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Experiments / Batch 24 CI

Batch 24 CI no result yet

also written as Lab Batch 24 C (I) · 24 C-I
Aim

To develop product equivalent to reference product

Observations

Expt Table remarks: AV-34.05 Amine-35.17

Raw materials
#MaterialSourceQtyPurity %
1Sun Surfol R-1400- ×2FOIL450 gms100
2P-Pentaoxide ×2FOIL22.95 gms100
3Epomine 018- ×290 gms100
42-ethyl hexyl acrylate ×2Loba210 gms100
Reaction conditions (optimized)
atmosphere: nitrogen
Process
Step Conditions Charged What happened Results
Step 1
Step- A
28112025 9076 Expt Table 2025.xls · Lab Batch 24 C(1).pdf · Lab Batch 24 C(1).pdf
temperature: 40-45 → 70-77 °C · ELN form table: temperature column '1-5', pressure N2 column '65-75'atmosphere: N2time: 0.5 + 4 h · ELN: 1-5 h
Sun Surfol R-1400- (HV-59) 450 g
P-Pentaoxide 22.95 gms [ELN] / Phosphorous pentaoxide 20.95 g [Table]
To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 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 clear non yellowish . Upon digestion cooled to RT. (180 gm ester + 37.3 g Butanol EO-PO) [ELN]
Yellowish floable liq [Table remark]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
0.5 40-45 N2 Table
4 70-77 N2 Table
AV 39.8AV 39.45AV 46.18
Step 2
Step-B
28112025 9076 Expt Table 2025.xls · Lab Batch 24 C(1).pdf · Lab Batch 24 C(1).pdf
temperature: 74-81 → 78-82 °C · ELN form table: temperature column '1-8', pressure N2 column '77-81'atmosphere: N2time: 2 + 6 h · ELN: 1-8 h
Epomine SP- 018 [Table] / Epomine 018- [ELN] 90 g
2-ethyl hexyl acrylate 210 g
To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 78 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. Reaction monitored with IV analysis. [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
2 74-81 N2 Feed [Table remark] Table
6 78-82 N2 Table
AV 0.2Amine 275IV 34.5
Step 3
Step-C
28112025 9076 Expt Table 2025.xls · Lab Batch 24 C(1).pdf · Lab Batch 24 C(1).pdf
temperature: 55-58 → 60 °C · ELN form table: temperature column '1-5', pressure N2 column '55-58'atmosphere: N2time: 0.4-hr feed + 4 h · ELN: 1-5 h
Step- 1 product (85) 170 g
Step- 2 Product (15) 30 g [Table]
To main reactor added Step- B reaction mass (15%) -30 g reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (85%) - 170 gm reaction mass in it. initially found clear reaction mass , yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. [ELN]
Flow able yellowish liquid. [ELN]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
0.4 (feed) 55-58 N2 feed Table
4 60 N2 Table
AV 35.56AV 34.05Amine 35.17
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1
av 43.2
Where this record comes from
Lab Batch 24 C(1).pdf — lab journal (primary source)
28112025 9076 Expt Table 2025.xls — researcher summary (cross-check)
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Field-by-field provenance (22 fields) — for auditors
3 extraction fragments · merged 2026-08-25 · 0 human-validated fields
FieldSourceExtractorConf.
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observations28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '24 C-I', csv rows 155-158 qwen-tasks/extract-expt-block.md@unversionedhigh
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  "aim": "To develop product equivalent to reference product",
  "materials": [
    {
      "sr_no": "1",
      "name": "Sun Surfol R-1400-",
      "source": "FOIL",
      "quantity": 450,
      "unit": "gms",
      "purity_pct": 100
    },
    {
      "sr_no": "2",
      "name": "P-Pentaoxide",
      "source": "FOIL",
      "quantity": 22.95,
      "unit": "gms",
      "purity_pct": 100
    },
    {
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      "name": "Epomine 018-",
      "quantity": 90,
      "unit": "gms",
      "purity_pct": 100
    },
    {
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      "name": "2-ethyl hexyl acrylate",
      "source": "Loba",
      "quantity": 210,
      "unit": "gms",
      "purity_pct": 100
    },
    {
      "sr_no": "1",
      "name": "Sun Surfol R-1400-",
      "source": "FOIL",
      "quantity": "450",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
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      "name": "P-Pentaoxide",
      "source": "FOIL",
      "quantity": "22.95",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": "3",
      "name": "Epomine 018-",
      "quantity": "90",
      "unit": "gms",
      "purity_pct": "100"
    },
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      "name": "2-ethyl hexyl acrylate",
      "source": "Loba",
      "quantity": "210",
      "unit": "gms",
      "purity_pct": "100"
    }
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  "process_steps": [
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      "step": 1,
      "time_hrs": "1-5",
      "temperature_c": "1-5",
      "pressure_n2_kg_cm2": "65-75",
      "procedure": [
        {
          "action": "To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 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 clear non yellowish . Upon digestion cooled to RT. (180 gm ester + 37.3 g Butanol EO-PO) AV-39.8"
        }
      ],
      "results": [
        {
          "value": "39.8",
          "verbatim": "AV-39.8",
          "parameter": "AV"
        }
      ]
    },
    {
      "step": 2,
      "time_hrs": "1-8",
      "temperature_c": "1-8",
      "pressure_n2_kg_cm2": "77-81",
      "procedure": [
        {
          "action": "To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 78 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. Reaction monitored with IV analysis. ( IV-34.5)"
        }
      ],
      "results": [
        {
          "value": "34.5",
          "verbatim": "IV-34.5",
          "parameter": "IV"
        }
      ]
    },
    {
      "step": 3,
      "time_hrs": "1-5",
      "temperature_c": "1-5",
      "pressure_n2_kg_cm2": "55-58",
      "procedure": [
        {
          "action": "To main reactor added Step- B reaction mass (15%) -30 g reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (85%) - 170 gm reaction mass in it. initially found clear reaction mass , yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. AV-35.56"
        }
      ],
      "observations": "Flow able yellowish liquid. AV-34.05 Amine-35.17",
      "results": [
        {
          "value": "35.56",
          "verbatim": "AV-35.56",
          "parameter": "AV"
        },
        {
          "value": "34.05",
          "verbatim": "AV-34.05",
          "parameter": "AV"
        },
        {
          "value": "35.17",
          "verbatim": "Amine-35.17",
          "parameter": "Amine"
        }
      ]
    },
    {
      "step": 1,
      "sr_no": "1",
      "time_hrs": "1-5",
      "temperature_c": "1-5",
      "pressure_n2_kg_cm2": "65-75",
      "procedure": [
        {
          "action": "Step- A To main reactor added Sun Surfol R-1400 under stirring and nitrogen atmosphere temp. 60 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 clear non yellowish . Upon digestion cooled to RT. (180 gm ester + 37.3 g Butanol EO-PO) AV-39.8"
        }
      ],
      "results": [
        {
          "measurement": "AV",
          "value": "39.8",
          "verbatim": "AV-39.8",
          "source_column": "procedure text",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 2,
      "sr_no": "2",
      "time_hrs": "1-8",
      "temperature_c": "1-8",
      "pressure_n2_kg_cm2": "77-81",
      "procedure": [
        {
          "action": "Step-B To main reactor added Epomine 018- reaction mass under stirring and nitrogen atmosphere temp. 78 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. Reaction monitored with IV analysis. ( IV-34.5)"
        }
      ],
      "remarks": "IV-34.5",
      "results": [
        {
          "measurement": "IV",
          "value": "34.5",
          "verbatim": "IV-34.5",
          "source_column": "remarks",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 3,
      "sr_no": "3",
      "time_hrs": "1-5",
      "temperature_c": "1-5",
      "pressure_n2_kg_cm2": "55-58",
      "procedure": [
        {
          "action": "Step-C To main reactor added Step- B reaction mass (15%) -30 g reaction mass under stirring and nitrogen atmosphere temp. 55 deg Started slowly addition of Step- A (85%) - 170 gm reaction mass in it. initially found clear reaction mass , yellowish in nature with viscosity. Mixed for 3 hrs then cooled to RT. AV-35.56"
        }
      ],
      "remarks": "Flow able yellowish liquid. AV-34.05 Amine-35.17",
      "results": [
        {
          "measurement": "AV",
          "value": "35.56",
          "verbatim": "AV-35.56",
          "source_column": "procedure text",
          "parameter": "unlabelled"
        },
        {
          "measurement": "AV",
          "value": "34.05",
          "verbatim": "AV-34.05",
          "source_column": "remarks",
          "parameter": "unlabelled"
        },
        {
          "measurement": "Amine value",
          "value": "35.17",
          "verbatim": "Amine-35.17",
          "source_column": "remarks",
          "parameter": "unlabelled"
        }
      ]
    },
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        }
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      "procedure": [
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          "time_h": 0.5,
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          "seq": 2,
          "temperature": "70-77",
          "time_h": 4,
          "verbatim": "70-77 °C / 4 h"
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      "conditions": {
        "atmosphere": "N2"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": 39.45,
          "verbatim": "39.45"
        }
      ],
      "remarks": "Yellowish floable liq AV adjusted to 39.8\n(180 gmAV-46.18+37.3 gm R-1400 to AV-39.45)"
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "Epomine SP- 018",
          "qty_g": 90
        },
        {
          "name": "2 ethyl hexyl acrylate",
          "qty_g": 210
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "74-81",
          "time_h": 2,
          "verbatim": "74-81 °C / 2 h"
        },
        {
          "seq": 2,
          "temperature": "78-82",
          "time_h": 6,
          "verbatim": "78-82 °C / 6 h"
        }
      ],
      "conditions": {
        "atmosphere": "N2"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": 0.2,
          "verbatim": "AV- 0.2"
        },
        {
          "parameter": "amine_value",
          "value": 275,
          "verbatim": "Amine -275"
        },
        {
          "parameter": "iodine_value",
          "value": 34.5,
          "verbatim": "IV-34.5"
        }
      ],
      "remarks": "Feed"
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "Step-  1 product  (85)",
          "qty_g": 170,
          "role": "intermediate"
        },
        {
          "name": "Step -  2 Product  (15)",
          "qty_g": 30,
          "role": "intermediate"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "temperature": "55-58",
          "time_h": 0.4,
          "verbatim": "55-58 °C / 0.4-hr feed"
        },
        {
          "seq": 2,
          "temperature": "60",
          "time_h": 4,
          "verbatim": "60 °C / 4 h"
        }
      ],
      "conditions": {
        "atmosphere": "N2"
      },
      "results": []
    }
  ],
  "critical_parameters": [
    {
      "s_no": "1",
      "parameter": "aminev",
      "reference_value": "30.1"
    },
    {
      "s_no": "2",
      "parameter": "av",
      "reference_value": "43.2"
    }
  ],
  "conditions": {
    "atmosphere": "nitrogen"
  },
  "observations": "Expt Table remarks: AV-34.05\nAmine-35.17"
}