本文選題：電感耦合等離子體原子發(fā)射光譜法 + 鈮鐵��； 參考：《冶金分析》2015年09期

【摘要】：鈮鐵樣品以氫氟酸和硝酸消解,直接在氫氟酸介質(zhì)中使用電感耦合等離子體原子發(fā)射光譜法(ICP-AES)測(cè)定鈮含量。試驗(yàn)考察了共存基體元素鐵以及常量雜質(zhì)硅、鈦、鋁、鉭等對(duì)測(cè)定的基體效應(yīng)、光譜干擾以及背景噪聲等因素的影響。通過(guò)采取優(yōu)化樣品稀釋比例、選擇適宜靈敏度分析譜線及其檢測(cè)積分與背景校正區(qū)域,優(yōu)化儀器工作條件等措施,將鈮元素的檢測(cè)信號(hào)強(qiáng)度調(diào)控在適宜水平,以確保方法具有良好線性范圍以及精密度和正確度水平。試驗(yàn)采用基體匹配法繪制校準(zhǔn)曲線,并進(jìn)行同步背景校正,檢驗(yàn)周期僅需10~15min。結(jié)果表明:在鈮質(zhì)量分?jǐn)?shù)為50%~80%范圍內(nèi),校準(zhǔn)曲線線性相關(guān)系數(shù)r0.999 5。按照實(shí)驗(yàn)方法進(jìn)行測(cè)定,實(shí)際鈮鐵合金樣品測(cè)定結(jié)果的相對(duì)標(biāo)準(zhǔn)偏差(RSD,n=8)不大于0.2%;鈮鐵標(biāo)準(zhǔn)樣品的測(cè)定結(jié)果與認(rèn)定值一致;實(shí)際鈮鐵合金產(chǎn)品的測(cè)試結(jié)果與紙上色層分離重量法的測(cè)試結(jié)果也一致。
[Abstract]:The samples of ferroniobiobiobiobium were digested with hydrofluoric acid and nitric acid, and the content of niobium was directly determined by ICP-AES- (inductively coupled plasma atomic emission spectrometry) in hydrofluoric acid medium. The influence of the coexisting matrix element iron and the constant impurities silicon titanium aluminum and tantalum on the matrix effect spectral interference and background noise were investigated. By optimizing sample dilution ratio, selecting appropriate sensitivity analysis spectrum line and its detection integral and background correction area, optimizing the working conditions of the instrument, the signal intensity of niobium detection is adjusted to the appropriate level. To ensure that the method has a good linear range and precision and accuracy level. The calibration curve was drawn by the matrix matching method, and the synchronous background correction was carried out. The inspection period was only 10 ~ 15 min. The results show that the linear correlation coefficient of calibration curve is r 0.999 5 when the mass fraction of niobium is 50%. According to the experimental method, the relative standard deviation of the determination results of the actual ferroniobiobiobiobium samples is not greater than 0.20.The results of the determination of the standard samples of ferroniobiobiobiobiobiobiobiobiobium are consistent with the determined values. The test results of the actual ferroniobium alloy products are in agreement with those obtained by the chromatographic separation gravimetric method on paper.
【作者單位】： 攀鋼集團(tuán)研究院有限公司釩鈦資源綜合利用國(guó)家重點(diǎn)實(shí)驗(yàn)室;
【分類號(hào)】：TG115.33

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