过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中的高含量钛

赵昕; 严慧; 禹莲玲; 汤行; 柳昭

doi:10.15898/j.cnki.11-2131/td.201911020150

过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中的高含量钛

湖南省地质测试研究院, 湖南长沙 410007

基金项目:
中央引导地方科技发展专项资金项目“湖南省地质测试研究院大型仪器科研购置”(2018KT5001)；湖南省地质矿产勘查开发局科研基金项目(201808)

详细信息

作者简介: 赵昕, 硕士, 工程师, 主要从事岩矿测试分析。E-mail:365827149@qq.com

通讯作者: 严慧, 硕士, 高级工程师, 主要从事地质实验测试技术方面的应用及研究。E-mail:223305564@qq.com

中图分类号: P578.44;O657.31

收稿日期: 2019-11-02

修回日期: 2020-02-23

录用日期: 2020-04-16

Determination of High Content of Titanium in Ilmenite by Inductively Coupled Plasma-Optical Emission Spectrometry with Sodium Peroxide Alkali Fusion

Geological Testing Institute of Hunan Province, Changsha 410007, China

More Information

Corresponding author: Hui YAN, 223305564@qq.com

Received Date: 02 November 2019

Revised Date: 23 February 2020

Accepted Date: 16 April 2020

摘要

摘要: 钛矿资源主要类型为钛铁矿岩矿、钛铁矿砂矿、金红石矿。钛铁矿属于难熔矿物，一般不溶于硝酸、盐酸或王水。对于高品位钛铁矿，即使采用盐酸-硝酸-氢氟酸-高氯酸混合酸溶解样品，钛元素也易水解形成难溶的偏钛酸析出，常给分析带来很大困难。容量法和分光光度法等传统方法测定钛存在操作流程长、步骤多、效率低等不足。因此，选择合适前处理方法的同时将大型仪器分析方法结合起来，有利于提高钛铁矿分析的准确度和测试效率。本文建立了以2.0g过氧化钠为熔剂，使用刚玉坩埚在700℃熔融样品15min，热水浸取后盐酸酸化，用电感耦合等离子体发射光谱(ICP-OES)测定钛铁矿中的高含量钛元素的方法。实验中采用全程空白试液稀释定容标准溶液消除了钠基体影响，通过优化熔融温度和时间使样品分解完全，考察了过氧化钠用量来降低待测溶液中盐分以保证测定的稳定性，通过选择合适的分析谱线并采用背景扣除法消除光谱干扰。本方法检出限为0.0035%，测试范围为0.0066%~62.50%(均以TiO₂含量计)；经钛铁矿国家标准物质(GBW07839、GBW07841)验证，相对标准偏差(RSD，n=12)为1.1%~2.1%，相对误差为-1.69%~1.11%。本方法应用于实际样品分析，相对标准偏差(RSD，n=12)均小于4%，TiO₂分析结果与国家标准方法(硫酸铁铵容量法)一致。本方法有效解决了钛铁矿分解不完全及高含量的钛易水解的问题，实现ICP-OES对不同类型钛铁矿样品中钛元素的定量分析。
- 钛铁矿 /
- 钛 /
- 刚玉坩埚 /
- 过氧化钠碱熔 /
- 电感耦合等离子体发射光谱法
Abstract: BACKGROUNDThe main types of ilmenite resources are ilmenite ore, ilmenite placer, and rutile ore. Ilmenite is a mineral that is difficult to be digested, and generally insoluble in nitric acid, hydrochloric acid or an aqua system. For high-grade ilmenite, even if the sample is dissolved by hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid mixture, titanium element is also easy to hydrolyze to form insoluble partial titanic acid precipitation, which often causes great difficulties in analysis. However, the traditional methods such as volumetric and spectrophotometry have the problems of long operation process, many steps and low efficiency. OBJECTIVESTo improve the accuracy of the analysis of titanium in ilmenite and test efficiency by choosing the appropriate pretreatment combined with large-scale instrument analysis methods. METHODSUsing 2.0g sodium peroxide as flux, the samples were melted in a corundum crucible at 700℃ for 15min. The resulted melts were soaked in hot water of 40-50℃, and then acidified with hydrochloric acid. The high content of titanium in the sample was determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). The effect of the sodium matrix was eliminated by diluting the standard solution with a blank test solution. The sample was decomposed completely by optimizing the melting temperature and time. The salt content in the solution was reduced by optimizing the quality of sodium peroxide to ensure the stability of the determination. The spectral interference was eliminated by optimizing the spectral lines and using the background deduction method. RESULTSThe detection limit of this method was 0.0035%, the analytical ranges were from 0.0066% to 62.50% (both were calculated by TiO₂ content). The relative standard deviations (RSD, n=12) were 1.1%-2.1% and the relative errors were -1.69%-1.11%, which was verified by the national standard materials (GBW07839, GBW07841) of ilmenite. For actual sample analysis, the relative standard deviations of the method (RSD, n=12) were less than 4%. The analytical results were consistent, compared with the national standard method (ferric ammonium sulfate volumetric method). CONCLUSIONSThis method is used to effectively solve the problems of incomplete digestion of ilmenite and easy hydrolysis of high content ilmenite, and achieve rapidly quantitative analysis of titanium content in different ilmenite samples by ICP-OES.
- ilmenite /
- titanium /
- sodium peroxide fusion /
- corundum crucible /
- inductively coupled plasma-optical emission spectrometry

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图 1 不同消解温度和熔融时间下TiO₂测定结果

Figure 1.

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表 1 王水、四酸、碱熔法处理样品TiO₂测定结果

Table 1. Analytical results of TiO₂ in samples dissoluted with aqua regia, four acids and alkali fusion methods

标准物质编号	TiO₂测定值(%)				三种溶解方法TiO₂测定值与认定值的相对误差(%)
标准物质编号	认定值	王水	四酸	碱熔	王水	四酸	碱熔
GBW07839	2.95±0.12	2.63	2.77	2.97	-10.85	-6.10	0.68
GBW07841	19.83±0.36	17.21	18.25	19.97	-13.21	-7.97	0.71

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表 2 不同用量过氧化钠对TiO₂测定的影响

Table 2. Effect of the quality of sodium peroxide on the determination of TiO₂

过氧化钠用量(g)	GBW07839			GBW07841
过氧化钠用量(g)	TiO₂认定值(%)	TiO₂测定值(%)	相对误差(%)	TiO₂认定值(%)	TiO₂测定值(%)	相对误差(%)
1.0	2.95±0.12	2.65	-10.17	19.83±0.36	17.16	-13.46
1.5	2.95±0.12	2.76	-6.44	19.83±0.36	18.29	-7.77
2.0	2.95±0.12	2.92	-1.02	19.83±0.36	19.77	-0.30
2.5	2.95±0.12	2.94	-0.34	19.83±0.36	19.80	-0.15
3.0	2.95±0.12	2.94	-0.34	19.83±0.36	19.79	-0.20

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表 3 实际样品采用X射线荧光光谱法测定结果

Table 3. Analytical results of TiO₂ in the actual samples by X-ray fluorescence spectrometry

样品编号	SiO₂(%)	Al₂O₃ (%)	CaO (%)	TFe₂O₃ (%)	MgO (%)	K₂O (%)	TiO₂ (%)	Na₂O (%)	Mn (%)
Ti-1	54.23	15.37	3.33	13.89	4.57	3.71	3.30	1.47	0.071
Ti-2	52.25	15.46	3.17	12.00	3.48	2.92	6.59	2.49	0.075
Ti-3	30.51	9.54	6.54	30.83	5.36	0.41	16.95	1.58	0.452
Ti-4	2.09	1.19	0.35	47.53	0.48	0.035	48.48	0.14	1.12

样品编号	P (%)	S (mg/kg)	V (mg/kg)	Ni (mg/kg)	Cu (mg/kg)	Zn (mg/kg)	Sr (mg/kg)	Y (mg/kg)	Zr (mg/kg)
Ti-1	0.248	46	212	180	57.3	127	246	33.9	382
Ti-2	0.254	63	282	109	35.3	99	287	34.0	681
Ti-3	0.096	2843	601	51	50.9	198	402	25.9	212
Ti-4	0.024	168	485	25	23.3	296	38	36.9	400

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表 4 实际样品采用本方法和传统化学方法测定结果比对

Table 4. Comparison of analytical results of TiO₂ in the actual sample by this study and chemical method

样品编号	碱熔法(本方法)12次测定TiO₂平均值(%)	容量法TiO₂测定值(%)	RSD(%)
Ti-1	3.11	3.10	2.6
Ti-2	6.39	6.43	3.5
Ti-3	16.52	16.67	2.6
Ti-4	48.30	48.43	1.7

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