电感耦合等离子体原子发射光谱法测定重晶石中碳酸钡和硫酸钡
发布时间：2018-10-08 14:54
【摘要】：通过采用不同的样品处理方法,对电感耦合等离子体原子发射光谱法(ICP-AES)测定重晶石中碳酸钡和硫酸钡含量的方法进行了探讨。采用不同浓度醋酸对纯硫酸钡进行溶解试验,结果表明,采用1.7mol/L醋酸常温溶解1h,硫酸钡的溶出率与用水进行溶解时保持一致。因而采用以下流程对样品中碳酸钡进行测定:采用水溶解样品,并用ICP-AES对样品溶液中钡进行测定,得到样品中水溶性钡的含量;采用1.7mol/L醋酸溶解样品,并用ICP-AES对样品溶液中钡进行测定,得到样品中水溶性钡、以碳酸钡形式存在的钡的含量总和;将后者减去前者可得到以碳酸钡形式存在的钡的含量,再进一步换算为碳酸钡含量,实现了ICPAES对重晶石中碳酸钡含量的测定。采用1.0mol/L盐酸加热煮沸30min处理样品,可有效溶解氯化钡、碳酸钡等含钡杂质,而采用1.0mol/L盐酸对纯硫酸钡的溶解试验表明,1.0mol/L盐酸对硫酸钡的溶出率为0.090%,与重晶石样品中硫酸钡质量分数(大于10%)相比可忽略不计。因而采用以下流程对样品中硫酸钡进行测定:样品经1.0mol/L盐酸处理后,过滤,采用过氧化钠熔融-碳酸钠溶液浸提的方法处理沉淀,并采用ICP-AES对浸取液中钡进行测定,可得到以硫酸钡形式存在的钡的含量,将其换算为硫酸钡含量,实现了ICP-AES对重晶石样品中硫酸钡含量的测定。考虑到重晶石样品中碳酸钡的含量较低而硫酸钡的含量较高,分别选择灵敏度最高的Ba 455.403nm谱线和灵敏度较低的Ba 230.424nm谱线为分析谱线对二者进行测定,其对应钡的校准曲线线性相关系数分别为0.999 1~0.999 9和0.999 5~1.000 0。按照实验方法测定重晶石样品中碳酸钡和硫酸钡,碳酸钡方法检出限为0.001%,硫酸钡方法检出限为0.003%;碳酸钡和硫酸钡测定结果的相对标准偏差(RSD,n=12)分别不大于21%和1.0%。实验方法用于样品中碳酸钡测定并加入碳酸钡进行加标回收试验,其回收率为90%~110%。实验方法用于测定重晶石矿石成分分析标准物质中硫酸钡,测定值与认定值相吻合。
[Abstract]:The determination of barium carbonate and barium sulfate in barite by inductively coupled plasma atomic emission spectrometry (ICP-AES) was studied by different sample processing methods. The dissolution test of pure barium sulfate with different concentration of acetic acid showed that the dissolution rate of barium sulfate with 1.7mol/L acetic acid at room temperature for 1 hour was the same as that with water. Therefore, the content of water-soluble barium in the sample was obtained by using water dissolved sample, ICP-AES method and 1.7mol/L acetic acid method, and the content of water-soluble barium carbonate in the sample was determined by the following procedures: the sample was dissolved in water and the content of water soluble barium in the sample solution was determined by ICP-AES. The content of water-soluble barium in the sample solution was determined by ICP-AES, and the total content of barium in the form of barium carbonate was obtained, and the content of barium in the form of barium carbonate was obtained by subtracting the latter. The determination of barium carbonate in barite by ICPAES has been realized by further conversion to the content of barium carbonate. By using 1.0mol/L hydrochloric acid to heat and boil the samples with 30min, barium chloride, barium carbonate and other impurities containing barium can be effectively dissolved. The dissolution test of pure barium sulfate with 1.0mol/L hydrochloric acid shows that the dissolution rate of Barium sulfate by 1.0 mol / L HCl is 0.090, which is negligible compared with the mass fraction of barium sulfate in barite samples (more than 10%). The sample was treated with 1.0mol/L hydrochloric acid, filtered, precipitated by molten sodium oxide solution and extracted by sodium carbonate solution, and barium in the leaching solution was determined by ICP-AES, so that barium sulfate in the sample was determined by the following procedure: after treated with 1.0mol/L hydrochloric acid, the sample was filtered, and precipitated by solution extraction of sodium peroxide-sodium carbonate. The content of barium in the form of barium sulfate can be obtained and converted into the content of barium sulfate. The determination of barium sulfate in barite samples by ICP-AES has been realized. Considering the lower content of barium carbonate and the higher content of barium sulfate in barite samples, the Ba 455.403nm lines with the highest sensitivity and the Ba 230.424nm lines with lower sensitivity are selected for the determination of the two lines, The linear correlation coefficients of the calibration curves for barium are 0.999 ~ 0.999 9 and 0.999 5 ~ 1.000 respectively. The detection limit of barium carbonate and barium sulfate in barite samples is 0.001, the detection limit of barium sulfate method is 0.003 and the relative standard deviation (RSD,n=12) of barium carbonate and barium sulfate determination results is less than 21% and 1.0%, respectively. The method was used for the determination of barium carbonate in the sample and the addition of barium carbonate for the standard recovery test. The recovery rate was 90% and 110%. The method has been applied to the determination of barium sulfate in barite ores.
【作者单位】： 湖北省地质实验测试中心;
【分类号】：O657.31;P575
，
本文编号：2257184
[Abstract]:The determination of barium carbonate and barium sulfate in barite by inductively coupled plasma atomic emission spectrometry (ICP-AES) was studied by different sample processing methods. The dissolution test of pure barium sulfate with different concentration of acetic acid showed that the dissolution rate of barium sulfate with 1.7mol/L acetic acid at room temperature for 1 hour was the same as that with water. Therefore, the content of water-soluble barium in the sample was obtained by using water dissolved sample, ICP-AES method and 1.7mol/L acetic acid method, and the content of water-soluble barium carbonate in the sample was determined by the following procedures: the sample was dissolved in water and the content of water soluble barium in the sample solution was determined by ICP-AES. The content of water-soluble barium in the sample solution was determined by ICP-AES, and the total content of barium in the form of barium carbonate was obtained, and the content of barium in the form of barium carbonate was obtained by subtracting the latter. The determination of barium carbonate in barite by ICPAES has been realized by further conversion to the content of barium carbonate. By using 1.0mol/L hydrochloric acid to heat and boil the samples with 30min, barium chloride, barium carbonate and other impurities containing barium can be effectively dissolved. The dissolution test of pure barium sulfate with 1.0mol/L hydrochloric acid shows that the dissolution rate of Barium sulfate by 1.0 mol / L HCl is 0.090, which is negligible compared with the mass fraction of barium sulfate in barite samples (more than 10%). The sample was treated with 1.0mol/L hydrochloric acid, filtered, precipitated by molten sodium oxide solution and extracted by sodium carbonate solution, and barium in the leaching solution was determined by ICP-AES, so that barium sulfate in the sample was determined by the following procedure: after treated with 1.0mol/L hydrochloric acid, the sample was filtered, and precipitated by solution extraction of sodium peroxide-sodium carbonate. The content of barium in the form of barium sulfate can be obtained and converted into the content of barium sulfate. The determination of barium sulfate in barite samples by ICP-AES has been realized. Considering the lower content of barium carbonate and the higher content of barium sulfate in barite samples, the Ba 455.403nm lines with the highest sensitivity and the Ba 230.424nm lines with lower sensitivity are selected for the determination of the two lines, The linear correlation coefficients of the calibration curves for barium are 0.999 ~ 0.999 9 and 0.999 5 ~ 1.000 respectively. The detection limit of barium carbonate and barium sulfate in barite samples is 0.001, the detection limit of barium sulfate method is 0.003 and the relative standard deviation (RSD,n=12) of barium carbonate and barium sulfate determination results is less than 21% and 1.0%, respectively. The method was used for the determination of barium carbonate in the sample and the addition of barium carbonate for the standard recovery test. The recovery rate was 90% and 110%. The method has been applied to the determination of barium sulfate in barite ores.
【作者单位】： 湖北省地质实验测试中心;
【分类号】：O657.31;P575
，
本文编号：2257184
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