炭素材料工業(yè)分析方法 編制說明

1《炭素材料工業(yè)分析方法》編制說明根據(jù)《國家標準化管理委員會關(guān)于下達2023年第四批推薦性國家標準計劃及相業(yè)協(xié)會提出，由全國鋼標準化技術(shù)委員會（SAC同時廣泛搜集相關(guān)標準和國內(nèi)外技術(shù)資料，進行了大量的研究分析、資料查證工作，2YB/T5189-2022，并根據(jù)產(chǎn)業(yè)需要以經(jīng)濟、社會效益，充分體現(xiàn)了標準在技術(shù)上的先3實際，避免試樣在制備過程中可能造成的污染，進一步保證了小于初始空白瓷方舟（鉑坩堝）質(zhì)量且灼燒殘余物沒有粘在瓷方舟（鉑坩堝）上時，4取根據(jù)樣品的種類:炭糊類、石墨制品、焙燒品按GB/T1427——修改了冷卻稱重具體操作步驟，便于實驗員進行堝在馬弗爐中加熱7min，以質(zhì)量損失計算揮發(fā)分——增加了6.5.3揮發(fā)分測試方法三（低溫）；的揮發(fā)分含量，又設(shè)備簡單、操作簡便，可較好滿足——增加了7固定碳的計算方法章節(jié)，解決了行業(yè)長期以來5針對標準修訂的內(nèi)容，我們收集了6種不同的代表性樣品進行了驗證測試，實驗樣品名稱負極粉針狀生焦針狀煅后焦普通煅后焦高純石墨樣品代號4#6#組織4家實驗室，將1#-3#樣品按第4章節(jié)水分測定方法實驗室名稱實驗次數(shù)（n）樣品代號#實驗室1：郴州質(zhì)檢所數(shù)據(jù)10.300.020.33數(shù)據(jù)20.320.020.34數(shù)據(jù)30.320.020.34數(shù)據(jù)40.280.020.32數(shù)據(jù)50.300.020.33數(shù)據(jù)60.310.020.33數(shù)據(jù)70.310.020.33數(shù)據(jù)80.300.020.34數(shù)據(jù)90.320.020.330.290.020.310.310.020.33有效測量次數(shù)nXmax0.320.020.34Xmin0.280.020.310.3050.0200.3300.0400.0000.030標準偏差(S)0.0130.0000.0090.00016900.0000816相對標準偏差(RSD)4.260.002.73實驗室內(nèi)的臨界極差CR0.95(n)3.07690.00003.3333臨界極差系數(shù)f（n）查表得f（n）實驗室是否通過通過通過通過格拉布斯（Grubbs）檢驗第一次通過格拉布斯（Grubbs）檢驗對每一個實驗室、每一個樣品進行分析，剔除離群數(shù)據(jù)作用是檢驗最大觀測值是否離群格拉布斯統(tǒng)計量Gp=（X（p）-X平均值）S最大值查表得上5%點2.3552.3552.355查表得上1%點2.5642.5642.564最大值0.000實驗室是否通過通過通過通過最小值查表得上5%點2.3552.3552.355查表得上1%點2.5642.5642.564最小值0.0002.222實驗室是否通過通過通過通過統(tǒng)計量水平1水平2水平3水平4均值的平均值0.20010.49930.99451.9719均值的標準差0.00100.00120.00090.0035最大均值0.20100.50050.99541.9755最小均值0.19900.49830.99371.9685Gmax0.92721.09731.01901.0185Gmin1.05960.86000.97980.9804G臨界值3.3曼德爾的h統(tǒng)計量實驗室郴州所省質(zhì)檢院永州所水平10.92720.1325-1.0596水平2-0.23731.0973-0.8600水平3-0.9798-0.03921.0190水平4-0.03811.0185-0.9804水平1水平2水平3水平4總平均值0.20010.49930.99451.9719T16.602316.475932.820165.0742T21.32108.226032.6411128.3232T3T4363363363363T50.00080.00140.00440.0185r20.0000360.0000640.0002020.000840L2（計算值）-0.7712-4.7392-18.7524-73.8153L2（取值）00008R20.0000360.0000640.0002020.000840r0.00600.00800.01420.0290R0.00600.00800.01420.0290r0.01670.02240.03980.0812R（計算值）0.01670.02240.03980.0812R（建議值）0.0200.0250.0500.100采用試劑級碳化硅，分別于650℃、700℃、800℃灼燒2h，測定其增重情況，實實驗溫度/℃坩堝質(zhì)量/g樣品質(zhì)量/g灼燒后坩堝加樣品質(zhì)量增重率/%平均增重率/%碳化硅氧化率/%65015.63691.002716.6420/16.64200.23940.24280.485615.81021.015516.81820.246270015.63731.030216.67040.28150.26560.531216.27451.041017.31810.249880016.10771.023517.13960.82070.79361.587215.73601.030616.77450.7665#樣品（灰分含量范圍≤0.300%）：稱取500g研磨過篩的干基高純石墨樣品（不），9#樣品（灰分含量范圍0.300%～0.600%）：稱取200g研磨過篩的干基高純石墨樣），），4#樣品（灰分含量范圍1.50%～3.00%）：稱取200g研磨過篩的干基高純石墨樣品），實驗室1#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%郴州市產(chǎn)商品質(zhì)量監(jiān)督檢驗所10.05980.20000.14870.49730.30251.01170.59872.002320.06010.20100.14810.49530.30181.00940.58731.964230.05890.19700.14520.48560.29850.99830.58841.967940.06060.20270.15050.50330.29510.98700.59351.984950.05960.19930.15230.50940.29730.99430.58971.972260.06080.20330.14730.49260.29240.97790.59992.006470.06050.20230.14750.49330.29780.99600.58611.960280.06030.20170.14940.49970.29310.98030.59181.979390.05670.18960.15060.50370.29250.97830.58911.97020.06210.20770.14990.50130.30121.00740.58371.95220.06160.20600.15170.50740.29610.99030.57701.9298平均值/%0.06010.20100.14920.49900.29710.99370.58961.9718S1/%0.00140.00480.00210.00700.00370.01230.00650.0217RSD/%2.38442.38441.40591.40591.23571.23571.10151.1015實驗室2#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%湖南省產(chǎn)商品質(zhì)量監(jiān)督檢驗研究院10.05810.19430.14770.49400.30111.00700.59671.995720.06060.20270.14920.49900.30261.01200.58171.945530.05810.19430.14680.49100.29911.00030.58911.970240.05980.20000.15190.50800.29490.98630.59992.006450.06130.20500.15210.50870.29680.99260.58271.948860.06090.20370.14710.49200.29340.98130.60022.007470.06080.20330.14890.49800.29911.00030.58411.953580.05730.19160.15010.50200.29420.98390.58211.946890.05880.19670.15160.50700.29210.97690.58911.97020.06080.20330.14960.50030.30091.00640.59271.98230.06210.20770.15120.50570.29680.99260.59922.0040平均值0.05990.20020.14970.50050.29740.99450.59071.9755S2S2/%0.00160.00520.00190.00640.00350.01160.00740.0249RSD/%2.60692.60691.27951.27951.16521.16521.26101.2610實驗室3#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%永州市產(chǎn)商品質(zhì)量監(jiān)督檢驗所10.05780.19330.14570.48730.30011.00370.58171.945520.06110.20430.14910.49870.30281.01270.58531.957530.05910.19770.14590.48800.29650.99160.58081.942540.06160.20600.15150.50670.29991.00300.59812.000350.05880.19670.15130.50600.29630.99100.57811.933460.05980.20000.15090.50470.29210.97690.59822.000770.06090.20370.14750.49330.30111.00700.58221.947280.06010.20100.14980.50100.29410.98360.58851.968290.05610.18760.15010.50200.29250.97830.60112.01040.06010.20100.14690.49130.30191.00970.58471.95550.05910.19770.15020.50230.29660.99200.59581.9926平均值0.05950.19900.14900.49830.29760.99540.58861.9685/%S3/%/%0.00160.00530.00210.00710.00380.01260.00820.0275RSD/%2.65742.65741.43341.43341.26491.26491.39721.3972統(tǒng)計量水平1水平2水平3水平4均值的平均值0.20010.49930.99451.9719均值的標準差0.00100.00120.00090.0035最大均值0.20100.50050.99541.9755最小均值0.19900.49830.99371.9685Gmax0.92721.09731.01901.0185Gmin1.05960.86000.97980.9804G臨界值3.3曼德爾的h統(tǒng)計量實驗室郴州所省質(zhì)檢院永州所水平10.92720.1325-1.0596水平2-0.23731.0973-0.8600水平3-0.9798-0.03921.0190水平4-0.03811.0185-0.9804水平1水平2水平3水平4總平均值0.20010.49930.99451.9719T16.602316.475932.820165.0742T21.32108.226032.6411128.3232T3T4363363363363T50.00080.00140.00440.0185r20.0000360.0000640.0002020.000840L2（計算值）-0.7712-4.7392-18.7524-73.8153L2（取值）0000R20.0000360.0000640.0002020.000840r0.00600.00800.01420.0290R0.00600.00800.01420.0290r0.01670.02240.03980.0812R（計算值）0.01670.02240.03980.0812R（建議值）0.0200.0250.0500.100采用試劑級碳化硅，分別于650℃、700℃、800℃灼燒2h，測定其增重情況，實實驗溫度/℃坩堝質(zhì)量/g樣品質(zhì)量/g灼燒后坩堝加樣品質(zhì)量增重率/%平均增重率/%碳化硅氧化率/%65015.63691.0027/16.64200.23940.24280.485615.81021.015516.81820.246270015.63731.030216.67040.28150.26560.531216.27451.041017.31810.249880016.10771.023517.13960.82070.79361.587215.73601.030616.77450.7665#樣品（灰分含量范圍≤0.300%）：稱取500g研磨過篩的干基高純石墨樣品（不），#樣品（灰分含量范圍0.300%～0.600%）：稱取200g研磨過篩的干基高純石墨樣），），4#樣品（灰分含量范圍1.50%～3.00%）：稱取200g研磨過篩的干基高純石墨樣品），實驗室1#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%郴州市產(chǎn)商品質(zhì)量監(jiān)督檢驗所10.05980.20000.14870.49730.30251.01170.59872.002320.06010.20100.14810.49530.30181.00940.58731.964230.05890.19700.14520.48560.29850.99830.58841.967940.06060.20270.15050.50330.29510.98700.59351.984950.05960.19930.15230.50940.29730.99430.58971.972260.06080.20330.14730.49260.29240.97790.59992.006470.06050.20230.14750.49330.29780.99600.58611.960280.06030.20170.14940.49970.29310.98030.59181.979390.05670.18960.15060.50370.29250.97830.58911.97020.06210.20770.14990.50130.30121.00740.58371.95220.06160.20600.15170.50740.29610.99030.57701.9298平均值/%0.06010.20100.14920.49900.29710.99370.58961.9718S1/%0.00140.00480.00210.00700.00370.01230.00650.0217RSD/%2.38442.38441.40591.40591.23571.23571.10151.1015實驗室2#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%湖南省產(chǎn)商品質(zhì)量監(jiān)督檢驗10.05810.19430.14770.49400.30111.00700.59671.995720.06060.20270.14920.49900.30261.01200.58171.945530.05810.19430.14680.49100.29911.00030.58911.970240.05980.20000.15190.50800.29490.98630.59992.006450.06130.20500.15210.50870.29680.99260.58271.948860.06090.20370.14710.49200.29340.98130.60022.007470.06080.20330.14890.49800.29911.00030.58411.953580.05730.19160.15010.50200.29420.98390.58211.946890.05880.19670.15160.50700.29210.97690.58911.97020.06080.20330.14960.50030.30091.00640.59271.98230.06210.20770.15120.50570.29680.99260.59922.0040平均值0.05990.20020.14970.50050.29740.99450.59071.9755S2S2/%0.00160.00520.00190.00640.00350.01160.00740.0249RSD/%2.60692.60691.27951.27951.16521.16521.26101.2610實驗室3#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%永州市產(chǎn)商品質(zhì)量監(jiān)督檢驗所10.05780.19330.14570.48730.30011.00370.58171.945520.06110.20430.14910.49870.30281.01270.58531.957530.05910.19770.14590.48800.29650.99160.58081.942540.06160.20600.15150.50670.29991.00300.59812.000350.05880.19670.15130.50600.29630.99100.57811.933460.05980.20000.15090.50470.29210.97690.59822.000770.06090.20370.14750.49330.30111.00700.58221.947280.06010.20100.14980.50100.29410.98360.58851.968290.05610.18760.15010.50200.29250.97830.60112.01040.06010.20100.14690.49130.30191.00970.58471.95550.05910.19770.15020.50230.29660.99200.59581.9926平均值0.05950.19900.14900.49830.29760.99540.58861.9685/S3/%0