鎳合金化學(xué)分析方法 第10部分：痕量元素含量的測(cè)定 輝光放電質(zhì)譜法 編制說明

1根據(jù)全國(guó)有色金屬標(biāo)準(zhǔn)化技術(shù)委員會(huì)《關(guān)于2有限公司運(yùn)營(yíng)管理著國(guó)家有色金屬及電子材料分析測(cè)試中心和國(guó)家有色金屬質(zhì)2004年至今共承擔(dān)了國(guó)家科技支撐計(jì)劃、國(guó)家863計(jì)劃、國(guó)家自然科學(xué)基金、軍工配套等省部級(jí)科技項(xiàng)目40余項(xiàng)；曾獲國(guó)家科技進(jìn)步獎(jiǎng)6項(xiàng)，國(guó)家發(fā)明獎(jiǎng)3利20余項(xiàng)；負(fù)責(zé)和參加起草制訂分析方法國(guó)家標(biāo)準(zhǔn)、行業(yè)標(biāo)準(zhǔn)300余項(xiàng)；國(guó)家標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品120個(gè)，在國(guó)內(nèi)外科技期刊上發(fā)表論文800余篇，撰寫論著表1人員分工表參與單位主要職責(zé)國(guó)標(biāo)（北京）檢驗(yàn)認(rèn)證有限公司標(biāo)準(zhǔn)工作前期調(diào)研、申報(bào)、樣品搜集、實(shí)驗(yàn)方案的確定、標(biāo)準(zhǔn)文本和編制說明的編寫、數(shù)理統(tǒng)計(jì)計(jì)算重復(fù)性限和再現(xiàn)性限深圳市中金嶺南有色金屬股份有限公司、紫金礦業(yè)集團(tuán)股份有限公司、昆明冶金研究院有限公司、上海有色金屬工業(yè)技術(shù)監(jiān)督監(jiān)測(cè)中心有限公司、峨嵋半導(dǎo)體材料研究所、國(guó)合通用（青島）測(cè)試評(píng)價(jià)認(rèn)證股份公司承擔(dān)一驗(yàn)的主要工作，包括對(duì)實(shí)驗(yàn)條件試驗(yàn)、實(shí)驗(yàn)步驟、試劑材料等的驗(yàn)證，并進(jìn)行實(shí)驗(yàn)樣品精密度試驗(yàn)并提供精密度數(shù)據(jù)標(biāo)準(zhǔn)文本、編制說明提出修改意見。金川集團(tuán)股份有限公司、鋼研納克檢測(cè)技術(shù)股份有限公司、廣東先導(dǎo)稀材股份有限公司、山東恒邦冶煉股份有限公司、寧波江豐電子材料股份有限公司承擔(dān)二驗(yàn)的主要工作，進(jìn)行實(shí)驗(yàn)樣品精密度試驗(yàn)并提供精密度數(shù)據(jù)，對(duì)標(biāo)準(zhǔn)文本、編制說明提出修改意見。金川集團(tuán)股份有限公司提供部分統(tǒng)一樣品。3委員會(huì)提交了《鎳合金化學(xué)分析方法第10部分：痕量元素含量年有色金屬國(guó)家標(biāo)準(zhǔn)制（修）訂項(xiàng)目計(jì)劃及征集起草單位的通知》（有色標(biāo)委），法第10部分：痕量元素含量的測(cè)定輝光放電質(zhì)譜法》，項(xiàng)目計(jì)劃編號(hào)為司、山東恒邦冶煉股份有限公司、寧波江豐電子材料股份有4公司為二驗(yàn)單位，負(fù)責(zé)提供精密度試驗(yàn)數(shù)據(jù)，并對(duì)標(biāo)專家對(duì)《鎳合金化學(xué)分析方法第10部分：痕量元素含其中4個(gè)標(biāo)準(zhǔn)樣品，4個(gè)對(duì)應(yīng)牌號(hào)的待測(cè)樣品，金川可補(bǔ)充提供幾個(gè)牌號(hào)的鎳合2024年7月底，主編單位將每塊統(tǒng)一樣品切成兩份，分別寄送給兩家驗(yàn)證5金化學(xué)分析方法第10部分：痕量元素含量的測(cè)定輝光預(yù)審會(huì)，來自XX等單位的XX名專家代表參會(huì)，對(duì)本文件的預(yù)審稿、編制說明進(jìn)行了充分、細(xì)致的討論，并提出修改意見。制組依據(jù)各家單位的意見和對(duì)標(biāo)準(zhǔn)文本進(jìn)行修改，結(jié)構(gòu)和起草規(guī)則》、GB/T20001.4-2015《標(biāo)準(zhǔn)編寫規(guī)則準(zhǔn)》、GB/T6379.2-2004《測(cè)量方法與結(jié)果的準(zhǔn)確度（正確度與精密度)第2部的測(cè)定》、GB/T223《鋼鐵及合金化學(xué)分析方法》系列標(biāo)準(zhǔn)、國(guó)軍標(biāo)GJB87816另外，GB/T14992-2005《高溫合金和金屬間化合物高溫材料的分類和牌號(hào)》中對(duì)鎳基高溫合金中元素含量有明確的規(guī)定，如鎳基高溫合金DD404中過預(yù)濺射可除去樣品表面的污染物。GDMS基體干擾小，測(cè)定下限可低至ng/g定已有非常成熟的應(yīng)用，并形成檢測(cè)標(biāo)準(zhǔn)。本標(biāo)準(zhǔn)發(fā)揮GDMS技術(shù)的優(yōu)勢(shì)，來量限值的要求，如鎳鉻鈷系合金要求Ag含量不大于0.0005%，Bi含量不大于放電條件直接影響樣品測(cè)定結(jié)果的準(zhǔn)確性和可靠7電壓設(shè)置的是最大放電電壓，一般設(shè)置1200V就可滿足絕大多數(shù)基體的測(cè)試需），8表2標(biāo)準(zhǔn)樣品單位：mg/kg值度值度值度值度值度值度度度B//////////////26/////33//////////////2024//////////////P////45//////////2//////////////////////V/////////1////////////2//////////473//553282//////////1/////////////////////////////////////////////////Y///////////////////////////////Nb////////////////////////3////////////////////////////////////32//////////////////////////////////////////////////////////////////////////////////////Hf/////////////////4//////////W/////////475////////////////////////////////////////////////////9表3檢出限單位：mg/kg值123456789B000P0V0000000Y0000Nb00000000HfW形成的質(zhì)譜干擾較多，對(duì)元素含量的測(cè)定可能產(chǎn)生一定所示。然而，理論存在的質(zhì)譜干擾的強(qiáng)度還與合金元素種類、合關(guān)，因此本標(biāo)準(zhǔn)只能給出推薦的測(cè)定分辨率，實(shí)際檢測(cè)中還要根表4質(zhì)譜干擾情況元素質(zhì)量數(shù)干擾離子強(qiáng)度/%理論所需分辨率測(cè)定分辨率Zn6668As7577YZr9091Ag93Nb16O+99.7631474高分辨，或Ag107中分辨Cd中分辨Te中分辨中分辨中分辨Ce高分辨按照標(biāo)準(zhǔn)文本的分析步驟對(duì)8個(gè)牌號(hào)的鎳合金統(tǒng)一樣中32種痕量元素含量進(jìn)行測(cè)定。），表52#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB29.7729.6229.6729.690.2528.3227.6627.6727.88Mg5.025.465.355.284.45.095.585.445.374.68Al////////////////////P72.3472.3772.3572.350.0270.6170.8970.9470.810.25Ca0.160.160.154.720.190.170.200.19Ti//////////V//////////Mn//////////Cu//////////Zn4.104.294.214.202.284.504.354.524.42Ga3.68As9.088.979.159.079.088.929.089.03<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y0.1380.1390.1340.1370.1430.140Zr5.395.595.475.485.585.485.495.52Nb//////////Mo//////////Ag0.2140.2170.2230.2182.100.2340.2130.2240.2204.70Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/8.288.558.558.468.768.898.778.810.782.412.422.412.410.322.592.652.642.63Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ce<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf0.0130.0130.0170.0140.0110.0140.0150.013Ta58.1758.7758.5658.500.5259.5860.4659.5859.970.75W37.0237.5937.1337.250.8238.5738.0538.0538.220.78Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb0.720.710.730.720.730.690.730.723.19Bi0.0240.0170.0190.0200.0270.0200.0200.022表64#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB38.7638.2238.7838.590.8240.1339.0039.2439.46Mg0.230.240.230.232.720.220.220.230.223.16Al//////////2.00.45P0.53Ca0.0660.0490.0540.0560.0620.0490.0530.055Ti//////////V//////////Mn64.2364.3464.4064.3265.9465.5565.6765.720.30Cu52.5753.7353.5553.2854.6554.4255.1354.730.66Zn0.210.230.220.225.940.210.220.260.23Ga8.938.838.858.870.639.259.179.139.180.66As2.012.062.022.033.53<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y0.510.520.540.523.350.530.580.560.56Zr//////////Nb206.5209.2208.3208.00.67205.5201.3202.6203.1Mo//////////Ag0.520.560.490.536.390.660.620.630.643.2Cd<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/7.037.166.847.012.276.936.906.886.910.370.780.800.770.782.180.780.840.820.814.05Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ce<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf0.710.9560.9540.9340.948Ta0.962.72W//////////Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb0.1010.1180.0980.1060.0990.0970.1060.1014.70Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表76#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB//////////Mg24.9225.4525.3525.2425.5125.5725.5225.53Al////////////////////P//////////Ca0.5090.4800.4130.4670.6000.5980.5890.5960.98Ti//////////V0.190.74Mn//////////Cu//////////Zn6.216.160.725.956.096.136.06Ga20.3720.1520.2920.270.5520.6320.5820.8420.680.66As4.564.764.704.672.224.204.234.274.230.86<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y0.0610.0640.0590.0614.100.0670.0720.0690.0693.63Zr2.222.202.272.232.892.842.912.88Nb//////////Mo//////////Ag//////////Cd//////////6.817.166.996.992.458.267.788.078.033.032.28Te0.0150.0150.0170.0167.370.0760.0530.0530.06121.9La0.0280.0280.0300.0294.030.0430.0460.0400.0436.98Ce<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf//////////Ta95.5996.5995.9796.050.53W//////////Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb0.8370.8100.8100.8190.8550.8910.9250.893.93Bi0.0100.0190.0070.01252.00.0090.0150.0100.01128.4表88#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB45.0344.1044.5344.5542.5942.3241.8542.250.89Mg2.742.772.742.750.642.672.742.812.742.63Al74.6574.7073.9474.430.5773.7574.3675.5274.54//////////PCa2.342.02Ti2.852.13V//////////Mn//////////Cu//////////Zn7.016.987.267.082.176.987.096.866.98Ga0.620.76As27.4127.1527.3327.300.4927.3727.4927.0527.300.84<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y//////////Zr4.814.814.964.865.025.265.345.213.17Nb//////////Mo20372025204620360.5120452083205720620.95Ag3.733.793.923.812.623.923.904.033.95Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/30.2031.1531.2530.8731.9232.6431.9032.157.427.227.517.382.027.447.437.597.49Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La0.0590.0610.0660.0625.820.0700.0670.0680.0682.23Ce0.1290.1250.1330.1293.100.1380.1370.1450.140Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf0.1350.1340.1250.1314.190.1430.1370.1402.18Ta36.5735.9336.8436.4538.3138.1838.0738.20.32W//////////Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb2.420.27Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表910#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB0.7820.7890.7860.7860.520.7030.6520.6940.6834.05Mg30.9231.2331.4831.210.8931.5631.6832.3331.86Al////////////////////P0.190.71Ca6.156.266.356.256.676.697.056.803.17Ti//////////V2.632.642.642.640.342.652.552.572.59Mn//////////Cu48.3248.7049.3348.7849.4948.9048.85Zn5.416.89Ga3.423.463.493.463.543.473.473.49As6.256.135.926.102.716.136.066.22<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Zr0.1450.1510.1560.1513.670.1470.1610.1690.159Nb0.88Mo//////////Ag0.1040.0700.0810.08520.20.0880.1090.1100.102Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/0.9190.8890.9390.9162.770.9130.8400.9920.9158.290.7590.7760.7140.7504.270.8220.7650.7850.7913.69Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La0.0820.0820.0810.0820.430.0830.0830.0940.0877.37Ce0.1600.1580.1580.1590.890.1670.1690.1630.166Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ta0.0500.0570.0620.0570.0570.0500.0450.051W3.073.023.073.163.273.283.23Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb2.75Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表1012#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB0.3870.3800.3690.3782.430.3720.3530.3380.3544.80Mg2.953.002.912.952.752.762.802.770.99Al////////////////////P2.06Ca//////////Ti//////////V0.100.24Mn0.590.84Cu//////////Zn8.949.71GaAs3.033.043.003.020.753.032.972.912.97<0.5<0.5<0.5<0.5/<0.5<0.5<0.5<0.5/Y0.0170.0190.0190.0195.400.0190.0170.0200.0198.06Zr0.1100.1010.0980.1036.070.1090.1186.50Nb//////////Mo//////////Ag0.1040.0840.1030.0970.1250.0830.1200.10921.3Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/0.5220.5800.5190.5406.430.5490.5890.4810.5400.1200.1360.1328.610.1350.1139.04Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ce<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ta3.613.723.693.673.943.843.893.89W52.3353.0851.9352.4554.8154.7254.9354.820.19Tl0.0080.0140.0150.01231.40.0140.0130.0140.0136.20Pb0.103.03Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表1114#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB0.3940.4430.3930.4136.490.4190.4450.4160.4273.78Mg5.57Al23.2823.1623.3323.260.3825.2723.9322.7824.095.83//////////P0.310.30Ca3.252.993.184.223.173.082.883.045.01Ti4.414.484.474.450.874.534.544.524.530.21V0.73Mn//////////Cu55.2955.7455.1355.390.5755.9156.2556.5356.230.55Zn0.200.200.170.190.220.230.220.22Ga5.085.105.160.805.255.245.315.270.77As7.077.137.100.387.437.367.317.370.812.282.68Y0.0110.0120.0110.0116.660.0120.0130.0090.011Zr0.4410.3840.4240.4177.100.4410.4270.4120.4273.40Nb0.3900.4110.4120.4040.4190.4100.4200.416Mo20.2320.000.99Ag0.0650.0670.0840.0720.0740.0730.0890.079Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/4.454.204.274.313.034.464.684.554.572.442.24Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La0.0240.0230.0220.0235.930.0230.0210.0250.023Ce0.0500.0480.0520.0504.340.0570.0470.0430.049Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ta0.0380.0380.0320.0369.050.0280.0300.0280.0294.51W0.76Tl<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Pb0.2710.2810.2840.2750.3040.2760.3050.2955.60Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表1216#鎳合金測(cè)定結(jié)果的精密度單位：mg/kg元素第一點(diǎn)第二點(diǎn)123平均RSD123平均RSDB0.3230.3810.3210.3410.3540.3410.3310.3423.45Mg0.9120.9040.8860.9010.9680.9710.8630.9346.60Al//////////P7.527.837.867.742.477.587.667.727.650.88Ca0.0990.1160.1097.700.0830.1020.1320.10623.6Ti6.566.656.586.590.716.656.706.696.680.37V0.8010.8020.8100.8040.670.8010.8020.8000.801Mn//////////Cu27.3427.2527.2727.290.1627.3227.4527.3727.380.24Zn0.2100.1400.1980.18320.60.1510.1360.2200.16926.7Ga0.72As2.943.023.063.013.073.032.963.028.958.35Y<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Zr0.0980.1010.1060.1023.910.1080.1030.0870.099Nb4.224.224.154.200.944.334.284.274.290.79Mo//////////Ag0.0620.0640.0860.0710.0840.0500.0590.06427.6Cd<0.1<0.1<0.1<0.1/<0.1<0.1<0.1<0.1/0.9880.9840.9960.9900.620.400.4690.4600.4750.4680.4910.4850.4950.490Te<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/La0.0660.0650.0620.0653.430.0620.0870.0830.078Ce<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Yb<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Hf<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/Ta0.0380.0330.0440.0380.0370.0380.0360.037W0.800.73Tl0.0340.0330.0270.0320.0290.0240.0120.02240.2Pb0.2770.2710.2710.2730.2770.2930.3200.2977.44Bi<0.01<0.01<0.01<0.01/<0.01<0.01<0.01<0.01/表13實(shí)驗(yàn)室序號(hào)及名稱序號(hào)單位名稱1國(guó)標(biāo)（北京）檢驗(yàn)認(rèn)證有限公司2鋼研納克檢測(cè)技術(shù)股份有限公司3金川集團(tuán)股份有限公司4寧波江豐電子材料股份有限公司5國(guó)合通用（青島）測(cè)試評(píng)價(jià)認(rèn)證股份公司6廣東先導(dǎo)稀材股份有限公司7深圳市中金嶺南有色金屬股份有限公司8上海有色金屬工業(yè)技術(shù)監(jiān)督監(jiān)測(cè)中心有限公司9紫金礦業(yè)集團(tuán)股份有限公司昆明冶金研究院有限公司峨嵋半導(dǎo)體材料研究所山東恒邦冶煉股份有限公司在每個(gè)樣品水平中將各實(shí)驗(yàn)室精密度測(cè)試結(jié)果的平均值重新組成一組新的數(shù)據(jù)組，視表14格拉布斯檢驗(yàn)結(jié)果元素樣品號(hào)實(shí)驗(yàn)室序號(hào)λ(0.05,n)Gmax有無離群值是否舍去B22N否44N否24N否43N否63Y是82Y是44N否P21N否44N否87N否84N否84N否V6Y是44N否41N否22N否45N否23N否26N否Nb42N否85N否22N否45N否64N否85N否22N否45N否Hf45N否25N否46N否63Y是W25Y是采用科克倫（Cochran）檢驗(yàn)法對(duì)每個(gè)樣品剔除離群值后的不同實(shí)值之間進(jìn)行等精度檢驗(yàn)。先計(jì)算m組數(shù)據(jù)的各表15科克倫檢驗(yàn)結(jié)果統(tǒng)計(jì)C(0.05,n)C43Y是86Y是P27Y是87Y是86Y是Nb46Y是86Y是45Y是22Y是44Y是根據(jù)GB/T6379.2-2004的要求對(duì)每個(gè)樣品水平的測(cè)試數(shù)據(jù)進(jìn)行統(tǒng)計(jì)，計(jì)算方法的重復(fù)表16重復(fù)性限和再現(xiàn)性限計(jì)算結(jié)果總平均值x/(mg/kg)/////////再現(xiàn)性方差sR2///////////////總平均值x/(mg/kg)//////再現(xiàn)性方差sR2////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)//////再現(xiàn)性方差sR2//////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2///////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)/////////再現(xiàn)性方差sR2///////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)////////////再現(xiàn)性方差sR2////////////////////總平均值x/(mg/kg)///再現(xiàn)性方差sR2/////總平均值x/(mg/kg)/////////再現(xiàn)性方差sR2//////////////總平均值x/(mg/kg)/////////再現(xiàn)性方差sR2///////////////總平均值x/(mg/kg)///再現(xiàn)性方差sR2/////總平均值x/(mg/kg)/////////再現(xiàn)性方差sR2///////////////表17各樣品水平的平均值、重復(fù)性限（r）和再現(xiàn)性限（R）R/(mg/kg)R/(mg/kg)BNbPHfVW鎳合金作為一類重要的戰(zhàn)略性材料，具有良好的高溫強(qiáng)度和優(yōu)良的耐磨損、耐高溫、抗熱震沖擊、抗氧化性能抗腐蝕、抗疲勞性能，主要用于石油、化工、環(huán)保、航天以及核工業(yè)等行業(yè)的各類零部件的制造、修復(fù)和預(yù)保護(hù)?！吨袊?guó)制造2025》等戰(zhàn)略規(guī)劃將高溫合金和金屬間化合物高溫材料的分類和牌號(hào)》中對(duì)鎳基高溫合金中元素含量有明確的規(guī)定，w(Zn)≤0.0005%，w(Pb)≤0.0002%，w(Sb)≤0.0005%，w(As)≤0.0005%，w(Ag)≤0.0005%，然而，目前，鎳合金中痕量元素的分析方法主要有基于分離技術(shù)的分光光度法、原子雜，受到的光譜和質(zhì)譜干擾嚴(yán)重，受到儀器及方法特性的影響，測(cè)定下限較高，無法滿足鎳合金中痕量元素的分析要求。迫切需要一種高靈敏度、低檢出限、固體直接進(jìn)樣的分析除去樣品表面的污染物。GDMS基體干擾小，分辨率高，可分辨絕大多數(shù)質(zhì)譜干擾，測(cè)定有輝光放電質(zhì)譜儀，輝光放電質(zhì)譜法在高純鎳、高純鈷、高純銅、高純鋁、高純鋅、高純鈦、高純錸、高純鎢、高純鈮、高純鉭等有色金屬中痕量元素含量的測(cè)定已有非常成熟的應(yīng)用，并形成檢測(cè)標(biāo)準(zhǔn)。本標(biāo)準(zhǔn)正是基于GDMS技術(shù)的優(yōu)勢(shì)，結(jié)合鎳合金測(cè)需求提出的，采GDMS法對(duì)鎳合金中痕量雜質(zhì)元素進(jìn)行測(cè)定。本標(biāo)準(zhǔn)對(duì)于價(jià)體系、提升產(chǎn)品質(zhì)量、指導(dǎo)產(chǎn)品應(yīng)用具、促鎳合金因其獨(dú)特的物理化學(xué)性質(zhì)和廣泛的應(yīng)用領(lǐng)域，市場(chǎng)需求持續(xù)攀升。特別是在航空航天、石油化工、能源電力、海洋工程等關(guān)鍵領(lǐng)域，鎳合金的應(yīng)用日益廣泛，推動(dòng)了市場(chǎng)規(guī)模的不斷擴(kuò)大。新能源汽車和高端裝備制造等新興領(lǐng)域的快速發(fā)展，進(jìn)一步增加了對(duì)根據(jù)產(chǎn)品標(biāo)準(zhǔn)的要求，不同牌號(hào)的鎳合金中元素含量有明確的限制，本標(biāo)準(zhǔn)屬于分析金化學(xué)分析方法》等標(biāo)準(zhǔn)的補(bǔ)充完善,與以上標(biāo)準(zhǔn)相比，降低了檢測(cè)下限，能夠滿足鎳合金鎳合金產(chǎn)業(yè)的快速發(fā)展離不開分析技術(shù)的支持,鎳合金分析檢測(cè)標(biāo)準(zhǔn)的制定與完善將帶本文件充分考慮了目前國(guó)內(nèi)鎳合金生產(chǎn)、研發(fā)、應(yīng)用和檢測(cè)的實(shí)際技術(shù)水平。本文件頒布執(zhí)行后，能夠推動(dòng)鎳合金檢測(cè)的標(biāo)準(zhǔn)化，提高數(shù)據(jù)的準(zhǔn)確度和一致性，助力我國(guó)鎳合金產(chǎn)本文件與有關(guān)的現(xiàn)行法律、法規(guī)和強(qiáng)制性國(guó)家標(biāo)準(zhǔn)沒有沖突。標(biāo)準(zhǔn)涉及內(nèi)容全面、條工鎳及鎳合金牌號(hào)和化學(xué)成分》、GB/T1499建議向鎳合金研發(fā)、生產(chǎn)、銷售、檢測(cè)的相關(guān)企業(yè)123456B123456789123456789P123456789123456789123456789123456789123456789123456789Y123456789123456789123456789123456789123456789123456789123456789123456789123456789123456789Hf123456789123456789W123456789123456789123456789123456789123456B123456789123456789123456789P1234567891234567891234567891234567891234567891234567891234567891<0.5<0.5<0.5<0.5<0.5<0.52<0.5<0.5<0.5<0.5<0.5<0.53<0.5<0.5<0.5<0.5<0.5<0.54<0.5<0.5<0.5<0.5<0.5<0.55<0.5<0.5<0.5<0.5<0.5<0.56<0.5<0.5<0.5<0.5<0.5<0.57<0.5<0.5<0.5<0.5<0.5<0.589Y123456789Nb123456789123456789123456789123456789123456789123456789123456789123456789123456789Hf123456789123456789123456789123456789123456789123456123456789123456789V123456789123456789120.3720.1520.2920.6320.5820.842321.4621.2520.97432.1734.3334.8537.7138.1738.35520.0720.6920.5720.226721.2721.0121.1321.3620.8920.34891234567891<0.5<0.5<0.5<0.5<0.5<0.52<0.5<0.5<0.5<0.5<0.5<0.53<0.5<0.5<0.5<0.5<0.5<0.54<0.5<0.5<0.5<0.5<0.5<0.55<0.5<0.5<0.5<0.5<0.5<0.56<0.5<0.5<0.5<0.5<0.5<0.57<0.5<0.5<0.5<0.5<0.5<0.589Y123456789123456789123456789123456789123456789123456789123456789123456789123456789123456789123456789123456B123456789123456789123456789P1234567891234567891234567891234567891234567891234567891<0.5<0.5<0.5<0.5<0.5<0.52<0.5<0.5<0.5<0.5<0.5<0.53<0.5<0.5<0.5<0.5<0.5<0.54<0.5<0.5<0.5<0.5<0.5<0.55<0.5<0.5<0.5<0.5<0.5<0.56<0.5<0.5<0.5<0.5<0.5<0.57<0.5<0.5<0.5<0.5<0.5<0.589123456789123456789123456789123456789123456789123456789123456789123456789123456789123456789Hf123456789123456789123456789123456789123456789表B.1格拉布斯檢驗(yàn)數(shù)據(jù)統(tǒng)計(jì)元素B的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507λ(0.05,10)=2.507//λ(0.01,10)=1.472λ(0.01,10)=1.472/NN//元素Mg的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%//λ(α,n)元素Al的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507/λ(0.01,10)=1.472Y/元素Si的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素P的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507λ(0.05,10)=2.507λ(0.05,10)=2.507/λ(0.01,10)=1.472λ(0.01,10)=1.472λ(0.01,10)=1.472NNN/元素Ca的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507/λ(0.01,10)=1.472N/元素Ti的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507/λ(0.01,10)=1.472N/元素V的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/NNY//元素Mn的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素Cu的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%//N//元素Ga的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507λ(0.05,10)=2.507//λ(0.01,10)=1.472λ(0.01,10)=1.472/NN//元素As的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素Zr的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素Nb的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素Mo的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507/λ(0.01,10)=1.472N/元素B的質(zhì)量分?jǐn)?shù)/%/1//2//3//4//5//6/7///s/%//λ(α,n)λ(0.05,10)=2.507λ(0.05,10)=2.507λ(0.05,10)=2.507λ(0.05,10)=2.507/λ(0.01,10)=1.472λ(0.01,10)=1.472λ(0.01,10)=1.472λ(0.01,10)=1.472NNNN/元素Sb的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%//λ(α,n)元素Hf的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/N//元素Ta的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507λ(0.05,10)=2.507λ(0.05,10)=2.507//λ(0.01,10)=1.472λ(0.01,10)=1.472λ(0.01,10)=1.472/NNY//元素W的質(zhì)量分?jǐn)?shù)/%/1////2////3////4////5////6//7//////s/%////λ(α,n)λ(0.05,10)=2.507//λ(0.01,10)=1.472/Y//表C.1各元素科克倫檢驗(yàn)結(jié)果B元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.0760.00630.3183///第2點(diǎn)0.37830.5950.3543///20.01330.890.7873///第2點(diǎn)0.02130.590.3513///30.700.49530.403///第2點(diǎn)0.250.06030.610.3733///40.890.79430.960.9173///第2點(diǎn)0.710.50631.9073///50.040.00230.353///第2點(diǎn)0.3830.0323///60.540.29731.0733///第2點(diǎn)0.210.04230.780.608370.460.21430.730.5283第2點(diǎn)0.4531.0783Cmax0.27000.2272C(α,m,n-1)C(0.05,14,2)=0.3346C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069C(0.01,14,2)=0.4069///結(jié)論等精度等精度///Mg元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s23s/(mg/kg)s2n10.2290.05230.00580.0000330.2820.0793///第2點(diǎn)0.2520.06430.00580.0000330.0320.0013///20.03830.01050.0001130.050.0033///第2點(diǎn)0.090.00830.00750.0000630.0383///30.220.04930.01370.0001930.250.061////第2點(diǎn)0.040.00130.01660.000283//3///40.01030.01050.0001130.600.3623///第2點(diǎn)0.090.00830.01350.0001830.070.0063///50.010.00030.00700.0000530.0263///第2點(diǎn)0.080.00730.00400.0000230.343///60.060.00430.00580.0000330.750.5633///第2點(diǎn)0.02230.01150.0001330.700.490370.3530.05030.002530.790.6253第2點(diǎn)0.070.00530.04510.002030.6250.0393Cmax0.31240.43770.4377C(α,m,n-1)C(0.05,14,2)=0.3346C(0.05,14,2)=0.3346C(0.05,13,2)=0.3924///C(0.01,14,2)=0.4069C(0.01,14,2)=0.4069C(0.01,13,2)=0.4751///結(jié)論等精度有離群值等精度///Al元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.425///第2點(diǎn)0.8990.808///2/////第2點(diǎn)3.7213.816///30.700.496///第2點(diǎn)0.720.520///41.851///第2點(diǎn)///51.297///第2點(diǎn)2.242///60.470.217///第2點(diǎn)4.9824.77470.070.006第2點(diǎn)2.566.546Cmax0.4435C(α,m,n-1)C(0.05,13,2)=0.3346///C(0.01,13,2)=0.4069///結(jié)論有離群值///Si元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n12.9098.4633///第2點(diǎn)0.6430.4133///21.0813///第2點(diǎn)3///3101.9823///第2點(diǎn)2.626.8523///47.7560.0833///第2點(diǎn)0.770.5963///58.9780.3793///第2點(diǎn)0.383///64.4533///第2點(diǎn)2.836373.9415.5073第2點(diǎn)2.9133Cmax0.3530C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有離群值///P元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.0150.00030.0710.00531.4982.2433///第2點(diǎn)0.03230.03131.5502.4033///20.8490.72230.080.00632.4473///第2點(diǎn)0.4990.24930.250.06230.730.5293///30.7660.58730.450.20130.343///第2點(diǎn)0.7700.59430.230.05430.200.0383///44.63530.200.03832.7793///第2點(diǎn)0.7360.54230.240.06030.760.5733///50.3090.09530.070.00530.670.4523///第2點(diǎn)0.3070.09430.210.04430.640.4093///61.5662.45430.4130.990.9733///第2點(diǎn)1.37930.720.52530.310.093373.0619.36730.03331.3211.7453第2點(diǎn)5.04425.44430.4790.22932.8077.8793Cmax0.55080.35970.3474C(α,m,n-1)C(0.05,14,2)=0.3346C(0.05,14,2)=0.3346C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069C(0.01,14,2)=0.4069C(0.01,14,2)=0.4069///結(jié)論有離群值有歧離值等精度///Ca元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.2800.0783///第2點(diǎn)0.2620.0693///20.270.0753///第2點(diǎn)0.363///30.353///第2點(diǎn)0.0103///40.353///第2點(diǎn)0.570.3263///50.0273///第2點(diǎn)0.0233///61.0213///第2點(diǎn)0.300.088370.0333第2點(diǎn)1.7593.0933Cmax0.5922C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有離群值///Ti元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n14.23417.9233///第2點(diǎn)3.26510.6633///23.2710.7233///第2點(diǎn)2.7833///32.2803///第2點(diǎn)3.5812.8043///42.797.7973///第2點(diǎn)0.680.4633///51.6473///第2點(diǎn)3.7714.2143///612.78163.2433///第2點(diǎn)4.2818.303370.7200.5193第2點(diǎn)2.7887.7753Cmax0.6021C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有離群值///V元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.2310.0533///第2點(diǎn)0.9870.9733///2//////第2點(diǎn)//////31.4553///第2點(diǎn)//////42.673///第2點(diǎn)0.950.9063///50.343///第2點(diǎn)0.0323///62.888.3203///第2點(diǎn)2.204.853370.353第2點(diǎn)1.7253Cmax0.3239C(α,m,n-1)C(0.05,11,2)=0.3924///C(0.01,11,2)=0.4751///結(jié)論有離群值///Mn元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.0860.0073///第2點(diǎn)0.2000.0403///20.333///第2點(diǎn)0.610.3673///30.970.9353///第2點(diǎn)0.423///41.3883///第2點(diǎn)0.520.2743///51.6633///第2點(diǎn)0.640.4143///60.710.4983///第2點(diǎn)0.530.284371.4011.9623第2點(diǎn)0.0333Cmax0.2408C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論等精度///Cu元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.6240.3903///第2點(diǎn)0.3623///20.540.2923///第2點(diǎn)0.0253///30.383///第2點(diǎn)0.0203///40.720.5183///第2點(diǎn)0.510.2633///50.060.0043///第2點(diǎn)0.353///61.3523///第2點(diǎn)3.219371.3741.8893第2點(diǎn)4.4493Cmax0.3470C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有歧離值///Ga元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.5800.33730.0530.0033///第2點(diǎn)0.03830.0610.0043///20.030.00130.020.0003///第2點(diǎn)0.080.00730.0103///30.230.05330.413///第2點(diǎn)0.02230.260.0693///40.02530.060.0033///第2點(diǎn)0.4330.090.0083///50.030.00130.080.0063///第2點(diǎn)0.01430.050.0023///60.3330.250.0633///第2點(diǎn)0.610.37330.270.075370.520.26930.230.0513第2點(diǎn)0.02430.220.0493Cmax0.25640.3314C(α,m,n-1)C(0.05,14,2)=0.3346C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069C(0.01,14,2)=0.4069///結(jié)論等精度等精度///As元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.0910.0083///第2點(diǎn)0.0920.0093///20.270.0723///第2點(diǎn)0.090.0083///30.353///第2點(diǎn)0.250.0653///40.210.0443///第2點(diǎn)0.0103///50.050.0033///第2點(diǎn)0.0183///60.060.0043///第2點(diǎn)0.020370.270.0713第2點(diǎn)0.250.0623Cmax0.2378C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論等精度///Zr元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.0103///第2點(diǎn)0.0550.0033///20.260.0683///第2點(diǎn)0.040.0013///30.060.0043///第2點(diǎn)0.050.0023///40.230.0553///第2點(diǎn)0.423///50.0343///第2點(diǎn)0.060.0043///60.0123///第2點(diǎn)0.240.060370.530.2823第2點(diǎn)0.250.0613Cmax0.3631C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有歧離值///Nb元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n11.3751.8903///第2點(diǎn)4.6233///22.5263///第2點(diǎn)2.375.6303///31.4393///第2點(diǎn)2.918.4823///45.7332.8513///第2點(diǎn)2.3133///54.263///第2點(diǎn)1.2983///66.9247.8643///第2點(diǎn)11.01121.228375.3728.8203第2點(diǎn)2.094.3473Cmax0.4308C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有歧離值///Mo元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n110.536111.003///第2點(diǎn)19.425377.333///243.251870.423///第2點(diǎn)32.911082.793///3230.083///第2點(diǎn)7.5456.843///40.000.003///第2點(diǎn)50.542554.333///584.393///第2點(diǎn)14.21202.023///6118.2113973.293///第2點(diǎn)171.6029445.94373.26510.663第2點(diǎn)17.039290.333Cmax0.5855C(α,m,n-1)C(0.05,14,2)=0.3346///C(0.01,14,2)=0.4069///結(jié)論有離群值///Sn元素科克倫（Cochran）檢驗(yàn)結(jié)果樣品編號(hào)2#4#6#8#單位序號(hào)s/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2ns/(mg/kg)s2n10.02430.02630.03130.5800.3363///第2點(diǎn)0.0720.00530.0250.00130.2420.05830.4223///20.03130.03030.01330.580.3363///第2點(diǎn)0.040.00230.03430.02230.590.3473///30.3230.3530.02630.0113///第2點(diǎn)0.4030.02830.03530.270.0703///40.02730.01130.01430.820.6