QJ020催化劑可燃碳測定法

1、 滄州分公司企業(yè)標(biāo)準(zhǔn) 催化劑可燃碳含量測定法 qj/czfgs 13.020-2008(a/o) 1 適用范圍本方法適用于催化劑可燃碳含量測定。2 方法概述 本方法系采用sb-3型自動(dòng)定碳儀進(jìn)行測定。 將試樣置于管式爐中、通入空氣在高溫（850）下進(jìn)行煅燒，使試樣中的可燃碳全部轉(zhuǎn)化為co2，生成的co2用堿液吸收，根據(jù)吸收前后的氣體變化計(jì)算出試樣的可燃碳含量，以百分?jǐn)?shù)表示。 化學(xué)反應(yīng)如下： 850 c+o2 co2 co2+2koh k2co3+h2o3 儀器與試劑3.1 儀器3.1.1 sb-3型自動(dòng)定碳儀；3.1.2 管狀高溫爐，配溫度自控器；3.1.3 燃燒管，瓷舟；3.1.4 氣體減壓

2、閥；3.2 試劑與材料3.2.1 氫氧化鉀：40%水溶液，3.2.2 硫酸：5%水溶液。3.2.3 氯化鈉飽和水溶液。4 準(zhǔn)備工作4.1 按儀器說明書要求接好高溫爐和定碳儀電源，將燃燒管與定碳儀連接，（見圖）同時(shí)將高溫爐升溫至850±10。4.2 將凈化風(fēng)與定碳儀連接。于定碳儀吸收瓶中裝滿40%koh水溶液。于水準(zhǔn) 滄州分公司2008-10-01發(fā)布 2008-10-15實(shí)施qj/czfgs 13.020-2008(a/o) 瓶中裝入適量的飽和食鹽水。燃燒管前面，要接有硫酸洗氣瓶、堿液瓶及干燥管，然后與凈化氣連接。接通電源，用減壓閥控制凈化風(fēng)壓力在0.3-0.4kg/cm2。使儀器的

3、集氣管處于待吸收狀態(tài)。調(diào)好后關(guān)閉電源。5 試驗(yàn)步驟5.1 稱量處理過的瓷舟（新瓷舟要經(jīng)稀鹽酸處理后方可使用），稱準(zhǔn)至0.0002克。然后向已知重量的瓷舟中稱入0.2±0.001克試樣（待生樣取0.1±0.001克）稱準(zhǔn)至0.0002克。5.2 開動(dòng)定碳儀，經(jīng)過排氣、通氧、吸收三部后燈亮，讀數(shù)“a”，同時(shí)關(guān)閉電源。5.3 燃燒取樣吸收讀數(shù)b：5.3.1 將盛有樣品的瓷舟以金屬鉤迅速推入高溫爐石英管最高溫度處，然后立即用橡皮塞塞緊，灼燒三分鐘。5.3.2 開啟儀器，經(jīng)排氣（通氧閥平放），通氧吸收（通氧閥立放），待封閉液將至量管的細(xì)管的三分之二處時(shí)，將通氧栓立即轉(zhuǎn)向關(guān)閉方向（既通

4、氧閥平放，這時(shí)量管隨通氧栓關(guān)閉，而通向大氣自行對零）。5.3.3 氣體進(jìn)吸收瓶后回到量管，燈量讀數(shù)“b”，關(guān)閉儀器。5.3.4 記錄量氣管中的溫度和大氣壓。6 計(jì)算6.1 試樣中的可燃碳x（%）按下式計(jì)算： （b-a）·k x= w 式中：a-燃燒氣吸收前讀數(shù)；b-燃燒氣吸收后讀數(shù)；w-稱取試樣重（克）；k-氣體的溫度壓力校正系數(shù)（由表2查處或由下列公式計(jì)算得出）。6.2 氣體的溫度壓力校正系數(shù)（k）可按下式計(jì)算： 289·（p-b） k= 760·（273+t）式中：p-試驗(yàn)時(shí)大氣壓力（mmhg） b-試驗(yàn)試驗(yàn)溫度下水的飽和蒸汽壓力（見表1）； t-實(shí)驗(yàn)時(shí)的溫度

5、 p-b-生成co2的壓力。qj/czfgs 13.020-2008(a/o) 7 精確度7.1 平行測定兩個(gè)結(jié)果的差數(shù)不應(yīng)大于0.04%7.2 取平行測定兩個(gè)結(jié)果的算術(shù)平均值，作為試樣的可燃碳含量。8 注意事項(xiàng)8.1 洗氣瓶中的h2so4溶液變黃更換；8.2 吸收瓶中koh溶液在使用500600次后更換；8.3 活塞應(yīng)定期更換（半個(gè)月）涂一次潤滑油（硅油或20#航空潤滑油）；8.4 量管應(yīng)經(jīng)常清洗，否則管壁出現(xiàn)油污，而產(chǎn)生附著水，影響讀數(shù)；8.5 儀器經(jīng)常不用時(shí)每天要開啟一次，否則通氣活栓容易粘結(jié)。表1 水的飽和蒸汽壓力表tpmmhgtpmmhgtpmmhgtpmmhg109.2091815

6、.482625.213439.90119.8401916.482726.743542.181210.522017.542828.353644.561311.232118.652930.043747.071411.992219.833031.823846.691512.792321.073133.703952.441613.632422.383235.664055.21714.532523.763337.734158.34編號(hào)部件名稱材料件數(shù)用途1水準(zhǔn)瓶玻璃1個(gè)盛裝用濃硫酸配制的5%甲基紅的酸性水，約500毫升。2調(diào)壓閥 調(diào)整風(fēng)壓3不比讀數(shù)標(biāo)尺白瓷板直接讀出含碳量。無須手持水準(zhǔn)瓶去比。4吸收瓶玻

7、璃盛裝40%的koh約1000毫升、裝至漏斗下端和細(xì)管銜接處。5量氣管6控制栓啟動(dòng)后、自動(dòng)改變通向、達(dá)到自動(dòng)吸收目的7微動(dòng)開關(guān)周期性使指示燈發(fā)出讀數(shù)信號(hào)qj/czfgs 13.020-2008(a/o) 8同步電機(jī)轉(zhuǎn)動(dòng)控制栓，達(dá)到自動(dòng)吸收9電木盤電木固定電機(jī)、控制栓10冷卻器玻璃可將燃燒后氣體溫度降低。11通氧栓用于通氧和混合氣體通入量氣管12過濾管內(nèi)裝脫脂棉、以除去燃燒過的氣體的塵埃13洗滌瓶（一）盛裝40%的koh高約40mm14插頭放入試樣和流出混合氣體通入量氣管15洗滌瓶（二）盛裝濃硫酸高約40mm sb68-3型 快速自動(dòng)定碳儀 qj/czfgs 13.020-2008(a/o) 表

8、2 氣體容量法測定碳含量用氣壓和溫度系數(shù)換算表 tommhg1213141516171819207200.9640.9590.9550.9510.9460.9420.9370.9330.9287220.9660.9620.9580.9530.9490.9450.9400.9350.9317240.9690.9650.9610.9560.9520.9470.9430.9380.9337260.9720.9680.9630.9590.9540.9500.9450.9410.9367280.9740.9700.9660.9610.9570.9530.9480.9430.9397300.9770.97

9、30.9690.9640.9600.9550.9510.9460.9417320.9800.9760.9710.9670.9620.9580.9530.9490.9447340.9830.9780.9740.9700.9650.9600.9560.9510.9477360.9850.9810.9770.9720.9680.9630.9580.9530.9497380.9880.9840.9790.9750.9700.9660.9610.9570.9527400.9910.9870.9820.9780.9730.9680.9640.9590.9557420.9940.9890.9850.9800

10、.9760.9710.9660.9620.9577440.9960.9920.9880.9830.9790.9740.9690.9650.9607460.9990.9950.9900.9860.9810.9760.9720.9670.9637481.0020.9970.9930.9890.9840.9790.9750.9700.9657501.0051.0000.9960.9910.9870.9820.9770.9730.9687521.0071.0030.9980.9940.9890.9840.9800.9750.9717541.0101.0051.0010.9970.9920.9860.9

11、830.9780.9737561.0131.0081.0040.9990.9950.9900.9850.9810.97675810.151.0111.0061.0020.9970.9930.9880.9830.9797601.0181.0141.0091.0051.0000.9950.9910.9860.9817621.0211.0161.0121.0071.0030.9980.9930.9890.9847641.0211.0191.0151.0101.0051.0010.9960.9910.9867661.0261.0221.0171.0131.0081.0030.9980.9940.989

12、7681.0291.0241.0201.0151.0111.0061.0010.9970.9927701.0321.0271.0231.0181.0131.0091.0040.9990.9947721.0341.0301.0251.0211.0161.0111.0061.0020.9977741.0371.0331.0281.0231.0191.0141.0091.0041.0007761.0401.0351.0311.0261.0211.0171.0121.0071.0027781.0421.0381.0331.0291.0241.0191.0141.0101.0057801.0451.04

13、11.0361.0311.0271.0241.0171.0121.008qj/czfgs 13.020-2008(a/o) 續(xù)表2 氣體容量法測定碳含量用氣壓和溫度系數(shù)換算表 tommhg212223242526272829307200.9240.9190.9140.9090.9060.9000.8950.8900.8850.8797220.9260.9220.9170.9120.9070.9020.8970.8920.8870.8837240.9290.9240.9190.9150.9100.9050.9000.8950.8900.8847260.9310.9270.9220.9170.91

14、20.9080.9030.8970.8920.8877280.9340.9290.9250.9200.9150.9100.9050.9000.8950.8907300.9370.9320.9270.9230.9180.9130.9080.9030.8970.8927320.9390.9350.9300.9250.9200.9150.9100.9050.9000.8957340.9420.9370.9330.9280.9230.9180.9130.9080.9020.8977360.9450.9400.9350.9300.9250.9210.9150.9100.9050.9007380.9470

15、.9430.9380.9330.9280.9230.9180.9130.9080.9027400.9500.9450.9400.9360.9310.9260.9210.9160.9100.9057420.9530.9480.9430.9380.9330.9280.9230.9180.9130.9077440.9550.9500.9460.9410.9360.9310.9260.9210.9160.9107460.9580.9530.9480.9430.9380.9330.9280.9230.9180.9137480.9610.9560.9510.9460.9410.9360.9310.9260

16、.9210.9157500.9630.9580.9540.9490.9440.9390.9340.9280.9230.9187520.9660.9610.9560.9510.9460.9410.9360.9310.9260.9207540.9680.9630.9590.9540.9490.9440.9390.9330.9280.9237560.9710.9660.9610.9560.9510.9460.9410.9360.9310.9257580.9740.9690.9640.9590.9540.9490.9440.9390.9330.9287600.9760.9710.9670.9620.9570.9520.9460.9410.9360.9317620.9790.9740.9690.9640.9590.9540.9490.9440.9380.9337640.9820.9770.9720.9670.9620.9570.9520.9460.9410.9367660.9840.9790.9740.9690.9640.9590.9540.9490.9440.9387680.9870.9820.9770.9720.9670.9620.9570.9520.9460.9417700.9900.9850.9800.9750.9700.9650.9590.9540.9490.9