《腐植酸尿素》编制说明（发布稿）

1《腐植酸尿素》编制说明检测方法，新的检测方法综合考虑了所有腐植酸含量检测的干扰项，使样品平行测定结果的相对偏差小于等于5%；腐植酸尿素中缩二脲心化学工业集团股份有限公司牵头《腐植酸尿素》团体标准的编写，23标准制定的格式按照GB/T1.1-2GB/T8170数值修约规则与极限数值4水分、粒度共6个技术指标项目。与含腐植酸尿素行标相比，本标项目Ⅳ型V型VI型总氮（N）的质量分数/%≥40.045.0水溶性腐植酸的质量分数/%≥0.500.300.220.12缩二脲的质量分数/%≤水不溶物含量/%≤5水分a（H2O）/%≤0.80亚甲基二脲以（HCHO计)c的质量分数≤0.60粒度c/%d0.85mm～2.80mm≥d1.18mm～3.35mm≥d2.00mm～4.75mm≥d4.00mm～8.00mm≥90.0a水分以生产企业出厂检验数据为准。b指标中粒度项只需符合四档中任一档即可，包装标识应标明。HG/T5045-2016《含腐植酸尿素》中腐植酸含量检测方法是重铬6称取8份对照尿素3.0g，分别加入不同量的防结块剂，用重铬序号样重g防结块剂加入量g测定值%腐植酸含量%13.0011800.034023.0055700.035032.991390.005500.1300.095542.993820.005610.1270.092552.995180.003230.0980.063563.002810.003010.0910.056573.003650.002880.0900.055583.007210.002110.0770.0425的沸点不同，在60℃左右的恒温水浴条件下油脂不被蒸出，只有溶7同时对试样中所提取出的含油量进行检测，检测结果为：0.21%序号样品编号样重g测定值%腐植酸含量%1对照尿素0.500550.222/2对照尿素0.500930.233/3样品一0.497871.8174样品一0.524031.84985样品一0.529601.7886样品一0.511141.7987样品一0.494951.7878样品一0.505091.7859样品一0.538251.775样品一0.525401.833样品一0.509151.822样品一0.496261.827最大值%最小值%极差%0.07平均值%平均偏差%0.021标准方差%0.028序号样品编号样重g测定值%腐植酸含量%平均值%1对照尿素1.005330.060//1.005250.061//2样品一0.999081.0250.960.961.024091.0120.953样品二1.020250.5900.530.531.013140.5930.534样品三1.007571.0920.992601.1055样品四0.995660.6400.580.5890.990820.6460.596样品五1.028701.4051.014991.3937样品六0.960111.4570.998741.4468样品七0.976392.0300.965362.0159样品八0.826541.7160.840201.724样品九0.499472.4982.442.450.509902.5232.46样品十0.189504.2074.154.160.177644.2324.17司样品标识样品fHG/T5045-2016《含腐植酸尿素》中缩二脲含量的检测GB/T22924的规定执行。GB/T22924团标编写组参考HG/T5045-2016《含腐植酸尿素》和GB/T取出经多次缩分后的待测样品约100g，快速用研磨器研磨至全35mg为宜）于250mL容量瓶中，加不含二氧化碳的水溶解并稀释至刻度，摇匀，超声脱气10min，取出。倒入已装好3KDa滤膜的超滤杯中，通氮气调节超滤杯压力为0.3MPa，弃去初滤液，得无色透明分别移取0.00mL、0.50mL、1.00mL、3.00mL、5.00mL、10.00mL色谱柱：S氨基或氨丙基柱，填料粒度为5um，柱长250mm，内径采用超滤前处理法分离尿素中腐植酸，滤液采用氨基/氨丙基柱序号样重g峰面积浓度mg/mL缩二脲%相对偏差%15.216052.27780.17780.86-225.151753.77280.18280.89135.216054.11840.18400.87-144.952550.36710.17080.87-154.984251.76570.17570.88064.025043.00430.14490.90275.031951.83800.17590.87-184.901749.35300.16720.85-394.379546.26830.15640.8914.560147.95100.16230.891平均值%0.88最大值%0.90最小值%0.85极差%0.05标准方差%0.02于9个250mL容量瓶中，用不含二氧化碳水溶解，依次加入0.5mg/mL缩二脲标准溶液5mL、5mL、5mL、10mL、10mL、10mL、15mL、15mL、15mL，用不含二氧化碳的水稀释至刻度，摇匀，超声脱气10min，超序号样重g样品含量mg加标量mg浓度mg/mL测得量mg回收率%12.965225.202.500.111427.8522.965025.202.500.111127.7833.000525.502.500.111227.809242.965425.215.000.124231.0552.953425.105.000.123330.8363.004725.545.000.123930.9872.970325.257.500.135833.9582.960425.167.500.13634.0093.000125.507.500.135533.88序号样品编号样重g缩二脲含量%平均值%1样品一3.02300.980.983.05160.972样品二3.00530.730.723.06600.723样品三3.03460.910.913.01950.914样品四3.20410.750.753.21020.755样品五3.08340.920.923.08560.926样品六3.01400.820.823.00970.827样品七3.14440.970.963.17700.968样品八3.11410.920.923.10590.929样品九3.05630.860.863.07940.85