改进的碳酸钠-氧化锌半熔-硫酸钡重量法测定重晶石中的硫

张志勇; 陈述; 李子尚; 周海波; 刘晓锋

doi:10.15898/j.cnki.11-2131/td.2015.05.013

改进的碳酸钠-氧化锌半熔-硫酸钡重量法测定重晶石中的硫

1.
长沙矿冶研究院, 湖南长沙 410012

2.
中南大学化学化工学院, 湖南长沙 410083

基金项目: 国家高技术研究发展计划(863计划)项目(2013AA064101)

详细信息

作者简介: 张志勇, 在读博士研究生, 高级工程师, 主要从事岩石矿物化学物相分析及冶金材料测试研究工作.E-mail: zyzhang@minerals.com

中图分类号: P578.71;O613.51;O655.1

收稿日期: 2014-06-23

修回日期: 2015-07-09

录用日期: 2015-09-05

刊出日期: 2015-05-25

Determination of Sulfur in Barite by Sodium Carbonate-Zinc Oxide Semi-molten Decomposition and Barium Sulfate Gravimetric Method

1.
Changsha Research Institute of Mining and Metallurgy, Changsha 410012, China

2.
School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China

Received Date: 23 June 2014

Revised Date: 09 July 2015

Accepted Date: 05 September 2015

Publish Date: 25 May 2015

摘要

摘要:
传统的碳酸钠-氧化锌半熔-硫酸钡重量法测定重晶石中的硫, 具有坩埚腐蚀小、干扰相对较少等优点, 但不能完全破坏重晶石矿物的晶格结构, 造成了硫的测定结果很不稳定。本文通过考察重晶石半熔分解过程中实验条件对硫的转化率的影响, 发现重晶石分解转化不彻底主要是由于样品粒度和熔剂粒度过粗, 故将传统的半熔法的实验条件改进为:采用瓷坩埚熔融, 重晶石样品粒度小于0.10 mm, 碳酸钠-氧化锌熔剂粒度小于0.18 mm, 半熔温度790℃, 半熔时间60 min。在此实验条件下重晶石可全部转化为BaCO₃与SO₄^2-定量分离, 因此不用使用昂贵的铂金坩埚, 也避免了强氧化性熔剂对坩埚的损毁, 减少了熔融时可能引入的干扰物质。本方法精密度(RSD)小于1.0%, 回收率大于99.5%, 适用于分析含重晶石的各类复杂地质样品。
- 重晶石 /
- 硫 /
- 碳酸钠-氧化锌半熔分解 /
- 硫酸钡重量法
Abstract:
The traditional sodium carbonate-zinc oxide semi fusion method causes little corrosion of the crucible and effects small interferences, but the analytical results of sulfur are unstable due to an incomplete break of the lattice structure of barite. The decomposition conditions during semi fusion that affect the conversion of sulfur are investigated and reported in this paper. Results show that the incomplete decomposition of barite was due to the grain sizes of samples and fluxes being too big. The modified method is that samples with sizes of less than 0.1 mm mixed with sodium carbonate-zinc oxide flux with sizes of less than 0.18 mm are decomposed at 790℃ for 60 min. Under these conditions, barite can be converted to BaCO₃ and isolated with SO₄^2- quantitatively through semi molten decomposition in a porcelain crucible, which avoids the use of the platinum crucible, damage of crucibles by strong oxidizing agents, and reduces the interference substances during melting. The RSD for this method was less than 1% and the recovery was more than 99.5%. This method can be applied to determine sulfur content of complex geological samples containing barite.
- barite /
- sulfate /
- sodium carbonate-zinc oxide semi-molten decomposition /
- barium sulfate gravimetric method

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图 1 半熔温度(a)和半熔时间(b)对硫转化率的影响

Figure 1.

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表 1 重晶石样品粒度对硫转化率的影响

Table 1. Effect of sample's size on the leaching rate of sulfur

重晶石粒度
(mm) 转化浸出率
(%) 重晶石粒度
(mm) 转化浸出率
(%)

0.30~0.60 20.30 0.10~0.125 99.85
0.18~0.30 40.55 0.075~0.10 99.88
0.15~0.18 96.57 0.050~0.075 99.89
0.125~0.15 99.57

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表 2 混合熔剂中碳酸钠粒度对硫转化率的影响

Table 2. Effect of sodium carbonate' size in mixed flux on the leaching rate of sulfur

碳酸钠粒度
(mm) 转化浸出率
(%) 碳酸钠粒度
(mm) 转化浸出率
(%)

0.60~1.00 92.30 0.125~0.18 99.87
0.30~0.60 98.05 0.10~0.125 99.75
0.18~0.30 99.56 0.075~0.10 99.65

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表 3 方法准确度与精密度试验

Table 3. Accuracy and precision tests of the method

重晶石
标准物质硫含量的
标准值(%) 硫含量的测定
平均值(%) 相对误差
(%) RSD
(%) 回收率
(%)

GBW07811 6.37 6.35 0.31 0.65 99.7
GBW07812 13.75 13.75 0 0.34 100.0

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参考文献(9)

[1]	岩石矿物分析编委会编著. 岩石矿物分析(第四版)[M]. 北京: 地质出版社, 2011: 427-428(第二分册), 205-206(第一分册). The Editorial Committee of Rock and Mineral Analysis. Rock and Mineral Analysis (Fourth Edition)[M]. Beijing: Geological Publishing House, 2011: 427-428 (Vol. 2), 205-206 (Vol. 1).
[2]	http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201002021.htm
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[7]	http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201102025.htm
[8]	http://www.cnki.com.cn/Article/CJFDTOTAL-YKCS201402009.htm
[9]

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重晶石粒度 (mm)	转化浸出率 (%)	重晶石粒度 (mm)	转化浸出率 (%)
0.30~0.60	20.30	0.10~0.125	99.85
0.18~0.30	40.55	0.075~0.10	99.88
0.15~0.18	96.57	0.050~0.075	99.89
0.125~0.15	99.57

碳酸钠粒度 (mm)	转化浸出率 (%)	碳酸钠粒度 (mm)	转化浸出率 (%)
0.60~1.00	92.30	0.125~0.18	99.87
0.30~0.60	98.05	0.10~0.125	99.75
0.18~0.30	99.56	0.075~0.10	99.65

重晶石标准物质	硫含量的标准值(%)	硫含量的测定平均值(%)	相对误差 (%)	RSD (%)	回收率 (%)
GBW07811	6.37	6.35	0.31	0.65	99.7
GBW07812	13.75	13.75	0	0.34	100.0

改进的碳酸钠-氧化锌半熔-硫酸钡重量法测定重晶石中的硫

1. 长沙矿冶研究院, 湖南 长沙 410012 2. 中南大学化学化工学院, 湖南 长沙 410083

作者简介: 张志勇, 在读博士研究生, 高级工程师, 主要从事岩石矿物化学物相分析及冶金材料测试研究工作.E-mail: zyzhang@minerals.com

Determination of Sulfur in Barite by Sodium Carbonate-Zinc Oxide Semi-molten Decomposition and Barium Sulfate Gravimetric Method

1. Changsha Research Institute of Mining and Metallurgy, Changsha 410012, China 2. School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China

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目录

1.
长沙矿冶研究院, 湖南长沙 410012

2.
中南大学化学化工学院, 湖南长沙 410083

1.
Changsha Research Institute of Mining and Metallurgy, Changsha 410012, China

2.
School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China