Determination of Sulfur in Barite and Pyrite by High Frequency Infrared Carbon-Sulfur Spectrometer
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摘要: 硫酸盐矿石和硫化物矿石大部分是低电磁性的物质，利用高频红外碳硫仪测定这类矿石中的硫时，在燃烧过程中难以产生较大的电磁感应涡流，导致矿石中的硫释放不完全，造成硫的测定结果偏低。本文采用二氧化硅将重晶石精矿和黄铁矿精矿稀释成不同硫含量的重晶石和黄铁矿样品，通过优化称样量及助熔剂等测试条件，建立了使用高频红外碳硫仪测定重晶石和黄铁矿中硫含量的分析方法。结果表明：当样品中的硫含量高于2%时确定称样量为0.07 g，当硫含量低于2%时确定称样量为0.1 g，加入助熔剂0.4 g锡粒+0.4 g铁粒+1.5 g钨粒，可使重晶石和黄铁矿中的硫完全释放进入仪器红外吸收区域，硫的回收率提高至95.8%~104.2%（重晶石）和95.3%~105.1%（黄铁矿），分别高于常规红外碳硫仪的回收率（83.39%~91.1%和91.5~97.5%）。本方法精密度高（RSD < 5%），实现了硫含量的准确测定。Abstract: Most sulfate and sulfide ores are composed of low electrical magnetic materials. In the process of combustion, the sulfur in sulfate and sulfide ores cannot be released completely, because it is difficult to produce a large enough electromagnetic induction eddy current. Thus, the results are lower than real values when the sulfur in sulfate and sulfide ores is determined by High Frequency Infrared Carbon-Sulfur Spectrometer. In this study, the barite and pyrite samples are diluted with silicon dioxide to acquire different contents of sulfur. By optimizing the sample weight and flux types, determination of sulfur by High Frequency Infrared Carbon-Sulfur Spectrometer was developed. Results show that the sample weight is 0.07 g when the content of sulfur is higher than 2% whereas sample weight is 0.1 g when the sulfur content is below 2%. Furthermore, the sulfur in barite and pyrite can be released completely into the infrared absorption area when adding 0.4 g of tin grain, 0.4 g of iron grain, and 0.5 g of tungsten grain to the sample. The recovery of sulfur can reach 95.8%-104.2%(barite) and 95.3%-105.1%(pyrite), which is far higher than the recovery of 83.3%-91.1% and 91.5-97.5% for the conventional analysis of sulfur by Infrared Carbon-Sulfur Spectrometer. This method precision is less than 5% and can determine the accurate content of sulfur.
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Key words:
- barite /
- pyrite /
- sulfur /
- High Frequency Infrared Carbon-Sulfur Spectrometer
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表 1 重晶石和黄铁矿的稀释倍数及硫的含量
Table 1. The dilution ratio and content of sulfur for the barite and pyrite
重晶石及
稀释后
样品编号稀释倍数 硫含量
参考值
(%)黄铁矿及
稀释后
样品编号稀释倍数 硫含量
参考值
(%)1 250 0.038 12 1000 0.047 2 200 0.048 13 800 0.059 3 150 0.064 14 400 0.12 4 100 0.096 15 200 0.24 5 50 0.19 16 80 0.59 6 20 0.48 17 40 1.18 7 10 0.96 18 20 2.35 8 8 1.20 19 8 5.88 9 4 2.40 20 4 11.75 10 2 4.80 21 2 23.50 11 1 9.61 22 1 47.00 
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表 2 称样量对重晶石和黄铁矿中硫含量测定的影响
Table 2. Effect of sample weight on determination of sulfur in barite and pyrite
称样量
(g)重晶石中的硫含量 (%) 称样量
(g)黄铁矿中的硫含量 (%) 样品7 样品8 样品9 样品10 样品17 样品18 样品19 样品20 0.03 0.88 1.09 2.35 4.78 0.03 1.05 2.21 5.72 11.55 0.05 0.92 1.13 2.35 4.84 0.05 1.09 2.26 5.79 11.66 0.07 0.96 1.16 2.44 4.99 0.07 1.15 2.34 5.86 11.73 0.10 0.97 1.18 2.42 4.87 0.10 1.17 2.29 5.80 11.68 0.15 0.95 1.16 2.39 4.82 0.15 1.07 2.20 5.74 11.60
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表 3 锡粒助熔剂用量对重晶石和黄铁矿中硫测定的影响
Table 3. Effect of tin flux weight on determination of sulfur in barite and pyrite
助熔剂加入量 (g) 硫含量测定值 (%) 锡粒 铁粒 钨粒 样品6
(重晶石)样品16
(黄铁矿)0 0.4 1.5 0.39 0.46 0.1 0.4 1.5 0.40 0.48 0.2 0.4 1.5 0.40 0.52 0.3 0.4 1.5 0.41 0.53 0.4 0.4 1.5 0.45 0.54 0.5 0.4 1.5 0.40 0.52
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表 4 重晶石和黄铁矿中硫的测定方法比对和加标回收率
Table 4. Comparison of analytical methods and the spiked recovery for barite and pyrite
重晶石
样品编号硫含量参考值
(%)本方法
测定结果文献[2]方法
测定结果黄铁矿
样品编号硫含量参考值
(%)本方法
测定结果文献[2]方法
测定结果硫含量
(%)回收率
(%)硫含量
(%)回收率
(%)硫含量
(%)回收率
(%)硫含量
(%)回收率
(%)1 0.038 0.038 100.0 0.032 84.2 12 0.047 0.048 102.1 0.043 91.5 2 0.048 0.05 104.2 0.04 83.3 13 0.059 0.062 105.1 0.055 93.2 3 0.064 0.066 103.1 0.056 87.5 14 0.12 0.12 100.0 0.11 91.7 4 0.096 0.1 104.2 0.085 88.5 15 0.24 0.25 104.2 0.22 91.7 5 0.19 0.19 100.0 0.15 88.2 16 0.59 0.57 96.6 0.55 93.2 6 0.48 0.46 95.8 0.43 89.6 17 1.18 1.17 99.2 1.08 91.5 7 0.96 0.97 101.0 0.86 89.6 18 2.35 2.24 95.3 2.2 93.6 8 1.2 1.18 98.3 1.04 86.7 19 5.88 5.61 95.4 5.44 92.5 9 2.4 2.44 101.7 2.18 90.8 20 11.75 11.36 96.7 11 93.6 10 4.8 4.89 101.9 4.34 90.4 21 23.5 22.76 96.8 22.07 93.9 11 9.61 9.76 101.6 8.7 90.5 22 47 46.97 99.9 45.06 95.9 GBW07813 11.64 11.59 99.6 10.6 91.1 ZBK327 29.95 29.88 99.8 29.21 97.5
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表 5 方法精密度
Table 5. Precision tests of the method
样品编号 硫含量 (%) RSD
(%)分次测定值 平均值 参考值 样品5
(重晶石)0.18 0.2 0.19 0.2 0.19 0.19 4.2 0.2 0.19 0.18 0.2 0.19 0.2 0.19 0.19 样品8
(重晶石)1.15 1.16 1.18 1.17 1.18 1.20 1.6 1.2 1.21 1.18 1.16 1.17 1.18 1.16 1.18 GBW07813
(重晶石)11.57 11.55 11.57 11.5 11.59 11.64 0.4 11.59 11.61 11.58 11.65 11.59 11.62 11.67 11.59 样品15
(黄铁矿)0.25 0.24 0.23 0.24 0.25 0.24 4.5 0.26 0.25 0.26 0.23 0.25 0.24 0.25 0.26 样品18
(黄铁矿)2.26 2.22 2.24 2.23 2.24 2.35 0.8 2.25 2.21 2.24 2.27 2.23 2.24 2.26 2.25 ZBK327
(硫铁矿)29.87 29.85 29.88 29.92 29.89 29.95 0.6 29.86 29.91 29.92 29.94 29.89 29.93 29.84 29.91
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