied by the National Standard silicon-molybdenum blue method,using laboratory water of both the first and the second grade.The results showed that the soluble silicon contents of the water samples evaporated by the glass beaker and the stainless steel plate were both higher than the 0.01 mg/mL silicon standard,which were also higher than that of the water sample evaporated by the platinum plate;however,the content of soluble silicon in the water sample evaporated by the polytetrafluoroethylene dish was lower than 0.01 mg/mL silicon standard,consistent with that of the water sample evaporated by the platinum dish,it showed that the effect of polytertrafluoroethylene dish was consistent with that of platinum dish.Furthermore,the difference of sample evaporation results between the polytetrafluoroethylene dish and the platinum plate was determined by ICP-AES,and the recovery rate of polytetrafluoroethylene dish samples was tested.Calculated by statistics of|t|=1.17<2.23=t_(0.05(10)),so the assume was acceptable.It showed that there was no significant difference between the two methods.The calibration curves of compounds showed good linearity in concentration range of 0.04-1.0 mg/L(R^(2)=0.995).The average recovery was between 92.0%-103.3%at three spiked levels(0.005 mg/L、0.015 mg/L、0.020 mg/L),while the relative standard deviations(RSD)was between 2.69%-3.52%.Through the above experimental verification,the platinum dish could be replaced by polytetrafluoroethylene dish in the evaporation experiment without affecting the experimental results,and thereby greatly reducing the detection cost.
关 键 词:可溶性硅 铂金皿 聚四氟乙烯皿 硅钼蓝法 电感耦合等离子体发射光谱法
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