X射线荧光光谱法测定生石灰中8种组分
1. 阳泉市综合检验检测中心, 山西阳泉 045000
2. 国家硅铝质耐火材料质量检验检测中心 (山西), 山西阳泉 045000
| 摘 要： | 生石灰的主要成分为CaO和MgO，在的生产运输过程中，容易吸收空气中的H2O和CO2，影响生石灰的品质，在传统的检测方法中，CaO和MgO采用EDTA滴定法，该方法在检测过程中，不可避免水中CO2对结果的影响，在实际应用时，不同实验室检测结果往往存在很大差异。本试验选择不同含量石灰石标准样品，在1000°C下灼烧1h，以获得生石灰标准样品。采用优级纯Li2B4O7为熔剂，以熔融玻璃片法制样，试样和熔剂比为1﹕10，加入0.2 mL 300 g/L NH4I溶液为脱模剂，在1000°C下熔融10 min，获得校准样片。在X射线荧光光谱仪中，通过设置合适测量条件，测量标准样片，以谱线校正消除谱线间干扰，依据经验系数法进行基体校正，建立测量标准工作曲线。通过测定待测样品的灼烧减量修正检测结果，建立了生石灰中CaO、MgO、SiO2、Al2O3、Fe2O3、TiO2、K2O、Na2O的化学成分分析方法。经过方法验证，该方法不同元素检测结果的相对标准偏差在0.02%-4.11%之间，采用有证标准样品和不同方法比对，结果误差在允许范围之内，证明该方法结果能够达到日常生产质量监控的需要。 |
| 关 键 词： | 生石灰; X射线荧光光谱法 (XRF); 熔融制样; 基体校正; 方法验证 |
| DOI： | 10.57237/j.mater.2023.05.002 |
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收稿日期: 2023-08-17
接受日期: 2023-10-08
在线出版日期: 2023-10-09
Based on X-ray Fluorescence Spectrometry, Determination of Eight Components in Quicklime
Yangquan Comprehensive Inspection and Testing Center, Yangquan 045000, China
| Abstract: | The main components of lime are CaO and MgO, in the production and transportation process, it is easy to absorb H2O and CO2 in the air, affecting the quality of lime, in the traditional detection method, CaO and MgO use EDTA titration method, the method in the detection process, it is inevitable to avoid the impact of CO2 in water on the results, in practical application, different laboratory detection nodes Results often vary greatly. In this experiment, the limestone standard sample was selected and burned it at 1000°C to obtain the quicklime standard sample. Li2B4O7 was used as the flux, and the molten glass sheet method was employed. The sample to flux ratio was 1:10, and 0.2 mL of 300 g/L NH4I solution was added as the release agent. The calibration sample was accomplished by melting at 1000°C for 10 min. In X-ray fluorescence spectrometer, spectral line interference was eliminated by spectral line correction, and matrix correction was carried out according to the empirical coefficient method to correct the effect of calcination in the sample on the results. A composition analysis method for CaO, MgO, SiO2, Al2O3, Fe2O3, TiO2, K2O, and Na2O in quicklime was established. Through the verification of the precision and accuracy of the method, it was proved that the results of the method could meet the needs of daily production quality monitoring. Through the method verification, the relative standard deviation of the detection results of different elements of the method is between 0.02%-4.11%. By comparing the certified standard samples with different methods, the result error is within the allowable range, which proves that the results of the method can meet the needs of daily production quality control. |
| Keywords: | Quicklime; X-ray Fluorescence Spectrometry; Fusion Sample Preparation; Matrix Correction; Method Validation |
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