Optimization of thorium content determination method in typical associated ore waste residue

Mingliang BI; Shen LIAO; Xiaoyan LI

doi:10.11889/j.1000-3436.2023-0024

Journal of Radiation Research and Radiation Processing, Volume. 41, Issue 4, 040701(2023)

Optimization of thorium content determination method in typical associated ore waste residue

Mingliang BI1,*... Shen LIAO2 and Xiaoyan LI3 |Show fewer author(s)

¹Radiation Environment Monitoring Center of Guangdong Province Nuclear Industry Geological Bureau, Guangzhou 510800, China

²Guangdong Nuclear Power Engineering Survey Institute, Guangzhou 510800, China

³School of Nuclear Science and Engineering, East China University of Technology, Nanchang 330013, China

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Figures & Tables(7)

Fig. 1. Concentration curves of thorium content detected in each sample under different digestion times

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Table 1. Verification of factors that may affect the results during the experimental process

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Table 1. Verification of factors that may affect the results during the experimental process

影响因素 Influence factors	不合格数 Unqualifi- ed quantity	影响因素 Influence factors	不合格数 Unqualifi-ed quantity
未确认仪器状况Unconfirmed instrument condition	0	消解环境温度变化大Digestion of environmental temperature changes	0
操作不熟练Unskilled in operation	0	加试剂的量不统一Different reagent quantities	0
配制试剂不准确Inaccurate reagents	0	样品残留萃取剂Sample residual extractant	11
消解设备控温差异Temperature difference of digestion equipment	0	重复消解次数不足Insufficient repeated digestion times	18
分液漏斗有漏液Leakage of separatory funnel	1	酸的纯度不够Insufficient purity of acid	0
光度计性能不合要求Unqualified photometer	0	萃取剂质量问题Quality issues with extractants	0
通风橱抽风速率不一致Inconsistent wind speed in fume hood	0	标准曲线线性不好Poor linearity of standard curve	0
试验用水纯度不够Insufficient purity of test water	0	比色时间过长Colorimetric time too long	9

Table 2. Thorium content detected in each sample under different digestion times

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Table 2. Thorium content detected in each sample under different digestion times

矿渣名称Slag name	测定值1 Measured value 1	测定值2 Measured value 2	测定值3 Measured value 3	测定值4 Measured value 4	测定值5 Measured value 5
锌废渣 Zinc waste residue	6.03	7.38	8.66	8.52	8.61
铜矿废渣 Copper mine waste residue	9.01	9.76	10.70	10.60	10.40
钒矿废渣 Vanadium ore waste	5.78	8.79	9.31	9.28	9.25
铅矿废渣 Lead ore waste	5.23	6.09	6.45	6.53	6.63
汞矿废渣 Mercury ore waste	2.01	2.08	2.33	2.41	2.27
钛冶炼渣 Titanium smelting slag	327	377	410	415	405
国标物 National standard GBW04119	10.1	11.5	11.9	11.8	11.7

Table 3. Absorbance measurements of thorium solutions at different concentrations at different colorimetric time

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Table 3. Absorbance measurements of thorium solutions at different concentrations at different colorimetric time

时间 / min Time	钍溶液浓度 / (μg·mL^-1) Concentration of thorium solution
时间 / min Time	0.05	0.20	0.60
1	0.056	0.235	0.684
2	0.061	0.248	0.695
3	0.063	0.249	0.695
4	0.063	0.248	0.695
5	0.062	0.245	0.694
6	0.059	0.243	0.691
7	0.056	0.240	0.689
8	0.054	0.237	0.687
9	0.051	0.234	0.684
10	0.048	0.231	0.683

Table 4. Determination values of thorium content in samples before and after the use of hydrogen peroxide and perchloric acid digestion extractants

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Table 4. Determination values of thorium content in samples before and after the use of hydrogen peroxide and perchloric acid digestion extractants

矿渣名称

Slag name

锌废渣

Zinc waste residue

铜矿废渣

Copper mine waste residue

钒矿废渣

Vanadium

ore waste

铅矿废渣

Lead ore waste

汞矿废渣

Mercury ore waste

钛冶炼渣

Titanium smelting slag

国标物

National standard GBW04119

消解前测定值 Measured value before digestion

6.15

9.12

6.35

5.68

1.45

329

10.4

消解后测定值 Measured value after digestion

8.66

10.7

9.31

6.45

2.33

410

11.9

Table 5. Analysis of measurement results after experimental optimization

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Table 5. Analysis of measurement results after experimental optimization

矿渣名称 Slag name	测定值1/ (mg‧kg^-1) Measured value 1	测定值2/ (mg‧kg^-1) Measured value 2	测定值3/ (mg‧kg^-1) Measured value 3	平均值/ (mg‧kg^-1) Average value	相对标准偏差 / % Relative standard deviation	回收率 / % Rate of recovery
锌废渣Zinc waste residue	8.66	8.64	8.72	8.67	0.48	99.3
铜矿废渣Copper mine waste residue	10.7	10.8	10.6	10.7	0.93	87.2
钒矿废渣Vanadium ore waste	9.19	9.26	9.24	9.23	0.39	104.9
铅矿废渣Lead ore waste	6.64	6.62	6.68	6.65	0.46	96.8
汞矿废渣Mercury ore waste	2.21	2.29	2.28	2.26	1.93	84.7
钛冶炼渣Titanium smelting slag	403	401	404	403	0.38	95.2
国标物National standard GBW04119	11.7	11.8	12.1	11.9	0.84	99.4

Table 6. Comparison results and relative standard deviation of three different methods

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Table 6. Comparison results and relative standard deviation of three different methods

矿渣名称Slag name	分光光度法/ (mg‧kg^-1) Spectrophotometry	ICP-MS法/ (mg‧kg^-1) ICP-MS method	γ谱仪法 / (mg‧kg^-1) γ Spectrometer method	相对标准偏差 / % Relative standard deviation
锌废渣Zinc waste residue	8.67	8.88	8.75	1.2
铜矿废渣Copper mine waste residue	10.7	10.9	11.3	2.8
钒矿废渣Vanadium ore waste	9.23	9.25	9.27	0.2
铅矿废渣Lead ore waste	6.65	6.73	6.65	0.7
汞矿废渣Mercury ore waste	2.26	2.46	2.30	4.5
钛冶炼渣Titanium smelting slag	403	408	406	0.6
国标物National standard GBW04119	11.9	11.7	11.9	1.0

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Mingliang BI, Shen LIAO, Xiaoyan LI. Optimization of thorium content determination method in typical associated ore waste residue[J]. Journal of Radiation Research and Radiation Processing, 2023, 41(4): 040701

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Paper Information

Category: Research Articles

Received: Mar. 27, 2023

Accepted: May. 4, 2023

Published Online: Sep. 21, 2023

The Author Email:

DOI:10.11889/j.1000-3436.2023-0024

Topics

laser devices and laser physics

Lasers and Laser Optics

Laser physics

laser manufacturing

Instrumentation, Measurement and Metrology

Table 1. Verification of factors that may affect the results during the experimental process

Table 1. Verification of factors that may affect the results during the experimental process

Table 2. Thorium content detected in each sample under different digestion times

Table 2. Thorium content detected in each sample under different digestion times

Table 3. Absorbance measurements of thorium solutions at different concentrations at different colorimetric time

Table 3. Absorbance measurements of thorium solutions at different concentrations at different colorimetric time

Table 4. Determination values of thorium content in samples before and after the use of hydrogen peroxide and perchloric acid digestion extractants

Table 4. Determination values of thorium content in samples before and after the use of hydrogen peroxide and perchloric acid digestion extractants

Table 5. Analysis of measurement results after experimental optimization

Table 5. Analysis of measurement results after experimental optimization

Table 6. Comparison results and relative standard deviation of three different methods

Table 6. Comparison results and relative standard deviation of three different methods

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