QJ020催化剂可燃碳测定法

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1、 沧州分公司企业标准 催化剂可燃碳含量测定法 QJ/CZFGS 13.020-2008(A/O) 1 适用范围本方法适用于催化剂可燃碳含量测定。2 方法概述 本方法系采用SB-3型自动定碳仪进行测定。 将试样置于管式炉中、通入空气在高温（850）下进行煅烧，使试样中的可燃碳全部转化为CO2，生成的CO2用碱液吸收，根据吸收前后的气体变化计算出试样的可燃碳含量，以百分数表示。 化学反应如下： 850 C+O2 CO2 CO2+2KOH K2CO3+H2O3 仪器与试剂3.1 仪器3.1.1 SB-3型自动定碳仪；3.1.2 管状高温炉，配温度自控器；3.1.3 燃烧管，瓷舟；3.1.4 气体减压

2、阀；3.2 试剂与材料3.2.1 氢氧化钾：40%水溶液，3.2.2 硫酸：5%水溶液。3.2.3 氯化钠饱和水溶液。4 准备工作4.1 按仪器说明书要求接好高温炉和定碳仪电源，将燃烧管与定碳仪连接，（见图）同时将高温炉升温至85010。4.2 将净化风与定碳仪连接。于定碳仪吸收瓶中装满40%KOH水溶液。于水准 沧州分公司2008-10-01发布 2008-10-15实施QJ/CZFGS 13.020-2008(A/O) 瓶中装入适量的饱和食盐水。燃烧管前面，要接有硫酸洗气瓶、碱液瓶及干燥管，然后与净化气连接。接通电源，用减压阀控制净化风压力在0.3-0.4Kg/Cm2。使仪器的集气管处于待

3、吸收状态。调好后关闭电源。5 试验步骤5.1 称量处理过的瓷舟（新瓷舟要经稀盐酸处理后方可使用），称准至0.0002克。然后向已知重量的瓷舟中称入0.20.001克试样（待生样取0.10.001克）称准至0.0002克。5.2 开动定碳仪，经过排气、通氧、吸收三部后灯亮，读数“A”，同时关闭电源。5.3 燃烧取样吸收读数B：5.3.1 将盛有样品的瓷舟以金属钩迅速推入高温炉石英管最高温度处，然后立即用橡皮塞塞紧，灼烧三分钟。5.3.2 开启仪器，经排气（通氧阀平放），通氧吸收（通氧阀立放），待封闭液将至量管的细管的三分之二处时，将通氧栓立即转向关闭方向（既通氧阀平放，这时量管随通氧栓关闭，而通

4、向大气自行对零）。5.3.3 气体进吸收瓶后回到量管，灯量读数“B”，关闭仪器。5.3.4 记录量气管中的温度和大气压。6 计算6.1 试样中的可燃碳X（%）按下式计算： （B-A）K X= W 式中：A-燃烧气吸收前读数；B-燃烧气吸收后读数；W-称取试样重（克）；K-气体的温度压力校正系数（由表2查处或由下列公式计算得出）。6.2 气体的温度压力校正系数（K）可按下式计算： 289（P-b） K= 760（273+t）式中：P-试验时大气压力（mmHg） b-试验试验温度下水的饱和蒸汽压力（见表1）； t-实验时的温度 P-b-生成CO2的压力。QJ/CZFGS 13.020-2008(A

5、/O) 7 精确度7.1 平行测定两个结果的差数不应大于0.04%7.2 取平行测定两个结果的算术平均值，作为试样的可燃碳含量。8 注意事项8.1 洗气瓶中的H2SO4溶液变黄更换；8.2 吸收瓶中KOH溶液在使用500600次后更换；8.3 活塞应定期更换（半个月）涂一次润滑油（硅油或20#航空润滑油）；8.4 量管应经常清洗，否则管壁出现油污，而产生附着水，影响读数；8.5 仪器经常不用时每天要开启一次，否则通气活栓容易粘结。表1 水的饱和蒸汽压力表TPmmHgTPmmHgTPmmHgTPmmHg109.2091815.482625.213439.90119.8401916.482726.

6、743542.181210.522017.542828.353644.561311.232118.652930.043747.071411.992219.833031.823846.691512.792321.073133.703952.441613.632422.383235.664055.21714.532523.763337.734158.34编号部件名称材料件数用途1水准瓶玻璃1个盛装用浓硫酸配制的5%甲基红的酸性水，约500毫升。2调压阀 调整风压3不比读数标尺白瓷板直接读出含碳量。无须手持水准瓶去比。4吸收瓶玻璃盛装40%的KOH约1000毫升、装至漏斗下端和细管衔接处。5量气管6

7、控制栓启动后、自动改变通向、达到自动吸收目的7微动开关周期性使指示灯发出读数信号QJ/CZFGS 13.020-2008(A/O) 8同步电机转动控制栓，达到自动吸收9电木盘电木固定电机、控制栓10冷却器玻璃可将燃烧后气体温度降低。11通氧栓用于通氧和混合气体通入量气管12过滤管内装脱脂棉、以除去燃烧过的气体的尘埃13洗涤瓶（一）盛装40%的KOH高约40mm14插头放入试样和流出混合气体通入量气管15洗涤瓶（二）盛装浓硫酸高约40mm SB68-3型 快速自动定碳仪 QJ/CZFGS 13.020-2008(A/O) 表2 气体容量法测定碳含量用气压和温度系数换算表 tommHg121314

8、1516171819207200.9640.9590.9550.9510.9460.9420.9370.9330.9287220.9660.9620.9580.9530.9490.9450.9400.9350.9317240.9690.9650.9610.9560.9520.9470.9430.9380.9337260.9720.9680.9630.9590.9540.9500.9450.9410.9367280.9740.9700.9660.9610.9570.9530.9480.9430.9397300.9770.9730.9690.9640.9600.9550.9510.9460.941

9、7320.9800.9760.9710.9670.9620.9580.9530.9490.9447340.9830.9780.9740.9700.9650.9600.9560.9510.9477360.9850.9810.9770.9720.9680.9630.9580.9530.9497380.9880.9840.9790.9750.9700.9660.9610.9570.9527400.9910.9870.9820.9780.9730.9680.9640.9590.9557420.9940.9890.9850.9800.9760.9710.9660.9620.9577440.9960.99

10、20.9880.9830.9790.9740.9690.9650.9607460.9990.9950.9900.9860.9810.9760.9720.9670.9637481.0020.9970.9930.9890.9840.9790.9750.9700.9657501.0051.0000.9960.9910.9870.9820.9770.9730.9687521.0071.0030.9980.9940.9890.9840.9800.9750.9717541.0101.0051.0010.9970.9920.9860.9830.9780.9737561.0131.0081.0040.9990

11、.9950.9900.9850.9810.97675810.151.0111.0061.0020.9970.9930.9880.9830.9797601.0181.0141.0091.0051.0000.9950.9910.9860.9817621.0211.0161.0121.0071.0030.9980.9930.9890.9847641.0211.0191.0151.0101.0051.0010.9960.9910.9867661.0261.0221.0171.0131.0081.0030.9980.9940.9897681.0291.0241.0201.0151.0111.0061.0

12、010.9970.9927701.0321.0271.0231.0181.0131.0091.0040.9990.9947721.0341.0301.0251.0211.0161.0111.0061.0020.9977741.0371.0331.0281.0231.0191.0141.0091.0041.0007761.0401.0351.0311.0261.0211.0171.0121.0071.0027781.0421.0381.0331.0291.0241.0191.0141.0101.0057801.0451.0411.0361.0311.0271.0241.0171.0121.008

13、QJ/CZFGS 13.020-2008(A/O) 续表2 气体容量法测定碳含量用气压和温度系数换算表 tommHg212223242526272829307200.9240.9190.9140.9090.9060.9000.8950.8900.8850.8797220.9260.9220.9170.9120.9070.9020.8970.8920.8870.8837240.9290.9240.9190.9150.9100.9050.9000.8950.8900.8847260.9310.9270.9220.9170.9120.9080.9030.8970.8920.8877280.9340.

14、9290.9250.9200.9150.9100.9050.9000.8950.8907300.9370.9320.9270.9230.9180.9130.9080.9030.8970.8927320.9390.9350.9300.9250.9200.9150.9100.9050.9000.8957340.9420.9370.9330.9280.9230.9180.9130.9080.9020.8977360.9450.9400.9350.9300.9250.9210.9150.9100.9050.9007380.9470.9430.9380.9330.9280.9230.9180.9130.

15、9080.9027400.9500.9450.9400.9360.9310.9260.9210.9160.9100.9057420.9530.9480.9430.9380.9330.9280.9230.9180.9130.9077440.9550.9500.9460.9410.9360.9310.9260.9210.9160.9107460.9580.9530.9480.9430.9380.9330.9280.9230.9180.9137480.9610.9560.9510.9460.9410.9360.9310.9260.9210.9157500.9630.9580.9540.9490.94

16、40.9390.9340.9280.9230.9187520.9660.9610.9560.9510.9460.9410.9360.9310.9260.9207540.9680.9630.9590.9540.9490.9440.9390.9330.9280.9237560.9710.9660.9610.9560.9510.9460.9410.9360.9310.9257580.9740.9690.9640.9590.9540.9490.9440.9390.9330.9287600.9760.9710.9670.9620.9570.9520.9460.9410.9360.9317620.9790

17、.9740.9690.9640.9590.9540.9490.9440.9380.9337640.9820.9770.9720.9670.9620.9570.9520.9460.9410.9367660.9840.9790.9740.9690.9640.9590.9540.9490.9440.9387680.9870.9820.9770.9720.9670.9620.9570.9520.9460.9417700.9900.9850.9800.9750.9700.9650.9590.9540.9490.9437720.9920.9870.9820.9770.9720.9670.9620.9570.9510.9467740.9950.9900.9850.9800.9750.9700.9640.9590.9540.9487760.9970.9920.9870.9830.9770.9720.9670.9620.9560.9517781.0000.9950.9900.9850.9800.9750.9700.9640.9590.9547801.0030.9980.9930.9880.9830.9770.9730.9670.9620.956