電感耦合等離子體原子發(fā)射光譜法測(cè)定鋁合金中硼
發(fā)布時(shí)間:2018-06-06 08:05
本文選題:電感耦合等離子體原子發(fā)射光譜法 + 萃取。 參考:《冶金分析》2015年08期
【摘要】:鋁合金樣品采用氫氧化鈉溶液和過(guò)氧化氫溶解,稀硫酸酸化,然后置于分液漏斗中,pH 3時(shí)溶液中硼酸和一定量的苯羥乙酸及孔雀石綠締合成三元絡(luò)合物,用苯定量萃取,萃取液直接進(jìn)入有機(jī)進(jìn)樣系統(tǒng)的電感耦合等離子體原子發(fā)射光譜儀(ICP-AES),選擇分析譜線B 249.678nm測(cè)定鋁合金中硼。通過(guò)樣品溶解方法、萃取劑、萃取方法及條件(時(shí)間和酸度)的選擇,采用基體匹配法消除物理干擾。方法中硼的質(zhì)量濃度在1.00mg/L以內(nèi)與其發(fā)射強(qiáng)度呈線性關(guān)系,校準(zhǔn)曲線的線性相關(guān)系數(shù)r=0.999 3,硼的檢出限為0.001mg/L。按照實(shí)驗(yàn)方法對(duì)標(biāo)準(zhǔn)樣品和自備樣品分別測(cè)定,標(biāo)準(zhǔn)樣品的測(cè)定值和認(rèn)定值基本吻合;自備樣品測(cè)定結(jié)果的相對(duì)標(biāo)準(zhǔn)偏差(RSD,n=10)小于5%,加標(biāo)回收率為80%~100%,方法可檢測(cè)鋁合金中質(zhì)量分?jǐn)?shù)最低為0.000 1%的硼。
[Abstract]:Aluminum alloy samples were dissolved in sodium hydroxide solution and hydrogen peroxide and acidified with dilute sulfuric acid. Boric acid and a certain amount of phenylglycolic acid and malachite green were synthesized in the solution of pH 3 in the funnel and extracted quantitatively by benzene. An inductively coupled plasma atomic emission spectrometer (ICP-AES-) for the determination of boron in aluminum alloy was developed. The analytical line B 249.678nm was selected for the determination of boron in aluminum alloy. The physical interference was eliminated by matrix matching method through the selection of sample dissolution method, extractant, extraction method and conditions (time and acidity). The linear correlation coefficient of calibration curve is 0.999 3 and the detection limit of boron is 0.001 mg / L. According to the experimental method, the standard sample and the self-provided sample were determined, and the measured value of the standard sample was basically consistent with the determined value. The relative standard deviation (RSD) of the determination results of self-provided samples is less than 5. The recovery rate of the added standard is 80 and 100. The method can be used to detect boron with the lowest mass fraction of 0.000 in aluminum alloy.
【作者單位】: 重慶工業(yè)職業(yè)技術(shù)學(xué)院;重慶市計(jì)量質(zhì)量檢測(cè)研究院鋁鎂中心;中原特鋼股份有限公司;
【分類號(hào)】:TG115.33;TG146.21
【參考文獻(xiàn)】
相關(guān)期刊論文 前8條
1 王倩,明芳;ICP-AES測(cè)定鋁合金中硼[J];光譜實(shí)驗(yàn)室;2003年04期
2 張e,
本文編號(hào):1985842
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