化肥成分分析系列标准物质研制

Development of Certified Reference Materials for the Chemical Composition of Chemical Fertilizers

研制了尿素、磷酸氢二铵、氯化钾、高氮磷低氯复合肥、高氮低氯复合肥、高钾硫基复合肥、高钾中氯复合肥、高磷低氯复合肥和平衡型硫基复合肥系列化肥标准物质,样品严格按照相关标准要求进行采集、加工制备、均匀性检验、稳定性检验,由15家不同行业的权威实验室进行协作定值,并对不确定度进行评定。结果表明,样品粒度分布满足样品加工要求,具有良好的均匀性和稳定性。本系列化肥标准物质共定值45项元素(指标),包括N、P_(2)O_(5)、水溶性P_(2)O_(5)、有效性P_(2)O_(5)、K_(2)O、S、Cl、As、Hg、Cr、Cd、Cu、Pb、Zn、Ni、B、Se、Ge、Fe、Na、Ca、Mg、Al、Ti、V、Mn、Co、Sr、Mo、Ba、Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,量值准确可靠、不确定度范围评估合理,符合国家一级标准物质的要求。研制的9个化肥化学成分标准物质定值的元素含量梯度范围合理,填补了国内复合肥料标准物质空白,可为化肥样品分析质量控制、实验室仪器校准、分析方法和实验室检测能力验证与评价提供基础技术支撑。

The set of chemical fertilizer CRMs were developed in this study include urea,diammonium hydrogen phosphate,potassium chloride,high nitrogen phosphorus low chlorine compound fertilizer,high nitrogen and low chlorine compound fertilizer,high potassium sulfur based compound fertilizer,high potassium and medium chlorine compound fertilizer,high phosphorus and low chlorine compound fertilizer and balanced sulfur based compound fertilizer.Samples were collected,processed,prepared,tested for uniformity and stability in strict accordance with the requirements of standards.Then,cooperative analyses for certification were performed by 15 authoritative laboratories from different departments.Results show that the particle size distribution of the processed samples meet the requirements of sample processing.The samples have good homogeneity,and the samples can be considered to be stable.Reference values of 45 elements(indexes)for this set of fertilizer reference materials were certified,including N,P_(2)O_(5),water-soluble P_(2)O_(5),available P_(2)O_(5),K_(2)O,S,Cl,As,Hg,Cr,Cd,Cu,Pb,Zn,Ni,B,Se,Ge,Fe,Na,Ca,Mg,Al,Ti,V,Mn,Co,Sr,Mo,Ba,Y,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu.The certified values are reliable with reasonable uncertainty ranges,which meet the requirements of national first-class reference materials.The gradient range of major element content of the nine certified reference materials for chemical composition of chemical fertilizer is reasonable,which improves the types of certified reference materials for chemical fertilizer,and provides basic technical support for quality control of chemical fertilizer sample analysis,calibration of laboratory instruments,analysis methods and evaluation of laboratory ability.