← Back batch 54 of 100 ← Batch 34 Batch 34 C →
av
31.7
target 43.2 · -26.6% vs target
Application test
not OK
2 tests
Conclusion — verbatim from the source
“Application test against violet- 27 / Black is good only re-solubility failed for violet 23 & Blue”
pdf/9076 Data for Raven POC project/Old ELN/LBN 34 -B.pdf, page 2
Aim

To develop product equivalent to reference product

Observations

Expt Table remarks: Brownish tincture Expt Table remarks: Initially turbid / After 1 hr clear mass Expt Table remarks: Yellowish after 1.5 hrs

Raw materials
#MaterialGrade / notesSourceRM noQtyPurity %Role
1Surfol R-1400(R-53/07032024Sun shieldR-53/07032024290 gmsreactant
2Phosphorous pentaoxideCommercial10.8 gmsreactant
3Epomine SP-018Nippon30 gms100reactant
4TolueneCommercial94 gms99solvent
5AIBN catalystHimedia0.2 gms100catalyst
52 ethyl hexyl acrylate70 gms100reactant
6AIBN catalyst0.32 gms103catalyst
Process
Step Conditions Charged What happened Results
Step 1
Phosphate ester
28112025 9076 Expt Table 2025.xls · LBN 34 -B.pdf
temperature: 58 → 75 °Catmosphere: N2time: 4 h · ELN: 5 h
Surfol R-1400 HV-59 (R-53/07032024) 290 g
Phosphorous pentaoxide 10.8 g
Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh [ELN]
Appearance- yellowish clear [ELN]
After digestion cool to RT and filter through Nylon mesh [Table remark]
Brownish tincture [Expt Table remark, carried in source order]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
58 N2 Table
4 75 N2 Table
AV 38.5
Step 2
Acrylate intermediate
28112025 9076 Expt Table 2025.xls · LBN 34 -B.pdf
temperature: 68-72 °C · ELN: 65-72 °Catmosphere: N2time: 1.15 hr feed + 3.5 h · ELN: 5.5 h
Epomine SP- 018 30 g
Toluene 95 ml [Table] / 94 gms [ELN materials list]
AIBN catalyst 0.2 g
2 ethyl hexyl acrylate 70 g
AIBN catalyst 0.32 g
Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent ( Dissolved AIBN- 0.2 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acrylate (with dissolved AIBN- 0.32 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. [ELN]
Appearance- yellowish clear [ELN]
Initially turbid / After 1 hr clear mass [Expt Table remark, carried in source order]
Step-by-step (3 entries)
Time (h)Temp (°C)AtmWhat happened
68-72 N2 Table
1.15 hr feed 68-72 N2 Feed [Table remark] Table
3.5 68-72 N2 Table
IV 10.5
Step 3
Neutralization
28112025 9076 Expt Table 2025.xls · LBN 34 -B.pdf
temperature: 58-60 °C · ELN: 56-61 °Catmosphere: N2time: 2.5 hr · ELN: 3.5 h
Step - 1 Product 80 g
Step - 2 Product 20 g [Table]
Step 3) Neutralization - RBF with acrylate intermediate of step-1) (20%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (80%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. [ELN]
Yellowish after 1.5 hrs [Expt Table remark, carried in source order]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
Feed slowly over 30 min Table
2.5 hr 58-60 N2 Stirrer well and disperse amine [Table remark] Table
AV 31.7
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1
av 43.2 31.7
Sample LBN 34 - B
OK Application test
good only
LBN 34 -B.pdf
not OK re-solubility — re-solubility failed
failed
LBN 34 -B.pdf
Where this record comes from
LBN 34 -B.pdf — lab journal (primary source)
28112025 9076 Expt Table 2025.xls — researcher summary (cross-check)
Something wrong on this page? Record a correction
Your correction is permanent: it survives every re-extraction and the field can no longer be changed by the system.
Field-by-field provenance (20 fields) — for auditors
2 extraction fragments · merged 2026-08-25 · 1 human-validated fields
Fix a wrong or missing extraction side-by-side with the original: qwen-extract--lbn-34-b--lbn-34-b expt-block--34b
FieldSourceExtractorConf.
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materials[1]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
materials[2]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
materials[3]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
materials[4]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
materials[5]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
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process_steps[0]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[1]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[2]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[0]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[1]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
samples[0]LBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
outcomeLBN 34 -B.pdf pages 1-2 (pages 3-4 blank) qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[3]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '34B' qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[4]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '34B' qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[5]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '34B' qwen-tasks/extract-expt-block.md@unversionedhigh
observations28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '34B' qwen-tasks/extract-expt-block.md@unversionedhigh
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  "aim": "To develop product equivalent to reference product",
  "conclusion": "Application test against violet- 27 / Black is good only re-solubility failed for violet 23 & Blue",
  "materials": [
    {
      "sr_no": 1,
      "name": "Surfol R-1400",
      "descriptor": "(R-53/07032024",
      "rm_no": "R-53/07032024",
      "source": "Sun shield",
      "quantity": 290,
      "unit": "gms",
      "role": "reactant"
    },
    {
      "sr_no": 2,
      "name": "Phosphorous pentaoxide",
      "source": "Commercial",
      "quantity": 10.8,
      "unit": "gms",
      "role": "reactant"
    },
    {
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      "source": "Nippon",
      "quantity": 30,
      "unit": "gms",
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      "role": "reactant"
    },
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      "source": "Commercial",
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      "unit": "gms",
      "purity_pct": 99,
      "role": "solvent"
    },
    {
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      "name": "AIBN catalyst",
      "source": "Himedia",
      "quantity": 0.2,
      "unit": "gms",
      "purity_pct": 100,
      "role": "catalyst"
    },
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      "quantity": 70,
      "unit": "gms",
      "purity_pct": 100,
      "role": "reactant"
    },
    {
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      "name": "AIBN catalyst",
      "quantity": 0.32,
      "unit": "gms",
      "purity_pct": 103,
      "role": "catalyst"
    }
  ],
  "process_steps": [
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      "step": 1,
      "name": "Phosphate ester",
      "procedure": [
        {
          "seq": 1,
          "time_h": 5,
          "temperature": "58-75",
          "atmosphere": "N2",
          "action": "Step 1) Phosphate ester- RBF with Surfol R-1400 heated to 58 deg C and then slowly added P2O5 into it under N2 atmosphere. Digested this for 3 hrs at 70-75 deg C. Cool to RT and filter through Nylon Mesh AV- 38.5",
          "observation": "Appearance- yellowish clear",
          "measurements": [
            {
              "parameter": "AV",
              "value": 38.5,
              "phase": "in-process",
              "verbatim": "AV- 38.5"
            }
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      "results": [
        {
          "parameter": "AV",
          "value": 38.5,
          "phase": "in-process",
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        }
      ]
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    {
      "step": 2,
      "name": "Acrylate intermediate",
      "procedure": [
        {
          "seq": 2,
          "time_h": 5.5,
          "temperature": "65-72",
          "atmosphere": "N2",
          "action": "Step 2) Acrylate intermediate- RBF with Epoimin SP-18 with Toluene solvent ( Dissolved AIBN- 0.2 gm) heated to 66-72 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acrylate (with dissolved AIBN- 0.32 gm) into it over 1.15 hrs and continue reaction for 3 hrs. Cool to RT removed toluene under reduced pressure. ( IV-10.5)",
          "observation": "Appearance- yellowish clear",
          "measurements": [
            {
              "parameter": "IV",
              "value": 10.5,
              "phase": "in-process",
              "verbatim": "IV-10.5"
            }
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        {
          "parameter": "IV",
          "value": 10.5,
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        }
      ]
    },
    {
      "step": 3,
      "name": "Neutralization",
      "procedure": [
        {
          "seq": 3,
          "time_h": 3.5,
          "temperature": "56-61",
          "atmosphere": "N2",
          "action": "Step 3) Neutralization - RBF with acrylate intermediate of step-1) (20%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-2) (80%) Phosphate ester into it over 30 min and continue for 3 hrs. Cool to RT and filter through Nylon Mesh. AV-31.7",
          "observation": "AV-31.7",
          "measurements": [
            {
              "parameter": "AV",
              "value": 31.7,
              "phase": "final",
              "verbatim": "AV-31.7"
            }
          ]
        }
      ],
      "results": [
        {
          "parameter": "AV",
          "value": 31.7,
          "phase": "final",
          "verbatim": "AV-31.7"
        }
      ]
    },
    {
      "step": 1,
      "materials": [
        {
          "name": "Surfol R-1400  HV-59  (R-53/07032024)",
          "qty": "290 g",
          "role": "reactant"
        },
        {
          "name": "Phosphorous pentaoxide",
          "qty": "10.8 g",
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "58 oC",
          "verbatim": "58"
        },
        {
          "seq": 2,
          "temperature": "75 oC",
          "time_h": "4",
          "verbatim": "75, 4"
        }
      ],
      "conditions": {
        "temperature": "58 to 75 oC",
        "atmosphere": "N2",
        "time_h": "4 h"
      },
      "results": [
        {
          "parameter": "AV",
          "value": "38.5",
          "verbatim": "38.5"
        }
      ],
      "remarks": "After digestion cool to RT and filter through Nylon mesh"
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "Epomine SP- 018",
          "qty": "30 gm",
          "role": "reactant"
        },
        {
          "name": "Toluene",
          "qty": "95 ml",
          "role": "solvent"
        },
        {
          "name": "AIBN catalyst",
          "qty": "0.2 gm",
          "role": "catalyst"
        },
        {
          "name": "2 ethyl hexyl acrylate",
          "qty": "70 gm",
          "role": "reactant"
        },
        {
          "name": "AIBN catalyst",
          "qty": "0.32 gm",
          "role": "catalyst"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "68-72 oC",
          "verbatim": "68-72",
          "time_h": "0.15"
        },
        {
          "seq": 2,
          "temperature": "68-72 oC",
          "time_h": "1.15 hr feed",
          "verbatim": "68-72, 1.15 hr feed"
        },
        {
          "seq": 3,
          "temperature": "68-72 oC",
          "time_h": "3.5",
          "verbatim": "68-72, 3.5"
        }
      ],
      "conditions": {
        "temperature": "68-72 oC",
        "atmosphere": "N2",
        "time_h": "1.15 hr feed, 3.5 h"
      },
      "results": [
        {
          "parameter": "IV",
          "value": "10.5",
          "verbatim": "IV-10.5"
        }
      ],
      "remarks": "Feed"
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "Step - 1 Product",
          "qty": "80 g",
          "role": "intermediate"
        },
        {
          "name": "Step -  2 Product",
          "qty": "20 g",
          "role": "intermediate"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "verbatim": "Feed slowly over 30 min"
        },
        {
          "seq": 2,
          "temperature": "58-60 oC",
          "time_h": "2.5 hr",
          "verbatim": "58-60, 2.5 hr"
        }
      ],
      "conditions": {
        "temperature": "58-60 oC",
        "atmosphere": "N2",
        "time_h": "2.5 hr"
      },
      "results": [
        {
          "parameter": "AV",
          "value": "31.7",
          "verbatim": "AV-31.7"
        }
      ],
      "remarks": "Stirrer well and disperse amine"
    }
  ],
  "critical_parameters": [
    {
      "parameter": "aminev",
      "reference_value": "30.1",
      "phase": "target-check",
      "verbatim": "aminev / 30.1"
    },
    {
      "parameter": "av",
      "reference_value": "43.2",
      "value": "31.7",
      "phase": "target-check",
      "verbatim": "av / 43.2 / 31.7"
    }
  ],
  "samples": [
    {
      "sample_id": "LBN 34 - B",
      "application_tests": [
        {
          "test": "Application test",
          "pigment": "violet- 27 / Black",
          "result": "good only",
          "verdict": "ok",
          "file": "pdf/9076 Data for Raven POC project/Old ELN/LBN 34 -B.pdf"
        },
        {
          "test": "re-solubility",
          "pigment": "violet 23 & Blue",
          "result": "failed",
          "verdict": "not ok",
          "failure_reason": "re-solubility failed",
          "file": "pdf/9076 Data for Raven POC project/Old ELN/LBN 34 -B.pdf"
        }
      ]
    }
  ],
  "outcome": {
    "status": "partial",
    "basis": "Application test against violet- 27 / Black is good only re-solubility failed for violet 23 & Blue",
    "citation": "pdf/9076 Data for Raven POC project/Old ELN/LBN 34 -B.pdf, page 2"
  },
  "observations": "Expt Table remarks: Brownish tincture\nExpt Table remarks: Initially turbid / After 1 hr clear mass\nExpt Table remarks: Yellowish after 1.5 hrs"
}