离子色谱法测定肥料中微量无机阴离子含量及国际标准制定研究
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摘要
研究开发了采用离子色谱法测定肥料中微量无机阴离子含量的新方法。该方法采用阴离子交换色谱柱,配合电导检测器,通过梯度洗脱或等度洗脱的策略,能有效地将肥料中6种常见的阴离子与其他干扰物质分离并准确测定,拓展了《化肥中微量阴离子的测定离子色谱法》(GB/T 29400—2012)国家标准的应用范围。组织了全球15家分析实验室针对一系列有代表性的肥料样品采用新方法进行了国际实验室间比对,统计结果表明,该方法的适用性广且精密度高,从而被推荐为新的国际标准ISO 20702:2017中所采用的标准测定方法。
A new method of determining microamount of inorganic anions in fertilizers by ion chromatography is researched and developed. Utilizing anion exchange column and electrical conductivity detector and adopting gradient elution or isocratic elution tactics, the method can effectively separate six common inorganic anions from other interfering materials in fertilizers and accurately determine these anions,it extends the application range of the national standard "GB/T29400—2012 Determination of microamount of inorganic anions in fertilizers by ion chromatography".15 participating laboratories all around the world are organized to conduct an interlaboratory comparison on a series of typical fertilizer samples. Statistical results show that the new method has the superiority of high adaptability and high accuracy,thereby it is recommended as standard determination method adopted in new international standard ISO 20702:2017.
A new method of determining microamount of inorganic anions in fertilizers by ion chromatography is researched and developed. Utilizing anion exchange column and electrical conductivity detector and adopting gradient elution or isocratic elution tactics, the method can effectively separate six common inorganic anions from other interfering materials in fertilizers and accurately determine these anions,it extends the application range of the national standard "GB/T29400—2012 Determination of microamount of inorganic anions in fertilizers by ion chromatography".15 participating laboratories all around the world are organized to conduct an interlaboratory comparison on a series of typical fertilizer samples. Statistical results show that the new method has the superiority of high adaptability and high accuracy,thereby it is recommended as standard determination method adopted in new international standard ISO 20702:2017.
引文
[1]奚振邦.现代化学肥料学[M].北京:中国农业出版社,2008:425-425.
[2]沈其荣,谭金芳,钱晓晴.土壤肥料学通论[M].北京:高等教育出版社,2011:80-81.
[3]买永彬,顾方乔,峋战.农业环境学[M].北京:中国农业出版社,1994:65-77.
[4]程明芳,金继运,李春花,等.氯离子对作物生长和土壤性质影响的研究进展[J].浙江农业科学,2010(1):12-14.
[5]张秀平.减少蔬菜硝酸盐积累的措施[J].安徽农业,2004(5):7-7.
[6]吴剑平,张鑫,顾欣,等.饲喂十字花科类植物对生鲜牛乳中硫氰酸钠含量的影响研究[J].中国兽药杂志,2012(10):16-19.
[7]焦立为.莫尔法沉淀滴定测定肥料中氯化物含量[J].理化检验(化学分册),2006(3):219-220.
[8]侯定军,郭扬武.原子吸收分光光度法测定复混肥料中氯含量[J].化肥工业,2003(6):53-53.
[9]冯素玲,张桂恩.动力学荧光法测定溴离子的研究[J].光谱学与光谱分析,1997(4):104-109.
[10]孙又宁,余梅玲.自动电位滴定法测定肥料和土壤中氯离子含量[J].中国土壤与肥料,2007(2):75-77.
[11]Association of Official Analytical Chemists International.AOAC Official Method 928.02 Chlorine(water-soluble)in fertilizers[S].Rockville:AOAC International,1985:1-1.
[12]European Committee for Standardization.FertilizersDetermination of chlorides in the absence of organic material:EN 16195:2011[S].Brussels:European Committee for Standardization,2011:3-6.
[13]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.尿素的测定方法第8部分:硫酸盐含量目视比浊法:GB/T 2441.8—2010[S].北京:中国标准出版社,2010:1-2.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.工业用碳酸氢铵的测定方法第2部分:氯化物含量电位滴定法:GB/T 6276.2—2010[S].北京:中国标准出版社,2010:1-3.
[15]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.工业用碳酸氢铵的测定方法第4部分:硫酸盐含量目视比浊法:GB/T 6276.4—2010[S].北京:中国标准出版社,2010:1-2.
[16]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.复混肥料中氯离子含量的测定:GB/T24890—2010[S].北京:中国标准出版社,2010:1-5.
[17]吴勣,孙明星,高运川,等.离子色谱法测定化肥中六种阴离子[J].理化检验(化学分册),2011(1):23-26.
[18]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.化肥中微量阴离子的测定离子色谱法:GB/T 29400—2012[S].北京:中国标准出版社,2012:1-8.
[19]International Organization for Standardization.ISO/FDIS20702 Fertilizers and soil conditioners-Determination of microamounts of inorganic anions in fertilizers by ion chromatography[S].Geneva:ISO General Secretary,2017:1-7.
[20]International Organization for Standardization.ISO/IEC Directives Part 1 and Consolidated ISO Supplement[M].8th Ed.Geneva:ISO General Secretary,2008:261-301.
[21]International Organization for Standardization.Accuracy(trueness and precision)of measurement methods and resultsPart 2:Basic method for the determination of repeatability and reproducibility of a standard measurement method:ISO 5725-2:1994[S].Geneva:ISO General Secretary,2017:1-21.
[22]LATIMER G W J.Official Methods of Analysis of AOAC International:Appendix F:Guideline for Standard Method Performance Requirements[M].19th Ed.Rockville:AOAC International,2012:1-16.
[23]American Society for Testing and Materials.Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method:ASTM E691-15[S].Philadelphia:American Society for Testing and Materials,2015:1-20.
[24]COCHRAN W G.The distribution of the largest of a set of estimated variances as a fraction of their total[J].Annals of Human Genetics,1941(1):47-52.
[25]GRUBBS F E.Procedures for detecting outlying observations in samples[J].Technometrics,1969(1):1-21.
[26]GRUBBS F E,BECK G.Extension of sample sizes and percentage points for significance tests of outlying observations[J].Technometrics,1972(4):847-854.
[2]沈其荣,谭金芳,钱晓晴.土壤肥料学通论[M].北京:高等教育出版社,2011:80-81.
[3]买永彬,顾方乔,峋战.农业环境学[M].北京:中国农业出版社,1994:65-77.
[4]程明芳,金继运,李春花,等.氯离子对作物生长和土壤性质影响的研究进展[J].浙江农业科学,2010(1):12-14.
[5]张秀平.减少蔬菜硝酸盐积累的措施[J].安徽农业,2004(5):7-7.
[6]吴剑平,张鑫,顾欣,等.饲喂十字花科类植物对生鲜牛乳中硫氰酸钠含量的影响研究[J].中国兽药杂志,2012(10):16-19.
[7]焦立为.莫尔法沉淀滴定测定肥料中氯化物含量[J].理化检验(化学分册),2006(3):219-220.
[8]侯定军,郭扬武.原子吸收分光光度法测定复混肥料中氯含量[J].化肥工业,2003(6):53-53.
[9]冯素玲,张桂恩.动力学荧光法测定溴离子的研究[J].光谱学与光谱分析,1997(4):104-109.
[10]孙又宁,余梅玲.自动电位滴定法测定肥料和土壤中氯离子含量[J].中国土壤与肥料,2007(2):75-77.
[11]Association of Official Analytical Chemists International.AOAC Official Method 928.02 Chlorine(water-soluble)in fertilizers[S].Rockville:AOAC International,1985:1-1.
[12]European Committee for Standardization.FertilizersDetermination of chlorides in the absence of organic material:EN 16195:2011[S].Brussels:European Committee for Standardization,2011:3-6.
[13]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.尿素的测定方法第8部分:硫酸盐含量目视比浊法:GB/T 2441.8—2010[S].北京:中国标准出版社,2010:1-2.
[14]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.工业用碳酸氢铵的测定方法第2部分:氯化物含量电位滴定法:GB/T 6276.2—2010[S].北京:中国标准出版社,2010:1-3.
[15]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.工业用碳酸氢铵的测定方法第4部分:硫酸盐含量目视比浊法:GB/T 6276.4—2010[S].北京:中国标准出版社,2010:1-2.
[16]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.复混肥料中氯离子含量的测定:GB/T24890—2010[S].北京:中国标准出版社,2010:1-5.
[17]吴勣,孙明星,高运川,等.离子色谱法测定化肥中六种阴离子[J].理化检验(化学分册),2011(1):23-26.
[18]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.化肥中微量阴离子的测定离子色谱法:GB/T 29400—2012[S].北京:中国标准出版社,2012:1-8.
[19]International Organization for Standardization.ISO/FDIS20702 Fertilizers and soil conditioners-Determination of microamounts of inorganic anions in fertilizers by ion chromatography[S].Geneva:ISO General Secretary,2017:1-7.
[20]International Organization for Standardization.ISO/IEC Directives Part 1 and Consolidated ISO Supplement[M].8th Ed.Geneva:ISO General Secretary,2008:261-301.
[21]International Organization for Standardization.Accuracy(trueness and precision)of measurement methods and resultsPart 2:Basic method for the determination of repeatability and reproducibility of a standard measurement method:ISO 5725-2:1994[S].Geneva:ISO General Secretary,2017:1-21.
[22]LATIMER G W J.Official Methods of Analysis of AOAC International:Appendix F:Guideline for Standard Method Performance Requirements[M].19th Ed.Rockville:AOAC International,2012:1-16.
[23]American Society for Testing and Materials.Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method:ASTM E691-15[S].Philadelphia:American Society for Testing and Materials,2015:1-20.
[24]COCHRAN W G.The distribution of the largest of a set of estimated variances as a fraction of their total[J].Annals of Human Genetics,1941(1):47-52.
[25]GRUBBS F E.Procedures for detecting outlying observations in samples[J].Technometrics,1969(1):1-21.
[26]GRUBBS F E,BECK G.Extension of sample sizes and percentage points for significance tests of outlying observations[J].Technometrics,1972(4):847-854.