鐠釹金屬化學(xué)分析方法主起草單位實(shí)驗(yàn)報(bào)告

鐠釹金屬化學(xué)分析方法碳、鐵、鉬、鋁、硅和鐠含量的測(cè)定火花放電原子發(fā)射光譜法主起草單位實(shí)驗(yàn)報(bào)告3鐠釹金屬化學(xué)分析方法碳、鐵、鉬、鋁、硅和鐠含量的測(cè)定火花放電原子發(fā)射光譜法含量。對(duì)此，我們進(jìn)行了詳細(xì)的條件實(shí)驗(yàn)和精密度實(shí)驗(yàn)，結(jié)果如下：共收集到30塊實(shí)驗(yàn)用樣品，先用稀土金屬快速分析儀檢驗(yàn)樣品均勻度，然黃色底紋和紅色底紋表示。從結(jié)果可以看出，樣品PNMo-10的Mo存在離群27個(gè)樣品均勻度較好，各元素測(cè)試結(jié)果不存在歧離值或離群值，可用于本次校4取紅外吸收法測(cè)定，其余元素均采用ICP-AES或ICP-MS法測(cè)定，為確保定值樣品CFeMoAlPr1<0.00052<0.00053<0.00054<0.0005<0.00051<0.000522<0.000523<0.000524<0.000583-187平均值0.0170.045<0.00050.0070.01520.6361<0.000572<0.00053<0.00054<0.000518-193平均值0.0310.183<0.00050.0100.02223.27416<0.00054<0.01020<0.00054<0.01036<0.00058<0.01045<0.00053<0.0104-187平均值0.0100.017<0.00050.004<0.01020.7151<0.0005522<0.000503<0.000574<0.000553-55平均值0.1070.180<0.00050.0070.0201<0.000582<0.00053<0.000534<0.000599-201平均值0.0800.168<0.00050.0060.01124.6821<0.000582<0.000523<0.000534<0.0005322-114平均值0.0230.049<0.00050.0060.00923.6901<0.000532<0.000533<0.000534<0.000546-59平均值0.0700.492<0.00050.0040.0111<0.00052<0.00053<0.00054<0.00051-167平均值0.0850.188<0.00050.0100.02620.0321<0.00052<0.00053<0.00054<0.000561-191平均值0.0310.133<0.00050.0160.02920.4611<0.000532<0.000593<0.000574<0.0005920-193平均值0.0120.034<0.00050.0080.01123.1271<0.000522<0.000533<0.000584<0.000531-1平均值0.1010.412<0.00050.0070.0201923489-200平均值0.4730.00090.0260.03633.2031<0.00052<0.00053<0.00054<0.00056-187平均值0.0260.146<0.00050.0240.04120.2461<0.000522<0.000523<0.000534<0.000562-1平均值0.159<0.00050.0080.02910.015820.015830.0159740.015727平均值0.0640.3230.0160.0220.04910.015020.015430.015340.0155502平均值0.0350.3450.0150.0360.04923.42010.0096320.0096630.009440.00967538平均值0.0380.4670.0100.0370.04310.0060220.0059230.0059140.00594503平均值0.0160.2040.0060.0670.07523.48510.0257（0.0813）20.0264（0.0829）30.0254（0.0763）40.0257（0.0801）539平均值0.0860.2750.0260.060（0.080）1<0.00052<0.00053<0.00054<0.000519#平均值0.0340.325<0.00050.1770.13825.7251<0.00052<0.00053<0.00054<0.00059#平均值0.0110.090<0.00050.0210.01810.053820.054030.053840.0537PNMo-7平均值0.0380.4140.0540.0130.03323.91710.060020.061230.061640.0603PNMo-8平均值0.0210.1460.0610.0150.01823.725810.064520.063630.063640.0623PNMo-9平均值0.0230.2880.0640.0300.03224.114名稱CAl9#0.0110.090/0.0210.01816.8900.0640.3230.0160.0220.04918.7210.0380.4670.0100.0370.04319.0823-550.1070.180/0.0070.02019.4302-10.1591.083/0.0080.02919.7124-1870.0100.017/0.004/20.71511-2010.0370.214/0.0410.10522.88220-1930.0120.034/0.0080.01123.1270.0160.2040.0060.0670.07523.48522-1140.0230.049/0.0060.00923.690PNMo-80.0210.1460.0610.0150.01823.725PNMo-70.0380.4140.0540.0130.03323.917PNMo-90.0230.2880.0640.0300.03224.1149-2010.0800.168/0.0060.01124.6820.0340.325/0.1770.13825.725NCS2030360.0901.4800.00780.00870.04530.829-2000.4731.2610.00090.0260.03633.203NCS2030350.0460.560.0320.0190.02320.850.0860.2750.0260.060（0.080）18.798曲線范圍0.010-0.4730.017-1.4800.0009-0.0.0009-0.0.004-0.1770.009-0.13816.890-33.203064064產(chǎn)品標(biāo)準(zhǔn)18.0-32.0表3精密度實(shí)驗(yàn)樣品參考含量C9/（0.080）//0光譜分解后，對(duì)選定的內(nèi)標(biāo)線和分析線的強(qiáng)度進(jìn)行測(cè)量，根據(jù)標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品制作的校準(zhǔn)曲線，求出分析樣品中待測(cè)元素的2.儀器主要工作條件：實(shí)驗(yàn)采用一次積分，充氣、預(yù)燃、積分各階段具體參數(shù)見(jiàn)表4。靜止流量0.07L/min，分析流量9L/min。實(shí)驗(yàn)過(guò)程中選用的分析//6C分別考察了砂帶機(jī)磨樣和銑床制樣兩種制樣方式，并給出了推薦標(biāo)準(zhǔn)偏差（RSD）的平均值作為衡量標(biāo)準(zhǔn)之間，測(cè)試結(jié)果無(wú)顯著差異，因此推薦采用40-80目砂帶制樣。本實(shí)驗(yàn)工作曲砂帶粒度統(tǒng)計(jì)結(jié)果CFeMoAlSiPr含量參考值40#第一次RSD%第二次RSD%RSD%平均值60#第一次RSD%4.921第二次RSD%RSD%平均值80#第一次RSD%4.978第二次RSD%RSD%平均值砂帶粒度統(tǒng)計(jì)結(jié)果CFeMoAlSiPr含量參考值40#第一次RSD%0第二次RSD%0RSD%平均值60#第一次RSD%第二次RSD%0RSD%平均值80#第一次RSD%第二次RSD%RSD%平均值60mm/min，對(duì)比轉(zhuǎn)速分別為90r/min、187r/min、270r/min時(shí)樣品測(cè)試結(jié)果統(tǒng)計(jì)值，表中用灰色底紋標(biāo)注了各元素RSD最小的數(shù)據(jù)。從表8、9可以看銑床轉(zhuǎn)速r/min統(tǒng)計(jì)結(jié)果CFeMoAlSiPr含量參考值90第一次RSD%4.326第二次RSD%RSD%平均值第一次RSD%第二次RSD%4.696RSD%平均值270第一次RSD%第二次RSD%4.316RSD%平均值銑床轉(zhuǎn)速r/min統(tǒng)計(jì)結(jié)果CFeMoAlSiPr含量參考值90第一次RSD%第二次RSD%4.716RSD%平均值第一次RSD%0第二次RSD%4.235RSD%平均值270第一次RSD%第二次RSD%4.084RSD%平均值4個(gè)點(diǎn)，測(cè)試點(diǎn)位置避開(kāi)樣品中心和樣品表面缺陷位置，均以各元素分析線強(qiáng)度與參比線強(qiáng)度比值（相對(duì)強(qiáng)度）為橫坐標(biāo)，以各元素強(qiáng)度校正樣品。本方法選取9-200、PNMo-8、503、9#等4塊樣品作為各元），C/82.測(cè)試精密度實(shí)驗(yàn)樣品所列9#，503，PNMo-8，PNMo-9，19#，502，539，2-1，9-200九塊樣11)=2.564,G單(0.01，10)=2.482,G雙(0.01，11)=0.1448，G樣品測(cè)定結(jié)果/%平均值/%標(biāo)準(zhǔn)偏差/%RSD/%123456789樣品1C//////////////樣品2C樣品3C樣品4C樣品5C//////////////樣品6C樣品7C樣品8C//////////////樣品9C43.97元素樣品號(hào)單大值單小值G單大G單小檢驗(yàn)結(jié)果（單大大）檢驗(yàn)結(jié)果（單?。╇p大值雙小值G雙大G雙小檢驗(yàn)結(jié)果 大)檢驗(yàn)結(jié)果(雙小)C1.39681.27530.00730.00730.00650.00650.52310.60241.65801.80490.01310.01290.01160.01210.49150.5649樣品32.03501.38860.02010.02030.01900.01920.21890.67661.47511.40960.02140.02150.02070.02080.58370.62412.07091.80800.03930.04110.03560.03670.41530.47691.91511.55150.03190.03270.03010.03022.23581.02090.08520.08630.08340.08360.47640.46022.35021.19250.15010.15190.14820.14850.28360.79571.52461.47300.46850.45350.30990.72690.46880.45531.24121.75580.07860.07870.07780.07790.45330.58281.77291.39620.17780.17900.16860.16960.71210.3770樣品31.37671.52400.12270.12330.11560.11640.37530.61721.27351.64410.26330.26510.25050.25090.60710.53451.89371.49600.29790.29990.28270.28530.70110.37061.80201.21820.30530.30780.29200.29240.28860.61112.05541.17950.23390.23690.22760.22810.39130.65941.18131.82231.08131.08641.01531.02670.37060.70671.24121.75580.07860.07870.07780.07790.71590.3770////////0.71210.3770//1.28781.70280.00730.00750.00560.0059//樣品31.74281.35550.06210.06320.05840.05850.68270.46302.00991.37550.06690.06830.06340.06380.50400.5718////////0.38380.6219//1.36301.67360.01540.01540.01380.0141//2.15861.38950.02630.02700.02310.02370.54590.5123////////0.15190.6804//2.00771.3726//Al1.69521.31240.01670.01680.01630.01630.29570.66811.45501.78650.06540.06560.06400.06420.50660.5789樣品31.02152.43580.01710.01560.60840.37850.01720.01620.95261.58070.03120.03130.02910.02940.79370.13491.87851.79270.17810.17880.17530.17620.80350.50951.13281.67090.03750.03770.03590.03600.41470.52911.56701.47480.0496004970.0491004910.76180.37850.70722.96610.00600.00610.00580.00580.56540.46832.05161.17230.03580.03610.03490.03490.21740.56161.29901.70920.01960.01970.01890.01900.30320.66402.11931.32450.07780.07880.07620.07620.69120.4273樣品31.81232.10360.02030.02060.01950.01980.39340.57121.71331.34280.03550.03570.03510.03510.54350.34081.64131.53930.13660.13700.13450.13610.59380.55921.90711.79490.04470.04510.04360.04390.87120.76911.34801.38720.06210.06030.46290.47640.06220.06042.06171.12750.02370.02410.02320.02320.60100.57611.54071.41840.03410.03420.03310.03320.45210.68921.86291.436217.08917.09716.93916.9640.51300.59341.16201.970023.62223.63323.49823.5130.22620.6494樣品31.64591.722923.84923.88623.70023.7130.73550.21141.48602.018624.14124.16524.02724.0720.55980.36401.42641.750225.63225.63625.56125.5650.64220.42301.38871.663923.74323.75323.65623.6630.55110.31961.41661.502918.83218.84118.74118.7520.62420.40471.52171.645620.14620.17920.03020.0310.58690.56131.45641.875733.44833.46333.32833.3660.64110.3532本方法采用砂帶機(jī)或小型銑床研磨鐠釹金屬樣品。用火花放電原子發(fā)射光譜法測(cè)定鐠釹金屬中碳、鐵、鉬、鋁、硅和鐠元素的含0.56%~1.40%、0.09%~0.28%之間。本方法操作簡(jiǎn)單快速、干擾小，測(cè)定結(jié)果的精密度好，能夠滿足鐠釹金屬的快FeMoAlPrNdAvg0.0610.2410.0090.0160.04380.7330.0010.0080.0010.0010.0510.055RSD3.4158.6070.2720.068極差0.0030.0230.0030.0030.1530.16310.0620.2540.010.0160.04418.89680.71820.0610.2320.0090.0160.04318.82780.81330.0590.2350.0090.0160.04318.81680.82240.0620.240.0090.0160.04418.94480.68450.0620.2390.0090.0160.04418.96980.66260.060.240.0090.0160.04318.87