{
  "record_id": "exp-9076-059",
  "project": "9076",
  "aliases": [
    "Batch NO-59",
    "Byk 9076",
    "Batch NO-59."
  ],
  "provenance": {
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      "qwen-extract--9076-exp-48-60-1--batch-59",
      "qwen-extract--9076-exp-48-60_1--batch-no-59"
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        "source_file": "pdf/9076 Data for Raven POC project/Handwritten  notes/9076 Exp 48-60_1.pdf",
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      "procedure_summary": {
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      "observations": {
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        "confidence": "medium",
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        "locator": "pages 23-24",
        "confidence": "medium",
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      },
      "process_steps[1]": {
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        "confidence": "medium",
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        "extracted_date": "",
        "locator": "pages 23-24",
        "confidence": "medium",
        "human_checked": true
      },
      "samples[0]": {
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        "locator": "pages 23-24",
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    },
    "last_merged": "2026-08-25"
  },
  "documents": [
    {
      "file": "pdf/9076 Data for Raven POC project/Handwritten  notes/9076 Exp 48-60_1.pdf",
      "role": "handwritten_notes",
      "link_basis": "human link (exp-9076-059)",
      "link_status": "user-confirmed"
    }
  ],
  "validation": {
    "validated_fields": {},
    "corrections_applied": []
  },
  "date": "6/3/26",
  "aim": "Handwritten lab-note for a BYK 9076 analogue batch (9076 Exp 48-60 series): Step-I phosphate ester of the polyol with P2O5, Step-II acylate/acrylate intermediate from SP-18 (or Lupasol G-20) with 2-ethyl hexyl acrylate/acylate, Step-III neutralisation of the phosphate ester with the acylate intermediate.",
  "conditions": {
    "atmosphere": "N2",
    "other": "Step I: RT-50 to 77-78°C; Step II: 77-78 to 78-81°C; Step III: 55-59 to 55-58°C"
  },
  "materials": [
    {
      "name": "Macrolub LUB 1010",
      "quantity": "300",
      "unit": "gm",
      "role": "reactant",
      "notes": "Be-12PO-10EO, 942.22 / 59.54"
    },
    {
      "name": "P2O5",
      "quantity": "15",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "Epimine 8p-18",
      "quantity": "50",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "2-ethyl hexyl Acylate",
      "quantity": "116.6",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "AIBN",
      "quantity": "0.16",
      "unit": "gm",
      "role": "catalyst",
      "notes": "0.1%"
    },
    {
      "name": "Macrolub LUB 1010, Be-12PO-10EO, 942.22 / 59.54",
      "quantity": "300",
      "unit": "gm",
      "molecular_weight": "942.22",
      "role": "reactant"
    },
    {
      "name": "P2O5",
      "quantity": "15",
      "unit": "gm",
      "molecular_weight": "141.94",
      "role": "reactant"
    },
    {
      "name": "2-ethyl hexyl Acylate",
      "quantity": "116.6",
      "unit": "gm",
      "molecular_weight": "184.27",
      "role": "reactant"
    },
    {
      "name": "AIBN - 0.1%",
      "quantity": "0.16",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "Phosphate Ester (Step-I)",
      "quantity": "85",
      "unit": "gm",
      "percentage": "85",
      "role": "reactant"
    },
    {
      "name": "Acylate Intermediate (Step-II)",
      "quantity": "15",
      "unit": "gm",
      "percentage": "15.1",
      "role": "reactant"
    }
  ],
  "procedure_summary": "Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis with AIBN. Step III: Neutralization.",
  "observations": "Step I: Yellowish, turbidity Mass, AV - 56.2, Mono - 15%, Diacid - 71%, Free Acid - 0.31%.\nStep II: TU - 34, Yellow turbid mass, TU - 15.8.\nStep III: No clarity, Turbidity, Foaming, Yellowish Mass, AV - 43.2, Amine - 24.2.\n\nCharged LUB 1010 - 300gm\nFeed of P2O5 - 15gm / over 20min. / raised temp\nYellowish / turbidity Mass. AV - 56.2, Mono - 15%, Diacid - 71%, Free Acid - 0.31%\n8p-18 charged\nFeed of (2-ethyl hexyl Acylate + AIBN) mix over 3 hrs.\nTU - 34 / Yellow turbid mass\nTU - 15.8 / Cool to RT\nchanged - Acylate Intermediate\nFeed of phosphate Ester\nOver - 15 min. / No clarity, Turbidity / Foaming, Yellowish Mass., AV - 43.2, Amine - 24.2",
  "process_steps": [
    {
      "name": "Step- I Phosphate ester",
      "process": [
        {
          "time": "0.5",
          "temperature": "RT-50 / N2",
          "observation": "Charged LUB 1010 - 300gm"
        },
        {
          "time": "1.5",
          "temperature": "RT-75 / N2",
          "observation": "Feed of P2O5 - 15gm / over 20min. / raised temp"
        },
        {
          "time": "2.5",
          "temperature": "77-78 / N2",
          "observation": "Yellowish / turbidity Mass. AV - 56.2, Mono - 15%, Diacid - 71%, Free Acid - 0.31%"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV - 56.2"
        },
        {
          "verbatim": "Mono - 15%"
        },
        {
          "verbatim": "Diacid - 71%"
        },
        {
          "verbatim": "Free Acid - 0.31%"
        }
      ],
      "step": 1
    },
    {
      "name": "Step- II Acylate Intermediate",
      "process": [
        {
          "time": "0.5",
          "temperature": "77-78 / N2",
          "observation": "8p-18 charged"
        },
        {
          "time": "1.5",
          "temperature": "78-81 / N2",
          "observation": "Feed of (2-ethyl hexyl Acylate + AIBN) mix over 3 hrs."
        },
        {
          "time": "4 hrs.",
          "temperature": "78-81 / N2",
          "observation": "TU - 34 / Yellow turbid mass"
        },
        {
          "time": "3.1 hrs",
          "temperature": "78-81 / N2",
          "observation": "TU - 15.8 / Cool to RT"
        }
      ],
      "measurements": [
        {
          "verbatim": "TU - 34"
        },
        {
          "verbatim": "TU - 15.8"
        }
      ],
      "step": 2
    },
    {
      "name": "Step-II Neutralisation",
      "process": [
        {
          "time": "0.5",
          "temperature": "55-59 / N2",
          "observation": "changed - Acylate Intermediate"
        },
        {
          "time": "1.5",
          "temperature": "55-59 / N2",
          "observation": "Feed of phosphate Ester"
        },
        {
          "time": "1.5 hrs.",
          "temperature": "55-58 / N2",
          "observation": "Over - 15 min. / No clarity, Turbidity / Foaming, Yellowish Mass., AV - 43.2, Amine - 24.2"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV - 43.2"
        },
        {
          "verbatim": "Amine - 24.2"
        }
      ],
      "step": 2
    }
  ],
  "samples": [
    {
      "id": "Batch NO-59.",
      "analytical": [
        {
          "verbatim": "AV - 56.2"
        },
        {
          "verbatim": "Mono - 15%"
        },
        {
          "verbatim": "Diacid - 71%"
        },
        {
          "verbatim": "Free Acid - 0.31%"
        },
        {
          "verbatim": "TU - 34"
        },
        {
          "verbatim": "TU - 15.8"
        },
        {
          "verbatim": "AV - 43.2"
        },
        {
          "verbatim": "Amine - 24.2"
        }
      ],
      "sample_id": "unspecified sample"
    }
  ]
}