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Experiments / Batch 48

Batch 48 OK

26.6.25 · vnmr1 · also written as LBN 48 · S 9076 #48 · P 76 B.NO 48 · Sample_P_76_B_NO_48 · Sample P 76 B.NO 48 · 48 · LBN-48 (Q)
LBN 48.pdf lab journal (primary source) APP DATA- BYK 9076 equivalent.xlsx application testing Fine Organics 13C zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report Fine Organics 1H zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report Fine Organics 1H zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf analytical report 28112025 9076 Expt Table 2025.xls researcher summary (cross-check)
aminev
36.25
target 30.1 · +20.4% vs target
av
44.36
target 43.2 · +2.7% vs target
Conclusion — verbatim from the source
“Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet”
[LBN 48.pdf, page 2]
Aim

To develop product equivalent to reference product

Observations

Expt Table remarks: Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet; Tested on Violet 23 resolubility ok

Raw materials
#MaterialSourceQtyPurity %Mol. wt.Moles
1Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900Viswaat178 gms9000.197
2P2O5Commercial9.357 gms141.940.0658
3Epomine SP-018Nippon30 gms100
42 ethyl hexyl acrylate70 gms100184.27
Reaction conditions (optimized)
atmosphere: N2other: Optimized Reaction Conditions table present but blank
Process
Step Conditions Charged What happened Results
Step 1
Phosphate ester
28112025 9076 Expt Table 2025.xls · LBN 48.pdf
 temperature: 58-75 °C · Table row: 45 °Catmosphere: N2time: 5 h · Table row: 0.2 h
Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 (MW 900, 0.197 mol) 178 g
P2O5 (MW 141.94, 0.0658 mol) 9.357 g
Step 1) Phosphate ester- RBF with Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 heated to 50 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 [ELN]
Step-by-step (1 entry)
Time (h)Temp (°C)AtmWhat happened
0.2 45 Table
AV 52.52Mono 24.44Di 51.76Free acid 0.24P 2.14%
Step 2
Acrylate intermediate
28112025 9076 Expt Table 2025.xls · LBN 48.pdf
 temperature: 78-82 °Catmosphere: N2time: 6.5 h · Table row: 0.2 h
Epomine SP- 018 30 g
2 ethyl hexyl acrylate (MW 184.27) 70 g
Step 2) Acrylate intermediate- RBF with Epomine SP- 018 heated to 78-81 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. Cool to RT [ELN]
Appearance- yellowish clear [ELN]
Step-by-step (1 entry)
Time (h)Temp (°C)AtmWhat happened
0.2 80 Table
AV 0.45IV 26.1Mono/Di/Free acid Mono-24.44 / Di- 51.76/ Free acid-0.24
Step 3
Neutralization
28112025 9076 Expt Table 2025.xls · LBN 48.pdf
 temperature: 56-61 °C · Table row: 80 °Catmosphere: N2time: 0.5 (feed) + 3.5 h · ELN: 3.5 h
Step - 1 Product Phosphate ester 0.85 [Table]
Step 3) Neutralization - RBF with acrylate intermediate of step-2) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) (85%) Phosphate ester into it over 30 min and contain 1ue for 3 hrs. Cool to RT and filter through Nylon Mesh. [ELN]
Yellowish clear transparent mass [Table remark]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
0.5 80 Feed of phosphate ester Table
3.5 Stirrer well, clear transparent mass Table
AV 44.36HV 46.58SAP 62.14Amine 36.25IV 5.8P 1.82%IV 26.1
Step 4
LBN-48 (Q)
28112025 9076 Expt Table 2025.xls
 temperature: 65-75 → 55-60 °Ctime: 1 hr + 2.5 hr
RM from above Batch
i) Acrylate 0.15
ii) Dimethyl sulphate 0.005
iii) Phosphate 0.85 [Table]
Single-source step: present only in the Expt Table block '48', where it is labelled LBN-48 (Q) and charged from 'RM from above Batch'. [Table]
Step-by-step (2 entries)
Time (h)Temp (°C)AtmWhat happened
1 hr 65-75 Dimethyl sulphate — Clear transparent mass Table
2.5 hr 55-60 Phosphate — Yellowish transparent clear mass Table
AV 52Amine 31.67IV 3.48SAP 84.9HV 38.6
Critical parameters — measured vs target
ParameterTargetMeasured
aminev 30.1 36.25
av 43.2 44.36
Sample unspecified sample
result Solubility/gloss over pigments (pigment Black, Blue, Violet-23/27 etc)
All having matching resolubility while reduced gloss in violet
AV 44.36
HV 46.58
SAP 62.14
Amine 36.25
IV 5.8
13C NMR Dec 25 2025 · cdcl3 note: 13C FS (full scan) plot covering 20-220 ppm; peak positions (ppm) as printed on the plot, no assignments printed · ppm: 77.358, 77.1, 76.85, 75.461, 75.302, 75.272, 75.127, 75.082, 74.93, 74.467, 73.284, 73.056, 72.828, 71.144, 70.711, 70.582, 70.522, 70.021, 67.206, 31.657, 30.094, 28.804, 22.916, 19.221, 18.432, 18.1… · Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
13C NMR Dec 25 2025 · cdcl3 note: 13C zoom1 plot covering 10-35 ppm; peak positions (ppm) as printed on the plot · ppm: 38.532, 31.657, 30.246, 30.094, 28.804, 23.592, 23.053, 22.916, 19.221, 18.432, 18.151, 18.113, 17.415, 17.294, 17.264, 17.218, 17.104, 16.937, 16.899, 14.069, 13.895, 10.905, 10.806 · Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
1H NMR Dec 25 2025 · cdcl3 ppm peaks: 7.315; 3.934; 3.922; 3.682; 3.655; 3.648; 3.632; 3.606; 3.588; 3.577; 3.568; 3.557; 3.547; 3.534; 3.522; 3.513; 3.502; 3.492; 3.482; 3.471; 3.458; 3.444; 3.424; 3.416; 3.407; 3.398; 3.390; 3.349; 3.338; 3.329; 3.323; 3.302; 3.161; 2.173; 1.593; 1.579; 1.565; 1.549; 1.535; 1.384; 1.370; 1.354; 1.339; 1.325; 1.278; 1.147; 1.134; 1.116; 1.111; 1.101; 1.088; 0.929; 0.914; 0.899; 0.884; 0.873; 0.000. Relative integrals: 0.26; 0.68; 1.73; 31.61; 17.23; 5.81; 1.38; 0.71; 2.60; 0.68; 0.11; 2.09; 8.02; 21.18; 5.91. · Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
Sample S 9076 #48
result Violet 23 (NC-PU ink)
ParameterThis sampleStandard (BYK 9076 Standard)
Viscosity 30 sec 29 sec
Gloss 53.3 62
Colour Strength 98-99.00% 1
Resolubility 3 4
Transparency Opaque Ref as Std
APP DATA- BYK 9076 equivalent.xlsx
result Violet 27 (NC-PU ink)
ParameterThis sampleStandard (BYK 9076 Standard)
Viscosity 31 sec 30 sec
Gloss 4.6 5.3
Colour Strength 1 1
Resolubility 4 4
Transparency Eq to Std Ref as Std
APP DATA- BYK 9076 equivalent.xlsx
result Black (NC-PU ink)
ParameterThis sampleStandard (BYK 9076 Standard)
Viscosity 34 sec 33 sec
Gloss 30.9 31
Colour Strength 1 1
Resolubility 4 4
Transparency Eq to Std Ref as Std
APP DATA- BYK 9076 equivalent.xlsx
result Blue (NC-PU ink)
ParameterThis sampleStandard (BYK 9076 Standard)
Viscosity 32 sec 31 sec
Gloss 34.8 34
Colour Strength 1 1
Resolubility 4 4
Transparency Transparent Ref as Std
APP DATA- BYK 9076 equivalent.xlsx
Sample P 76 B.NO 48
13C NMR 25December2025 · CDCL3 · Fine Organics 13C zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
1H NMR 25December2025 · CDCL3 · Fine Organics 1H zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
13C NMR 25December2025 · CDCL3 · Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
13C NMR 25December2025 · CDCL3 · Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
1H NMR 25December2025 · CDCL3 · Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
1H NMR 25December2025 · CDCL3 · Fine Organics 1H zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf
Where this record comes from
LBN 48.pdf — lab journal (primary source)
APP DATA- BYK 9076 equivalent.xlsx — application testing
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 (24 fields) — for auditors
12 extraction fragments · merged 2026-08-25 · 9 human-validated fields
Fix a wrong or missing extraction side-by-side with the original: qwen-extract--lbn-48--lbn-48 app-data--S 9076 #48 analytical-name--15e694ba0c09 analytical-name--169cdbf3e74b analytical-name--2da192277dff analytical-name--a2a1e959b7c9 analytical-name--ae3970a4da38 analytical-name--b2f38d9eb7df qwen-extract--fine-organics-13c-fs-plot-sample-p-76-b-no-48--p-76-b-no-48 qwen-extract--fine-organics-13c-zoom1-plot-sample-p-76-b-no-48--p-76-b-no-48 qwen-extract--fine-organics-1h-fs-plot-sample-p-76-b-no-48--p-76-b-no-48 expt-block--48
FieldSourceExtractorConf.
aimLBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
conclusionLBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
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materials[2]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
materials[3]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[0]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[1]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
process_steps[2]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[0]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
critical_parameters[1]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
samples[0]LBN 48.pdf [LBN 48.pdf, pages 1-2] qwen-tasks/extract-fragment.md@unversionedhigh
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samples[1]APP DATA- BYK 9076 equivalent.xlsx sheet BYK_9076_equivalent, rows 53-53 parse_app_data.py@unversionedhigh
samples[2]Fine Organics 13C zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf filename parse_analytical_names.py@unversionedhigh
dateFine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf page 1 qwen-tasks/extract-fragment.md@unversionedhigh
scientistFine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf page 1 qwen-tasks/extract-fragment.md@unversionedhigh
record_type28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[3]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[4]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[5]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
process_steps[6]28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
observations28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '48', csv rows 1-11 qwen-tasks/extract-expt-block.md@unversionedhigh
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      "file": "pdf/9076 Data for Raven POC project/Analytical Report/NMR/#48/Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
      "role": "analytical",
      "link_basis": "alias match: P 76 B.NO 48",
      "link_status": "rule"
    },
    {
      "file": "pdf/9076 Data for Raven POC project/Analytical Report/NMR/#48/Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
      "role": "analytical",
      "link_basis": "alias match: P 76 B.NO 48",
      "link_status": "rule"
    },
    {
      "file": "pdf/9076 Data for Raven POC project/Analytical Report/NMR/#48/Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
      "role": "analytical",
      "link_basis": "alias match: P 76 B.NO 48",
      "link_status": "rule"
    },
    {
      "file": "pdf/9076 Data for Raven POC project/Analytical Report/NMR/#48/Fine Organics 1H zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
      "role": "analytical",
      "link_basis": "alias match: P 76 B.NO 48",
      "link_status": "rule"
    },
    {
      "file": "docs/Project Expt Report/28112025  9076 Expt Table 2025.xls",
      "role": "summary_table",
      "link_basis": "alias match: 48",
      "link_status": "rule"
    }
  ],
  "validation": {
    "validated_fields": {
      "conclusion": {
        "validated_by": "FOIL review",
        "date": "2026-08-20"
      },
      "outcome.status": {
        "validated_by": "FOIL review",
        "date": "2026-08-20"
      },
      "date": {
        "validated_by": "FOIL review",
        "date": "2026-08-21"
      },
      "materials[0].molecular_wt": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "materials[0].moles": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "materials[1].molecular_wt": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "materials[1].moles": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "materials[3].molecular_wt": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      },
      "process_steps[4].conditions.temperature": {
        "validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
        "date": "2026-08-21"
      }
    },
    "corrections_applied": [
      "corr-0001",
      "corr-0002",
      "corr-0005",
      "corr-0014",
      "corr-0015",
      "corr-0016",
      "corr-0017",
      "corr-0018",
      "corr-0041",
      "corr-0043"
    ]
  },
  "aim": "To develop product equivalent to reference product",
  "conclusion": "Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet",
  "conditions": {
    "atmosphere": "N2",
    "other": "Optimized Reaction Conditions table present but blank"
  },
  "materials": [
    {
      "sr_no": 1,
      "name": "Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900",
      "source": "Viswaat",
      "quantity": "178",
      "unit": "gms",
      "molecular_wt": "900",
      "moles": "0.197"
    },
    {
      "sr_no": 2,
      "name": "P2O5",
      "source": "Commercial",
      "quantity": "9.357",
      "unit": "gms",
      "molecular_wt": "141.94",
      "moles": "0.0658"
    },
    {
      "sr_no": 3,
      "name": "Epomine SP-018",
      "source": "Nippon",
      "quantity": "30",
      "unit": "gms",
      "purity_pct": "100"
    },
    {
      "sr_no": 4,
      "name": "2 ethyl hexyl acrylate",
      "quantity": "70",
      "unit": "gms",
      "purity_pct": "100",
      "molecular_wt": "184.27"
    }
  ],
  "process_steps": [
    {
      "step": 1,
      "time_hrs": "5",
      "temp_c": "58-75",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 1) Phosphate ester- RBF with Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 heated to 50 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 AV--52.52"
        }
      ],
      "results": [
        {
          "measurement": "AV",
          "value": "52.52",
          "verbatim": "AV--52.52",
          "parameter": "unlabelled"
        },
        {
          "measurement": "Mono",
          "value": "24.44",
          "verbatim": "Mono-24.44",
          "parameter": "unlabelled"
        },
        {
          "measurement": "Di",
          "value": "51.76",
          "verbatim": "Di- 51.76",
          "parameter": "unlabelled"
        },
        {
          "measurement": "Free acid",
          "value": "0.24",
          "verbatim": "Free acid-0.24",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 2,
      "time_hrs": "6.5",
      "temp_c": "78-82",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 2) Acrylate intermediate- RBF with Epomine SP- 018 heated to 78-81 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. IV-26.1 @ 5.5 hrs Cool to RT"
        }
      ],
      "results": [
        {
          "measurement": "Appearance",
          "value": "yellowish clear",
          "verbatim": "Appearance- yellowish clear",
          "parameter": "unlabelled"
        },
        {
          "measurement": "AV",
          "value": "0.45",
          "verbatim": "AV-0.45",
          "parameter": "unlabelled"
        },
        {
          "measurement": "IV",
          "value": "26.1 @ 5.5 hrs",
          "verbatim": "IV-26.1 @ 5.5 hrs",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 3,
      "time_hrs": "3.5",
      "temp_c": "56-61",
      "pressure": "N2",
      "procedure": [
        {
          "action": "Step 3) Neutralization - RBF with acrylate intermediate of step-2) (15%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) (85%) Phosphate ester into it over 30 min and contain 1ue for 3 hrs. Cool to RT and filter through Nylon Mesh."
        }
      ],
      "results": [
        {
          "measurement": "AV",
          "value": "44.36",
          "verbatim": "AV-44.36",
          "parameter": "unlabelled"
        },
        {
          "measurement": "HV",
          "value": "46.58",
          "verbatim": "HV-46.58",
          "parameter": "unlabelled"
        },
        {
          "measurement": "SAP",
          "value": "62.14",
          "verbatim": "SAP-62.14",
          "parameter": "unlabelled"
        },
        {
          "measurement": "Amine",
          "value": "36.25",
          "verbatim": "Amine-36.25",
          "parameter": "unlabelled"
        },
        {
          "measurement": "IV",
          "value": "5.8",
          "verbatim": "IV-5.8",
          "parameter": "unlabelled"
        }
      ]
    },
    {
      "step": 1,
      "materials": [
        {
          "name": "i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900",
          "role": "unknown",
          "quantity_g": "178",
          "verbatim": "i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO\\nHV-62.3/ MW-900",
          "role_verbatim": "raw_material"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "react",
          "temperature": "45",
          "time_h": "0.2",
          "verbatim": "Temp. 45, Time 0.2"
        }
      ],
      "conditions": {
        "temperature": "45",
        "time_h": "0.2"
      },
      "results": [
        {
          "parameter": "unlabelled",
          "value": "P-2.14%",
          "verbatim": "P-2.14%",
          "note": "P value, likely phosphorus content; parameter not labelled in cell"
        }
      ]
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "i) Epomine SP- 018",
          "role": "unknown",
          "quantity_g": "30",
          "verbatim": "i)  Epomine SP- 018",
          "role_verbatim": "raw_material"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "react",
          "temperature": "80",
          "time_h": "0.2",
          "verbatim": "Temp. 80, Time 0.2"
        }
      ],
      "conditions": {
        "temperature": "80 / 79-81",
        "time_h": "0.2"
      },
      "results": [
        {
          "parameter": "unlabelled",
          "value": "Mono-24.44 / Di- 51.76/ Free acid-0.24",
          "verbatim": "Mono-24.44 / Di- 51.76/ Free acid-0.24",
          "note": "Epoxy distribution (mono/di) and free acid; not a single A.V. parameter"
        }
      ]
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "Step - 1 Product Phosphate ester",
          "role": "intermediate",
          "quantity_g": "0.85",
          "verbatim": "Step - 1 Product\\nPhosphate ester"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "react",
          "temperature": "80",
          "time_h": "0.5",
          "verbatim": "Temp. 80, Time 0.5, Feed of phosphate ester",
          "note": "Feed-of-phosphate-ester sub-stage per the cell annotation; the Temp-80 stage is inferred from column position (same temp cell as Step 2)"
        },
        {
          "seq": 2,
          "action": "react",
          "time_h": "3.5",
          "verbatim": "Time 3.5; Stirrer well, clear transparent mass",
          "note": "Temperature blank in the cell for this stage"
        }
      ],
      "conditions": {
        "note": "Two stages: 80 oC / 0.5 h (feed of phosphate ester), then 3.5 h at unstated temperature; see procedure"
      },
      "results": [
        {
          "parameter": "phosphorus_content",
          "value": "1.82%",
          "verbatim": "P-1.82%"
        },
        {
          "parameter": "iodine_value",
          "value": "26.1",
          "verbatim": "IV-26.1  @ 5.5 hrs",
          "note": "Iodine value measured at 5.5 hrs"
        },
        {
          "parameter": "acid_value",
          "value": "44.36",
          "verbatim": "AV-44.36"
        },
        {
          "parameter": "hydroxyl_value",
          "value": "46.58",
          "verbatim": "HV-46.58"
        },
        {
          "parameter": "saponification_value",
          "value": "62.14",
          "verbatim": "SAP-62.14"
        },
        {
          "parameter": "amine_value",
          "value": "36.25",
          "verbatim": "Amine-36.25"
        },
        {
          "parameter": "iodine_value",
          "value": "5.8",
          "verbatim": "IV-5.8"
        }
      ],
      "remarks": "Stirrer well , clear transparent mass; Yellowish clear transparent mass"
    },
    {
      "step": 4,
      "note": "Downstream modification labelled LBN-48 (Q); its material list includes 'RM from above Batch'. Kept as a distinct process step because it has its own materials, conditions and results.",
      "materials": [
        {
          "name": "RM from above Batch",
          "role": "intermediate",
          "verbatim": "RM from above Batch"
        },
        {
          "name": "i) Acrylate",
          "role": "unknown",
          "quantity_g": "0.15",
          "verbatim": "i) Acrylate",
          "role_verbatim": "raw_material"
        },
        {
          "name": "ii) Dimethyl sulphate",
          "role": "unknown",
          "quantity_g": "0.005",
          "verbatim": "ii) Dimethyl sulphate",
          "role_verbatim": "raw_material"
        },
        {
          "name": "iii) Phosphate",
          "role": "unknown",
          "quantity_g": "0.85",
          "verbatim": "iii) Phosphate",
          "role_verbatim": "raw_material"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "react",
          "temperature": "65-75",
          "time_h": "1 hr",
          "verbatim": "Dimethyl sulphate, Temp. 65-75, 1 hr; Clear transparent mass"
        },
        {
          "seq": 2,
          "action": "react",
          "temperature": "55-60",
          "time_h": "2.5 hr",
          "verbatim": "Phosphate, Temp. 55-60, 2.5 hr; Yellowish transparent clear mass"
        }
      ],
      "conditions": {
        "note": "Two staged conditions: 65-75 oC / 1 hr (dimethyl sulphate) then 55-60 oC / 2.5 hr (phosphate); see procedure"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "52",
          "verbatim": "AV-52"
        },
        {
          "parameter": "amine_value",
          "value": "31.67",
          "verbatim": "Amine-31.67"
        },
        {
          "parameter": "iodine_value",
          "value": "3.48",
          "verbatim": "IV-3.48"
        },
        {
          "parameter": "saponification_value",
          "value": "84.9",
          "verbatim": "SAP-84.9"
        },
        {
          "parameter": "hydroxyl_value",
          "value": "38.6",
          "verbatim": "HV-38.6"
        }
      ],
      "remarks": "Clear transparent mass; Yellowish transparent clear mass"
    }
  ],
  "critical_parameters": [
    {
      "s_no": 1,
      "parameter": "aminev",
      "reference_value": "30.1",
      "value": "36.25"
    },
    {
      "s_no": 2,
      "parameter": "av",
      "reference_value": "43.2",
      "value": "44.36"
    }
  ],
  "samples": [
    {
      "description": "Neutralized phosphate ester-acrylate product (step 3), filtered through Nylon Mesh",
      "analytical": [
        {
          "technique": "AV",
          "value": "44.36"
        },
        {
          "technique": "HV",
          "value": "46.58"
        },
        {
          "technique": "SAP",
          "value": "62.14"
        },
        {
          "technique": "Amine",
          "value": "36.25"
        },
        {
          "technique": "IV",
          "value": "5.8"
        },
        {
          "technique": "13C NMR",
          "date": "Dec 25 2025",
          "solvent": "cdcl3",
          "instrument": "NMR500-vnmrs500",
          "file": "Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "parameters": "{\"observe\": \"C13, 125.6866595 MHz\", \"decouple\": \"H1, 499.8496240 MHz\", \"pulse_sequence\": \"CARBON (s2pul)\", \"fid_file\": \"CARBON\", \"temperature\": \"20.0 C / 293.1 K\", \"operator\": \"vnmr1\", \"relax_delay\": \"1.000 sec\", \"pulse\": \"45.0 degrees\", \"acq_time\": \"1.049 sec\", \"width\": \"31250.0 Hz\", \"repetitions\": \"1166\", \"power\": \"41 dB\", \"decoupling\": \"continuously on, WALTZ-16 modulated\", \"line_broadening\": \"1.0 Hz\", \"ft_size\": \"65536\", \"total_time\": \"1 hr, 8 min\"}",
          "printed_result": "{\"note\": \"13C FS (full scan) plot covering 20-220 ppm; peak positions (ppm) as printed on the plot, no assignments printed\", \"ppm\": [77.358, 77.1, 76.85, 75.461, 75.302, 75.272, 75.127, 75.082, 74.93, 74.467, 73.284, 73.056, 72.828, 71.144, 70.711, 70.582, 70.522, 70.021, 67.206, 31.657, 30.094, 28.804, 22.916, 19.221, 18.432, 18.151, 17.415, 17.294, 17.264, 17.218, 17.104, 16.937, 16.899, 14.069, 13.895, 10.905]}"
        },
        {
          "technique": "13C NMR",
          "date": "Dec 25 2025",
          "solvent": "cdcl3",
          "instrument": "NMR500-vnmrs500",
          "file": "Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "parameters": "{\"observe\": \"C13, 125.6866595 MHz\", \"decouple\": \"H1, 499.8496240 MHz\", \"pulse_sequence\": \"CARBON (s2pul)\", \"fid_file\": \"CARBON\", \"temperature\": \"20.0 C / 293.1 K\", \"operator\": \"vnmr1\", \"relax_delay\": \"1.000 sec\", \"pulse\": \"45.0 degrees\", \"acq_time\": \"1.049 sec\", \"width\": \"31250.0 Hz\", \"repetitions\": \"1166\", \"power\": \"41 dB\", \"decoupling\": \"continuously on, WALTZ-16 modulated\", \"line_broadening\": \"1.0 Hz\", \"ft_size\": \"65536\", \"total_time\": \"1 hr, 8 min\"}",
          "printed_result": "{\"note\": \"13C zoom1 plot covering 10-35 ppm; peak positions (ppm) as printed on the plot\", \"ppm\": [38.532, 31.657, 30.246, 30.094, 28.804, 23.592, 23.053, 22.916, 19.221, 18.432, 18.151, 18.113, 17.415, 17.294, 17.264, 17.218, 17.104, 16.937, 16.899, 14.069, 13.895, 10.905, 10.806]}"
        },
        {
          "technique": "1H NMR",
          "date": "Dec 25 2025",
          "solvent": "cdcl3",
          "file": "Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "conditions": "{\"temperature\": \"20.0 C / 293.1 K\", \"frequency_mhz\": \"499.8471010\", \"relaxation_delay_sec\": \"5.000\", \"pulse_degrees\": \"45.0\", \"acquisition_time_sec\": \"2.045\", \"width_hz\": \"8012.8\", \"repetitions\": \"64\", \"line_broadening_hz\": \"0.3\", \"ft_size\": \"32768\", \"total_time\": \"7 min 31 sec\"}",
          "instrument": "NMR500-vnmrs500",
          "pulse_sequence": "PROTON (s2pul)",
          "printed_result": "ppm peaks: 7.315; 3.934; 3.922; 3.682; 3.655; 3.648; 3.632; 3.606; 3.588; 3.577; 3.568; 3.557; 3.547; 3.534; 3.522; 3.513; 3.502; 3.492; 3.482; 3.471; 3.458; 3.444; 3.424; 3.416; 3.407; 3.398; 3.390; 3.349; 3.338; 3.329; 3.323; 3.302; 3.161; 2.173; 1.593; 1.579; 1.565; 1.549; 1.535; 1.384; 1.370; 1.354; 1.339; 1.325; 1.278; 1.147; 1.134; 1.116; 1.111; 1.101; 1.088; 0.929; 0.914; 0.899; 0.884; 0.873; 0.000. Relative integrals: 0.26; 0.68; 1.73; 31.61; 17.23; 5.81; 1.38; 0.71; 2.60; 0.68; 0.11; 2.09; 8.02; 21.18; 5.91."
        }
      ],
      "application_tests": [
        {
          "test": "Solubility/gloss over pigments",
          "system": "pigment Black, Blue, Violet-23/27 etc",
          "result": "All having matching resolubility while reduced gloss in violet",
          "verbatim": "Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet"
        }
      ],
      "sample_id": "unspecified sample"
    },
    {
      "sample_id": "S 9076 #48",
      "application_tests": [
        {
          "test": "Violet 23",
          "system": "NC-PU ink",
          "conditions": "trial 31.10.2025",
          "result": "Viscosity: 30 sec; Gloss: 53.3; Colour Strength: 98-99.00%; Resolubility: 3; Transparency: Opaque",
          "vs_reference": "BYK 9076 Standard — Viscosity: 29 sec; Gloss: 62; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
          "file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
        },
        {
          "test": "Violet 27",
          "system": "NC-PU ink",
          "conditions": "trial 31.10.2025",
          "result": "Viscosity: 31 sec; Gloss: 4.6; Colour Strength: 1; Resolubility: 4; Transparency: Eq to Std",
          "vs_reference": "BYK 9076 Standard — Viscosity: 30 sec; Gloss: 5.3; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
          "file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
        },
        {
          "test": "Black",
          "system": "NC-PU ink",
          "conditions": "trial 31.10.2025",
          "result": "Viscosity: 34 sec; Gloss: 30.9; Colour Strength: 1; Resolubility: 4; Transparency: Eq to Std",
          "vs_reference": "BYK 9076 Standard — Viscosity: 33 sec; Gloss: 31; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
          "file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
        },
        {
          "test": "Blue",
          "system": "NC-PU ink",
          "conditions": "trial 31.10.2025",
          "result": "Viscosity: 32 sec; Gloss: 34.8; Colour Strength: 1; Resolubility: 4; Transparency: Transparent",
          "vs_reference": "BYK 9076 Standard — Viscosity: 31 sec; Gloss: 34; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
          "file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
        }
      ]
    },
    {
      "sample_id": "P 76 B.NO 48",
      "analytical": [
        {
          "technique": "13C NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 13C zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        },
        {
          "technique": "1H NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 1H zoom2 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        },
        {
          "technique": "13C NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 13C FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        },
        {
          "technique": "13C NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 13C zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        },
        {
          "technique": "1H NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 1H FS plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        },
        {
          "technique": "1H NMR",
          "file": "Analytical Report/NMR/#48/Fine Organics 1H zoom1 plot Sample P 76 B.NO 48 CDCL3 25December2025.pdf",
          "solvent": "CDCL3",
          "date": "25December2025"
        }
      ]
    }
  ],
  "outcome": {
    "status": "ok",
    "basis": "Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet",
    "citation": "[LBN 48.pdf, page 2]"
  },
  "date": "26.6.25",
  "scientist": "vnmr1",
  "record_type": "synthesis",
  "observations": "Expt Table remarks: Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility while reduced gloss in violet; Tested on Violet 23 resolubility ok"
}