{
  "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.",
  "abstract_shown": true,
  "affiliations": [
    "School of Materials Science & Engineering, Gyeongsang National University, Jinju 52828, Republic of Korea",
    "Industry Support Division, Korea Institute of Ceramic Engineering & Technology, Jinju 52851, Republic of Korea",
    "Advanced Materials Technology Division, Korea Testing & Research Institute, Gwacheon 13810, Republic of Korea"
  ],
  "article_type": null,
  "arxiv": null,
  "author_total": 6,
  "authors": [
    {
      "affs": [
        0,
        1
      ],
      "name": "Myung-Gyu Lee",
      "orcid": "0009-0006-5292-6341"
    },
    {
      "affs": [
        1
      ],
      "name": "Tae-Young Kim"
    },
    {
      "affs": [
        0,
        1
      ],
      "name": "Sam-Hang Yi"
    },
    {
      "affs": [
        1
      ],
      "name": "Joo-Seok Park"
    },
    {
      "affs": [
        2
      ],
      "name": "Young-Jun Yoon"
    },
    {
      "affs": [
        0
      ],
      "name": "Kyoung-Seok Moon",
      "orcid": "0000-0002-7326-9495"
    }
  ],
  "bibtex": "https://research.draconitic.com/paper/667j29w0e6xv7.bib",
  "cited_by": 0,
  "doi": "10.3390/molecules31213915",
  "fulltext_url": null,
  "id": "667j29w0e6xv7",
  "issns": [
    "1420-3049"
  ],
  "landing_url": "https://www.mdpi.com/1420-3049/31/21/3915",
  "language": null,
  "licence": "CC-BY-4.0",
  "licence_label": "CC BY 4.0",
  "licence_source": "article",
  "licence_url": "https://creativecommons.org/licenses/by/4.0/",
  "metadata_licence": null,
  "native_subjects": [],
  "openalex": null,
  "pdf_url": null,
  "pmcid": null,
  "pmid": null,
  "published": "2026-10-30",
  "publisher": "MDPI AG",
  "ris": "https://research.draconitic.com/paper/667j29w0e6xv7.ris",
  "sources": [
    {
      "first_seen": "2026-10-31T00:20:49Z",
      "native_id": "10.3390/molecules31213915",
      "source": "crossref",
      "url": "https://www.mdpi.com/1420-3049/31/21/3915"
    }
  ],
  "subjects": [
    {
      "field": "chemistry",
      "origin": "issn:1420-3049",
      "subfield": "general"
    }
  ],
  "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",
  "title_text": "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",
  "type": "peer-reviewed",
  "updated_at": "2026-11-01T00:20:47Z",
  "url": "https://research.draconitic.com/paper/667j29w0e6xv7",
  "venue": "Molecules",
  "versions": []
}