离子色谱法快速测定土壤中的亚硝酸盐氮和硝酸盐氮
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摘要
建立离子色谱法快速测定土壤中亚硝酸盐氮和硝酸盐氮的方法。土壤样品采用250 mL 0.01 moL/L氯化钙溶液提取,于20℃水浴振荡60 min,静置离心。采用Ion Pac AS19离子色谱柱,以20 mmoL/L氢氧化钾溶液为淋洗液,流量为1.0 mL/min,进样体积为25μL,以电导检测器进行检测。亚硝酸盐氮和硝酸盐氮的质量浓度在0.20～5.00 mg/L范围内与色谱峰面积呈良好的线性关系,线性相关系数均为0.999 9,方法检出限分别为0.005,0.007mg/L。样品的加标回收率为95.0%～97.4%,测定结果的相对标准偏差为0.89%～2.11%(n=12)。该方法适用于土壤中亚硝酸盐氮和硝酸盐氮含量的快速测定。
A method for rapid determination of nitrite nitrogen and nitrate nitrogen in soil by ion chromatography was established. The soil samples were extracted by 250 mL 0.01 moL/L calcium chloride solution, shaken for 60 min in 20℃water bath, and centrifuged in static state. Ion Pac AS19 was used as ion chromatography column, 20 mmoL/L potassium hydroxide solution was used as eluent, the flow rate was 1.0 mL/min, the injection volume was 25 μL. It was detected by conductive detector. The mass concentration of nitrite nitrogen and nitrate nitrogen showed good linear relationships with its chromatographic peak area in the range of 0.20–5.00 mg/L, and the correlation coefficients were 0.999 9, the detection limits were 0.005, 0.007 mg/L, respectively. The recoveries of standard addition were 95.0%–97.4%, and the relative standard deviation of the results was 0.89%–2.11%(n=12). The method is suitable for the rapid determination of nitrite nitrogen and nitrate nitrogen content in soil.
A method for rapid determination of nitrite nitrogen and nitrate nitrogen in soil by ion chromatography was established. The soil samples were extracted by 250 mL 0.01 moL/L calcium chloride solution, shaken for 60 min in 20℃water bath, and centrifuged in static state. Ion Pac AS19 was used as ion chromatography column, 20 mmoL/L potassium hydroxide solution was used as eluent, the flow rate was 1.0 mL/min, the injection volume was 25 μL. It was detected by conductive detector. The mass concentration of nitrite nitrogen and nitrate nitrogen showed good linear relationships with its chromatographic peak area in the range of 0.20–5.00 mg/L, and the correlation coefficients were 0.999 9, the detection limits were 0.005, 0.007 mg/L, respectively. The recoveries of standard addition were 95.0%–97.4%, and the relative standard deviation of the results was 0.89%–2.11%(n=12). The method is suitable for the rapid determination of nitrite nitrogen and nitrate nitrogen content in soil.
引文
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[14]王祖翔,余杨,孙莉,等.离子色谱法测定食品中的无机铵[J].食品与机械,2012,28(4):96-99.
[15]杨春霞.离子色谱法测定土壤中无机阴阳离子含量[J].理化检验(化学分册),2012,48(10):1 199-1 202.
[16]莫紫梅,杨黎,郑娟,等.离子色谱法测定FAPAS比对肉粉样品中亚硝酸盐、硝酸盐含量[J].肉类研究,2018(3):46-50.
[17]郑小玲,郭小喜,李晓华,等.离子色谱法测定婴幼儿米粉中硝酸盐和亚硝酸盐[J].食品研究与开发,2018(4):152-156.
[18]DAHNKE W C.Recommended chemical soil test procedures for the North Central Region[M].North Central Regional Research Publication No.221(Revised).
[19]刘帅,吕亮.离子色谱法测定土壤中的硝态氮[J].农业工程,2011(3):61-64.
[2]HJ 634-2012土壤氨氮、亚硝酸盐氮、硝酸盐氮的测定氯化钾溶液提取-分光光度法[S].
[3]李亚男,王宇新.离子色谱技术在环境监测中的应用及预处理技术[J].环境科学与管理,2005,30(4):105-106.
[4]王梅英,王敏捷,李鹏程,等.离子色谱法同时测定天然碱矿中氯离子和硫酸根离子[J].岩矿测试,2013,32(4):586-589.
[5]李苗,冯光.离子色谱技术在药物分析领域的研究进展[J].中国药品标准,2011,12(5):342-345.
[6]林琳,劳月娥,许健,等.在线渗析-离子色谱法测定土壤中有效氟[J].岩矿测试,2011,30(4):497-500.
[7]赵新颖,屈锋,牟世芬.离子色谱技术的重要进展和我国近年的发展概况[J].色谱,2017(3):223-228.
[8]钟坚海,郑瑞娟,陈金凤,等.连续自动再生化学抑制-离子色谱法测定石膏及其制品中的氟和氯[J].岩矿测试,2015,34(3):330-334.
[9]熊文明,张志军.碱熔-离子色谱法同时测定玻璃中的氟和硫[J].岩矿测试,2011,30(6):768-771.
[10]齐竹华,刘克纳,牟世芬.离子色谱法测定海水中的铵离子[J].环境化学,2000,19(1):79-83.
[11]MICHALSKI R.Determination of nitrogen species(nitrate,nitrite and ammonia ions)in environmental samples by ion chromatography[J].Polish journal of environmental studies,2006,15(1):5-18.
[12]GB 5009.33-2010食品安全国家标准食品中亚硝酸盐和硝酸盐的测定[S].
[13]何清,郑爱华.离子色谱法测定土壤中的总氮量[J].实验室研究与探索,2011,30(11):221-223.
[14]王祖翔,余杨,孙莉,等.离子色谱法测定食品中的无机铵[J].食品与机械,2012,28(4):96-99.
[15]杨春霞.离子色谱法测定土壤中无机阴阳离子含量[J].理化检验(化学分册),2012,48(10):1 199-1 202.
[16]莫紫梅,杨黎,郑娟,等.离子色谱法测定FAPAS比对肉粉样品中亚硝酸盐、硝酸盐含量[J].肉类研究,2018(3):46-50.
[17]郑小玲,郭小喜,李晓华,等.离子色谱法测定婴幼儿米粉中硝酸盐和亚硝酸盐[J].食品研究与开发,2018(4):152-156.
[18]DAHNKE W C.Recommended chemical soil test procedures for the North Central Region[M].North Central Regional Research Publication No.221(Revised).
[19]刘帅,吕亮.离子色谱法测定土壤中的硝态氮[J].农业工程,2011(3):61-64.