沸水振荡浸提-电感耦合等离子体质谱(ICP-MS)法测定土壤中有效硼  

Determination of Available Boron in Soil by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)with Boiling Water Shock Extraction

作　　者：于聪灵 刘安 王立平 李龙飞 宋娟娟 李晓敬 金倩 YU Congling;LIU An;WANG Liping;LI Longfei;SONG Juanjuan;LI Xiaojing;JIN Qian(Hebei Research Center for Geoanalysis,Baoding,Hebei 071051,China;Key Laboratory of Mineral Resources and Ecological Environment Monitoring of Hebei Province,Baoding,Hebei 071051,China)

机构地区：[1]河北省地质实验测试中心,河北保定071051 [2]河北省矿产资源与生态环境监测重点实验室,河北保定071051

出　　处：《中国无机分析化学》2024年第9期1306-1312,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：河北省三三三人才基金资助项目(A201803015);河北省地矿局地质科技项目(13000022P00329410152H)。

摘　　要：传统的土壤有效硼提取和测定的方法具有前处理操作繁琐、实验流程长,检测结果误差较大且双样平行性较差等问题。为提高检测效率、降低操作难度,通过对浸提时间、振荡频率、提取器皿、分析同位素和内标元素选择等因素的考察,确定了最优条件,建立了沸水振荡浸提-电感耦合等离子体质谱(ICP-MS)法测定土壤中有效硼的方法。结果显示,在选用100 mL具盖聚乙烯离心管中沸水浸提13 min、振荡频率为180 r/min前处理条件下,使用电感耦合等离子质谱(ICP-MS)仪,以11 B为目标同位素、6 Li为内标元素进行测定,不同酸碱性土壤中的有效硼测定结果均在标准物质不确定度范围内。测定元素在浓度0~2.0μg/mL呈良好的线性关系,相关系数r为0.9998,方法的检出限为0.004 mg/kg,相对标准偏差RSD(n=7)为1.9%~4.7%。采用6种土壤有效态成分分析标准物质按照建立的方法进行处理,测定结果均在认定值的误差范围内。方法具有精密度好、操作简单、分析快速、绿色环保等特点,适用于大批量样品的检测,大大提高了检测分析效率,为土壤重金属污染检测及防治工作提供理论支撑及科学依据。The traditional methods for extraction and determination of available boron in soil have many problems,such as cumbersome pretreatment,long experimental process,large error of detection results and poor parallelism of two samples.In order to improve the detection efficiency and reduce the difficulty of operation,the optimal conditions were determined by investigating the extraction time,oscillation frequency,extraction vessel,selection of analytical isotope and internal standard element,and the method for the determination of available boron in soil by inductively coupled plasma mass spectrometry(ICP-MS)with boiling water shock extraction was established.The results showed that the pretreatment conditions were boiling water extraction for 13 min in a 100 mL polyethylene centrifuge with a cover and an oscillation frequency of 180 r/min.The determination was performed using ICP-MS with 11 B as the target isotope and 6 Li as the internal standard element.The results of the determination of available boron in different acid-base soils were all within the uncertainty range of the reference material.The determined elements showed a good linear relationship in the concentration range of 0—2.0μg/mL,with a correlation coefficient r of 0.9998.The detection limit of the method was 0.004 mg/kg,and the relative standard deviation(RSD)(n=7)was 1.9%—4.7%.Six kinds of soil available component analysis reference materials were processed according to the method,and the determination results were all within the error range of the identified value.This method has the characteristics of good precision,simple operation,rapid analysis,and environmental protection,and is suitable for the detection of large quantities of samples.It can greatly improve the efficiency of detection and analysis,and provide theoretical support and scientific basis for the detection and prevention of soil heavy metal pollution.

关 键 词：有效硼 沸水振荡浸提 电感耦合等离子体质谱法 土壤 

分 类 号：O657.63[理学—分析化学]