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Experiments / Batch 10

Batch 10 OK

19.05.23 · also written as Lab Batch 10 · 10 · Step 10 B
Conclusion — verbatim from the source
“Product was Yellowish flow able liquid”
[Lab Batch 10.pdf, page 2]
Aim

To develop product equivalent to reference product

Observations

Step-A: Appearance was yellowish with slight gripped in viscosity. Upon digestion cooled to RT. Step-B: initially found clear reaction mass , later on changed to yellowish in nature. Built viscosity at end of reaction. Step-C: initially found clear reaction mass , later on changed to slight turbid yellowish in nature with viscosity. Expt Table remarks: Initial feed of Step 10 B slowly found clear transparent mass ( still 20%) then slowly increased turbidity. Upon total feed reaction mass became viscous non flowable yellowish white mass. AV-55 Expt Table remarks: Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product.

Raw materials
#MaterialSourceQtyPurity %
1Vicasurf -1010FOIL230 gms100
2Polyphosphoric acidFOIL15.2 gms100
3Epomine 018-105 gms100
42- ethyl hexyl acrylateLoba245 gms100
Process
Step Conditions Charged What happened Results
Step 1
Step A
28112025 9076 Expt Table 2025.xls · Lab Batch 10.pdf
temperature: 60 / 75 °C · ELN narrative: start 40 degatmosphere: N2time: 1 / 3 h · ELN: 1-5 h
Vicasurf -1010 (HV-115-120) 230 g
Polyphosphpric acid 15.2 g (ELN materials table: Polyphosphoric acid; ELN narrative: P- pentaoxide)
To main reactor added Vicasurf 1010 under stirring and nitrogen atmosphere temp. 40 deg increased temp slowly with addition of P- pentaoxide. Upon feed completion temp raised to 75 deg C and digested for 2-3 hrs. Appearance was yellowish with slight gripped in viscosity. Upon digestion cooled to RT. [ELN]
Clear reaction mass, no charing/residue in mass [Table, Other column]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
1 60 stage 1 Table
3 75 N2 stage 2 Table
acid_value 183
Step 2
Step B
28112025 9076 Expt Table 2025.xls · Lab Batch 10.pdf
temperature: 68 / 78 °C · ELN: 55-80 °Catmosphere: N2time: 2 / 4 h · ELN: 1-8 h
Epomine SP- 018 105 g
2 ethyl hexyl acrylate 245 g
To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 55-65 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass , later on changed to yellowish in nature. Built viscosity at end of reaction. [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
2 68 stage 1 Table
4 78 N2 stage 2 Table
acid_value 257
Step 3
Step C
28112025 9076 Expt Table 2025.xls · Lab Batch 10.pdf
temperature: 60 / 62 °C · ELN: 60-65 °Catmosphere: N2time: 0.5 / 3 h · ELN: 1-5 h
Step 1- product -80 248 gm %
Step-2 Product -20% 62 gm %
To main reactor added Step- B reaction mass (20%) - reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (80%) reaction mass in it. initially found clear reaction mass , later on changed to slight turbid yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. [ELN]
Initial feed of Step 10 B slowly found clear transparent mass ( still 20%) then slowly increased turbidity. Upon total feed reaction mass became viscous non flowable yellowish white mass. [Table remarks]
Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product. [Table remarks]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
0.5 60 stage 1 Table
3 62 stage 2 Table
acid_value 55
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1
av 43.2
SPDu
Where this record comes from
Lab Batch 10.pdf — lab journal (primary source)
28112025 9076 Expt Table 2025.xls — researcher summary (cross-check)
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Field-by-field provenance (18 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--lab-batch-10--lab-batch-10 expt-block--10
FieldSourceExtractorConf.
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materials[0]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
materials[1]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
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materials[3]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
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process_steps[1]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[2]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[0]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedmedium
critical_parameters[1]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedmedium
critical_parameters[2]Lab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedmedium
observations28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '10', csv rows 35-37 qwen-tasks/extract-expt-block.md@unversionedhigh
outcomeLab Batch 10.pdf pages 1-2 qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[3]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '10', csv rows 35-37 qwen-tasks/extract-expt-block.md@unversionedhigh
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process_steps[5]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '10', csv rows 35-37 qwen-tasks/extract-expt-block.md@unversionedhigh
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  "validation": {
    "validated_fields": {
      "outcome.status": {
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    ]
  },
  "date": "19.05.23",
  "aim": "To develop product equivalent to reference product",
  "conclusion": "Product was Yellowish flow able liquid",
  "materials": [
    {
      "sr_no": "1",
      "name": "Vicasurf -1010",
      "source": "FOIL",
      "quantity": "230",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "2",
      "name": "Polyphosphoric acid",
      "source": "FOIL",
      "quantity": "15.2",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "3",
      "name": "Epomine 018-",
      "quantity": "105",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "4",
      "name": "2- ethyl hexyl acrylate",
      "source": "Loba",
      "quantity": "245",
      "unit": "gms",
      "purity_pct": "100"
    }
  ],
  "process_steps": [
    {
      "step": 1,
      "time_hrs": "1-5",
      "temperature_c": "60-75",
      "n2": "Yes",
      "procedure": [
        {
          "action": "To main reactor added Vicasurf 1010 under stirring and nitrogen atmosphere temp. 40 deg increased temp slowly with addition of P- pentaoxide . Upon feed completion temp raised to 75 deg C and digested for 2-3 hrs. Appearance was yellowish with slight gripped in viscosity. Upon digestion cooled to RT."
        }
      ]
    },
    {
      "step": 2,
      "time_hrs": "1-8",
      "temperature_c": "55-80",
      "n2": "Yes",
      "procedure": [
        {
          "action": "To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 55-65 deg Started slowly addition of 2- ethyl hexyl acrylate slowly. initially found clear reaction mass , later on changed to yellowish in nature. Built viscosity at end of reaction."
        }
      ]
    },
    {
      "step": 3,
      "time_hrs": "1-5",
      "temperature_c": "60-65",
      "n2": "Yes",
      "procedure": [
        {
          "action": "To main reactor added Step- B reaction mass (20%) - reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (80%) reaction mass in it. initially found clear reaction mass , later on changed to slight turbid yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT."
        }
      ]
    },
    {
      "step": 1,
      "materials": [
        {
          "name": "Vicasurf -1010 (HV-115-120)",
          "qty_g": "230",
          "role": "unknown",
          "role_verbatim": "raw_material"
        },
        {
          "name": "Polyphosphpric acid",
          "qty_g": "15.2",
          "role": "unknown",
          "role_verbatim": "raw_material"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "60",
          "time_h": "1",
          "verbatim": "60 / 1"
        },
        {
          "seq": 2,
          "temperature": "75",
          "time_h": "3",
          "verbatim": "75 / 3"
        }
      ],
      "conditions": {
        "temperature": "60 / 75",
        "atmosphere": "N2",
        "time_h": "1 / 3"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "183",
          "verbatim": "A.V. cell: 183"
        }
      ],
      "remarks": "Other column: Clear reaction mass, \nno charing/residue in mass"
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "Epomine SP- 018",
          "qty_g": "105",
          "role": "unknown",
          "role_verbatim": "raw_material"
        },
        {
          "name": "2 ethyl hexyl acrylate",
          "qty_g": "245",
          "role": "unknown",
          "role_verbatim": "raw_material"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "68",
          "time_h": "2",
          "verbatim": "68 / 2"
        },
        {
          "seq": 2,
          "temperature": "78",
          "time_h": "4",
          "verbatim": "78 / 4"
        }
      ],
      "conditions": {
        "temperature": "68 / 78",
        "atmosphere": "N2",
        "time_h": "2 / 4"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "257",
          "verbatim": "A.V. cell: 257"
        }
      ],
      "remarks": ""
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "Step 1- product -80",
          "qty_g": "248 gm %",
          "role": "intermediate"
        },
        {
          "name": "Step-2  Product  -20%",
          "qty_g": "62 gm %",
          "role": "intermediate"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "60",
          "time_h": "0.5",
          "verbatim": "60 / 0.5"
        },
        {
          "seq": 2,
          "temperature": "62",
          "time_h": "3",
          "verbatim": "62 / 3"
        }
      ],
      "conditions": {
        "temperature": "60 / 62",
        "time_h": "0.5 / 3"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "55",
          "verbatim": "AV-55"
        }
      ],
      "remarks": ""
    }
  ],
  "critical_parameters": [
    {
      "s_no": "1",
      "parameter": "aminev",
      "reference_value": "30.1"
    },
    {
      "s_no": "2",
      "parameter": "av",
      "reference_value": "43.2"
    },
    {
      "parameter": "SPDu"
    }
  ],
  "observations": "Step-A: Appearance was yellowish with slight gripped in viscosity. Upon digestion cooled to RT.\nStep-B: initially found clear reaction mass , later on changed to yellowish in nature. Built viscosity at end of reaction.\nStep-C: initially found clear reaction mass , later on changed to slight turbid yellowish in nature with viscosity.\n\nExpt Table remarks: Initial feed of Step 10 B slowly\n found clear transparent mass ( still 20%) then slowly\n increased turbidity. Upon total feed reaction mass became viscous non flowable yellowish white mass.\nAV-55\nExpt Table remarks: Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product.",
  "outcome": {
    "status": "ok",
    "basis": "Product was Yellowish flow able liquid",
    "citation": "[Lab Batch 10.pdf, page 2]"
  }
}