摘要
溴主要以离子形式分布在地壳水圈的溴化物型卤水、卤化物硫酸盐型卤水中,目前应用波长色散X射线荧光光谱（WDXRF）测定卤水中的溴,主要采用粉末载体压片法前处理待检样品,制样工作量大,制样均匀性和制样过程中的污染都会影响准确度,方法实用性不强。本文借助薄膜吸附前处理卤水样品,通过优化筛选薄膜材料及卤水取样量,确定移取50μL卤水样品滴于Ф=40 mm的3#层析滤纸的圆心位置,自然晾干后高压压平来前处理待检样品,采用人工配制标准样品校正溴的标准曲线,用WDXRF测定溴的含量。钾钠钙镁氯和硫酸根等共存离子的影响可以忽略,方法检出限（3σ）为0.95 mg/L,精密度（RSD,n=11）不大于0.8%,加标回收率为99.4%~101.2%。本方法操作简便,不需要使用化学试剂,解决了现行卤水中溴的分析方法流程复杂、分析成本高的问题。
Bromine exists mainly as ions in bromide brine and halide sulfate brine in the hydrosphere of the crust.Powder carrier pellet method is commonly used in analyzing bromine in brine by Wavelength Dispersive X-ray Fluorescence Spectrometry（ WDXRF）. However,this sample preparation method has the disadvantages of large work load,sample inhomogeneity and outer contamination,which affects the analytical accuracy. Samples were pretreated by film adsorption,and film material and sample weight were optimized and are reported in this paper.Firstly,50 μL of brine is dropped to the center of a chromatography filter paper（ Ф = 40 mm）,air dried,and then flattened by high pressure to prepare the film sample for WDXRF test. A standard curve of Br was calibrated by self-prepared standard solution. Experimental results show that the impact of coexisting ions such as K＋,Na＋,Ca2 ＋,Mg2 ＋,Cl-and SO2-4on the detection of Br is negligible. The detection limit of this method is 0. 95 mg/L,the precision is less than 0. 8%（ n = 11）,and the recoveries are 99. 4%-101. 2%. The new sample preparation method is very economical and easy to operate,avoiding the use of chemical reagent.
出处
《岩矿测试》
CAS
CSCD
北大核心
2015年第5期570-574,共5页
Rock and Mineral Analysis
基金
山东省地矿局地质科技攻关项目(KY201403)
关键词
卤水
溴
薄膜吸附
X射线荧光光谱法
brine
bromine
thin film adsorption
X-ray Fluorescence Spectrometry
