粮油检验 粮食、油料的杂质、不完善粒检验编制说明

2《粮油检验粮食、油料的杂质、不完善粒检验》编制说明根据国家标准化管理委员会《关于下达2023年第一批推荐性国家标准计划质量监督检测中心、河南省食品和盐业检验技术研究院（河南省粮油饲料产品质量监督检验中心）、深圳市计量质量检测研究院、中储粮质检有限公司、迩言(上海）科技有限公司、北京中检葆泰生物技术有限公司、中储粮成都储藏研3用人工智能的粮食AI识别系统，学习完善数据库，准确率、重复性、稳定性和霉变粒、损伤粒、杂质等指标数智化检测，在图像识别、模型建立和AI智能学4图1糙米未熟粒图2糙米病斑粒图3糙米生芽粒图4玉米生霉粒图5玉米热损伤粒图6玉米虫蚀粒图7玉米双面扫描图片家粮食和物资储备局办公室关于下达2020通知》，由北京东孚久恒仪器技术有限公司牵头制定《52023年6月-2023年12月，标准并形成标准文本及编制说明征求意见稿。2024年3月，召开起草组第一次研讨分析，对文本提出修改意见和建议，并协助起草单6效降低人工劳动强度、提高效率，从而提高粮食基层检验情况，本次修订增加了不完善粒子项的计算公式，7），出黍粒；稷米拣出稷粒；高粱米拣出高粱壳善粒检验试样质量（m5’米类小样用量与其原粮相同）”，修8糙米并称量（m5精确至0.01g。”的检测程序，将大样杂质含量（u1）录入仪器，启动仪器进行图像采集和图像分析。仪器自动计算得到不完善粒含量、谷外果的平均数，即为测试结果，以质量分数（%）表示，结果保留小数点后一位。本次修订增加了不完善粒子项的计算公式，东、海南等主产区的意见确定油菜籽筛层孔径为1.0mm；花生上层筛层孔径为9表1原始数据：粮食的大样杂质含量人员i小麦-1小麦-2小麦-3稻谷-1稻谷-2稻谷-3玉米-1玉米-2玉米-3大豆-1大豆-2大豆-3水平j12345678910.492.150.570.970.690.60.592.250.620.570.540.620.710.530.612.0820.622.160.750.930.510.392.230.710.880.740.810.640.562.150.540.912.050.570.550.472.0230.430.520.430.980.400.512.160.510.480.462.080.552.030.490.480.462.3040.610.500.552.030.602.010.562.050.720.460.960.382.150.510.560.990.610.860.572.0650.582.190.640.950.700.490.522.310.600.880.590.552.050.452.030.550.610.950.5760.560.950.620.480.650.920.462.180.660.960.470.542.010.520.632.020.620.990.57表2粮食大样杂质含量实验结果分析（%）实验员1实验员2实验员3实验员4实验员5实验员6平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数736216012350475830878290446708234890592370444712271557671272137068471452435117954602566365321772871774227948102703492656673074746不应超过3次测定重复性临界极差，即极差表3对单元平均值的格拉布斯检验水平单个低值单个高值两个低值两个高值检验类型10.5250.200格拉布斯检验统计量20.1620.56830.48040.2250.47450.1500.38760.8090.1340.54070.7890.2740.32680.2170.52490.2960.2840.2090.3270.0830.5120.3270.359岐离值0.03490.0349格拉布斯检验临界值0.01160.0116表4粮食大样杂质含量的mj,srj,sRj计算值（%）水平jmj回收率2.8*Srj2.8*SRj10.550.05260.06350.14720.177920.08220.09350.23020.261832.060.10460.11490.29290.321640.610.05860.07710.16410.215850.07370.09870.20630.2763690.50.09830.11100.27520.310970.550.05610.07500.15720.210080.08010.09400.22440.2632990.00.09360.11390.26190.31910.520.05680.07490.15910.20970.08280.09860.23170.27622.030.09820.11040.27490.3092参与的一致水平试验获得重复性标准差srj=0.056，再现性标准差SRj=0.073；mj水平时，重复性标准差srj=0.099，再现性标准差SRj=0.113。现行标准GB/T试结果绝对差值不大于0.3%。本次试验中，大样杂质含量在较高水平，即性标准差2.8SRj=2.8×0.113＝0.31≈0表5小样杂质含量人员i小麦-1小麦-2小麦-3稻谷-1稻谷-2稻谷-3玉米-1玉米-2玉米-3大豆-1大豆-2大豆-3水平j12345678910.481.890.390.882.080.570.860.510.521.990.280.790.510.820.680.980.571.630.360.900.380.760.7120.550.980.270.890.330.920.550.632.060.240.800.520.790.560.570.950.372.040.400.7230.442.040.440.920.380.882.050.660.970.490.360.910.352.010.680.860.412.150.410.420.920.4540.580.520.962.090.550.870.390.990.622.010.380.800.310.960.550.440.400.880.330.790.640.8650.580.982.090.440.852.070.500.560.560.500.980.420.920.480.400.550.350.850.700.822.0460.420.990.512.050.380.920.660.880.492.090.380.940.240.850.760.810.600.370.430.770.68表6粮食小样杂质含量实验结果分析（%）实验员1实验员2实验员3实验员4实验员5实验员6平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数表7对单元平均值的格拉布斯检验水平单个低值单个高值两个低值两个高值检验类型10.2780.339格拉布斯检验统计量20.5410.06130.3410.25540.1960.39750.4990.3080.39860.3230.28270.4290.22280.2970.29190.4040.2790.5300.2410.5700.0830.5650.060岐离值0.03490.0349格拉布斯检验临界值0.01160.0116表8粮食大样杂质含量的mj,srj,sRj计算值（%）水平jmj回收率2.8*Srj2.8*SRj10.520.05990.06690.16770.187420.07570.10520.21210.2947396.50.11180.11250.31310.315140.4080.00.05200.08300.14570.232550.9292.00.06530.07480.18280.2094697.00.10360.10630.29000.297670.4182.00.07670.07770.21480.217680.8989.00.07750.08640.21710.2420991.50.10330.28930.31480.610.08710.09150.24370.25630.08940.10030.25020.280989.00.10540.11090.29500.3106参与的一致水平试验获得重复性标准差srj=0.069，再现性标准差SRj=0.080；mj水平时，重复性标准差srj=0.106，再现性标准差SRj=0.110。现行标准GB/T试结果绝对差值不大于0.3%。本次试验中，小样杂质含量在较高水平，即一致。大样杂质含量和小样杂质含量小于2.0%时方法的重复性符合GB/T量国家标准有关问题的规定》中要求原粮杂质含量的允许偏差要求为不大于对小麦、玉米样品的不完善粒含量进行测定，从准确度和表9原始数据：粮食的不完善粒含量（%）人员i小麦-1小麦-2小麦-3小麦-4小麦-5小麦-6玉米-1玉米-2玉米-3玉米-4玉米-5玉米-6水平j1234567898.09.86.58.49.96.48.721.02.09.97.32.76.08.020.72.052.56.79.08.69.8表10粮食不完善粒含量实验结果分析（%）实验员1实验员2实验员3实验员4实验员5实验员6平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数平均值极差标准差变异系数）；）；表11对单元平均值的格拉布斯检验水平单个低值单个高值两个低值两个高值检验类型10.3190.358格拉布斯检验统计量20.5570.08130.4350.18140.1430.48150.1150.48760.4060.19270.3300.23180.2310.31590.3560.2330.3670.2430.3060.3490.3360.238岐离值0.03490.0349格拉布斯检验临界值0.01160.0116表12粮食不完善粒含量的mj,srj,sRj计算值（%）水平jmj回收率2.8*Srj2.8*SRj197.50.10890.10990.30480.307822.4397.20.10540.14310.29510.400736.340.16330.20180.45720.565248.190.18760.31500.52520.881950.24800.30200.69430.8456620.920.30060.38890.84171.088872.160.10000.16390.28000.458884.090.22360.24350.62610.681895.8297.00.29310.35750.82081.00118.090.35220.47370.98631.32629.9799.70.37320.38661.04491.082599.60.52770.89871.47772.5163图8中粒粮的重复性和再现性图图9大粒粮的重复性和再现性性限R存在相关性，进一步分析见图8和图9，相关系数大于0.9。a.对于中粒粮，通过y=0.0292x+0.2806可以计算出重复性要求不高于0.5%时，对应的不完善粒含量为7.5%，即大于8.0%时应考虑调整精密度要求。例如5等和等外小麦要考虑调整精密度要求。通过对我国中小粒粮中总产量排名第一的小麦质量等级情况分析，不完善粒含量为再叠加分样误差，将5等和等外小麦不完善粒的两次独立测试结果的绝大于0.5当不完善粒总量＞8.0%时，在重复性条件下，获得的两次b.对于大粒粮，通过y=0.0803x+0.2555可以计算出重复性要求不高于要求。例如5等和等外玉米要考虑调整精密度要求。通过对我国大粒、特大粒粮中总产量排名第一的玉米质量等级情况再叠加分样误差，将5等和等外玉米不完善粒的两次独立测试结果的绝不完善粒总量≤10.0%时，在重复性条件下，获得的两次独立测试结果在实验室内使用品牌1不完善粒测定仪仪器检验法分别对粮食不完善粒含间是否存在显著性差异，小麦和玉米测定结果计算出统计量|t|<t0.05(p<0.05，两种测定方法无显著性差异。采用x2检验进行标准差检验，按照现行国标GB/T5494-2019中规定的不完善粒含量重复性要求计算得出小麦和玉米的平的小麦测定结果计算统计量x2<x20.95(2)=5.99，极差<CrR95(3)=0.594，说明小麦测定结果均符合现行国标GB/T5494-2019中的重复性要求。不完善粒含量量x2<x20.95(2)=5.99，极差>CrR95(3)=1.188说明当玉米不完善粒含量小于8%时，测定结果均符合现行国标GB/T5494-2019中的重复性要求，但当玉米不完善粒含量大于8%时，测定结果不再符合现行国标GB/T5494-2019中的重复性要求。表13实验室内小麦仪器检验法不完善粒含量测定结果样品测定次数感官分析测定结果(%)仪器检验法测定结果(%)仪器检验法测定平均值(%)标准偏tt0.05(2)x2x20.95(2)差(%)CrR95(3)小麦麦110.22-2.944.3032.8815.990.50.59423麦0.160.422.632.8麦315.86.06.00.21-1.692.6060.526.335.8麦40.212.6060.528.038.5麦510.19-3.982.1950.423麦6121.120.821.00.170.4221.2320.9表14实验室内玉米仪器检验法不完善粒含量测定结果样品测定次数工测定结果(%)仪器测定结果(%)仪器测定平均值(%)标准偏tt0.05(2)x2x20.95(2)差(%)CrR95(3)玉米玉米0.190.614.3030.5495.990.422.232.6玉0.310.7米223.934.6玉米31-1.702.57226.637.1玉米40.45-2.033.18928.937.8玉米50.630.366.20729.83玉米61-0.4917.5932.423器检测，将检测结果与定值进行配对T检验，考察两组结果是否存在显著性差表15小麦不完善粒准确性测试数据编号人工测定结果(%)仪器测定结果(%)差值di均值d标准偏差sdtdt0.05,2916.958.52-1.57-0.282.0452-0.7937.477.65-0.1844.315-0.7762.872.740.1370.2486.706.550.1592.420.553.455.535.305.56-0.264.695.48-0.796.296.49-0.204.275.98-1.713.573.45-0.723.246.28-3.04-0.32202.272.61-0.34216.989.39-2.41223.403.72-0.32234.204.33-0.13240.00254.95-0.81262.592.170.42272.442.91-0.47282.152.93-0.78292.283.51-1.23302.263.19-0.93表16玉米不完善粒准确性数据分析表编号人工测定结果(%)仪器测定结果(%)差值di均值d标准偏差sdtdt0.05,2914.173.310.860.250.792.04523.474.21-0.7433.782.790.9943.883.380.5152.943.52-0.5864.335.27-0.9474.665.67-1.0184.034.27-0.2492.823.45-0.633.182.980.205.694.830.865.615.330.285.055.09-0.045.805.600.207.717.420.294.935.20-0.276.976.040.935.666.39-0.734.724.530.19208.647.780.86217.557.100.46227.466.42238.337.620.71246.737.69-0.96257.716.720.99269.770.7727280.56292.56300.39准方法中规定的重复性要求，同时采用6次测定极差与现有国家标准（GB/T6379.6-2009）规定的6次测定重复性临界极差进行对照，考察表17低值样重复性分析表测定次数不完善粒（%）平均值标准偏差sx2x20.95（5）极差12.642.6011.07050.2822.4232.742.6652.6462.52表18中值样重复性分析表测定次数不完善粒（%）平均值标准偏差sx2x20.95（5）极差19.3411.07050.5529.3038.9149.0959.4669.31表19高值样重复性分析表测定次数不完善粒（%）平均值标准偏差sx2x20.95（5）极差10.238.6011.07050.6323456三个水平不完善粒含量的x2计算值均不超过查表值，极差也均不超过重复a.决定修改感官检验法的精密度要求，对于中小粒粮食、油料，当不完善值不大于0.5当不完善粒总量＞8.0%时，在重复性条件下，获得的测试结果保留到小数点后一位。对于大粒、特大粒粮食、油料，当不完善粒总量≤10.0%时，在重复性条件下，获得的两次独立测试结果的绝％；b.第二法仪器检验法重复性与第一法感官检验法要求一致。得的两次独立测试结果的绝对差值不大于0.5％，求其平均数，即为表20原始数据：稻谷的谷外糙米含量人员iDG-1DG-2DG-3DG-4DG-5DG-6水平j12345614.365.046.213.043.844.256.322.063.404.324.996.9422.384.085.647.170.832.854.034.696.520.622.252.573.624.647.1633.533.694.466.510.953.003.685.207.003.324.005.8642.993.785.237.330.842.073.214.075.906.892.853.905.566.5550.942.763.974.886.170.853.204.365.326.492.894.676.7760.732.693.624.336.583.053.745.027.150.812.944.054.416.88表21稻谷的谷外糙米含量实验结果分析（%）人员i结果分析DG-1DG-2DG-3DG-4DG-5DG-6水平j1234561平均值66.49极差0.130.470.360.520.790.73标准差0.040.360.32变异系数5.104.755.667.594.952平均值0.842.603.914.996.95极差0.460.490.470.460.65标准差90.210.460.30变异系数22.307.435.279.224.383平均值3.283.795.176.88极差0.500.530.320.61标准差0.210.070.26变异系数2.426.643.923.844平均值3.023.925.566.92极差0.320.330.360.290.670.78标准差70.32变异系数7.274.913.044.924.615平均值0.952.954.154.966.48极差40.390.650.60标准差0.090.070.25变异系数9.476.263.895.463.796平均值0.852.893.804.596.87极差0.280.350.360.430.690.57标准差80.310.23变异系数8.065.214.766.723.39同一人员3次测定结果极差在0.57%-0.72%之间。按照稻谷谷外糙米含量重复复性临界极差，即极差<CrR95(3)=0.589。说明当稻谷谷外糙米含量水平小于4.0%时，测定结果均符合在重复性条件下两次独立测试结果的绝0.38%、0.98%、0.47%。不同人员测定稻谷谷外糙米含量的标准差在0.045-0.572之间，变异系数在2.412=0.481表22对单元平均值的格拉布斯检验水平单个低值单个高值两个低值两个高值检验类型10.3760.174格拉布斯检验统计量20.1670.45630.2450.34840.4430.09950.9940.31460.9250.018*0.630岐离值0.03490.0349格拉布斯检验临界值0.01160.0116表23稻谷谷外糙米含量的mj,Srj,SRj计算值（%）水平jmj回收率2.8*Srj2.8*SRj10.18830.39600.5272294.00.14750.15350.41290.429732.9999.70.17630.28100.49360.786743.9699.00.17950.22160.50260.620555.010.38990.46571.09181.304066.7696.60.28330.31910.79330.8935因此本次文本修订确定稻谷谷外糙米含量方法精密度为：当谷外糙米含量≤其平均数，即为测试结果，测试结果保留到小数点后一位；当谷外糙米含量＞其平均数，即为测试结果，测试结果保留到小数表24谷外糙米含量准确性数据分析表编号人工测定结果仪器测定结果差值di均值d标准偏差Sdtdt0.05,291-0.16-0.060.350.932.04520.170.52-0.3530.500.370.1340.470.320.1550.340.39-0.0560.520.280.2470.370.42-0.0580.790.85-0.0690.640.70-0.06-0.480.800.550.250.340.68-0.340.460.51-0.050.650.520.920.97-0.050.750.85-0.100.260.730.80-0.070.740.42200.290.56-0.2721-0.64220.43232.01-0.92240.480.53-0.05250.74260.81-0.27270.620.69-0.0728-0.41290.730.78-0.05300.560.99-0.43a.修改感官检验法的精密度要求当谷外糙米含量≤4.b.仪器检验法可以用于测定稻谷中的谷外糙米含量。表25技术内容的对比1/是仪器检验法融入标准文2是不完善粒含量和稻谷中谷外糙米含量将适用于谷外糙米含量3食、油料检验油检验感官检是增加了4个文件：GB/T5490粮油检验一般规则、GB/T36091粮油机械检验4义是增加了6项术语定义：图像采集、图像质质的内容提取出来总结5是6是7否），8是修改了不完善粒含量精密度要求。结果的绝对差值：大粒、特大粒粮食、油料当不完善粒子项含量≤10.0%时，不大于1.0当不完善粒子项含量＞料当不完善粒子项含量≤8.0%时，不大于0.5％；当不完善粒子项含量＞精密度要求：当谷外糙米含量≤4.0%时，在重复性条件下获得的两次独立测试结果的绝对差值不大于0.5%;当谷外糙米含量＞4.0%时，在重复性条件下获得的两次独立测试结果/9无是在第二法仪器检验法中增加了原理：采用相机或扫描仪等图像采集装置采谷外糙米含量和不完善粒含量质量分“粮食和油料容是按照第一法7.1.3进行大样杂质检验，检验结果计算和重复性要求同第一法8.1.1。从检验过大样杂质的试样中缩注：不完善粒检验试样质量不得少于/是分析。仪器自动计算得到不完善粒含无是结果均需从仪器上读取，以质量分数（%）表示，在重复性条件下，两次独测定结果保留位数和精密度要求均与/。是终输出的数据应为质量格通过对粮食和油料产品和花生缺少筛层孔径规附录A中增加油菜籽和产区的意见确定油菜籽生上层筛层孔径为12.0参照GB/T6379.2-2004《测试方法与结果的准确度（表26质量控制样品样品编号样品名称小样杂质含量（%）无机杂质含量（%）不完善粒含量（%）QC202401硬质白小麦QC202402软质红小麦QC202403黄玉米0.6/6.0QC202404粳米0.100.024.0QC202405籼米0.100.024.0QC202406粳稻0.5谷外糙米含量：2.5%QC202407籼稻0.5谷外糙米含量：2.5%表27验证用样品含量水平序号样品编号样品名称小样杂质含量（%）无机杂质含量不完善粒含量1XM-1硬质白小麦0.2-0.40.10-0.252.0-3.02XM-2硬质白小麦0.5-0.70.25-0.455.0-8.03XM-3硬质白小麦0.8-1.20.45-0.559.0-12.04XM-4软质红小麦0.2-0.40.10-0.252.0-3.05XM-5软质红小麦0.8-1.20.45-0.557.0-9.06YM-1黄玉米0.2-0.4/3.0-5.07YM-2黄玉米0.5-0.7/6.0-10.08YM-3黄玉米0.8-1.2/11.0-18.09DM-1粳米0.05-0.150.010-0.0250.5-1.5DM-2粳米0.15-0.250.020-0.0354.0-7.0DM-3籼米0.05-0.150.01-0.021.0-4.0DM-4籼米0.15-0.250.02-0.044.0-7.0DG-1粳稻0.2-0.4谷外糙米含量：1.0%-3.0%DG-2粳稻0.4-0.7谷外糙米含量：4.0%-8.0%DG-3籼稻0.2-0.4谷外糙米含量：1.0%-3.0%DG-4籼稻0.4-0.7谷外糙米含量：4.0%-8.0%表28各机构杂质含量测定结果（第一法感官检验法）机XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4水平j12345678910.350.590.300.980.320.600.940.200.080.200.300.640.200.560.310.590.990.290.960.300.600.210.080.200.260.620.280.560.210.630.280.300.600.940.210.040.200.5620.380.600.280.940.340.590.010.260.500.300.580.340.580.280.960.300.620.990.210.300.640.280.580.320.580.280.980.310.590.900.340.630.280.6230.360.600.300.330.680.240.280.360.360.820.300.600.280.920.300.650.990.260.060.240.320.580.440.720.360.620.300.300.610.220.080.220.280.360.420.8240.360.620.280.340.630.000.580.280.580.300.580.280.940.290.680.580.280.560.340.640.300.980.290.610.900.200.300.570.300.5650.360.620.240.300.560.950.060.540.320.580.320.580.300.900.300.530.9080.280.480.360.620.280.940.220.520.900.020.510.280.5460.380.620.380.340.600.360.570.300.560.300.580.320.980.310.630.080.240.530.300.560.360.640.300.940.310.630.900.240.550.280.5270.320.590.310.270.600.200.080.220.300.610.300.630.320.610.990.350.300.550.080.670.250.600.290.570.290.980.300.580.980.290.510.270.59表29第一法感官检验法测定杂质含量重复性和再现性分析项目硬质白小麦软质红小麦黄玉米粳米籼米粳稻籼稻XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4参与实验室的数量7777777777777777排除异常值后实验室数量7777777777777766杂质含量平均值/%0.330.600.300.980.300.600.910.280.560.280.57重复性标准偏差，sr/%0.03940.02280.03910.02380.04250.02520.01720.03400.02120.01600.00910.01430.04850.06540.02490.0263重复性限，r（2.8×sr）/%0.11020.06370.10950.06660.11900.07050.04800.09530.05940.04470.02550.04010.13570.18300.06960.0736再现性标准偏差，SR/%0.03890.02130.04170.02890.04020.02640.03750.04260.02390.02730.01550.02120.04300.08530.03280.0351再现性限，R（2.8×SR）/%0.10890.05970.11670.08090.11260.07380.10490.11930.06690.07660.04340.05920.12030.23880.09200.0982图10重复性限r、再现性限R与杂质含量平均值的关系（第一法）对表29的数据进行分析，显示使用第一法测定杂质含量的重复性限r的范围为0.0255%-0.183%，且重复性限r与杂质含量的相关系表示显著的依赖关系。米类杂质重复性限r的范围为0.0091%-0.0212%，符合在重复性条件下，获得的两次独立测试结果的绝对差值不表30各机构杂质含量测定结果（第二法仪器检验法）机XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4水平j12345678910.370.430.920.280.650.130.390.720.010.590.810.590.640.470.490.990.670.230.440.730.260.080.220.510.660.510.970.390.400.990.150.710.190.390.670.190.540.650.540.6220.480.600.290.570.160.310.530.360.510.330.600.980.320.630.080.180.070.190.350.580.340.530.300.690.290.660.080.260.430.070.090.160.320.670.380.5930.290.580.180.400.700.050.250.470.350.650.340.620.190.980.400.650.240.390.550.400.650.370.700.180.920.320.590.490.330.6240.350.770.940.350.830.310.73////0.250.480.260.520.300.640.430.300.72////0.380.540.250.440.480.600.990.300.290.70////0.320.490.270.4050.440.480.300.840.160.470.720.010.210.570.560.510.960.320.790.220.510.690.070.130.590.220.430.330.600.320.820.190.480.760.050.160.000.190.4960.650.520.710.922.390.230.400.570.020.070.030.030.170.080.600.320.680.200.500.620.020.090.030.060.310.540.170.450.780.100.060.010.070.1770.350.640.320.910.330.650.920.240.550.310.550.880.240.270.560.660.310.590.270.590.950.340.310.580.940.080.310.520.310.66表31第二法仪器检验法测定杂质含量重复性和再现性分析项目硬质白小麦软质红小麦黄玉米粳米籼米粳稻籼稻XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4参与实验室的数量7777777766667777排除异常值后实验室数量6766677765657677杂质含量平均值/%0.370.550.270.860.240.510.810.090.200.080.200.310.580.300.54重复性标准偏差，sr/%0.07880.07240.07370.04770.10180.03410.03670.05620.04790.03420.02770.02940.04810.06420.03290.1285重复性限，r（2.8×sr）/%0.22060.20270.20620.13360.28490.09540.10270.15730.13410.09570.07760.08230.13450.17990.09210.3597再现性标准偏差，SR/%0.08050.12300.09570.08100.19840.09650.16080.25840.05280.03980.04530.03630.13950.09200.13910.1746再现性限，R（2.8×SR）/%0.22540.34430.26800.22680.55540.27030.45020.72360.14780.11160.12690.10160.39050.25770.38950.4889图11重复性限r、再现性限R与杂质含量平均值的关系（第二法）对表31的数据进行分析，显示使用第二法测定杂质含量的重的依赖关系。米类杂质重复性限r的范围为0.0776%-0.1341%，很难符合在重复性条件下，获得的两次独立测试结果的绝对差值不大于表32第一法和第二法杂质含量测定结果分析序号第一法测定结果Xi第二法测定结果Xj差值d差值的标准偏差tdt0.05,1510.330.370.0440.0582.0612.13120.600.55-0.0483-0.00940.300.27-0.02250.980.86-0.12060.300.24-0.06770.600.51-0.09580.980.81-0.17090.09-0.0190.210.20-0.0070.100.08-0.0110.210.20-0.0010.280.310.0230.560.580.0230.280.300.0270.570.54-0.028平均值0.460.43-0.03///////F=S12/S22=1.23，在显著性水平α=0.051/F0.975（15，15）=0.349，判断：由于0.34此，两方法测定结果的标准差不存在显著性差异，即图12第一法与第二法测定杂质含量重复性限r比较图13第一法与第二法测定杂质含量再现性限R比较质限量的粮食，每高0.3个百分点，扣量0.3%；实际杂质含量低于标准规定杂质c.第一法感官检验法与第二法仪器检验法结果一致一定条件。但仍然三个难题不易解决：①轻型杂含量的测定，有的仪器在设计时会将轻型杂质吹表33各机构不完善粒含量测定结果（第一法感官检验法）机构iXM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4水平j12345678913.095.589.442.747.744.208.406.502.955.682.955.539.632.897.664.258.016.302.986.203.055.979.713.107.684.288.356.182.885.7223.416.089.752.867.444.257.766.343.455.936.039.822.267.934.497.646.302.995.873.376.469.792.667.564.307.966.802.905.7932.896.009.472.767.244.317.896.043.875.803.055.709.573.007.394.557.506.263.705.862.965.739.442.727.384.977.976.213.855.7443.015.949.442.767.403.838.176.033.066.012.955.849.522.487.583.938.066.002.925.942.905.909.962.637.943.637.766.012.875.9453.355.579.792.767.623.908.015.882.735.963.275.649.712.847.743.928.465.692.815.703.016.002.927.783.907.895.762.585.7863.943.417.636.533.906.933.866.173.027.573.427.306.443.816.754.236.743.178.083.477.656.803.826.5373.006.019.982.957.834.218.035.993.276.253.026.039.972.987.954.018.016.003.016.033.015.972.997.923.777.986.002.875.86表34第一法感官检验法测定不完善粒含量重复性和再现性分析项目硬质白小麦软质红小麦黄玉米粳米籼米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4参与实验室的数量777777777777排除异常值后实验室数量666777767776不完善粒含量平均值/%3.085.899.742.847.674.057.99重复性标准偏差，sr/%0.10960.18150.18850.16110.18410.17020.21070.28020.09150.15220.15310.1580重复性限，0.30700.50810.52790.45090.51540.47640.59000.78460.25610.42630.42870.4425再现性标准偏差，SR/%0.16860.23750.25110.22360.22790.41320.29770.34150.22340.31470.46240.1602再现性限，0.47220.66490.70320.62600.63801.15690.83370.95630.62560.88121.29480.4485图14重复性限r、再现性限R与不完善粒含量平均值的关系（第一法）对表34的数据进行分析，显示使用第一法测定不完善粒含量的重复性限r，小麦的范围为0.3070%-0.5279%；玉米的范围为表35各机构不完善粒含量测定结果（第二法仪器检验法）机构iXM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4水平j12345678913.337.635.108.906.322.805.482.495.799.312.257.393.847.976.283.066.252.715.467.598.406.272.955.8623.956.442.367.924.007.056.382.835.553.455.902.297.494.357.356.072.965.473.497.289.622.818.275.588.646.022.775.4733.106.327.255.913.066.673.326.415.883.035.933.226.083.158.323.607.245.702.975.9643.636.189.723.387.394.287.31////3.516.029.813.257.374.417.36////3.466.399.643.587.104.277.59////53.243.018.404.547.706.305.529.583.247.904.348.080.986.163.085.963.224.887.715.922.826.2863.646.253.367.315.419.756.202.785.213.422.867.583.565.909.936.042.715.493.976.243.428.402.514.526.512.725.1072.926.259.983.017.943.828.235.982.965.895.999.722.927.817.706.152.936.153.025.772.947.963.958.016.083.045.99表36第二法仪器检验法测定不完善粒含量重复性和再现性分析项目硬质白小麦软质红小麦黄玉米粳米籼米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4参与实验室的数量777777776666排除异常值后实验室数量777776666666不完善粒含量平均值/%3.306.139.972.957.834.227.722.925.83重复性标准偏差，sr/%0.23800.35280.32020.21720.29080.45520.46580.39310.09070.16160.10380.2611重复性限，r（2.8×sr）/%0.66650.98790.89660.60830.81421.27471.30421.10070.25400.45250.29070.7311再现性标准偏差，SR/%0.36910.37240.49260.44800.41650.57870.62970.66670.21590.21190.14090.4263再现性限，R（2.8×SR）/%1.03361.04281.37921.25431.16611.62031.76311.86690.60440.59330.39441.1938图15重复性限r、再现性限R与不完善粒含量平均值的关系（第二法）表38第二法各机构不完善粒含量测定结果极差（%）机构仪器品牌硬质白小麦软质红小麦黄玉米粳米籼米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4机构10.900.740.190.660.240.930.780.250.050.260.77机构20.500.520.780.390.180.360.190.08机构30.300.200.060.270.840.020.210.090.74机构40.170.370.170.330.290.280.30////机构50.060.650.470.230.500.540.380.660.180.400.340.32机构60.550.560.560.190.470.070.39机构70.190.480.550.090.150.290.530.66图16小麦不完善粒含量测定极差图17玉米不完善粒含量测定极差图18大米不完善粒含量测定极差表39第二法仪器检验法测定不完善粒含量重复性和再现性分析（去除明显异常）项目硬质白小麦软质红小麦黄玉米粳米籼米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4参与实验室的数量777777776666排除异常值后实验室数量555555566664不完善粒含量平均值/%3.176.039.802.997.837.722.925.73重复性标准偏差，sr/%0.22040.27720.18600.17670.15300.33310.34290.39310.09070.16160.10380.1465重复性限，r（2.8×sr）/%0.61700.77600.52090.49480.42840.93270.96021.10070.25400.45250.29070.4103再现性标准偏差，SR/%0.31250.28220.41130.44910.43490.51180.62080.66670.21590.21190.14090.4294再现性限，R（2.8×SR）/%0.87490.79031.15170.25760.21761.43301.73811.86690.60440.59330.39441.2022粒含量的相关系数R2为0.4183，表示小麦的范围为0.2176%-0.8749%；玉米的表40第一法和第二法不完善粒含量测定结果分析序号第一法测定结果Xi第二法测定结果Xj差值d差值的标准偏差tdt0.05,1113.083.300.2260.2800.2022.20125.896.130.24239.749.970.22842.842.9557.677.830.16164.054.220.17777.937.72-0.2138-0.7119-0.0036.19-0.0723.202.92-0.2775.895.83-0.066平均值6.066.04-0.02/// ∑(Xi/j-X)2152.73////表A.5.3得到F1-α/2（v1，v2）=F0.975（1