岩矿测试2025，Vol.44Issue(3)：460-468,9.DOI:10.15898/j.ykcs.202411290248
碱熔分解-电感耦合等离子体质谱/发射光谱法测定黑土地地表基质中33种元素
Determination of 33 Elements in Ground Substrate of Black Soil by ICP-MS/OES with Alkali Melting Digestion
摘要
Abstract
The organic matter content in black soil samples is high,typically ranging from 3％ to 10％.Traditional pretreatment methods such as open acid dissolution digestion,microwave acid dissolution and digestion,high-pressure closed acid dissolution and digestion,and ashing method cannot completely digest the sample,and different elements need to adopt different digestion and determination methods,resulting in long experiments,complex operation processes,high analysis costs,and are not suitable for the simultaneous determination of multiple elements.Sodium carbonate,lithium tetraborate and lithium metaborate were selected as mixed fluxes to digest the samples,and a method of adding tartaric acid to the acid extractor was proposed to extract the samples.33 elements in the ground substrate of black soil were determined by inductively coupled plasma-mass spectrometry/optical emission spectrometry(ICP-MS/OES).The traditional method for analyzing black-soil sample is not suitable for the simultaneous determination of rare earth and other multiple elements, nor for elements prone to hydrolysis such as tantalum and hafnium,while ICP-MS/OES is suitable.The effects of different extraction systems on the extraction of tantalum and hafnium were studied,and the optimal ratio of 30mL of hydrochloric acid and 10mL of 100g/L tartaric acid was determined.On this basis,the detection limit of the samples was 0.01-41.04μg/g by the experimental method of control samples,and the results satisfied the requirements of soil analysis and detection.At the same time,different kinds of soil reference materials were selected for practical testing,and the measured values of each element were basically consistent with the standard values,with the relative standard deviations(RSDs)between 0.48％-4.36％ and the relative errors between-5.23％-4.85％.In addition,to further verify the feasibility of the method,the relative standard deviations were all between 0.16％-4.97％ when applied to actual samples.关键词
稀土元素/钽/铪/电感耦合等离子体质谱法/电感耦合等离子体发射光谱法/酒石酸/碱熔/黑土Key words
rare earth elements/Ta/Hf/inductively coupled plasma-mass spectrometry/inductively coupled plasma-optical emission spectrometry/tartaric acid/alkali fusion/black soil分类
化学化工引用本文复制引用
于海月,张淇,卢兵,韩晨灏,王桃源,李明亮..碱熔分解-电感耦合等离子体质谱/发射光谱法测定黑土地地表基质中33种元素[J].岩矿测试,2025,44(3):460-468,9.基金项目
中国地质调查局地质调查项目"战略性矿产勘查岩矿测试技术支撑(哈尔滨中心)"(DD20243204) （哈尔滨中心）
