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(biāo)準(zhǔn)化管理委員會(huì)關(guān)于下達(dá)2023年第四批推薦性國家標(biāo)準(zhǔn)計(jì)劃及相業(yè)協(xié)會(huì)提出，由全國鋼標(biāo)準(zhǔn)化技術(shù)委員會(huì)（SAC同時(shí)廣泛搜集相關(guān)標(biāo)準(zhǔn)和國內(nèi)外技術(shù)資料，進(jìn)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(jì)、社會(huì)效益，充分體現(xiàn)了標(biāo)準(zhǔn)在技術(shù)上的先3實(shí)際，避免試樣在制備過程中可能造成的污染，進(jìn)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(shí)，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(shí)驗(yàn)員進(jìn)行堝在馬弗爐中加熱7min，以質(zhì)量損失計(jì)算揮發(fā)分——增加了6.5.3揮發(fā)分測(cè)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(jì)算方法章節(jié)，解決了行業(yè)長期以來5針對(duì)標(biāo)準(zhǔn)修訂的內(nèi)容，我們收集了6種不同的代表性樣品進(jìn)行了驗(yàn)證測(cè)試，實(shí)驗(yàn)樣品名稱負(fù)極粉針狀生焦針狀煅后焦普通煅后焦高純石墨樣品代號(hào)4#6#組織4家實(shí)驗(yàn)室，將1#-3#樣品按第4章節(jié)水分測(cè)定方法實(shí)驗(yàn)室名稱實(shí)驗(yàn)次數(shù)（n）樣品代號(hào)#實(shí)驗(yàn)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(cè)量次數(shù)nXmax0.320.020.34Xmin0.280.020.310.3050.0200.3300.0400.0000.030標(biāo)準(zhǔn)偏差(S)0.0130.0000.0090.00016900.0000816相對(duì)標(biāo)準(zhǔn)偏差(RSD)4.260.002.73實(shí)驗(yàn)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(shí)驗(yàn)室是否通過通過通過通過格拉布斯（Grubbs）檢驗(yàn)第一次通過格拉布斯（Grubbs）檢驗(yàn)對(duì)每一個(gè)實(shí)驗(yàn)室、每一個(gè)樣品進(jìn)行分析，剔除離群數(shù)據(jù)作用是檢驗(yàn)最大觀測(cè)值是否離群格拉布斯統(tǒng)計(jì)量Gp=（X（p）-X平均值）S最大值查表得上5%點(diǎn)2.3552.3552.355查表得上1%點(diǎn)2.5642.5642.564最大值0.000實(shí)驗(yàn)室是否通過通過通過通過最小值查表得上5%點(diǎn)2.3552.3552.355查表得上1%點(diǎn)2.5642.5642.564最小值0.0002.222實(shí)驗(yàn)室是否通過通過通過通過統(tǒng)計(jì)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(biāo)準(zhǔn)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(jì)量實(shí)驗(yàn)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(jì)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(jì)算值）0.01670.02240.03980.0812R（建議值）0.0200.0250.0500.100采用試劑級(jí)碳化硅，分別于650℃、700℃、800℃灼燒2h，測(cè)定其增重情況，實(shí)實(shí)驗(yàn)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(shí)驗(yàn)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(yàn)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(shí)驗(yàn)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(yàn)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(shí)驗(yàn)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(yàn)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(jì)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(biāo)準(zhǔn)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(jì)量實(shí)驗(yàn)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(jì)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(jì)算值）0.01670.02240.03980.0812R（建議值）0.0200.0250.0500.100采用試劑級(jí)碳化硅，分別于650℃、700℃、800℃灼燒2h，測(cè)定其增重情況，實(shí)實(shí)驗(yàn)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(shí)驗(yàn)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(yàn)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(shí)驗(yàn)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(yàn)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(shí)驗(yàn)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(yàn)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