X-熒光在壓片法測定纖維玻璃成份中的應(yīng)用(陳建良,巨石集團(tuán))

1、在壓片法測定纖維玻璃成份中的應(yīng)用陳建良X-熒光Content1實驗室概覽2問題與設(shè)計3解決方法標(biāo)線建立4方法論證56Q&A1實驗室概覽2問題與設(shè)計面臨的問題X熒光對纖維玻璃測定熔片法壓片法B2O3F溶劑經(jīng)濟(jì)性基體效應(yīng)顆粒度效應(yīng)面臨的問題X熒光對纖維玻璃測定熔片法B2O3F溶劑經(jīng)濟(jì)性壓片法基體效應(yīng)顆粒度效應(yīng)壓片法基體效應(yīng)顆粒度效應(yīng)纖維玻璃組成很穩(wěn)定，基體效應(yīng)影響小主要解決粒度效應(yīng)；樣品與粘結(jié)劑之間的比例3解決方法樣品顆粒度的控制選取多種試樣震動磨采用30S、60S、90S、120S、180S、240S磨樣激光料度分析儀分析粒度確定磨樣時間檢測結(jié)果做比對120各樣品粒度分布已基本相同，最大

2、差值不大于1.2%。0.0740.050mm粒徑隨磨樣時間分布圖稀釋比10:110:2稀釋比樣品號化學(xué)成分(%)SiO2Al2O3Fe2O3CaONa2OTiO2B2O3F10：1159.1916.010.4325.020.520.407.170.47259.1816.050.4325.120.520.407.190.48359.2316.070.4325.070.520.407.200.48459.1316.040.4325.050.520.407.100.47極差0.100.060.000.100.000.000.100.0110：2153.1114.500.3822.580.520.40

3、7.400.47253.1814.490.3822.640.520.407.280.48353.1514.550.3822.520.520.407.350.48453.2614.550.3822.590.520.407.330.47極差0.150.060.000.120.000.000.120.01樣品經(jīng)120S研磨粒徑0.074 mm0.0740.050 mm分布最大差值1%兩種稀釋比制成樣片后，其化學(xué)成分檢測結(jié)果最大差值0.15%重現(xiàn)性都能夠滿足檢測要求兩種稀釋比采用10:1的稀釋比4標(biāo)線建立元素分析線分析晶體電流(mA)電壓（KV）測量時間（S）2角（度）探測器準(zhǔn)直器()PHASiSi

4、KA1XS-CEM50303029.272流氣0.4650150AlAl KA1XS-CEM100302034.362流氣0.4650150FeFe KA1LiF20050601057.527閃爍0.4660140CaCa KA1LiF200405020113.082流氣0.2340250MgMg KA1XS-55100302020.713流氣0.4640160KK KA1LiF200506010136.655流氣0.4640160NaNa KA1XS-55100303024.896流氣0.4650150TiTi KA1LiF20050601086.165流氣0.4640160BB KA1XS

5、-B1353010039.898流氣2.040170FF KA1XS-55135305039.304流氣0.4640250分析元素測量條件為布魯克S4Pioneer 型X射線熒光光譜儀的最佳條件，可供其它儀器選擇條件時參考成分測量范圍(%)成分測量范圍(%)SiO250.372.5K2O0.10.5Al2O311.717.4Na2O0.211.6Fe2O30.20.7TiO20.20.8CaO12.825.8F0.10.9MgO0.210.2B2O34.89.0測量范圍5方法論證樣品重現(xiàn)性 F 和B2O3測量最大誤差最大為0.01%、0.12%化學(xué)成分SiO2Al2O3Fe2O3CaOMgOK

6、2ONa2OTiO2B2O3F1#53.1514.430.4222.660.450.290.510.407.160.452#53.0514.440.4222.680.450.290.510.407.100.463#53.0914.470.4222.660.450.290.510.407.110.464#53.0614.410.4222.690.440.290.510.407.030.455#53.0514.470.4222.670.440.290.510.407.150.466#53.0514.430.4222.680.440.290.510.407.090.457#53.1314.450.4

7、222.730.440.290.520.407.100.468#53.0014.450.4322.650.440.290.520.407.120.46平均值53.0714.440.4222.680.440.290.510.407.110.46極差0.150.060.010.080.010.000.010.000.120.01標(biāo)準(zhǔn)偏差0.040.020.000.020.010.000.000.000.040.01相對標(biāo)準(zhǔn)偏差0.0010.0010.0080.0010.0110.0000.0090.0000.0050.011方法精密度化學(xué)成分SiO2Al2O3Fe2O3CaOMgOK2ONa2OT

8、iO2B2O3F1#56.4814.030.4720.580.450.280.510.406.250.462#56.4214.070.4720.550.450.280.510.406.270.453#56.4514.010.4720.590.450.280.510.416.240.454#56.5014.020.4720.590.450.280.510.416.240.465#56.4514.060.4720.610.440.280.510.416.360.466#56.4414.080.4720.610.440.280.510.416.320.467#56.4514.010.4720.620.440.280.510.416.290.468#56.5114.090.4720.620.440.280.510.416.290.46956.5114.090.4720.620.440.280.510.416.290.461056.5114.090.4720.620.440.280.510.416.290.46平均值56.4714.050.4720.600.440.280.510.416.280.46極差0.090.080.000.070.010.000.000.010.120.01標(biāo)準(zhǔn)偏差0.0340.0360.