钼蓝分光光度法联合测定铁矿石中磷和二氧化硅
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摘要
以往铁矿石中磷和二氧化硅含量的测定需要分别采用钼蓝分光光度法。在使用磷钼蓝分光光度法时,常会因钒、砷等的干扰使得磷测定结果不准确,需要将样品再处理后才能测定。实验采用石墨垫底铁坩埚,碳酸钠和硼酸混合熔剂高温熔融铁矿石,使铁矿石样品分解彻底,再分别采用铋磷钼蓝和硅钼蓝分光光度法测定磷和二氧化硅含量,从而实现了采用钼蓝分光光度法联合测定铁矿石中磷和二氧化硅。干扰试验表明,在高温熔融时,石墨可将钒(V)还原为钒(III),使样品中钒不干扰磷的测定;显色液中加入15mg硫代硫酸钠溶液可将砷(V)还原为砷(III),继而消除砷对磷测定的干扰。磷的质量浓度在0～3μg/mL范围内遵守比尔定律,校准曲线的线性相关系数为0.999 9,表观摩尔吸光系数为2.242×104 L·mol-1·cm-1;二氧化硅的质量浓度在0～5μg/mL范围内遵守比尔定律,校准曲线的线性相关系数为0.999 5,表观摩尔吸光系数为9.342×103 L·mol-1·cm-1。方法中磷和二氧化硅的检出限分别为0.002 6μg/mL和0.008 1μg/mL。按照实验方法测定6个铁矿石标准样品中磷和二氧化硅,磷测定结果的相对标准偏差(n=8)小于5%,相对误差小于2%;二氧化硅测定结果的相对标准偏差(n=8)小于2%,相对误差小于1.5%。按照实验方法测定5个铁矿石样品中磷和二氧化硅,磷测定结果的相对标准偏差(RSD,n=8)小于7%,二氧化硅测定结果的相对标准偏差(n=8)小于1%;磷和二氧化硅的测定值均与电感耦合等离子体原子发射光谱法的测定值相一致。
In the past,the content of phosphorus and silicon dioxide in iron ore were determined separately by molybdenum blue spectrophotometry.When the phosphorus molybdenum blue spectrophotometry was used,the determination results of phosphorus were often inaccurate due to the interference by vanadium and arsenic.As a result,the sample should be retreated before determination.With bottom of iron crucible covered by graphite,the iron ore was melted at high temperature with sodium carbonate-boric acid mixture as flux.After complete decomposition,the content of phosphorus and silicon dioxide in iron ore sample was determined by bismuth phosphorus molybdenum blue spectrophotometry and silicon molybdenum blue spectrophotometry,respectively.Therefore,the combined determination of phosphorus and silicon dioxide in iron ore by molybdenum blue spectrophotometry was realized.The interference test indicated that vanadium(V)was reduced to vanadium(III)by graphite during the melting at high temperature,which eliminated the interference of vanadium with the determination of phosphorus.15 mg of sodium thiosulfate solution was added into the coloring solution to reduce arsenic(V)to arsenic(III),which eliminated the interference of arsenic with the determination of phosphorus.Beer′s law was obeyed for phosphorus with mass concentration in the range of 0-3μg/mL.The linear correlation coefficient of calibration curve was 0.999 9.The apparent molar absorptivity was 2.242×104 L·mol-1·cm-1.Beer′s law was obeyed for silicon dioxide with mass concentration in the range of 0-5μg/mL.The linear correlation coefficient of calibration curve was 0.999 5.The apparent molar absorptivity was 9.342×103 L·mol-1·cm-1.The detection limit of phosphorus and silicon dioxide in this method was 0.002 6μg/mL and 0.008 1μg/mL,respectively.The contents of phosphorus and silicon dioxide in six certified reference materials of iron ore were determined according to the experimental method.The relative standard deviations(RSD,n=8)of determination results for phosphorus were less than 5%,and the relative error was less than 2%.The RSDs(n=8)of determination results for silicon dioxide were less than 2%,and the relative error was less than 1.5%.The contents of phosphorus and silicon dioxide in five iron ore samples were determined according to the experimental method.The RSDs(n=8)was less than 7% and 1%for phosphorus and silicon dioxide,respectively.The determination results of phosphorus and silicon dioxide were consistent with those obtained by inductively coupled plasma atomic emission spectrometry.
In the past,the content of phosphorus and silicon dioxide in iron ore were determined separately by molybdenum blue spectrophotometry.When the phosphorus molybdenum blue spectrophotometry was used,the determination results of phosphorus were often inaccurate due to the interference by vanadium and arsenic.As a result,the sample should be retreated before determination.With bottom of iron crucible covered by graphite,the iron ore was melted at high temperature with sodium carbonate-boric acid mixture as flux.After complete decomposition,the content of phosphorus and silicon dioxide in iron ore sample was determined by bismuth phosphorus molybdenum blue spectrophotometry and silicon molybdenum blue spectrophotometry,respectively.Therefore,the combined determination of phosphorus and silicon dioxide in iron ore by molybdenum blue spectrophotometry was realized.The interference test indicated that vanadium(V)was reduced to vanadium(III)by graphite during the melting at high temperature,which eliminated the interference of vanadium with the determination of phosphorus.15 mg of sodium thiosulfate solution was added into the coloring solution to reduce arsenic(V)to arsenic(III),which eliminated the interference of arsenic with the determination of phosphorus.Beer′s law was obeyed for phosphorus with mass concentration in the range of 0-3μg/mL.The linear correlation coefficient of calibration curve was 0.999 9.The apparent molar absorptivity was 2.242×104 L·mol-1·cm-1.Beer′s law was obeyed for silicon dioxide with mass concentration in the range of 0-5μg/mL.The linear correlation coefficient of calibration curve was 0.999 5.The apparent molar absorptivity was 9.342×103 L·mol-1·cm-1.The detection limit of phosphorus and silicon dioxide in this method was 0.002 6μg/mL and 0.008 1μg/mL,respectively.The contents of phosphorus and silicon dioxide in six certified reference materials of iron ore were determined according to the experimental method.The relative standard deviations(RSD,n=8)of determination results for phosphorus were less than 5%,and the relative error was less than 2%.The RSDs(n=8)of determination results for silicon dioxide were less than 2%,and the relative error was less than 1.5%.The contents of phosphorus and silicon dioxide in five iron ore samples were determined according to the experimental method.The RSDs(n=8)was less than 7% and 1%for phosphorus and silicon dioxide,respectively.The determination results of phosphorus and silicon dioxide were consistent with those obtained by inductively coupled plasma atomic emission spectrometry.
引文
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[9]梁文君,聂纬,郑金云.铋磷钼蓝分光光度法测定金属硅中磷[J].光谱实验室,2002,19(1):124-126.LIANG Wen-jun,NIE Wei,ZHENG Jin-yun.Study on spectrophotometric determination of phosphorus in silicon metal with the blue made from bismuth,phosphorus &molybdenum[J].Chinese Journal of Spectroscopy Laboratory,2002,19(1):124-126.
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[11]许卉,贺萍.多波长线性回归分光光度法同时测定磷和硅[J].光谱实验室,1999,16(1):60-62.XU Hui,HE Ping.Simultaneous spectrophotometric determination of trace phosphorus and silicon in natural water by multi-wavelength linear regression[J].Chinese Journal of Spectroscopy Laboratory,1999,16(1):60-62.
[12]袁秉鉴,戴祥胜.分光光度法快速测定钢铁中的锰、磷、硅[J].化学分析计量,2001,10(4):24-26.YUAN Bing-jian,DAI Xiang-sheng.Quick determination of Mn,P and Si in steel and iron by spectrophotometry[J].Chemical Analysis and Meterage,2001,10(4):24-26.
[13]潘永平.分光光度法测定铁矿石中硅和磷含量[J].金属矿山(Metal Mine),2000,29(9):51-52,54.
[14]迟少婷.分光光度法连续测定铁矿石中磷和钛[J].冶金分析(Metallurgical Analysis),2002,22(1):68-69.
[15]杨莲瑛.分光光度法测定铁矿石中的二氧化硅和五氧化二磷[J].化工管理(Chemical Enterprise Management),2013,27(5):63,65,156.
[16]王丽君,胡述戈,杜建民,等.应用ICP-AES法测定铁矿石中6元素[J].冶金分析,2003,23(3):67,50.WANG Li-jun,HU Shu-ge,DU Jian-min,et al.Determination of 6elements in iron ore by ICP-AES[J].Metallurgical Analysis,2003,23(3):67,50.
[17]云作敏,金丽.电感耦合等离子体发射光谱法测定铁矿石中硅、磷、锰、钙、镁、铝、钛[J].矿产勘查(Mineral Exploration),2010,1(Z1):184-186.
[2]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 6730.19—2016铁矿石分析方法铋磷钼蓝光度法测定磷量[S].北京:中国标准出版社,2016.
[3]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 6730.9—2016铁矿石硅含量的测定硫酸亚铁还原-硅钼蓝分光光度法[S].北京:中国标准出版社,2016.
[4]李文宽.硅钼蓝分光光度法测定磷矿石中的二氧化硅[J].云南化工(Yunnan Chemical Technology),1998(1):42-43.
[5]梁中.碱熔、铋磷钼蓝分光光度法测定钒钛铁矿、钛精矿的磷含量[J].矿业快报(Express Information of Mining Industry),2002,18(1):4-6.
[6]方芳,张然.铋磷钼兰光度法快速测定铁矿石中的磷[J].中国化工贸易(China Chemical Trade),2013,6(4):265.
[7]潘永平.双波长分光光度法同时测定铁矿中磷和砷[J].冶金分析,2002,22(4):42-43.PAN Yong-ping.Simultaneous determination of phosphorus and arsenic in iron ore by dual-wavelength spectrophotometry[J].Metallurgical Analysis,2002,22(4):42-43.
[8]刘金,彭元,程先忠.铋盐-钼蓝分光光度法测定铁矿石中的微量磷[J].武汉工业学院学报(Journal of Wuhan Polytechnic University),2012,29(4):35-37.
[9]梁文君,聂纬,郑金云.铋磷钼蓝分光光度法测定金属硅中磷[J].光谱实验室,2002,19(1):124-126.LIANG Wen-jun,NIE Wei,ZHENG Jin-yun.Study on spectrophotometric determination of phosphorus in silicon metal with the blue made from bismuth,phosphorus &molybdenum[J].Chinese Journal of Spectroscopy Laboratory,2002,19(1):124-126.
[10]王慧卿,刘静.光度法快速测定硼铁中硅和磷及其理论探讨[J].莱钢科技(Laigang Science &Technology),2016,34(1):26-28.
[11]许卉,贺萍.多波长线性回归分光光度法同时测定磷和硅[J].光谱实验室,1999,16(1):60-62.XU Hui,HE Ping.Simultaneous spectrophotometric determination of trace phosphorus and silicon in natural water by multi-wavelength linear regression[J].Chinese Journal of Spectroscopy Laboratory,1999,16(1):60-62.
[12]袁秉鉴,戴祥胜.分光光度法快速测定钢铁中的锰、磷、硅[J].化学分析计量,2001,10(4):24-26.YUAN Bing-jian,DAI Xiang-sheng.Quick determination of Mn,P and Si in steel and iron by spectrophotometry[J].Chemical Analysis and Meterage,2001,10(4):24-26.
[13]潘永平.分光光度法测定铁矿石中硅和磷含量[J].金属矿山(Metal Mine),2000,29(9):51-52,54.
[14]迟少婷.分光光度法连续测定铁矿石中磷和钛[J].冶金分析(Metallurgical Analysis),2002,22(1):68-69.
[15]杨莲瑛.分光光度法测定铁矿石中的二氧化硅和五氧化二磷[J].化工管理(Chemical Enterprise Management),2013,27(5):63,65,156.
[16]王丽君,胡述戈,杜建民,等.应用ICP-AES法测定铁矿石中6元素[J].冶金分析,2003,23(3):67,50.WANG Li-jun,HU Shu-ge,DU Jian-min,et al.Determination of 6elements in iron ore by ICP-AES[J].Metallurgical Analysis,2003,23(3):67,50.
[17]云作敏,金丽.电感耦合等离子体发射光谱法测定铁矿石中硅、磷、锰、钙、镁、铝、钛[J].矿产勘查(Mineral Exploration),2010,1(Z1):184-186.