Rapid complexometric determination of ytterbium in laser-fiber grade ytterbium chelate

Liu Rongli; Zhang Sijin; Luo Mian; Zhu Qipeng; Wang Chengyuan; Shi Xuefeng

doi:10.11884/HPLPB202638.250419

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Article Navigation > High Power Laser and Particle Beams > 2026 > Accepted Manuscript

Liu Rongli, Zhang Sijin, Luo Mian, et al. Rapid complexometric determination of ytterbium in laser-fiber grade ytterbium chelate[J]. High Power Laser and Particle Beams. doi: 10.11884/HPLPB202638.250419

Citation:

Liu Rongli, Zhang Sijin, Luo Mian, et al. Rapid complexometric determination of ytterbium in laser-fiber grade ytterbium chelate[J]. High Power Laser and Particle Beams. doi: 10.11884/HPLPB202638.250419

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Rapid complexometric determination of ytterbium in laser-fiber grade ytterbium chelate

doi: 10.11884/HPLPB202638.250419

Hunan Rare-Earth Metal Materials Research Institute Co, Ltd, Changsha 410126, China

Received Date: 2025-11-25
Accepted Date: 2026-01-07
Rev Recd Date: 2026-01-13

Available Online: 2026-01-28

Abstract

Abstract

Background
Yb(TMHD)₃ (ytterbium tris (2,2,6,6-tetramethyl-3,5-heptanedionate)) is the irreplaceable vapor-phase dopant for fabricating high-gain Yb-doped silica laser fibers, and its exact Yb content dictates final fiber performance. The conventional oxalate gravimetric method requires 6 h per sample, incompatible with the real-time feedback demanded by modern preform manufacture.
Purpose
In order to enhance the production efficiency,
Methods
we report a “nitric acid-hydrogen peroxide open-vessel digestion/EDTA complexometric titration” protocol. After 3 min oxidative decomposition of the organic matrix, the solution is buffered with hexamethylenetetramine (pH=5-6) and titrated with standard EDTA using xylenol orange (XO) as indicator.
Results
The stoichiometric Yb³⁺ : EDTA ratio is 1∶1; the sharp colour change from rose-red to bright yellow with a relative standard deviation (RSD, n=11) of ≤ 0.5%. Mean recoveries for spiked Yb(TMHD)₃ ranged 98.2%-100.2%. Results for ten commercial lots deviated <0.3% from the gravimetric reference, while the total analysis time was reduced from 6 h to 15 min.
Conclusions
The procedure is accurate, precise, inexpensive and field-robust, enabling on-site monitoring of Yb loading and immediate optimisation of preform deposition parameters.
- Yb(TMHD)₃,
- ytterbium,
- EDTA,
- rapid titration

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References(20)

References

[1]	Snitzer E, Po H, Tumminelli R P, et al. Double-clad fiber amplifier and laser[J]. Opt. Lett., 1988, 13(7): 591-593.
[2]	Jackson S D, King T A. High-power diode-cladding-pumped Tm-doped silica fiber laser[J]. Optics Letters, 1998, 23(18): 1462-1464. doi: 10.1364/OL.23.001462
[3]	Richardson D J, Nilsson J, Clarkson W A. High power fiber lasers: current status and future perspectives [invited][J]. Journal of the Optical Society of America B, 2010, 27(11): B63-B92. doi: 10.1364/JOSAB.27.000B63
[4]	Digonnet M J F. Rare-earth-doped fiber lasers and amplifiers[M]. 2nd ed. Boca Raton: CRC Press, 2001.
[5]	Ainslie B J. A review of the fabrication and properties of erbium-doped fibers for optical amplifiers[J]. Journal of Lightwave Technology, 1991, 9(2): 220-227. doi: 10.1109/50.65880
[6]	Koponen J, Söderlund M, Hoffman H J, et al. Measuring photodarkening from Yb-doped silica fibers[M]. Proc. SPIE, 2006, 6102: 61020R.
[7]	Jetschke S, Unger S, Schwuchow A, et al. Efficiency and photodarkening of Yb-doped fibers: dependence on the core composition[M]. Proc. SPIE, 2007, 6453: 64530I.
[8]	Dong L. Chemical composition and photodarkening of Yb-doped silica fibers[J]. J. Opt. Soc. Am. B, 2019, 36(6): 1583-1590.
[9]	IEC 60793-2-50: 2018, Optical fibers-part 2-50: product specifications-sectional specification for class B single-mode fibers[S].
[10]	叶再兴. 草酸盐重量法测定锆矿石中稀土总量[J]. 广东化工, 2024, 51(6): 119-121 Ye Zaixing. Determination of the total amount of rare earth in zirconium ore by oxalate gravimetric method[J]. Guangdong Chemical Industry, 2024, 51(6): 119-121
[11]	李净岩, 包香春, 张秀艳, 等. 草酸盐重量法测定镨钕熔盐渣废料中稀土总量[J]. 理化检验-化学分册, 2022, 58(3): 350-353 doi: 10.11973/lhjy-hx202203019 Li Jingyan, Bao Xiangchun, Zhang Xiuyan, et al. Determination of total amount of rare earth in molten salt slag waste of praseodymium-neodymium by oxalate gravimetric method[J]. Physical Testing and Chemical Analysis(Part B: Chemical Analysis), 2022, 58(3): 350-353 doi: 10.11973/lhjy-hx202203019
[12]	刘春, 张慧珍, 张翼明, 等. 草酸盐重量法和电感耦合等离子体原子发射光谱法相结合测定钇铝合金中钇[J]. 冶金分析, 2020, 40(2): 24-28 Liu Chun, Zhang Huizhen, Zhang Yiming, et al. Determination of yttrium in yttrium-aluminum alloy by oxalate gravimetry and inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis, 2020, 40(2): 24-28
[13]	ISO 11438-6: 1993(E), Ferronickel-Determination of trace-element content by electrothermal atomic absorption spectrometric method-part 6: determination of thallium content[S].
[14]	Li J, Wang Q, Zhang Y. Gravimetric determination of ytterbium in rare-earth ores with oxalate[J]. J. Chin. Soc. Rare Earths, 2015, 33(2): 245-249.
[15]	Todoli J L, Mermet J M. Sample introduction systems in ICP spectrometry[M]. Elsevier, 2020.
[16]	Nelms S M. Inductively coupled plasma mass spectrometry handbook[M]. Blackwell, 2005.
[17]	Cheng K L, Bray R H. EDTA titration of yttrium and rare earths in silicate rocks[J]. Anal. Chem., 1955, 27(5): 782-785.
[18]	Van Der Walt T N, Strelow F W W. Complexometric titration of yttrium and ytterbium with EDTA after separation on AG50W-X8[J]. Anal. Chim. Acta, 1983, 153: 209-212.
[19]	Zhao Y, Li D, Guo F. Rapid EDTA titration of total rare earths in Ba-Y-Cu oxides[J]. Talanta, 1988, 35(10): 809-811.
[20]	Liu H, Zhang T, Chen Y. Interference of β-diketonate ligands in EDTA complexation of Yb³⁺: a spectroscopic study[J]. J. Coord. Chem., 2022, 75(12): 1987-1995.