Multi-Element Quantitative Analysis of Shale and Sandstone Based on Laser Induced Breakdown Spectroscopy

Mingxin Shi; Jian Wu; Di Wu; Jinghui Li; Yan Qiu; Xinyu Guo; Ying Zhou; Ziyuan Song; Minxin Chen

doi:10.3788/CJL231332

Chinese Journal of Lasers, Volume. 51, Issue 8, 0811002(2024)

Multi-Element Quantitative Analysis of Shale and Sandstone Based on Laser Induced Breakdown Spectroscopy

Mingxin Shi¹, Jian Wu^1、*, Di Wu¹, Jinghui Li¹, Yan Qiu², Xinyu Guo¹, Ying Zhou¹, Ziyuan Song¹, and Minxin Chen¹

¹State Key Laboratory of Electrical Insulation and Power Equipment, School of Electrical Engineering, Xi an Jiaotong University, Xi an 710049, Shaanxi , China

²Ministry of Education Key Laboratory of Electronic Physics and Devices, School of Electronic Science and Engineering, Xi an Jiaotong University, Xi an 710049, Shaanxi , China

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Figures & Tables(10)

Fig. 1. A diagram for the micro-LIBS system setup

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Fig. 2. Photos of representative shale and sandstone samples

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Fig. 3. Typical spectra of shale and sandstone samples

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Fig. 4. PLSR parameter optimization flow chart

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Fig. 5. Parameter optimization process of Si element

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Fig. 6. Input spectrum after parameter optimization (shale No. 2)

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Fig. 7. Calibration curves of Si, Ca, Fe, Al, and Mg elements. (a) Si element; (b) Ca element; (c) Fe element; (d) Al element; (e) Mg element

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Table 1. Mass fraction of each element in shale and sandstone samples

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Table 1. Mass fraction of each element in shale and sandstone samples

Data set		Mass fraction /%
Data set		Si	Ca	Fe	Al	Mg
Shale （sample size is 23）	Mean	26.51	2.77	5.61	12.92	2.13
	Median	27.28	2.75	4.67	10.03	2.07
	Min	17.15	0.92	0.79	4.20	0.38
	Max	35.09	5.28	16.67	37.10	5.33
	STD	4.49	1.16	3.42	7.43	1.04
	RSD /%	16.93	41.77	61.13	57.48	49.06
Sandstone （sample size is 22）	Mean	29.06	6.67	2.29	4.61	1.67
	Median	31.43	6.54	2.20	4.49	1.23
	Min	13.57	0.94	1.54	2.69	0.55
	Max	41.02	17.21	3.61	6.61	5.66
	STD	7.39	4.54	0.67	1.18	1.15
	RSD /%	25.42	68.02	29.07	25.69	69.12

Table 2. Relative standard deviation of spectra before and after pretreatment

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Table 2. Relative standard deviation of spectra before and after pretreatment

Data set		Si	Ca	Fe	Al	Mg
Shale	$R_{s i n g l e}^{O r i g i n}$	21.00±6.39	57.27±27.04	29.90±16.49	26.15±11.78	28.16±18.22
	$R_{S - S}^{O r i g i n}$	27.51	63.54	51.44	27.17	40.13
	$R_{s i n g l e}^{P r e t r e a t e d}$	10.70±5.15	10.69±17.66	20.99±10.37	14.52±6.71	15.77±7.63
	$R_{S - S}^{P r e t r e a t e d}$	24.83	61.56	52.58	26.19	37.89
Sandstone	$R_{s i n g l e}^{O r i g i n}$	20.52±8.78	88.06±63.69	72.98±29.58	44.30±15.51	54.18±22.18
	$R_{S - S}^{O r i g i n}$	26.22	81.11	58.69	29.86	56.10
	$R_{s i n g l e}^{P r e t r e a t e d}$	7.83±3.22	44.31±28.02	42.49±24.95	34.30±21.73	40.67±16.69
	$R_{S - S}^{P r e t r e a t e d}$	15.22	73.79	58.69	31.35	53.21

Table 3. Evaluation indexes of quantitative analysis of Si, Ca, Fe, Al, Mg elements

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Table 3. Evaluation indexes of quantitative analysis of Si, Ca, Fe, Al, Mg elements

Sample and element		R²	RMSEC /%	RMSEP /%	RMSECV /%
Shale	Si	0.9524	1.0270	1.7494	1.9027
	Ca	0.9170	0.3286	0.3615	0.7467
	Fe	0.9915	0.3369	0.9181	1.0515
	Al	0.9870	0.9177	2.8818	3.8290
	Mg	0.9909	0.1071	0.7705	0.3389
Sandstone	Si	0.9697	1.2171	2.6230	3.4010
	Ca	0.9737	0.7594	0.9745	1.5270
	Fe	0.9457	0.1529	0.1355	0.3406
	Al	0.9661	0.2448	0.7133	0.7810
	Mg	0.9093	0.2090	0.3744	0.3809

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Mingxin Shi, Jian Wu, Di Wu, Jinghui Li, Yan Qiu, Xinyu Guo, Ying Zhou, Ziyuan Song, Minxin Chen. Multi-Element Quantitative Analysis of Shale and Sandstone Based on Laser Induced Breakdown Spectroscopy[J]. Chinese Journal of Lasers, 2024, 51(8): 0811002

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Paper Information

Category: spectroscopy

Received: Oct. 27, 2023

Accepted: Dec. 11, 2023

Published Online: Mar. 29, 2024

The Author Email: Jian Wu (jxjawj@mail.xjtu.edu.cn)

DOI:10.3788/CJL231332

CSTR:32183.14.CJL231332

Topics

laser devices and laser physics

Lasers and Laser Optics

Laser physics

laser manufacturing

Instrumentation, Measurement and Metrology