Determination of primary metal elements in LiF-UF<sub>4</sub> and LiF-ThF<sub>4</sub> molten salts via inductively coupled plasma atomic emission spectrometry

Ling HAN; Yuanyuan TANG; Min GE; Yuan QIAN; Hongtao LIU

doi:10.11889/j.0253-3219.2024.hjs.47.030603

NUCLEAR TECHNIQUES, Volume. 47, Issue 3, 030603(2024)

Determination of primary metal elements in LiF-UF₄ and LiF-ThF₄ molten salts via inductively coupled plasma atomic emission spectrometry

Ling HAN^1,2, Yuanyuan TANG^1、*, Min GE¹, Yuan QIAN¹, and Hongtao LIU¹

Author Affiliations

¹Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201800, China

²University of Chinese Academy of Sciences, Beijing 100049, China

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Figures & Tables(9)

Table 1. Operating parameters of ICP-AES

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Table 1. Operating parameters of ICP-AES

仪器参数

Parameters

、

设定值

Settings

、

仪器参数

Parameters

、

设定值

Settings

、

RF功率

RF power

1 350 W

等离子气

Plasma gas

13.0 mL·min^-1

观测方式

Observation mode

轴向

Axis

雾化气

Nebulizer gas

0.8 mL·min^-1

重复测定次数

Replicates

辅助气

Auxiliary gas

0.8 mL·min^-1

Table 2. Samples with different mass ratios

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Table 2. Samples with different mass ratios

样品编号 Sample number 、	FLiU元素质量比 Element mass ratio of FLiU / % 、		样品编号 Sample number 、	FLiTh元素质量比 Element mass ratio of FLiTh / % 、
样品编号 Sample number 、	Li	U	样品编号 Sample number 、	Li	Th
FLiU-1#	3.87	64.89	FLiTh-1#	4.43	62.93
FLiU-2#	4.73	62.50	FLiTh-2#	5.44	60.11
FLiU-3#	5.84	59.35	FLiTh-3#	6.80	56.31

Table 3. Comparison of four FLiU dissolution methods

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Table 3. Comparison of four FLiU dissolution methods

方法

Method

、

实验条件

Experimental condition

、

实验现象

Experimental phenomena

、

称取0.2 g FLiU-2#，加入5 mL HNO₃，密封，微波消解仪加热

A mixture of FLiU-2# (0.2 g), and HNO₃ (5 mL) in a closed Tefon beaker (50 mL)

was heated (MARS 7) at 120 ℃

底部有大量不溶物

Large amount of insoluble material

称取0.2 g FLiU-2#，加入5 mL HNO₃、2 mL H₂O₂，密封，微波消解仪加热

A mixture of FLiU-2# (0.2 g), HNO₃ (5 mL), and H₂O₂ (2 mL) in a closed Tefon beaker (50 mL) was heated (MARS 7) at 120 ℃

溶解完全，溶液澄清

Completely dissolved

称取0.2 g FLiU-2#，加入10 mL 20% HNO₃、2 mL H₂O₂，密封，微波消解仪加热

A mixture of FLiU-2# (0.2 g), HNO₃ (10 mL 20%), and H₂O₂ (2 mL) in a closed Tefon beaker (50 mL) was heated (MARS 7) at 120 ℃

溶解完全，溶液澄清

Completely dissolved

称取0.2 g FLiU-2#，加入10 mL 20% HNO₃、2 mL H₂O₂，密封，石墨消解仪加热

A mixture of FLiU-2# (0.2 g), HNO₃ (10 mL 20%), and H₂O₂ (2 mL) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 120 ℃

溶解完全，溶液澄清

Completely dissolved

Table 4. Comparison of four FLiTh dissolution methods

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Table 4. Comparison of four FLiTh dissolution methods

方法

Method

、

实验条件

Experimental condition

、

实验现象

Experimental phenomena

、

称取0.2 g FLiTh-2#A mixture of FLiTh-2# (0.2 g)

加入0.5 g硝酸铝、10 mL 10% HNO₃，90 ℃加热

Al(NO₃)₃ (0.5 g), and HNO₃ (10 mL 10%) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 90 ℃

底部有大量不溶物

Large amount of insoluble material

加入1.0 g硝酸铝、10 mL 10% HNO₃，90 ℃加热

Al(NO₃)₃ (1.0 g), and HNO₃ (10 mL 10%) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 90 ℃

底部有大量不溶物

Large amount of insoluble material

加入1.5 g硝酸铝、10 mL 10% HNO₃，90 ℃加热

Al(NO₃)₃ (1.5 g), and HNO₃ (10 mL 10%) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 90 ℃

底部有少量不溶物

Small amount of insoluble material

加入2.0 g硝酸铝、10 mL 10% HNO₃，90 ℃加热

Al(NO₃)₃ (2.0 g), and HNO₃ (10 mL 10%) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 90 ℃

溶解完全，溶液澄清

Completely dissolved

加入2.5 g硝酸铝、10 mL 10% HNO₃，90 ℃加热

Al(NO₃)₃ (2.5 g), and HNO₃ (10 mL 10%) in a closed Tefon beaker (50 mL) was heated (HotBlock 100) at 90 ℃

溶解完全，溶液澄清

Completely dissolved

Table 5. Effect of Al content on Li test results

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Table 5. Effect of Al content on Li test results

Al含量

Content of Al / μg·mL^-1

、

Li含量-理论值

Theoretical value of Li / μg·mL^-1

、

Li含量-测试值

Measured value of Li / μg·mL^-1

、

相对误差

Relative error / %

、

20.00

2.000

2.013

0.6

30.00

2.000

1.995

-0.2

40.00

2.000

2.015

0.8

Table 6. Sample precision test results (using FLiU, %)

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Table 6. Sample precision test results (using FLiU, %)

样品编号 Sample number 、	元素 Elemental 、	测定值 Measured value / %(w/w) 、							平均值 Average value / % (w/w) 、	相对标准偏差Relative standard deviation / %
FLiU-1#	Li	3.82	3.79	3.85	3.92	3.89	3.85	3.83	3.85	1.1
FLiU-1#	U	64.75	64.98	65.02	65.04	64.95	64.69	64.97	64.91	0.2
FLiU-2#	Li	4.59	4.68	4.75	4.62	4.81	4.82	4.64	4.70	2.0
FLiU-2#	U	62.93	62.46	62.85	62.08	62.97	63.14	63.52	62.85	0.7
FLiU-3#	Li	5.93	5.91	5.78	5.82	5.89	5.97	5.96	5.89	1.2
FLiU-3#	U	59.52	59.46	59.58	59.12	59.37	59.42	59.67	59.45	0.3

Table 7. Sample precision test results (using FLiTh, %)

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Table 7. Sample precision test results (using FLiTh, %)

样品编号 Sample number 、	元素 Elemental 、	测定值 Measured value / %(w/w) 、							平均值 Average value / % (w/w) 、	相对标准偏差Relative standard deviation / %
FLiTh-1#	Li	4.35	4.56	4.52	4.39	4.35	4.37	4.48	4.43	2.0
FLiTh-1#	Th	62.98	62.76	62.56	62.96	62.48	62.37	62.65	62.68	0.4
FLiTh-2#	Li	5.58	5.62	5.42	5.51	5.54	5.32	5.41	5.49	1.9
FLiTh-2#	Th	60.23	60.35	60.41	60.21	60.07	60.45	60.05	60.25	0.3
FLiTh-3#	Li	6.92	6.72	6.68	6.75	6.91	6.65	6.59	6.75	1.9
FLiTh-3#	Th	56.38	56.68	56.27	56.15	56.42	56.59	56.21	56.39	0.3

Table 8. Content accuracy test results of lithium and uranium (n=10)

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Table 8. Content accuracy test results of lithium and uranium (n=10)

元素

Elemental

、

理论值

Theoretical value / μg·g^-1

、

测定值

Measured value / μg·g^-1

、

回收率

Recovery / %

、

平均回收率

Average recovery / %

、

2.000

2.002, 2.012, 2.013, 1.996, 2.047, 2.018, 2.024, 2.031, 2.019, 1.992

100.1, 100.6, 100.7, 99.8, 102.4, 100.9, 101.2, 101.6, 101.0, 99.6

100.8

24.566

24.871, 24.890, 24.951, 24.476, 24.534, 24.912, 24.897, 24.965, 24.689, 24.998

101.2, 101.3, 101.6, 99.6, 99.9, 101.4, 101.3, 101.6, 100.5, 101.8

101.0

Table 9. Content accuracy test results of lithium and thorium (n=10)

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Table 9. Content accuracy test results of lithium and thorium (n=10)

元素

Elemental

、

理论值

Theoretical value/ μg·g^-1

、

测定值

Measured value / μg·g^-1

、

回收率

Recovery / %

、

平均回收率

Average recovery / %

、

2.000

2.046, 2.008, 2.017, 2.021, 1.995, 2.023, 2.008, 1.992, 2.041, 2.019

102.3, 100.4, 100.9, 101.1, 99.8, 101.2, 100.4, 99.6, 102.1, 101.0

100.9

24.000

24.452, 23.897, 24.213, 24.089, 23.998, 24.568, 23.858, 24.567, 24.421, 24.531

101.9, 99.6, 100.9, 100.4, 100.0, 102.4, 99.4, 102.4, 101.8, 102.2

101.1

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Ling HAN, Yuanyuan TANG, Min GE, Yuan QIAN, Hongtao LIU. Determination of primary metal elements in LiF-UF₄ and LiF-ThF₄ molten salts via inductively coupled plasma atomic emission spectrometry[J]. NUCLEAR TECHNIQUES, 2024, 47(3): 030603

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Paper Information

Category: Research Articles

Received: Sep. 1, 2023

Accepted: --

Published Online: Apr. 29, 2024

The Author Email: Yuanyuan TANG (TANGYuanyuan)

DOI:10.11889/j.0253-3219.2024.hjs.47.030603

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laser devices and laser physics

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