Skip to content
DraconiticResearch
Search Sources API
201,818 studies31 sourcesUpdated 35 min ago
Peer-reviewedCC BY 4.0Molecules

Overcoming Incomplete Digestion of Ti-Doped LiFePO4 Cathode Materials: Microwave-Assisted Sample Preparation and Single-Laboratory Validated ICP-OES Determination of Li, Fe, P, and Ti

  • Myung-Gyu Lee1,2
  • Tae-Young Kim2
  • Sam-Hang Yi1,2
  • Joo-Seok Park2
  • Young-Jun Yoon3
  • Kyoung-Seok Moon1
  1. 1School of Materials Science & Engineering, Gyeongsang National University, Jinju 52828, Republic of Korea
  2. 2Industry Support Division, Korea Institute of Ceramic Engineering & Technology, Jinju 52851, Republic of Korea
  3. 3Advanced Materials Technology Division, Korea Testing & Research Institute, Gwacheon 13810, Republic of Korea
Open at sourceDOICite

Abstract

Reliable compositional quality control of Ti-doped LiFePO4 (LFP) requires quantitative release of the low-level Ti dopant from a carbon-coated phosphate matrix. We evaluated aqua regia hot-plate digestion and developed a closed-vessel microwave digestion–inductively coupled plasma optical emission spectrometry (ICP-OES) method for Li, Fe, P, and Ti. Aqua regia left a carbon-rich residue containing Ti; mass balance on seven digestions showed that 5.86 ± 0.37% of total Ti was retained, compared with 0.39 ± 0.12%, 0.53 ± 0.11%, and 0.81 ± 0.13% for Li, Fe, and P. The mean Ti recovery across the 14 aqua regia digestions was 92.8% of the assigned value, compared with 100.0% for the microwave procedure. Digestion with 6 mL HNO3 and 2 mL HCl at 240 °C gave quantitative Ti release: between 220 and 240 °C the Ti result rose by 14.0% to a plateau, while Li, Fe, and P changed by less than 2%. Calibration R2 values exceeded 0.999. Recoveries were 98.6–99.8%, repeatability RSDs 0.49–1.51%, and relative expanded uncertainties 0.64–2.20%; the lower calibration limit for Ti was 250 mg kg−1. Method means agreed with values assigned by 14–16 laboratories (compatibility indices ≤ 0.49). Under routine conditions, the method would support Ti specifications of ±13.4% relative or wider.

Related

  1. PARAFAC-Assisted Excitation–Emission Matrix Fluorescence for Minimal-Preparation Co-Determination of Norfloxacin and Metoclopramide in Human Urine: Overcoming Severe Concentration Imbalance Without Chromatography
    Mahmoud M. Elkhoudary, Randa A. Abdel Salam, Mohamed S. Abdel-Maksoud +1
    MoleculesPeer-reviewedCC BY 4.0General chemistryCrossref
  2. ICRF-assisted Box–Behnken design and optimization for rapid UPLC–PDA determination of dorzolamide hydrochloride and timolol maleate in an ophthalmic preparation
    Erdal Dinç, Eda Büker
    Journal of AOAC InternationalPeer-reviewedCC BY 4.0Full textAnalytical chemistryPMC
  3. Digestion and Orthogonal Click Conjugation Enables Nanopore Reading of Proteins
    Jasper W. van de Sande, Xiuqi Chen, Cees Dekker +1
    ChemRxivPreprintLicence not statedGeneral chemistryChemRxiv
  4. Machine learning based distribution mapping of gold in soil samples using aqua regia digestion and solid phase extraction
    Maryam Rezazadeh, Dariush Esmaeily
    Scientific ReportsPeer-reviewedCC BY-NC-ND 4.0Full textAnalytical chemistryCrossref
  5. From Food Structure to L-Cell Exposure: How Processing and Digestion Shape Endogenous GLP-1 Responses
    Roko Šantić, Marko Kumrić, Tina Tičinović Kurir +2
    Molecules (Basel, Switzerland)Peer-reviewedCC BYFull textGeneral chemistryEurope PMC

Cite

BibTeXRIS
BibTeX
@article{lee2026overcoming,
  title = {{Overcoming Incomplete Digestion of Ti-Doped LiFePO4 Cathode Materials: Microwave-Assisted Sample Preparation and Single-Laboratory Validated ICP-OES Determination of Li, Fe, P, and Ti}},
  author = {Myung-Gyu Lee and Tae-Young Kim and Sam-Hang Yi and Joo-Seok Park and Young-Jun Yoon and Kyoung-Seok Moon},
  journal = {Molecules},
  year = {2026},
  month = oct,
  doi = {10.3390/molecules31213915},
  url = {https://www.mdpi.com/1420-3049/31/21/3915},
  note = {CC BY 4.0},
}
RIS
TY  - JOUR
TI  - Overcoming Incomplete Digestion of Ti-Doped LiFePO4 Cathode Materials: Microwave-Assisted Sample Preparation and Single-Laboratory Validated ICP-OES Determination of Li, Fe, P, and Ti
AU  - Myung-Gyu Lee
AU  - Tae-Young Kim
AU  - Sam-Hang Yi
AU  - Joo-Seok Park
AU  - Young-Jun Yoon
AU  - Kyoung-Seok Moon
PY  - 2026
DA  - 2026/10/30
JO  - Molecules
DO  - 10.3390/molecules31213915
UR  - https://www.mdpi.com/1420-3049/31/21/3915
AB  - Reliable compositional quality control of Ti-doped LiFePO4 (LFP) requires quantitative release of the low-level Ti dopant from a carbon-coated phosphate matrix. We evaluated aqua regia hot-plate digestion and developed a closed-vessel microwave digestion–inductively coupled plasma optical emission spectrometry (ICP-OES) method for Li, Fe, P, and Ti. Aqua regia left a carbon-rich residue containing Ti; mass balance on seven digestions showed that 5.86 ± 0.37% of total Ti was retained, compared with 0.39 ± 0.12%, 0.53 ± 0.11%, and 0.81 ± 0.13% for Li, Fe, and P. The mean Ti recovery across the 14 aqua regia digestions was 92.8% of the assigned value, compared with 100.0% for the microwave procedure. Digestion with 6 mL HNO3 and 2 mL HCl at 240 °C gave quantitative Ti release: between 220 and 240 °C the Ti result rose by 14.0% to a plateau, while Li, Fe, and P changed by less than 2%. Calibration R2 values exceeded 0.999. Recoveries were 98.6–99.8%, repeatability RSDs 0.49–1.51%, and relative expanded uncertainties 0.64–2.20%; the lower calibration limit for Ti was 250 mg kg−1. Method means agreed with values assigned by 14–16 laboratories (compatibility indices ≤ 0.49). Under routine conditions, the method would support Ti specifications of ±13.4% relative or wider.
SN  - 1420-3049
ER  -