X射线荧光光谱法测定冶金渣料中主次成分

doi:10.13228/j.issn.1000-7571.2014.08.008

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摘要以L₂B₄O₇和LiBO₂ [m(L₂B₄O₇) ∶m(LiBO₂)=2∶1] 为熔剂,LiNO₃为氧化剂,LiBr为脱模剂,熔融法制备样品,建立了X射线荧光光谱对冶金渣料中的TFe、SiO₂、TCa、MgO、TiO₂_、MnO、P₂O₅、Al₂O₃、K₂O和Na₂O的快速检测方法。采用高炉渣、转炉渣、电炉渣系列标样绘制校准曲线,并通过加入钾长石、钠长石等适宜标准样品进行曲线分析范围扩展,使曲线既可以用于高炉渣、转炉渣、电炉渣等炉渣类样品分析,也可用于保护渣样品的检测分析。试验对稀释比、熔样温度、保护渣试样预处理温度等主要条件进行了探讨。结果表明,当试样与熔剂质量比为1∶10和熔样温度为1 050 ℃(熔样前保护渣样品预处理温度以700 ℃为宜)时,所得试样在熔剂中分散度(浓度)适当,同时适用于中高、低含量组分的测定。对一标准样品进行10次测定,各组合测定结果的相对标准偏差为0.07%~1.9%。方法用于各类实际冶金渣料分析时,结果与其他分析方法相一致。

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	朱春要
	顾锋
	年季强
	张良芬

关键词 ： X射线荧光光谱法, 炉渣, 保护渣, 熔融制样, 基体校正

Abstract：A rapid method was developed for the determination of TFe、SiO₂、TCa、MgO、TiO₂、MnO、P₂O₅、Al₂O₃、K₂O and Na₂O in metallurgical slag by X-ray fluorescence spectrometry (XRF). The sample was prepared by the fused method, using L₂B₄O₇and LiBO₂ [m(L₂B₄O₇)∶m(LiBO₂)=2∶1] as flux, LiNO₃as oxidizer and LiBr as release agent. A series of standard reference materials of blast furnace slag, converter slag, and electric furnace slag were used for establishing calibration curves. By addition of the reference materials of potassium feldspar and soda feldspar, the test range of curve was extended from slag to mould powder. The main experimental conditions of dilution ratio, fusion temperature and pre-treatment temperature were studied. The results showed that, when the mass ratio of sample to flux was chosen as 1∶10 and the fusion temperature and the pre-treatment temperature of the mould powder were at 1 050 ℃ and 700 ℃ respectively, the concentration of the sample in the flux was proved to be suitable for determination of both major and minor contents by XRF. The relative standard deviations (RSDs, n=10) for analysis of a reference materialwere from 0.07% to 1.9%. The test results were consistent with those of other methods in the determination of actual metallurgical slags.

Key words： X-ray fluorescence spectrometry slag mould powder fusion sample preparation matrix correction

收稿日期: 2014-02-13

ZTFLH:

O657.34

作者简介: 朱春要(1982-), 男, 本科, 工程师, 从事冶金分析工作; E-mail:zhucy316@sohu.com

引用本文:

朱春要, 顾锋, 年季强, 张良芬. X射线荧光光谱法测定冶金渣料中主次成分[J]. 冶金分析, 2014, 34(8): 39-44. ZHU Chun-yao, GU Feng, NIAN Ji-qiang, ZHANG Liang-fen. Determination of major and minor components in metallurgical slags by X-ray fluorescence spectrometry. , 2014, 34(8): 39-44.

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http://47.93.29.245/Jweb_yjfx/CN/10.13228/j.issn.1000-7571.2014.08.008 或 http://47.93.29.245/Jweb_yjfx/CN/Y2014/V34/I8/39

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