炭素材料工业分析方法 编制说明

1《炭素材料工业分析方法》编制说明根据《国家标准化管理委员会关于下达2023年第四批推荐性国家标准计划及相业协会提出，由全国钢标准化技术委员会（SAC同时广泛搜集相关标准和国内外技术资料，进行了大量的研究分析、资料查证工作，2YB/T5189-2022，并根据产业需要以经济、社会效益，充分体现了标准在技术上的先3实际，避免试样在制备过程中可能造成的污染，进一步保证了小于初始空白瓷方舟（铂坩埚）质量且灼烧残余物没有粘在瓷方舟（铂坩埚）上时，4取根据样品的种类:炭糊类、石墨制品、焙烧品按GB/T1427——修改了冷却称重具体操作步骤，便于实验员进行埚在马弗炉中加热7min，以质量损失计算挥发分——增加了6.5.3挥发分测试方法三（低温）；的挥发分含量，又设备简单、操作简便，可较好满足——增加了7固定碳的计算方法章节，解决了行业长期以来5针对标准修订的内容，我们收集了6种不同的代表性样品进行了验证测试，实验样品名称负极粉针状生焦针状煅后焦普通煅后焦高纯石墨样品代号4#6#组织4家实验室，将1#-3#样品按第4章节水分测定方法实验室名称实验次数（n）样品代号#实验室1：郴州质检所数据10.300.020.33数据20.320.020.34数据30.320.020.34数据40.280.020.32数据50.300.020.33数据60.310.020.33数据70.310.020.33数据80.300.020.34数据90.320.020.330.290.020.310.310.020.33有效测量次数nXmax0.320.020.34Xmin0.280.020.310.3050.0200.3300.0400.0000.030标准偏差(S)0.0130.0000.0090.00016900.0000816相对标准偏差(RSD)4.260.002.73实验室内的临界极差CR0.95(n)3.07690.00003.3333临界极差系数f（n）查表得f（n）实验室是否通过通过通过通过格拉布斯（Grubbs）检验第一次通过格拉布斯（Grubbs）检验对每一个实验室、每一个样品进行分析，剔除离群数据作用是检验最大观测值是否离群格拉布斯统计量Gp=（X（p）-X平均值）S最大值查表得上5%点2.3552.3552.355查表得上1%点2.5642.5642.564最大值0.000实验室是否通过通过通过通过最小值查表得上5%点2.3552.3552.355查表得上1%点2.5642.5642.564最小值0.0002.222实验室是否通过通过通过通过统计量水平1水平2水平3水平4均值的平均值0.20010.49930.99451.9719均值的标准差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临界值3.3曼德尔的h统计量实验室郴州所省质检院永州所水平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总平均值0.20010.49930.99451.9719T16.602316.475932.820165.0742T21.32108.226032.6411128.3232T3T4363363363363T50.00080.00140.00440.0185r20.0000360.0000640.0002020.000840L2（计算值）-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（计算值）0.01670.02240.03980.0812R（建议值）0.0200.0250.0500.100采用试剂级碳化硅，分别于650℃、700℃、800℃灼烧2h，测定其增重情况，实实验温度/℃坩埚质量/g样品质量/g灼烧后坩埚加样品质量增重率/%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#样品（灰分含量范围≤0.300%）：称取500g研磨过筛的干基高纯石墨样品（不），9#样品（灰分含量范围0.300%～0.600%）：称取200g研磨过筛的干基高纯石墨样），），4#样品（灰分含量范围1.50%～3.00%）：称取200g研磨过筛的干基高纯石墨样品），实验室1#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%郴州市产商品质量监督检验所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实验室2#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%湖南省产商品质量监督检验研究院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实验室3#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%永州市产商品质量监督检验所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统计量水平1水平2水平3水平4均值的平均值0.20010.49930.99451.9719均值的标准差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临界值3.3曼德尔的h统计量实验室郴州所省质检院永州所水平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总平均值0.20010.49930.99451.9719T16.602316.475932.820165.0742T21.32108.226032.6411128.3232T3T4363363363363T50.00080.00140.00440.0185r20.0000360.0000640.0002020.000840L2（计算值）-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（计算值）0.01670.02240.03980.0812R（建议值）0.0200.0250.0500.100采用试剂级碳化硅，分别于650℃、700℃、800℃灼烧2h，测定其增重情况，实实验温度/℃坩埚质量/g样品质量/g灼烧后坩埚加样品质量增重率/%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#样品（灰分含量范围≤0.300%）：称取500g研磨过筛的干基高纯石墨样品（不），#样品（灰分含量范围0.300%～0.600%）：称取200g研磨过筛的干基高纯石墨样），），4#样品（灰分含量范围1.50%～3.00%）：称取200g研磨过筛的干基高纯石墨样品），实验室1#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%郴州市产商品质量监督检验所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实验室2#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%湖南省产商品质量监督检验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实验室3#4#ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%ωC/%ωSiC/%永州市产商品质量监督检验所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