《腐植酸尿素》編制說明（發(fā)布稿）

1《腐植酸尿素》編制說明檢測方法，新的檢測方法綜合考慮了所有腐植酸含量檢測的干擾項(xiàng)，使樣品平行測定結(jié)果的相對偏差小于等于5%；腐植酸尿素中縮二脲心化學(xué)工業(yè)集團(tuán)股份有限公司牽頭《腐植酸尿素》團(tuán)體標(biāo)準(zhǔn)的編寫，23標(biāo)準(zhǔn)制定的格式按照GB/T1.1-2GB/T8170數(shù)值修約規(guī)則與極限數(shù)值4水分、粒度共6個技術(shù)指標(biāo)項(xiàng)目。與含腐植酸尿素行標(biāo)相比，本標(biāo)項(xiàng)目Ⅳ型V型VI型總氮（N）的質(zhì)量分?jǐn)?shù)/%≥40.045.0水溶性腐植酸的質(zhì)量分?jǐn)?shù)/%≥0.500.300.220.12縮二脲的質(zhì)量分?jǐn)?shù)/%≤水不溶物含量/%≤5水分a（H2O）/%≤0.80亞甲基二脲以（HCHO計(jì))c的質(zhì)量分?jǐn)?shù)≤0.60粒度c/%d0.85mm～2.80mm≥d1.18mm～3.35mm≥d2.00mm～4.75mm≥d4.00mm～8.00mm≥90.0a水分以生產(chǎn)企業(yè)出廠檢驗(yàn)數(shù)據(jù)為準(zhǔn)。b指標(biāo)中粒度項(xiàng)只需符合四檔中任一檔即可，包裝標(biāo)識應(yīng)標(biāo)明。HG/T5045-2016《含腐植酸尿素》中腐植酸含量檢測方法是重鉻6稱取8份對照尿素3.0g，分別加入不同量的防結(jié)塊劑，用重鉻序號樣重g防結(jié)塊劑加入量g測定值%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的沸點(diǎn)不同，在60℃左右的恒溫水浴條件下油脂不被蒸出，只有溶7同時對試樣中所提取出的含油量進(jìn)行檢測，檢測結(jié)果為：0.21%序號樣品編號樣重g測定值%腐植酸含量%1對照尿素0.500550.222/2對照尿素0.500930.233/3樣品一0.497871.8174樣品一0.524031.84985樣品一0.529601.7886樣品一0.511141.7987樣品一0.494951.7878樣品一0.505091.7859樣品一0.538251.775樣品一0.525401.833樣品一0.509151.822樣品一0.496261.827最大值%最小值%極差%0.07平均值%平均偏差%0.021標(biāo)準(zhǔn)方差%0.028序號樣品編號樣重g測定值%腐植酸含量%平均值%1對照尿素1.005330.060//1.005250.061//2樣品一0.999081.0250.960.961.024091.0120.953樣品二1.020250.5900.530.531.013140.5930.534樣品三1.007571.0920.992601.1055樣品四0.995660.6400.580.5890.990820.6460.596樣品五1.028701.4051.014991.3937樣品六0.960111.4570.998741.4468樣品七0.976392.0300.965362.0159樣品八0.826541.7160.840201.724樣品九0.499472.4982.442.450.509902.5232.46樣品十0.189504.2074.154.160.177644.2324.17司樣品標(biāo)識樣品fHG/T5045-2016《含腐植酸尿素》中縮二脲含量的檢測GB/T22924的規(guī)定執(zhí)行。GB/T22924團(tuán)標(biāo)編寫組參考HG/T5045-2016《含腐植酸尿素》和GB/T取出經(jīng)多次縮分后的待測樣品約100g，快速用研磨器研磨至全35mg為宜）于250mL容量瓶中，加不含二氧化碳的水溶解并稀釋至刻度，搖勻，超聲脫氣10min，取出。倒入已裝好3KDa濾膜的超濾杯中，通氮?dú)庹{(diào)節(jié)超濾杯壓力為0.3MPa，棄去初濾液，得無色透明分別移取0.00mL、0.50mL、1.00mL、3.00mL、5.00mL、10.00mL色譜柱：S氨基或氨丙基柱，填料粒度為5um，柱長250mm，內(nèi)徑采用超濾前處理法分離尿素中腐植酸，濾液采用氨基/氨丙基柱序號樣重g峰面積濃度mg/mL縮二脲%相對偏差%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極差%0.05標(biāo)準(zhǔn)方差%0.02于9個250mL容量瓶中，用不含二氧化碳水溶解，依次加入0.5mg/mL縮二脲標(biāo)準(zhǔn)溶液5mL、5mL、5mL、10mL、10mL、10mL、15mL、15mL、15mL，用不含二氧化碳的水稀釋至刻度，搖勻，超聲脫氣10min，超序號樣重g樣品含量mg加標(biāo)量mg濃度mg/mL測得量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序號樣品編號樣重g縮二脲含量%平均值%1樣品一3.02300.980.983.05160.972樣品二3.00530.730.723.06600.723樣品三3.03460.910.913.01950.914樣品四3.20410.750.753.21020.755樣品五3.08340.920.923.08560.926樣品六3.01400.820.823.00970.827樣品七3.14440.970.963.17700.968樣品八3.11410.920.923.10590.929樣品九3.05630.860.863.07940.85