摘要
选取7种不同的植物类样品,按GB/T 28730-2012所述方法制备分析样品。经试验提出其最佳样品前处理及色谱分析条件:取样品0.500 0g,于镍坩埚中用(1.0±0.1)g氢氧化钾,先后在250℃和550℃熔融30min和30min。取出坩埚,冷却至室温。用水10mL浸取熔块,溶液定容至100 mL。用Metrosep A16-150色谱柱作为分离柱,淋洗液为7.5 mmol·L^(-1)碳酸钠-0.75mmol·L^(-1)氢氧化钠溶液,用抑制型电导检测器测定。氟的线性范围在0.02~1.0mg·L^(-1)内,检出限为7.6μg·L^(-1)。在实样的基础上用标准加入法进行回收试验,测得回收率在96.2%~103%之间,测定值的相对标准偏差(n=6)均小于5.0%。
Seven kinds of botanic substances were sampled as described in GB/T 28730-2012 and the optimized conditions for sample-pretreatment and IC analysis were found as follows： the sample （0. 500 0 g） was fused with （1.0±0. 1） g KOH in a nickel crucible at 250 ℃ and 550 ℃ for 30 min and 30 min in succession. The melt in the cooled crucible was taken up with 10 mL of water and then made up to 100 mL. Metrosep A16-150 column was used for IC-separation with mixed solution of 7.5 mmol·L^-1 Na2CO3 and 0. 75 mmol·L^-1 NaOH as mobil phase. Restrain conductance detector was used in the determinations. Linearity range for fluorine was found between 0. 02 and 1.0 mg ·L^-1 , with detection limit of 7. 6μg·L^-1. On the base of substantial samples, test for recovery was made by standard addition method, giving values of recovery in the range of 96. 2% to 103% and values of RSD＇s （n=6） found were all less than 5.0%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第5期581-584,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家能源局标准资助项目(20140707)
南方电网有限责任公司科技项目(K-GD2013-057)
