Determination of Vanadium, Iron, Manganese and Phosphorus Contents in Ferrovanadium Slag by Alkali Fusion-Inductively Coupled Plasma Atomic Emission Spectrometry
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摘要:
采用碳酸钠-硼酸高温熔融样品，经盐酸浸取熔块，选择钒310.230 nm、铁259.940 nm、锰257.610 nm和磷213.618 nm为分析谱线，选用基体匹配法来消除基体效应的影响，建立了碱熔-电感耦合等离子体原子发射光谱法测定钒铁炉渣中钒铁锰磷的方法。结果表明，各元素校准曲线的线性相关系数均不小于0.999；方法中各元素检出限分别为：钒0.0076 μg/mL、铁0.0093 μg/mL、锰0.0065 μg/mL、磷0.0051 μg/mL。按照实验方法测定两个钒铁炉渣标准样品，测定结果的相对标准偏差（RSD，n=8）不大于3.9%，测定值与认定值基本一致。
Abstract:The ferrovanadium slag sample was fused with sodium carbonate-boric acid at high temperature, then acidified with hydrochloric. Vanadium 310.230 nm, iron 259.940 nm, manganese 257.610 nm and phosphorus 213.618 nm were selected as the analytical lines. The matrix matching method was used to eliminate the influence of matrix effect, the determination method of vanadium, iron, manganese and phosphorus contents in ferrovanadium slag by alkali fusion-inductively coupled plasma atomic emission spectrometry was established. The results showed that the linear correlation coefficients of calibration curves were all higher than 0.999, the limit of detection for vanadium, iron, manganese and phosphorus was 0.0076 μg/mL, 0.0093 μg/mL, 0.0065 μg/mL and 0.0051 μg/mL, respectively. Two ferrovanadium slag certified reference materials were determined according to the experimental method, the relative standard deviations(RSD, n=8) were less than 3.9 %.
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表 1 标准溶液系列中各元素质量浓度/（mg∙L-1）
Table 1. Mass concentration of each element in standard solution series
元素 S0 S1 S2 S3 S4 S5 钒 0 5.0 10 15 20 25 铁 0 2.0 4.0 6.0 8.0 10 锰 0 2.0 4.0 6.0 8.0 10 磷 0 0.04 0.08 0.12 0.16 0.20 
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表 2 校准曲线相关系数、检出限和测定下限
Table 2. Calibration curve correlation coefficients, detection limits and limit of determination
元素 波长
/nm相关系数R2 检出限
/（μg·mL-1）测定下限
/（μg·mL-1）测定范围
/%钒 310.230 0.9995 0.0076 0.025 0.002~2.50 铁 259.940 0.9997 0.0093 0.031 0.003~1.00 锰 257.610 0.9998 0.0065 0.022 0.002~1.00 磷 213.618 0.9996 0.0051 0.017 0.002~0.20
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表 3 国家标准物质测定结果
Table 3. Determination results of CRMs
元素 YSBC 19823-2017 YSBC 19824-2017 测定值% 认定值/% 相对标准偏
差RSD（n=8） /%相对误差RE /% 测定值/% 认定值/% 相对标准偏
差RSD（n=8） /%相对误差RE /% 钒 1.76 1.78±0.03 1.6 1.1 1.93 1.91±0.04 1.0 1.0 铁 0.691 0.695±0.017 2.7 0.6 0.445 0.442±0.016 1.8 1.7 锰 0.063 0.062±0.002 2.1 1.6 0.047 0.046±0.002 2.4 2.2 磷 0.014 0.013±0.001 3.2 7.7 0.006 0.006±0.001 3.9 0.0
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