糧油檢驗 糧食、油料的雜質、不完善粒檢驗編制說明

2《糧油檢驗糧食、油料的雜質、不完善粒檢驗》編制說明根據(jù)國家標準化管理委員會《關于下達2023年第一批推薦性國家標準計劃質量監(jiān)督檢測中心、河南省食品和鹽業(yè)檢驗技術研究院（河南省糧油飼料產(chǎn)品質量監(jiān)督檢驗中心）、深圳市計量質量檢測研究院、中儲糧質檢有限公司、邇言(上海）科技有限公司、北京中檢葆泰生物技術有限公司、中儲糧成都儲藏研3用人工智能的糧食AI識別系統(tǒng)，學習完善數(shù)據(jù)庫，準確率、重復性、穩(wěn)定性和霉變粒、損傷粒、雜質等指標數(shù)智化檢測，在圖像識別、模型建立和AI智能學4圖1糙米未熟粒圖2糙米病斑粒圖3糙米生芽粒圖4玉米生霉粒圖5玉米熱損傷粒圖6玉米蟲蝕粒圖7玉米雙面掃描圖片家糧食和物資儲備局辦公室關于下達2020通知》，由北京東孚久恒儀器技術有限公司牽頭制定《52023年6月-2023年12月，標準并形成標準文本及編制說明征求意見稿。2024年3月，召開起草組第一次研討分析，對文本提出修改意見和建議，并協(xié)助起草單6效降低人工勞動強度、提高效率，從而提高糧食基層檢驗情況，本次修訂增加了不完善粒子項的計算公式，7），出黍粒；稷米揀出稷粒；高粱米揀出高粱殼善粒檢驗試樣質量（m5’米類小樣用量與其原糧相同）”，修8糙米并稱量（m5精確至0.01g?！钡臋z測程序，將大樣雜質含量（u1）錄入儀器，啟動儀器進行圖像采集和圖像分析。儀器自動計算得到不完善粒含量、谷外果的平均數(shù)，即為測試結果，以質量分數(shù)（%）表示，結果保留小數(shù)點后一位。本次修訂增加了不完善粒子項的計算公式，東、海南等主產(chǎn)區(qū)的意見確定油菜籽篩層孔徑為1.0mm；花生上層篩層孔徑為9表1原始數(shù)據(jù)：糧食的大樣雜質含量人員i小麥-1小麥-2小麥-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糧食大樣雜質含量實驗結果分析（%）實驗員1實驗員2實驗員3實驗員4實驗員5實驗員6平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)736216012350475830878290446708234890592370444712271557671272137068471452435117954602566365321772871774227948102703492656673074746不應超過3次測定重復性臨界極差，即極差表3對單元平均值的格拉布斯檢驗水平單個低值單個高值兩個低值兩個高值檢驗類型10.5250.200格拉布斯檢驗統(tǒng)計量20.1620.56830.48040.2250.47450.1500.38760.8090.1340.54070.7890.2740.32680.2170.52490.2960.2840.2090.3270.0830.5120.3270.359岐離值0.03490.0349格拉布斯檢驗臨界值0.01160.0116表4糧食大樣雜質含量的mj,srj,sRj計算值（%）水平jmj回收率2.8*Srj2.8*SRj10.550.05260.06350.14720.177920.08220.09350.23020.261832.060.10460.11490.29290.321640.610.05860.07710.16410.215850.07370.09870.20630.2763690.50.09830.11100.27520.310970.550.05610.07500.15720.210080.08010.09400.22440.2632990.00.09360.11390.26190.31910.520.05680.07490.15910.20970.08280.09860.23170.27622.030.09820.11040.27490.3092參與的一致水平試驗獲得重復性標準差srj=0.056，再現(xiàn)性標準差SRj=0.073；mj水平時，重復性標準差srj=0.099，再現(xiàn)性標準差SRj=0.113?，F(xiàn)行標準GB/T試結果絕對差值不大于0.3%。本次試驗中，大樣雜質含量在較高水平，即性標準差2.8SRj=2.8×0.113＝0.31≈0表5小樣雜質含量人員i小麥-1小麥-2小麥-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糧食小樣雜質含量實驗結果分析（%）實驗員1實驗員2實驗員3實驗員4實驗員5實驗員6平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)表7對單元平均值的格拉布斯檢驗水平單個低值單個高值兩個低值兩個高值檢驗類型10.2780.339格拉布斯檢驗統(tǒng)計量20.5410.06130.3410.25540.1960.39750.4990.3080.39860.3230.28270.4290.22280.2970.29190.4040.2790.5300.2410.5700.0830.5650.060岐離值0.03490.0349格拉布斯檢驗臨界值0.01160.0116表8糧食大樣雜質含量的mj,srj,sRj計算值（%）水平jmj回收率2.8*Srj2.8*SRj10.520.05990.06690.16770.187420.07570.10520.21210.2947396.50.11180.11250.31310.315140.4080.00.05200.08300.14570.232550.9292.00.06530.07480.18280.2094697.00.10360.10630.29000.297670.4182.00.07670.07770.21480.217680.8989.00.07750.08640.21710.2420991.50.10330.28930.31480.610.08710.09150.24370.25630.08940.10030.25020.280989.00.10540.11090.29500.3106參與的一致水平試驗獲得重復性標準差srj=0.069，再現(xiàn)性標準差SRj=0.080；mj水平時，重復性標準差srj=0.106，再現(xiàn)性標準差SRj=0.110?，F(xiàn)行標準GB/T試結果絕對差值不大于0.3%。本次試驗中，小樣雜質含量在較高水平，即一致。大樣雜質含量和小樣雜質含量小于2.0%時方法的重復性符合GB/T量國家標準有關問題的規(guī)定》中要求原糧雜質含量的允許偏差要求為不大于對小麥、玉米樣品的不完善粒含量進行測定，從準確度和表9原始數(shù)據(jù)：糧食的不完善粒含量（%）人員i小麥-1小麥-2小麥-3小麥-4小麥-5小麥-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糧食不完善粒含量實驗結果分析（%）實驗員1實驗員2實驗員3實驗員4實驗員5實驗員6平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)平均值極差標準差變異系數(shù)）；）；表11對單元平均值的格拉布斯檢驗水平單個低值單個高值兩個低值兩個高值檢驗類型10.3190.358格拉布斯檢驗統(tǒng)計量20.5570.08130.4350.18140.1430.48150.1150.48760.4060.19270.3300.23180.2310.31590.3560.2330.3670.2430.3060.3490.3360.238岐離值0.03490.0349格拉布斯檢驗臨界值0.01160.0116表12糧食不完善粒含量的mj,srj,sRj計算值（%）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圖8中粒糧的重復性和再現(xiàn)性圖圖9大粒糧的重復性和再現(xiàn)性性限R存在相關性，進一步分析見圖8和圖9，相關系數(shù)大于0.9。a.對于中粒糧，通過y=0.0292x+0.2806可以計算出重復性要求不高于0.5%時，對應的不完善粒含量為7.5%，即大于8.0%時應考慮調整精密度要求。例如5等和等外小麥要考慮調整精密度要求。通過對我國中小粒糧中總產(chǎn)量排名第一的小麥質量等級情況分析，不完善粒含量為再疊加分樣誤差，將5等和等外小麥不完善粒的兩次獨立測試結果的絕大于0.5當不完善?？偭浚?.0%時，在重復性條件下，獲得的兩次b.對于大粒糧，通過y=0.0803x+0.2555可以計算出重復性要求不高于要求。例如5等和等外玉米要考慮調整精密度要求。通過對我國大粒、特大粒糧中總產(chǎn)量排名第一的玉米質量等級情況再疊加分樣誤差，將5等和等外玉米不完善粒的兩次獨立測試結果的絕不完善?？偭俊?0.0%時，在重復性條件下，獲得的兩次獨立測試結果在實驗室內(nèi)使用品牌1不完善粒測定儀儀器檢驗法分別對糧食不完善粒含間是否存在顯著性差異，小麥和玉米測定結果計算出統(tǒng)計量|t|<t0.05(p<0.05，兩種測定方法無顯著性差異。采用x2檢驗進行標準差檢驗，按照現(xiàn)行國標GB/T5494-2019中規(guī)定的不完善粒含量重復性要求計算得出小麥和玉米的平的小麥測定結果計算統(tǒng)計量x2<x20.95(2)=5.99，極差<CrR95(3)=0.594，說明小麥測定結果均符合現(xiàn)行國標GB/T5494-2019中的重復性要求。不完善粒含量量x2<x20.95(2)=5.99，極差>CrR95(3)=1.188說明當玉米不完善粒含量小于8%時，測定結果均符合現(xiàn)行國標GB/T5494-2019中的重復性要求，但當玉米不完善粒含量大于8%時，測定結果不再符合現(xiàn)行國標GB/T5494-2019中的重復性要求。表13實驗室內(nèi)小麥儀器檢驗法不完善粒含量測定結果樣品測定次數(shù)感官分析測定結果(%)儀器檢驗法測定結果(%)儀器檢驗法測定平均值(%)標準偏tt0.05(2)x2x20.95(2)差(%)CrR95(3)小麥麥110.22-2.944.3032.8815.990.50.59423麥0.160.422.632.8麥315.86.06.00.21-1.692.6060.526.335.8麥40.212.6060.528.038.5麥510.19-3.982.1950.423麥6121.120.821.00.170.4221.2320.9表14實驗室內(nèi)玉米儀器檢驗法不完善粒含量測定結果樣品測定次數(shù)工測定結果(%)儀器測定結果(%)儀器測定平均值(%)標準偏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器檢測，將檢測結果與定值進行配對T檢驗，考察兩組結果是否存在顯著性差表15小麥不完善粒準確性測試數(shù)據(jù)編號人工測定結果(%)儀器測定結果(%)差值di均值d標準偏差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玉米不完善粒準確性數(shù)據(jù)分析表編號人工測定結果(%)儀器測定結果(%)差值di均值d標準偏差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準方法中規(guī)定的重復性要求，同時采用6次測定極差與現(xiàn)有國家標準（GB/T6379.6-2009）規(guī)定的6次測定重復性臨界極差進行對照，考察表17低值樣重復性分析表測定次數(shù)不完善粒（%）平均值標準偏差sx2x20.95（5）極差12.642.6011.07050.2822.4232.742.6652.6462.52表18中值樣重復性分析表測定次數(shù)不完善粒（%）平均值標準偏差sx2x20.95（5）極差19.3411.07050.5529.3038.9149.0959.4669.31表19高值樣重復性分析表測定次數(shù)不完善粒（%）平均值標準偏差sx2x20.95（5）極差10.238.6011.07050.6323456三個水平不完善粒含量的x2計算值均不超過查表值，極差也均不超過重復a.決定修改感官檢驗法的精密度要求，對于中小粒糧食、油料，當不完善值不大于0.5當不完善?？偭浚?.0%時，在重復性條件下，獲得的測試結果保留到小數(shù)點后一位。對于大粒、特大粒糧食、油料，當不完善?？偭俊?0.0%時，在重復性條件下，獲得的兩次獨立測試結果的絕％；b.第二法儀器檢驗法重復性與第一法感官檢驗法要求一致。得的兩次獨立測試結果的絕對差值不大于0.5％，求其平均數(shù)，即為表20原始數(shù)據(jù)：稻谷的谷外糙米含量人員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實驗結果分析（%）人員i結果分析DG-1DG-2DG-3DG-4DG-5DG-6水平j1234561平均值66.49極差0.130.470.360.520.790.73標準差0.040.360.32變異系數(shù)5.104.755.667.594.952平均值0.842.603.914.996.95極差0.460.490.470.460.65標準差90.210.460.30變異系數(shù)22.307.435.279.224.383平均值3.283.795.176.88極差0.500.530.320.61標準差0.210.070.26變異系數(shù)2.426.643.923.844平均值3.023.925.566.92極差0.320.330.360.290.670.78標準差70.32變異系數(shù)7.274.913.044.924.615平均值0.952.954.154.966.48極差40.390.650.60標準差0.090.070.25變異系數(shù)9.476.263.895.463.796平均值0.852.893.804.596.87極差0.280.350.360.430.690.57標準差80.310.23變異系數(shù)8.065.214.766.723.39同一人員3次測定結果極差在0.57%-0.72%之間。按照稻谷谷外糙米含量重復復性臨界極差，即極差<CrR95(3)=0.589。說明當?shù)竟裙韧獠诿缀克叫∮?.0%時，測定結果均符合在重復性條件下兩次獨立測試結果的絕0.38%、0.98%、0.47%。不同人員測定稻谷谷外糙米含量的標準差在0.045-0.572之間，變異系數(shù)在2.412=0.481表22對單元平均值的格拉布斯檢驗水平單個低值單個高值兩個低值兩個高值檢驗類型10.3760.174格拉布斯檢驗統(tǒng)計量20.1670.45630.2450.34840.4430.09950.9940.31460.9250.018*0.630岐離值0.03490.0349格拉布斯檢驗臨界值0.01160.0116表23稻谷谷外糙米含量的mj,Srj,SRj計算值（%）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因此本次文本修訂確定稻谷谷外糙米含量方法精密度為：當谷外糙米含量≤其平均數(shù)，即為測試結果，測試結果保留到小數(shù)點后一位；當谷外糙米含量＞其平均數(shù)，即為測試結果，測試結果保留到小數(shù)表24谷外糙米含量準確性數(shù)據(jù)分析表編號人工測定結果儀器測定結果差值di均值d標準偏差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.修改感官檢驗法的精密度要求當谷外糙米含量≤4.b.儀器檢驗法可以用于測定稻谷中的谷外糙米含量。表25技術內(nèi)容的對比1/是儀器檢驗法融入標準文2是不完善粒含量和稻谷中谷外糙米含量將適用于谷外糙米含量3食、油料檢驗油檢驗感官檢是增加了4個文件：GB/T5490糧油檢驗一般規(guī)則、GB/T36091糧油機械檢驗4義是增加了6項術語定義：圖像采集、圖像質質的內(nèi)容提取出來總結5是6是7否），8是修改了不完善粒含量精密度要求。結果的絕對差值：大粒、特大粒糧食、油料當不完善粒子項含量≤10.0%時，不大于1.0當不完善粒子項含量＞料當不完善粒子項含量≤8.0%時，不大于0.5％；當不完善粒子項含量＞精密度要求：當谷外糙米含量≤4.0%時，在重復性條件下獲得的兩次獨立測試結果的絕對差值不大于0.5%;當谷外糙米含量＞4.0%時，在重復性條件下獲得的兩次獨立測試結果/9無是在第二法儀器檢驗法中增加了原理：采用相機或掃描儀等圖像采集裝置采谷外糙米含量和不完善粒含量質量分“糧食和油料容是按照第一法7.1.3進行大樣雜質檢驗，檢驗結果計算和重復性要求同第一法8.1.1。從檢驗過大樣雜質的試樣中縮注：不完善粒檢驗試樣質量不得少于/是分析。儀器自動計算得到不完善粒含無是結果均需從儀器上讀取，以質量分數(shù)（%）表示，在重復性條件下，兩次獨測定結果保留位數(shù)和精密度要求均與/。是終輸出的數(shù)據(jù)應為質量格通過對糧食和油料產(chǎn)品和花生缺少篩層孔徑規(guī)附錄A中增加油菜籽和產(chǎn)區(qū)的意見確定油菜籽生上層篩層孔徑為12.0參照GB/T6379.2-2004《測試方法與結果的準確度（表26質量控制樣品樣品編號樣品名稱小樣雜質含量（%）無機雜質含量（%）不完善粒含量（%）QC202401硬質白小麥QC202402軟質紅小麥QC202403黃玉米0.6/6.0QC202404粳米0.100.024.0QC202405秈米0.100.024.0QC202406粳稻0.5谷外糙米含量：2.5%QC202407秈稻0.5谷外糙米含量：2.5%表27驗證用樣品含量水平序號樣品編號樣品名稱小樣雜質含量（%）無機雜質含量不完善粒含量1XM-1硬質白小麥0.2-0.40.10-0.252.0-3.02XM-2硬質白小麥0.5-0.70.25-0.455.0-8.03XM-3硬質白小麥0.8-1.20.45-0.559.0-12.04XM-4軟質紅小麥0.2-0.40.10-0.252.0-3.05XM-5軟質紅小麥0.8-1.20.45-0.557.0-9.06YM-1黃玉米0.2-0.4/3.0-5.07YM-2黃玉米0.5-0.7/6.0-10.08YM-3黃玉米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秈米0.05-0.150.01-0.021.0-4.0DM-4秈米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秈稻0.2-0.4谷外糙米含量：1.0%-3.0%DG-4秈稻0.4-0.7谷外糙米含量：4.0%-8.0%表28各機構雜質含量測定結果（第一法感官檢驗法）機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第一法感官檢驗法測定雜質含量重復性和再現(xiàn)性分析項目硬質白小麥軟質紅小麥黃玉米粳米秈米粳稻秈稻XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4參與實驗室的數(shù)量7777777777777777排除異常值后實驗室數(shù)量7777777777777766雜質含量平均值/%0.330.600.300.980.300.600.910.280.560.280.57重復性標準偏差，sr/%0.03940.02280.03910.02380.04250.02520.01720.03400.02120.01600.00910.01430.04850.06540.02490.0263重復性限，r（2.8×sr）/%0.11020.06370.10950.06660.11900.07050.04800.09530.05940.04470.02550.04010.13570.18300.06960.0736再現(xiàn)性標準偏差，SR/%0.03890.02130.04170.02890.04020.02640.03750.04260.02390.02730.01550.02120.04300.08530.03280.0351再現(xiàn)性限，R（2.8×SR）/%0.10890.05970.11670.08090.11260.07380.10490.11930.06690.07660.04340.05920.12030.23880.09200.0982圖10重復性限r(nóng)、再現(xiàn)性限R與雜質含量平均值的關系（第一法）對表29的數(shù)據(jù)進行分析，顯示使用第一法測定雜質含量的重復性限r(nóng)的范圍為0.0255%-0.183%，且重復性限r(nóng)與雜質含量的相關系表示顯著的依賴關系。米類雜質重復性限r(nóng)的范圍為0.0091%-0.0212%，符合在重復性條件下，獲得的兩次獨立測試結果的絕對差值不表30各機構雜質含量測定結果（第二法儀器檢驗法）機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第二法儀器檢驗法測定雜質含量重復性和再現(xiàn)性分析項目硬質白小麥軟質紅小麥黃玉米粳米秈米粳稻秈稻XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4DG-1DG-2DG-3DG-4參與實驗室的數(shù)量7777777766667777排除異常值后實驗室數(shù)量6766677765657677雜質含量平均值/%0.370.550.270.860.240.510.810.090.200.080.200.310.580.300.54重復性標準偏差，sr/%0.07880.07240.07370.04770.10180.03410.03670.05620.04790.03420.02770.02940.04810.06420.03290.1285重復性限，r（2.8×sr）/%0.22060.20270.20620.13360.28490.09540.10270.15730.13410.09570.07760.08230.13450.17990.09210.3597再現(xiàn)性標準偏差，SR/%0.08050.12300.09570.08100.19840.09650.16080.25840.05280.03980.04530.03630.13950.09200.13910.1746再現(xiàn)性限，R（2.8×SR）/%0.22540.34430.26800.22680.55540.27030.45020.72360.14780.11160.12690.10160.39050.25770.38950.4889圖11重復性限r(nóng)、再現(xiàn)性限R與雜質含量平均值的關系（第二法）對表31的數(shù)據(jù)進行分析，顯示使用第二法測定雜質含量的重的依賴關系。米類雜質重復性限r(nóng)的范圍為0.0776%-0.1341%，很難符合在重復性條件下，獲得的兩次獨立測試結果的絕對差值不大于表32第一法和第二法雜質含量測定結果分析序號第一法測定結果Xi第二法測定結果Xj差值d差值的標準偏差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，在顯著性水平α=0.051/F0.975（15，15）=0.349，判斷：由于0.34此，兩方法測定結果的標準差不存在顯著性差異，即圖12第一法與第二法測定雜質含量重復性限r(nóng)比較圖13第一法與第二法測定雜質含量再現(xiàn)性限R比較質限量的糧食，每高0.3個百分點，扣量0.3%；實際雜質含量低于標準規(guī)定雜質c.第一法感官檢驗法與第二法儀器檢驗法結果一致一定條件。但仍然三個難題不易解決：①輕型雜含量的測定，有的儀器在設計時會將輕型雜質吹表33各機構不完善粒含量測定結果（第一法感官檢驗法）機構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第一法感官檢驗法測定不完善粒含量重復性和再現(xiàn)性分析項目硬質白小麥軟質紅小麥黃玉米粳米秈米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4參與實驗室的數(shù)量777777777777排除異常值后實驗室數(shù)量666777767776不完善粒含量平均值/%3.085.899.742.847.674.057.99重復性標準偏差，sr/%0.10960.18150.18850.16110.18410.17020.21070.28020.09150.15220.15310.1580重復性限，0.30700.50810.52790.45090.51540.47640.59000.78460.25610.42630.42870.4425再現(xiàn)性標準偏差，SR/%0.16860.23750.25110.22360.22790.41320.29770.34150.22340.31470.46240.1602再現(xiàn)性限，0.47220.66490.70320.62600.63801.15690.83370.95630.62560.88121.29480.4485圖14重復性限r(nóng)、再現(xiàn)性限R與不完善粒含量平均值的關系（第一法）對表34的數(shù)據(jù)進行分析，顯示使用第一法測定不完善粒含量的重復性限r(nóng)，小麥的范圍為0.3070%-0.5279%；玉米的范圍為表35各機構不完善粒含量測定結果（第二法儀器檢驗法）機構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第二法儀器檢驗法測定不完善粒含量重復性和再現(xiàn)性分析項目硬質白小麥軟質紅小麥黃玉米粳米秈米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4參與實驗室的數(shù)量777777776666排除異常值后實驗室數(shù)量777776666666不完善粒含量平均值/%3.306.139.972.957.834.227.722.925.83重復性標準偏差，sr/%0.23800.35280.32020.21720.29080.45520.46580.39310.09070.16160.10380.2611重復性限，r（2.8×sr）/%0.66650.98790.89660.60830.81421.27471.30421.10070.25400.45250.29070.7311再現(xiàn)性標準偏差，SR/%0.36910.37240.49260.44800.41650.57870.62970.66670.21590.21190.14090.4263再現(xiàn)性限，R（2.8×SR）/%1.03361.04281.37921.25431.16611.62031.76311.86690.60440.59330.39441.1938圖15重復性限r(nóng)、再現(xiàn)性限R與不完善粒含量平均值的關系（第二法）表38第二法各機構不完善粒含量測定結果極差（%）機構儀器品牌硬質白小麥軟質紅小麥黃玉米粳米秈米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4機構10.900.740.190.660.240.930.780.250.050.260.77機構20.500.520.780.390.180.360.190.08機構30.300.200.060.270.840.020.210.090.74機構40.170.370.170.330.290.280.30////機構50.060.650.470.230.500.540.380.660.180.400.340.32機構60.550.560.560.190.470.070.39機構70.190.480.550.090.150.290.530.66圖16小麥不完善粒含量測定極差圖17玉米不完善粒含量測定極差圖18大米不完善粒含量測定極差表39第二法儀器檢驗法測定不完善粒含量重復性和再現(xiàn)性分析（去除明顯異常）項目硬質白小麥軟質紅小麥黃玉米粳米秈米XM-1XM-2XM-3XM-4XM-5YM-1YM-2YM-3DM-1DM-2DM-3DM-4參與實驗室的數(shù)量777777776666排除異常值后實驗室數(shù)量555555566664不完善粒含量平均值/%3.176.039.802.997.837.722.925.73重復性標準偏差，sr/%0.22040.27720.18600.17670.15300.33310.34290.39310.09070.16160.10380.1465重復性限，r（2.8×sr）/%0.61700.77600.52090.49480.42840.93270.96021.10070.25400.45250.29070.4103再現(xiàn)性標準偏差，SR/%0.31250.28220.41130.44910.43490.51180.62080.66670.21590.21190.14090.4294再現(xiàn)性限，R（2.8×SR）/%0.87490.79031.15170.25760.21761.43301.73811.86690.60440.59330.39441.2022粒含量的相關系數(shù)R2為0.4183，表示小麥的范圍為0.2176%-0.8749%；玉米的表40第一法和第二法不完善粒含量測定結果分析序號第一法測定結果Xi第二法測定結果Xj差值d差值的標準偏差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