原料糖蜜分析操作规程一、取样 每车取一个有代表性的样品 (约500g)作为分析样品二、分析项目1、锤度的测定方法一：密度法1.1 测定方法:将糖蜜试样搅拌均匀后，于工业天平上称取试样200克，再加水800 mL，搅拌均匀后即得5倍稀释糖液（也可用测总糖的样液A测定，此时N=43.333/G样液A）用少许稀释糖液将250 mL量筒内壁冲洗两次，然后再盛满稀释糖液，静止片刻，待内部气泡逸出后，吹除表面泡沫，然后徐徐插入糖锤度计和温度计，待温度计的温度不再上升（约5分钟左右）时，即读取锤度和温度1.2 结果计算密度锤度（%）=N×（Bx+K）式中：N——稀释倍数 Bx——t℃样液的观测锤度，0Bx； K——t℃样液的观测锤度温度校正系数（查表1），0Bx表1：观测锤度温度更正表（20℃）观察糖度／Bx温度／℃1234567应 减05101112131415161718190.340.380.330.320.300.270.240.200.170.130.090.050.380.400.340.330.300.270.240.200.170.130.090.050.410.430.360.330.310.280.240.200.180.140.100.050.450.450.370.340.310.280.250.210.180.140.100.050.490.470.380.350.320.290.260.220.180.140.100.05O。
520.490.390.360.330.300.270.220.180.140.100.050.550.510.400.370.340.300.270.230.190.140.100.05应 加21222324252627282930313233343536373839400.040.100.160.210.270.330.400.460.540.610.690.760.840.910.991.071.151．Z51.341.430.040.100.160.210.270.330.400.460.540.610.690.770.850.921.001.081.161.251.341.430.050.100.160.220.280.340.410.470.550.620.700.770.850.921.001.081.161.261.351.440.050.100.160.220.280.340.410.470.550.620.700.780.850.931.011.091.171.261.351.440.050.100.160.220.280.340.410.470.550.620.700.780.850.931.011.091.171．Z71.361,450.050.100.160.220.280.340.410.470.550.620.700.780.850.931.011.091.171.271.361.450.050.100.160.220.290.350.410.480.550.620.700.780.860.931.011.091.171.281.371.46续表观察糖度／。
Bx温度／℃891011121314应 减05101112131415161718190.590.520.410.380.340.310.280.230.190.150.100.050.620.540.420.390.350.310.280.240.200.150.100.050.650.560.430.400.360.320.290.240.200.150.100.050.670.580.440.410.370.330.290.240.200.150.100.050.700.600.450.420.380.330.300.250.210.160.100.050.720.610.460.420.380.340.300.250.210.160.110.060.750.630.470.430.390.340.310.260.220.160.110.06应 加21222324252627282930313233343536373839400.060.110.170.230.290.350.420.480.560.630.710.790.860.941.021.101.181.291.381.460.060.110.170.230.300.360.420.490.560.630.710.790.860.941.021.101.181.291.381.470.060.110.170.230.300.360.420.490.560.630.710.790.860.941.021.101.181.301.381.470.060.110.170.230.300.360.420.490.570.640.720.800.870.951.031.111.191.311.391.480.060.110.170.230.300.360.430.500.570.640.720.800.880.961.041.121.201.321.401.490.060.120.170.240.310.370.430.500.580.650.730.810.880.961.051.131.211.321.411.500.060.120.170.240.310.370.440.510.580.650.730.810.890.971.051.131.211.331.411.50续表观察糖度／。
Bx温度／℃15161718192021应 减05101112131415161718190.770.650.480.440.400.350.310.260.220.160.110.060.790.670.490.450.410.360.320.260.220.160.110.060.820.680.500.460.410.360.320.270.220.160.110.060.840.700.500.460.420.370.330.270.230.170.120.060.870.710.510.470.420.370.330.280.230.170.120.060.890.730.520.480.430.380.340.280.230.180.120.060.910.740.530.490.440.390.340.280.230.180.120.06应 加21222324252627282930313233343536373839400.060.120.170.240.310.370.440.510.590.660.740.820.900.981.061.141.221.331.421.510.060.120.170.240.310.380.44,0.520.590.660.740.830.910.991.071.151.231.341.431.520.060.120.180.250.310.380.450.520.600.670.750.830.911.001.081.161.241.351.441.530.060.120.180.250.320.390.450.530.600.670.750.840.921.001.081.161.241.351.441.530.060.120.190.260.320.390.460.530.610.680.760.840.921．Ol1.091.171.251.361.451.540.060.120.190.260.320.400.460.540.610.680.760.850.931.021.101.181.261.361.451.540.060.120.190.260.320.400.460.540.610.680.770.850.941.021.111.191.271.371.461.55续表观察糖度／。
Bx温度／℃22232425303540应 减05101112131415161718190.930.750.540.490.440.390.350.290.240.180.120.060.950.760.550.500.450.400.360.290.240.190.130.060.970.770.570.500.450.400.360.300.250.190.130.060.990.800.570.510.460.410.360.300.250.190.130.061.080.860.600.550.500.440.380.320.260.200.130.071.160.910.640.580.520.460.400.330.270.200.140.071.240.970.670.600.540.480.410.340.280.210.140.07应 加212223242526Z7282930313233343536373839400.060.120.190.260.330.400.470.550.620.690.770.860.941.031.111.191.271.371.461.550.070.130.200.270.330.400.470.550.620.690.780.860.951.031.121.201.281.381.471.560.070.130.200.270.340.400.480.560.630.700.780.870.951.041.121.201.281.381.471.560.070.130.200.270.340.400.480.560.630.710.790.870.961.041.131.211.291.391.481.570.070.140.2l0.280．350.420.500.580.660.730.820.900.991.071.161.241.311.421.531.600.070.140.210.290.360.440.520.600.680.760.830.921.001.091.181.261.331.441.531.620.070.150.220.300.380.460.540.610.700.780.850.941.021.111.201.281.351.461.551.64 方法二：折射法（QB/T 2684一2005）甘蔗糖蜜经稀释一定倍数后，在折射仪上测其可溶性固体物质，经温度校正，乘以稀释倍数可得糖蜜的折射锤度。
1.1 仪器、设备1.1.1阿贝折射仪，折射率测量范围1.300-1.700分划板上折射率最小分度值0.001糖量浓度度测量范围(%)0~95 分划板上糖量浓度(%)最小分度值0.51.1.2 温度计，0℃-30℃，刻度0.1℃ 1.2 测定步骤1.2.1 糖蜜样品经充分搅拌后加蒸馏水进行质量稀释3-4倍，或直接用2.4.2样液测定1.2.2 校正_ 用蒸馏水校正仪器，20℃ 时蒸馏水的折射率为1.33299，若温度不在20℃，可查蒸馏水折射率表，调节仪器的示值与该温度对应的折射率相符即可1.2.3 测定 打开折射仪的棱镜，滴加适量的样液于棱镜上，迅速闭合并锁紧待样液达到棱镜温度时，调节光源及读数反射镜，使视场明亮，转动棱镜手轮，使视场中明暗分界线恰在十字线中心，读取样液的折射锤度及测定时的温度1.2.4 计算及结果表示 甘蔗糖蜜的折射锤度按下式计算，数值以%表示，计算结果取到小数点后一位数折射锤度（%）=N×（Bt +K）式中：N——稀释倍数； Bt——t℃糖蜜的折射锤度； K——t℃折射锤度温度校正数（查表2）；表2：折射锤度温度校正数折射锤度/ 0Bx0510152025303540455055606570温度/℃温度低于20℃应减之数100.500.540.580.610.640.660.680.700.720.730.740.750.760.780.79110.460.490.530.550.580.600.620.640.650.660.670.680.690.700.71120.420.450.480.500.520.540.560.570.580.590.600.610.610.6+30.63130.370.400.420.440.460.480.490.500.510.520.530.540.540.550.55140.330.350.370.390.400.410.420.430.440.450.450.460.460.470.48150.270.290.310.330.340.340.350.360.370.370.380.390.390.400.40160.220.240.250.260.270.280.280.290.300.300.300.310.310.320.32170.170.180.190.200.210.210.210.220.220.230.230.230.230.240.24180.120.130.130.140.140.140.140.150.150.150.150.160.160.160.16190.060.060.060.070.070.070.080.080.080.080.080.080.080.080.08温度/℃温度高于20℃应加之数210.060.070.070.070.070.080.080.080.080.080.080.080.080.080.08220.130.130.140.140.150.150.150.150.150.160.160.160.160.160.16230.190.200.210.220.220.230.230.230.230.240.240.240.240.240.24240.260.270.280.290.300.300.310.310.310.310.310.320.320.320.32250.330.350.360.370.380.380.390.400.400.400.400.400.400.400.40260.400.420.430.440.450.460.470.480.480.480.480.480.480.480.48270.480.500.520.530.540.550.550.560.560.560.560.560.560.560.56280.560.570.600.610.620.630.630.640.640.640.640.640.640.640.64290.640.660.680.690.710.720.720.730.730.730.730.730.730.730.73300.700.740.770.780.790.800.800.810.810.810.810.810.810.810.81温度/℃锤 度温度/℃锤 度15202530354015202530354010-0.61-0.64-0.66-0.68-0.70-0.7221+0.07+0.07+0.08+0.08+0.08+0.0811-0.55-0.58-0.60-0.62-0.64-0.6522+0.14+0.15+0.15+0.15+0.15+0.1512-0.50-0.52-0.54-0.56-0.57-0.5823+0.22+0.22+0.23+0.23+0.23+0.2313-0.44-0.46-0.48-0.49-0.50-0.5124+0.29+0.30+0.30+0.31+0.31+0.3114-0.39-0.40-0.41-0.42-0.43-0.4425+0.37+0.38+0.38+0.39+0.40+0.4015-0.33-0.34-0.34-0.35-0.36-0.3726+0.44+0.45+0.46+0.47+0.48+0.4816-0.26-0.27-0.28-0.28-0.29-0.3027+0.53+0.54+0.55+0.55+0.56+0.5617-0.20-0.21-0.21-0.21-0.22-0.2228+0.61+0.62+0.63+0.63+0.64+0.6418-0.14-0.14-0.14-0.14-0.15-0.1529+0.69+0.71+0.72+0.72+0.73+0.7319-0.07-0.07-0.07-0.07-0.08-0.0830+0.78+0.79+0.80+0.80+0.81+0.812、总糖的测定方法一：化学法2.1、原理将一定量的碱性酒石酸铜乙液和甲液等体积混合时，硫酸铜与氢氧化钠反应，生成氢氧化铜沉淀：2NaOH + CuSO4 = Cu(OH)2 + Na2SO4所生成的氢氧化铜沉淀与酒石酸钾钠反应，生成可溶性的酒石酸钾钠铜：COOKCOHHCOHCOONaHCOOKCOHCOCOONaHCu(OH)2+=Cu + 2H2 H2 O 在加热条件下，用样液滴定，样液中的还原糖与酒石酸钾钠铜反应，酒石酸钾钠铜被还原糖还原，产生红色氧化亚铜沉淀，还原糖则被氧化和降解，其反应如下：△滴定时以亚甲基蓝为氧化－还原指示剂。
因为亚甲基蓝氧化能力比二价铜弱，待二价铜离子全部被还原后，稍过量的还原糖可使蓝色的氧化型亚甲基蓝还原为无色的还原型的亚甲基蓝，此时溶液呈滴加亚甲基蓝溶液前的红色，即达滴定终点根据消耗的样液量可计算出还原糖含量 2．2试剂2.2.1 标准转化糖溶液（10g/L）A、准确称量经105℃烘干并冷却的蔗糖（AR）23.750克，用蒸馏水约120mL溶解并移入250ml容量瓶中，加入浓盐酸（相对密度1.19）9mL，摇匀，在室温20℃~25℃下静置8天，然后用蒸馏水稀释至刻度B、吸取A液100mL于1000mL的容量瓶中，用蒸馏水稀释至刻度得标准转化糖溶液（10g/L）溶于水中，再转移到1升的容量瓶中，再定容到刻度，即可得到1mg/ml的转化糖溶液2.2.2 标准转化糖溶液（2.5g/L）准确吸取标准转化糖溶液（10g/L）50mL移入200mL的容量瓶中，加酚酞指示剂5滴，用10%氢氧化钠溶液调至微红色，加水稀释至刻度，摇匀2.2.3 费林氏试剂甲液：称取硫酸铜（CuSO4·5H2O）69.28g，用蒸馏水溶解后，移入1000ml容量瓶中，加水至刻度，摇匀，过滤即成乙液：称取酒石酸钾钠（NaKC4H4O6.4H2O）346g溶于蒸馏水约500ml中，另取氢氧化钠(NaOH)100g溶于蒸馏水约200ml中。
将二者混合，移入1000ml容量瓶中，加水至刻度，放置2天，如液面降低，应加水至刻度，摇匀，过滤即成2.2.4 中性乙酸铅溶液（540Bx） 称取500g中性乙酸铅，加蒸馏水1000ml溶解后静置，取上层清澈过滤在滤液中滴加乙酸调节成中性或弱酸性（用石蕊试纸检验），再用不含二氧化碳的水稀释到54°Bx（相对密度1.25）2.2.5 脱铅剂 称取磷酸氢二钠（Na2HPO4.12H2O）70g，草酸钾（K2C2O4.H2O ）30g ，加蒸馏水溶解后稀释至1000ml2.2.6 四甲基蓝溶液（10g/L）称取四甲基蓝1.0g，加蒸馏水溶解后定容至100ml2.2.7 盐酸溶液（1+1）2.2.8氢氧化钠溶液10%2.3 器材电热恒温水浴锅，调温电炉，250ml锥形瓶，滴定管2.4 测定2.4.1费林氏试剂的标定准确吸取费林氏试剂乙液和甲液各5.00ml，移入250ml锥形瓶中，加蒸馏水29ml，从滴定管加入标准转化糖溶液（2.5g/L）19.5mL，轻轻摇匀，将锥形瓶加热使溶液在4~5min内沸腾，准确煮沸2min，加四甲基蓝溶液（10g/L）3滴，在溶液保持沸腾的状态下，从滴定管继续滴加转化糖液（控制在1min内）至加四甲基蓝蓝色刚刚消失出现砖红色即为终点。
记录消耗标准转化糖溶液的总体积（到达终点时锥形瓶中溶液的总体积控制在60mL）平行操作3次，取其平均值，按下式计算10mL费林氏甲乙混合液相当转化糖的量： 式中：A──10mL费林氏甲乙混合液相当转化糖的量，g； V──标定时消耗标准转化糖溶液的总体积，mL2.4.2 样液制备A、称取甘蔗糖蜜样品（43.333±0.001g）于烧杯中，加入适量的蒸馏水使之完全溶解，定容于500mL的容量瓶中B、用移液管取A溶液50mL于200mL的容量瓶中，加入中性乙酸铅溶液（540Bx） 2mL，充分摇匀后加入脱铅剂6mL，摇匀后加蒸馏水至刻度，充分摇匀，过滤C、 转化后样液制备 用移液管取B溶液25mL于100mL的容量瓶中，加水20mL，加盐酸溶液（1+1）5mL，用少量蒸馏水清洗其颈部盐酸，插入温度计，摇匀后在68℃的水浴中加热待温度到达66℃（一般在5min内到达）起计算转化时间，控制在66~68℃，转化10min，转化期间应不断地摇动转化完毕，迅速冷至室温，取出温度计，用少许蒸馏水冲洗温度计入容量瓶中，加入1g/L的酚酞指示剂2滴，用氢氧化钠溶液（10%）中和至微红色，加水至100mL，摇匀备用。
D、转化前样液制备用移液管取B溶液50mL于100mL的容量瓶中，加水至100mL，摇匀备用 2.4.3 样品溶液测定：准确吸取费林氏试剂乙液和甲液各5.00ml于250ml锥形瓶中，加蒸馏水（转化前：20ml；转化后：25ml加水量应使滴定完毕后锥形瓶中溶液的总体积为60mL例：如预定的检液量为25mL，费林氏混合液量为10mL，则加水量应为25mL），加热使溶液在4~5min内沸腾，准确煮沸2min，加四甲基蓝溶液（10g/L）3滴，在溶液保持沸腾的状态下，从滴定管继续滴加样品溶液（控制在1min内）至溶液蓝色刚刚消失，砖红色出现即为终点记录消耗样品溶液的总体积此操作转化前、转化后样液各重复操作3次，第1次是预滴，第2、3次是正式滴定，第2 、3次于煮沸前预加样液的量比第1次预滴的样液总量约少1mL取第2、3次的平均值计算结果2.4.4、结果计算转化前还原糖含量（%）=式中：m──样品重量，g；A──10mL费林氏甲乙混合液相当转化糖的量，g；V──测定时平均消耗转化前样液的总体积，mL；4000──稀释倍数转化后还原糖含量（%）=式中：m──样品重量，g；A──10mL费林氏甲乙混合液相当转化糖的量，g；V──测定时平均消耗转化前样液的总体积，mL；8000──稀释倍数。
总糖分（%）=蔗糖分+还原糖分=（转化后还原糖含量-转化前还原糖含量）0.95 + 转化前还原糖含量 式中：0.95——换算系数（0.95g蔗糖可转化为1g转化糖）方法二：仪器法（二次旋光法测定蔗糖分，化学法测定还原糖）（一）蔗糖分测定：二次旋光法2.1 方法提要 采用二次旋光法测定测得甘蔗糖蜜溶液转化前后的旋光读数，按相关公式进行计算，求得其蔗糖分2.2 仪器、设备、试剂2.2.1 WZZ-2SS自动旋光糖量计2.2.2 旋光观测管：长度：200.00±0.02mm2.2.3 容量瓶，100mL；500mL2.2.4 天平，精确至±0.001g2.2.5 精密温度计，0.1℃刻度2.2.6 碱性乙酸铅[Pb（CH3COO）2.Pb（OH）2]2.2.7 盐酸溶液（24.850Bx） 以浓盐酸（相对密度1.19）1000mL缓缓加入蒸馏水850mL中，并准确修正其密度至24.850Bx（20℃）.2.2.8 氯化钠溶液（231.5g/L） 称取在120℃干燥过的氯化钠231.5g，溶于适量蒸馏水中，移入1000mL容量瓶，加蒸馏水稀释至刻度。
2.3 测定步骤2.3.1 校准WZZ-2SS自动旋光糖量计用标准石英管校准2.3.2 样液制备称取甘蔗糖蜜样品（43.333±0.001g）于烧杯中，加入适量的蒸馏水使之完全溶解，定容于500mL的容量瓶中2.3.3 蔗糖分测定 取样液约200mL于锥形瓶中，加入碱式乙酸铅约7g，迅速摇匀，过滤，以移液管吸取两份50mL滤液，分别移入两个100mL容量瓶中，其中一瓶加入氯化钠溶液（231.5g/L）10mL，然后加蒸馏水至刻度，摇匀，如发现混浊则应过滤，滤液用200mm观测管测其旋光度，以此数乘2即得直接旋光读数P，并记录读数时糖液的温度在另一瓶中先加蒸馏水20mL，再加盐酸溶液（24.850Bx）10mL，插入温度计，在水浴中准确加热至60℃，并在此温度下保持10min（在最初3min内应不断摇荡）浸入冷水中，迅速冷却至读取直接旋光读数时的温度，用少量蒸馏水冲洗沾在温度计上的糖液于容量瓶内，取出温度计，加水至刻度（如溶液色泽较深可加入少量锌粉），充分摇匀，如发现混浊则应过滤用200mm观测管测其旋光读数，以此数乘2即得转化旋光读数P/（负值），并用0.1℃刻度温度计测出读数时糖液的温度t（测P及P/时的糖液的温度，二者相差应不超过1℃）。
2.3.4 计算及结果表示甘蔗糖蜜样品蔗糖分S，数值以%表示，按下式计算，结果取到小数点后一位数S=100（P-P/）×3/[132.56-0.0794（13-g）-0.53（t-20）]式中：、S——蔗糖分，%；P——直接旋光读数；P/——转化旋转光读数（负值）；t——测P/时糖液的温度，℃；g——8.6667×锤度/2 2.3.5允许误差 两次测定值之差应不超过其平均值的2%二） 还原糖测定：化学法操作步骤同方法一中转化前还原糖含量三） 总糖分（%）=蔗糖分+还原糖分 3、酸度：按QB/T2684-2005执行3.1 方法提要 甘蔗糖蜜酸度是以100g样品所耗用氢氧化钠溶液（1mol/L）的毫升数表示本法采用PH酸度计控制被测溶液的PH值在7.00±0.02 . ， 通过滴定耗用的氢氧化钠溶液量可计算出糖蜜的酸度。
3.2 仪器、设备3.2.1 PH计，分度值0.02PH；3.2.2 滴定管，刻度0.1mL；3.3 试剂3.3.1 氢氧化钠标准溶液（0.1mol/L）；3.3.2 中性蒸馏水 用氢氧化钠标准溶液（0.1mol/L）调节蒸馏水至PH（7.0±0.1）3.4 测定步骤3.4.1 样液制备 糖蜜经搅拌均匀后，称取5.00g于烧杯中用中性蒸馏水100mL溶解3.4.2 测定 以合适的缓冲溶液校正PH计，将用中性蒸馏水冲洗过的电极插入样液中，边搅拌边滴加氢氧化钠标准溶液（0.1mol/L），至样液的PH为7.00±0.02为止，即为终点记录耗用标准溶液的毫升数3.4.3计算及结果表示 甘蔗糖蜜酸度按下式计算，结果取到小数点后一位 酸度=100cV/5=20cV式中： c ——氢氧化钠标准溶液的浓度，mol/L； V——滴定耗用氢氧化钠标准溶液量，mL3.4.4 允许误差 两次测定值之差不得超过其平均值的5%4、总灰分测定 4.1方法提要 甘蔗糖蜜经浓硫酸处理后于高温炉中灼烧，得到的残留物即是样品的硫酸灰分4.2 仪器、设备4.2.1 高温炉，0℃~1000℃；4.2.2 石英坩埚，100mL。
4.3 试剂：浓硫酸4.4 测定步骤4.4.1 测定 用燃烧至恒重的石英坩埚，称取样品5~10g，加入浓硫酸5mL~10mL，于电炉上加热至完全碳化，放入高温炉中在550℃下灼烧至灰白色（约5h）取出置于干燥器中冷却，加入浓硫酸几滴润湿，再放入高温炉中，在650℃下灼烧至恒重（约1.5h），冷却，称重4.4.2 计算及结果表示 甘蔗糖蜜的总灰分（硫酸灰分）数值以%表示，按下式计算，结果取到小数点后一位 硫酸灰分（%）= 100（m3— m2）/m1式中： m1——样品质量，g； m2——坩埚质量，g； m3——灼烧后坩埚与残留物的总质量，g4.4.3允许误差 两次测定值之差不得超过其平均值的2%表2：折射锤度温度校正数折射锤度/ 0Bx0510152025303540455055606570温度/℃温度低于20℃应减之数100.500.540.580.610.640.660.680.700.720.730.740.750.760.780.79110.460.490.530.550.580.600.620.640.650.660.670.680.690.700.71120.420.450.480.500.520.540.560.570.580.590.600.610.610.6+30.63130.370.400.420.440.460.480.490.500.510.520.530.540.540.550.55140.330.350.370.390.400.410.420.430.440.450.450.460.460.470.48150.270.290.310.330.340.340.350.360.370.370.380.390.390.400.40160.220.240.250.260.270.280.280.290.300.300.300.310.310.320.32170.170.180.190.200.210.210.210.220.220.230.230.230.230.240.24180.120.130.130.140.140.140.140.150.150.150.150.160.160.160.16190.060.060.060.070.070.070.080.080.080.080.080.080.080.080.08温度/℃温度高于20℃应加之数210.060.070.070.070.070.080.080.080.080.080.080.080.080.080.08220.130.130.140.140.150.150.150.150.150.160.160.160.160.160.16230.190.200.210.220.220.230.230.230.230.240.240.240.240.240.24240.260.270.280.290.300.300.310.310.310.310.310.320.320.320.32250.330.350.360.370.380.380.390.400.400.400.400.400.400.400.40260.400.420.430.440.450.460.470.480.480.480.480.480.480.480.48270.480.500.520.530.540.550.550.560.560.560.560.560.560.560.56280.560.570.600.610.620.630.630.640.640.640.640.640.640.640.64290.640.660.680.690.710.720.720.730.730.730.730.730.730.730.73300.700.740.770.780.790.800.800.810.810.810.810.810.810.810.8113。