钒钛磁铁矿的微波消解及极谱法测定钒的研究
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摘要
铁矿石是国家建设进程中大量使用的资源,随着铁矿石的大量开采以及进口带来的质量问题也不容忽视。钒钛磁铁矿是我国大量进口的一种铁矿石,同时也是一种较为难溶的矿石,因此具有代表性。本课题通过采用钒钛磁铁矿标准品作为研究对象,进行了微波消解及主元素测定研究,具体研究内容与结果如下:
1.建立了以下四种微波消解体系:
(1)硫磷混酸消解体系:0.2000g样品,少量水润湿,9.00mL浓磷酸,3.00mL浓硫酸及少量浓硝酸,在微波功率350 W持续2 min,560 W持续6 min,350 W持续2 min的消解程序下进行样品消解。
(2)氢氟酸与磷酸消解体系:0.1000g样品,少量水润湿,2.00mL氢氟酸,8.00mL浓磷酸,在微波功率280W持续6min,350W持续2min的消解程序下对样品进行消解。
(3)添加络合物的消解体系:0.1000g样品,0.0400g 8-羟基喹啉,少量水润湿,10.00~12.00mL浓盐酸,在微波功率385W下对样品消解10~12min。
(4)碱熔体系:0.1000g样品加入到高铝坩埚中,3.000g溶剂(m_(NaOH):m_(Na2O2)=1:2),在微波功率385W下对样品消解10min。
体系(1)与体系(2)采用钛铁连续测定的方法来确定其中铁与钛的含量,体系(3)与体系(4)采用重铬酸钾法对铁进行测定,通过对样品中钛、铁含量的测定来判断微波消解的完全程度。结果表明,建立的四种微波消解体系对钒钛磁铁矿均能消解完全,结果符合分析化学的要求。
2.建立了醋酸-醋酸钠—邻菲罗啉测定钒钛磁铁矿中微量钒的新方法。
经过实验优化,最佳试剂条件:5.00mL pH≈4.5醋酸-醋酸钠缓冲溶液,3.00mL 1.00g/L邻菲罗啉,蒸馏水定容至25.00mL;最佳测定条件:测试波形为一阶导数波,起始电位为-0.20V,扫描速率为1.00V/s,扫描次数为4次,静止时间为14s。在最佳试剂和测定条件下,钒(V)浓度在0.050~5.0μg/mL的范围内,峰电流的峰高与钒的浓度呈线性关系,线性回归方程Ip’(×10~4nA) = 13.631-1.7678c(μg/mL) (n=7,R~2 = 0.9953),方法的检出限为0.0042μg/mL。该方法灵敏度高,测定范围宽,操作简便快速。新建立的方法应用于实际样品钒钛磁铁矿中微量钒的测定,分析的准确度和精密度满足分析化学要求。
本文研究了电极反应物的反应机理,结果表明,主要电极反应物为质子化的邻菲罗啉,该极谱波为不可逆的吸附波。
Iron ore was the resource that largely used in national construction process. The quality problem of iron ore would not be igored with minings and imports of plenty of iron ore. Vanadium and titanium magnetite was one of the inport iron ores in our country, and it was hard to digest, so the vanadium and titanium magnetite was representative. This topic had studied microwave digestion and determination of main element of vanadium and titanium magnetite standard sample. The main research content and results were followed:
1. Four kinds of microwave digestion system had been established:
(1) Mixed system of sulfuric acid and phosphoric acid: 0.2000g of vanadium and titanium magnetite sample, 3.00mL of concentrated H_2SO_4, 9.00mL of concentrated H_3PO_4, 5 droplets of HNO_3, The digestion procedure was: holding 2min in microwave power of 350W and holding 6min in microwave power of 560W, holding 2min in microwave power of 350W at last.
(2) Mixed system of hydrofluoric acid and phosphoric acid: 0.1000g of vanadium and titanium magnetite sample, 10.00mL of mixed acid (VH_3PO_4 / V_(HF) was 2:8), The digestion procedure was: holding 6min in microwave power of 280W and holding 2min in microwave power of 350W.
(3) Digestion system with complex: 0.1000g of vanadium and titanium magnetite, 0.0400g of complexant(8-hydroxyquinoline), 12.00mL of concentrated HCl, digestion time was 10~12min, microwave power was 385W.
(4) Alkali fusion: 0.1000g of vanadium and titanium magnetite, 3.000g of total mixed-flux (m_(NaOH)/m_(Na2O2) was 1:2), holding 10 min in microwave power of 385W.
Titanium and iron were determined one after another in the first and second system. Iron was determined by dichromatemethod in the third and forth system. The level of digestion was judged by the concentrations of titanium and iron in samples. The results showed that the four systems could digest vanadium and titanium magnetite completely and the consequences had met the analytical chemistry requirements.
2. A new method had been developed for the determination of micro amounts of vanadium in a buffer solution of HAc-NaAc.
Optimization reagent conditions: 5.00mL of buffer solution of HAc-NaAc at a pH of 4.5, 3.00mL of 1.00g/L phenanthroline(Phen) solution, then final volume was 25.00mL through adding distilled water. Optimization instrument conditions: determination waveform was the first order derivative wave, starting potential was -0.20V, scanning rate was 1.00V/s, scanning times was four and static time was 14s. Under the optimal condition, the linear range of vanadium determination was 0.050-5.0μg/mL, the linear equation was Ip’(×10~4nA) = 13.631-1.7678c(μg/mL) (n=7,R~2 = 0.9953), the detection limit was 0.0042μg/ml. The method had the advantage of the high sensitivity, wide linear range, simpleness and celerity. This method had been successfully applied to determination of micro amounts of vanadium in vanadium and titanium magnetite. The results had met with requirements of analytical chemistry.
The mechanism of electrode reactant had been also studied. The results showed that the main electrode reactant was protonated Phen, and the polarographic wave was an irreversible adsorption wave.
1.建立了以下四种微波消解体系:
(1)硫磷混酸消解体系:0.2000g样品,少量水润湿,9.00mL浓磷酸,3.00mL浓硫酸及少量浓硝酸,在微波功率350 W持续2 min,560 W持续6 min,350 W持续2 min的消解程序下进行样品消解。
(2)氢氟酸与磷酸消解体系:0.1000g样品,少量水润湿,2.00mL氢氟酸,8.00mL浓磷酸,在微波功率280W持续6min,350W持续2min的消解程序下对样品进行消解。
(3)添加络合物的消解体系:0.1000g样品,0.0400g 8-羟基喹啉,少量水润湿,10.00~12.00mL浓盐酸,在微波功率385W下对样品消解10~12min。
(4)碱熔体系:0.1000g样品加入到高铝坩埚中,3.000g溶剂(m_(NaOH):m_(Na2O2)=1:2),在微波功率385W下对样品消解10min。
体系(1)与体系(2)采用钛铁连续测定的方法来确定其中铁与钛的含量,体系(3)与体系(4)采用重铬酸钾法对铁进行测定,通过对样品中钛、铁含量的测定来判断微波消解的完全程度。结果表明,建立的四种微波消解体系对钒钛磁铁矿均能消解完全,结果符合分析化学的要求。
2.建立了醋酸-醋酸钠—邻菲罗啉测定钒钛磁铁矿中微量钒的新方法。
经过实验优化,最佳试剂条件:5.00mL pH≈4.5醋酸-醋酸钠缓冲溶液,3.00mL 1.00g/L邻菲罗啉,蒸馏水定容至25.00mL;最佳测定条件:测试波形为一阶导数波,起始电位为-0.20V,扫描速率为1.00V/s,扫描次数为4次,静止时间为14s。在最佳试剂和测定条件下,钒(V)浓度在0.050~5.0μg/mL的范围内,峰电流的峰高与钒的浓度呈线性关系,线性回归方程Ip’(×10~4nA) = 13.631-1.7678c(μg/mL) (n=7,R~2 = 0.9953),方法的检出限为0.0042μg/mL。该方法灵敏度高,测定范围宽,操作简便快速。新建立的方法应用于实际样品钒钛磁铁矿中微量钒的测定,分析的准确度和精密度满足分析化学要求。
本文研究了电极反应物的反应机理,结果表明,主要电极反应物为质子化的邻菲罗啉,该极谱波为不可逆的吸附波。
Iron ore was the resource that largely used in national construction process. The quality problem of iron ore would not be igored with minings and imports of plenty of iron ore. Vanadium and titanium magnetite was one of the inport iron ores in our country, and it was hard to digest, so the vanadium and titanium magnetite was representative. This topic had studied microwave digestion and determination of main element of vanadium and titanium magnetite standard sample. The main research content and results were followed:
1. Four kinds of microwave digestion system had been established:
(1) Mixed system of sulfuric acid and phosphoric acid: 0.2000g of vanadium and titanium magnetite sample, 3.00mL of concentrated H_2SO_4, 9.00mL of concentrated H_3PO_4, 5 droplets of HNO_3, The digestion procedure was: holding 2min in microwave power of 350W and holding 6min in microwave power of 560W, holding 2min in microwave power of 350W at last.
(2) Mixed system of hydrofluoric acid and phosphoric acid: 0.1000g of vanadium and titanium magnetite sample, 10.00mL of mixed acid (VH_3PO_4 / V_(HF) was 2:8), The digestion procedure was: holding 6min in microwave power of 280W and holding 2min in microwave power of 350W.
(3) Digestion system with complex: 0.1000g of vanadium and titanium magnetite, 0.0400g of complexant(8-hydroxyquinoline), 12.00mL of concentrated HCl, digestion time was 10~12min, microwave power was 385W.
(4) Alkali fusion: 0.1000g of vanadium and titanium magnetite, 3.000g of total mixed-flux (m_(NaOH)/m_(Na2O2) was 1:2), holding 10 min in microwave power of 385W.
Titanium and iron were determined one after another in the first and second system. Iron was determined by dichromatemethod in the third and forth system. The level of digestion was judged by the concentrations of titanium and iron in samples. The results showed that the four systems could digest vanadium and titanium magnetite completely and the consequences had met the analytical chemistry requirements.
2. A new method had been developed for the determination of micro amounts of vanadium in a buffer solution of HAc-NaAc.
Optimization reagent conditions: 5.00mL of buffer solution of HAc-NaAc at a pH of 4.5, 3.00mL of 1.00g/L phenanthroline(Phen) solution, then final volume was 25.00mL through adding distilled water. Optimization instrument conditions: determination waveform was the first order derivative wave, starting potential was -0.20V, scanning rate was 1.00V/s, scanning times was four and static time was 14s. Under the optimal condition, the linear range of vanadium determination was 0.050-5.0μg/mL, the linear equation was Ip’(×10~4nA) = 13.631-1.7678c(μg/mL) (n=7,R~2 = 0.9953), the detection limit was 0.0042μg/ml. The method had the advantage of the high sensitivity, wide linear range, simpleness and celerity. This method had been successfully applied to determination of micro amounts of vanadium in vanadium and titanium magnetite. The results had met with requirements of analytical chemistry.
The mechanism of electrode reactant had been also studied. The results showed that the main electrode reactant was protonated Phen, and the polarographic wave was an irreversible adsorption wave.
引文
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