電感耦合等離子體原子發(fā)射光譜法測定重晶石中碳酸鋇和硫酸鋇
發(fā)布時間：2018-10-08 14:54
【摘要】：通過采用不同的樣品處理方法,對電感耦合等離子體原子發(fā)射光譜法(ICP-AES)測定重晶石中碳酸鋇和硫酸鋇含量的方法進行了探討。采用不同濃度醋酸對純硫酸鋇進行溶解試驗,結(jié)果表明,采用1.7mol/L醋酸常溫溶解1h,硫酸鋇的溶出率與用水進行溶解時保持一致。因而采用以下流程對樣品中碳酸鋇進行測定:采用水溶解樣品,并用ICP-AES對樣品溶液中鋇進行測定,得到樣品中水溶性鋇的含量;采用1.7mol/L醋酸溶解樣品,并用ICP-AES對樣品溶液中鋇進行測定,得到樣品中水溶性鋇、以碳酸鋇形式存在的鋇的含量總和;將后者減去前者可得到以碳酸鋇形式存在的鋇的含量,再進一步換算為碳酸鋇含量,實現(xiàn)了ICPAES對重晶石中碳酸鋇含量的測定。采用1.0mol/L鹽酸加熱煮沸30min處理樣品,可有效溶解氯化鋇、碳酸鋇等含鋇雜質(zhì),而采用1.0mol/L鹽酸對純硫酸鋇的溶解試驗表明,1.0mol/L鹽酸對硫酸鋇的溶出率為0.090%,與重晶石樣品中硫酸鋇質(zhì)量分數(shù)(大于10%)相比可忽略不計。因而采用以下流程對樣品中硫酸鋇進行測定:樣品經(jīng)1.0mol/L鹽酸處理后,過濾,采用過氧化鈉熔融-碳酸鈉溶液浸提的方法處理沉淀,并采用ICP-AES對浸取液中鋇進行測定,可得到以硫酸鋇形式存在的鋇的含量,將其換算為硫酸鋇含量,實現(xiàn)了ICP-AES對重晶石樣品中硫酸鋇含量的測定�？紤]到重晶石樣品中碳酸鋇的含量較低而硫酸鋇的含量較高,分別選擇靈敏度最高的Ba 455.403nm譜線和靈敏度較低的Ba 230.424nm譜線為分析譜線對二者進行測定,其對應(yīng)鋇的校準(zhǔn)曲線線性相關(guān)系數(shù)分別為0.999 1~0.999 9和0.999 5~1.000 0。按照實驗方法測定重晶石樣品中碳酸鋇和硫酸鋇,碳酸鋇方法檢出限為0.001%,硫酸鋇方法檢出限為0.003%;碳酸鋇和硫酸鋇測定結(jié)果的相對標(biāo)準(zhǔn)偏差(RSD,n=12)分別不大于21%和1.0%。實驗方法用于樣品中碳酸鋇測定并加入碳酸鋇進行加標(biāo)回收試驗,其回收率為90%~110%。實驗方法用于測定重晶石礦石成分分析標(biāo)準(zhǔn)物質(zhì)中硫酸鋇,測定值與認定值相吻合。
[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.
【作者單位】： 湖北省地質(zhì)實驗測試中心;
【分類號】：O657.31;P575
，
本文編號：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.
【作者單位】： 湖北省地質(zhì)實驗測試中心;
【分類號】：O657.31;P575
，
本文編號：2257184
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