振荡浸提-电感耦合等离子体原子发射光谱法测定盐渍化土壤中水溶性阳离子和硫酸根  

Simultaneous determination of water-soluble cations and sulfate in saline soil by oscillation extraction-inductively coupled plasma atomic emission spectrometry

作　　者：聂高升 阿米娜·胡吉 刘权 韦应明 孙文明 徐国强 NIE Gaosheng;HOJI·Amina;LIU Quan;WEI Yingming;SUN Wenming;XU Guoqiang(Urumqi Comprehensive Survey Center on Natural Resources,China Geological Survey,Urumqi 830057,China)

机构地区：[1]中国地质调查局乌鲁木齐自然资源综合调查中心,新疆乌鲁木齐830057

出　　处：《冶金分析》2025年第1期76-83,共8页Metallurgical Analysis

基　　金：中国地质调查局项目(DD20220964)。

摘　　要：土壤盐渍化已成为威胁土壤健康的重要因素,土壤中的水溶性盐作为表征土壤盐渍化的重要指标,为盐渍化土分类和利用改良提供依据。目前,水溶性盐分分析前处理多采用林业标准方法LY/T 1251—1999《森林土壤水溶性盐分分析》,难以制备出澄清的溶液,导致水溶性盐分测定结果偏高。本文通过振荡浸提方式,采用20 g土壤样品中加入100 mL水,放入振荡机,振荡频率为200 r/min,振荡3 min后离心,单层慢速定量滤纸过滤土壤浸提液;选择K 766.490 nm、Na 818.326 nm、Ca 317.933 nm、Mg 279.079 nm、S 182.034 nm为K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-)的分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定盐渍化土壤中K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-)。方法中各离子检出限为0.01~0.02 g/kg。按照实验方法测定土壤有效态成分分析质控标准物质ASA-8a-CZ、ASA-2b-CZ、ASA-3b-CZ和土壤有效态成分分析标准物质GBW(E)070336(ASA-15)中水溶性K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-),结果的相对标准偏差(RSD,n=12)小于9%,相对误差(RE)小于8%,精密度和正确度均满足DZ/T 0258—2014《多目标区域地球化学调查规范(1∶250 000)》的要求。分别使用本法和LY/T 1251—1999测定土壤有效态成分分析质控标准物质ASA-8a-CZ中水溶性K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-),测定结果相一致。选择20件盐渍化土壤实际样品,采用本法制备浸提液,并测定K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-);同时分取一定量此浸提液,采用LY/T 1251—1999测定Cl^(-)、HCO_(3)^(-)、CO_(3)^(2-)和全盐量;用水溶性K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)、SO_(4)^(2-)、Cl^(-)、HCO_(3)^(-)、CO_(3)^(2-)这8种离子总和计算离子总量;全盐量同离子总量相对偏差小于15%。该方法无需加絮凝剂,能够同时测定土壤中水溶性K^(+)、Na^(+)、Ca^(2+)、Mg^(2+)和SO_(4)^(2-),适合于大批量区域地球化学样品中Soil salinization has become an important factor that threatens the soil health.As an important indicator of soil salinization,the water-soluble salts in soil provide a basis for the classification,utilization and improvement of salinized soil.At present,the pretreatment of water-soluble salt before analysis is mostly carried out using the forestry standard LY/T 1251-1999 Analysis methods of water-soluble salt of forest soil.However,it is difficult to prepare a clear solution,which leads to higher determination results of water-soluble salt.In this study,the oscillation extraction method was used:100 mL of water was added to 20 g of sample,which was then put into an oscillator;the oscillation frequency was 200 r/min,and the centrifugation was conducted after 3 min;the soil leaching solution was filtered by single-layer slow quantitative filter paper.K 766.490 nm,Na 818.326 nm,Ca 317.933 nm,Mg 279.079 nm and S 182.034 nm were selected as analytical spectral lines,and the content of K^(+),Na^(+),Ca^(2+),Mg^(2+) and SO<sup>2-4 in saline soil was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES). The limits of detection of ions were between 0.01 g/kg and 0.02 g/kg.The water-soluble K^(+),Na^(+),Ca^(2+),Mg^(2+) and SO<sup>2-4 in the quality control certified materials (ASA-8a-CZ,ASA-2b-CZ,ASA-3b-CZ) and certified reference materials[GBW(E)070336(ASA-15)] of soil for available components analysis were determined according to the experimental method.The relative standard deviations (RSD,n=12) of results were less than 9%,and the relative errors (RE) were less than 8%.The precision and accuracy could meet the requirements of DZ/T 0258-2014 Specification for Multi-objective Regional Geochemical Survey (1∶250 000).The content of K^(+),Na^(+),Ca^(2+),Mg^(2+) and SO<sup>2-4 in quality control reference material of soil for available components analysis(ASA-8a-CZ) was determined according to the experimental method and LY/T 1251-1999,and the found results were consistent.Twenty samples of saline

关 键 词：盐渍化土壤 水溶性阳离子 硫酸根 振荡提取 电感耦合等离子体原子发射光谱(ICP-AES) 区域地球化学样品 

分 类 号：O657.31[理学—分析化学]