摘要
对连续光源石墨炉原子吸收测定土壤中的镉的实验条件进行优化,最终确定用盐酸-硝酸-氢氟酸-过氧化氢四酸法进行消解,选择0.1%的硝酸钯作为基体改进剂,灰化分两步进行,温度分别为300℃、450℃,保持时间分别为20 s、40 s,原子化温度为1 550℃,保持时间为3 s。研究表明,此方法测定土壤中的镉标准曲线的相关系数为0.999 9,方法检出限为0.006 mg/kg,相对标准偏差为5%~11%,加标回收率为85%~94%,对质控样的分析结果与标准值吻合。
The experimental conditions for determination of cadmium in soil by continuum source graphite furnace atomic absorption were optimized. The final determination was to use hydrochloric acid-nitric acid-hydrofluoric acid-hydrogen for digestion, 0.1% of Palladium nitrate as a collective modifier, the ash was carried out in two steps, the optimum pyrolysis temperature were 300 ℃ and450 ℃, and the retention times were 20 s and 40 s, respectively, the atomization temperature was 1 550 ℃, and the retention time was 3 s. Studies had shown that the correlation coefficient of cadmium standard curve in soil measured by this method was 0.999 9, the detection limit of the method was 0.006 mg/kg, and the relative standard deviation was from 5% to 11%, and the recovery for the samples was from 85%~94%. The analysis results of the quality control samples were consistent with the standard value.
引文
[1]周宝宣,袁琦.土壤重金属检测技术研究现状及发展趋势[J].应用化工,2015,44(1):131-138+145.
[2]中国环境监测总站.土壤质量铅镉的测定石墨炉原子吸收分光光度法GB/T 17141—1997[S].北京:中国环境科学出版社,1998.
[3]肖波,陈子学,齐璐璐,等.连续光源原子吸收光谱仪在测定土壤有效态锌、锰、铁、铜中的应用[J].现代科学仪器,2007(6):108-110.
[4]王丽娟,胡军妹,严正,等.石墨炉原子吸收法测定食品中铅和镉的基体改进剂的研究[J].中外健康文摘,2011,8(45):58-60.
[5]王畅,游进.以硝酸钯为基体改进剂石墨炉原子吸收光谱法测定水和空气中痕量镉[J].中国卫生检验杂志,2003(3):355-356.
[6]德国耶拿分析仪器股份公司.高分辨连续光源石墨炉原子吸收光谱法测定土壤提取液中镉和铜[J].岩矿测试,2009,28(4):401-401.
[7]任婷,赵丽娇,钟儒刚.高分辨连续光源石墨炉原子吸收光谱法测定面制食品中的铝[J].光谱学与光谱分析,2011,31(12):3388-3391.
[8]易湘仁.原子吸收分析土壤中镉的测定[J].科研,2015(12):249.
[9]王晓雯.不同酸消解方法在土壤重金属测定中的比较研究[J].中国环境管理干部学院学报,2014,24(6):66-68.
[10]中国环境科学院.环境监测分析方法标准制修订技术导则HJ 168—2010[S].北京:中国环境科学出版社,2010.