Experiments / Batch 49
Batch 49 OK
1/11/25 ·
also written as LBN 48 · S 9076 #49 · Batch- NO-49 · BYK 9076 · 49
aminev
20.2
target 30.1 · -32.9% vs target
av
46.5
target 43.2 · +7.6% vs target
Conclusion — verbatim from the source
“Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments”
LBN 49.pdf, page 2
Aim
Prepare phosphate ester, acrylate intermediate, and neutralised product (BYK-9076 equivalent)
Observations
Appearance of acrylate intermediate: yellowish clear Tested over pigment Black, Blue, Violet-23/27 etc - all having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments Step-I: No Particles, Clear mass, No Turbidity Step-II: Clear Neutralisation: clear transparent Mass Step I: No - Particles, Clear mass, No Turbidity, HV - 51.87, mono - 22.56, di - 48, Free Acid - 1.096. Step II: Clear. Step III: AV - 46.5, Amine - 20.2. Charged LUB 1010- Feed of P205 / 10, Dispersion of P205 No - Particles., Clear mass., No Turbidity, HV - 51.87, mono - 22.56 / di - 48, Free Acid - 1.096 Charged SP-18 feed of 2ethyl hexyl Acrylate / 2hr Clear Acylate Intermediate 13 gm Feed of phosphate Ester over clear transparent Mass. AV - 46.5, Amine - 20.2 Expt Table remarks: 0.5,Feed of phosphate ester Expt Table remarks: IV-26.1 @ 5.5 hrs Expt Table remarks: Stirrer well , clear transparent mass
Procedure summary
Three-step synthesis: (1) Phosphate ester - Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/MW-900 heated to 50 deg C, P2O5 added under N2, digested 3 hrs at 70-75 deg C, cooled to RT. (2) Acrylate intermediate - Epomine SP-018 heated to 78-81 deg C under N2, 2-ethyl hexyl acrylate fed over 2 hrs, reaction continued 5 hrs, monitored by IV, cooled to RT. (3) Neutralization - acrylate intermediate of step 2 (13%) heated to 56 deg C under N2, phosphate ester of step 1 (87%) fed over 30 min, continued 3 hrs, cooled to RT, filtered through Nylon Mesh. Step-I: Charged LUB 1010 (208 gm) at RT-50/N2, fed P2O5 over 1.5 hrs at 50-77°C/N2, held 1.5 hrs at 77-80°C/N2. Step-II: Charged SP-18 (30 gm) at 75-79°C/N2, fed 2-ethyl hexyl Acrylate over 2 hrs, held 5.5 hrs at 77-79°C/N2. Neutralisation: Charged Acylate Intermediate (13 gm) at 55-58°C/N2, fed phosphate ester (87 gm) over 1.5 hrs at 55-57°C/N2. Step I: Phosphate ester synthesis. Step II: Acrylate intermediate synthesis. Step III: Neutralization.
Raw materials
| # | Material | Source | Qty | Purity % | Mol. wt. | Moles | Role |
|---|---|---|---|---|---|---|---|
| 1 | Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 ×3 | Viswaat | 208 gms | 900 | 0.2311 | reactant | |
| 2 | P2O5 ×4 | Commercial | 10.93 gms | 141.94 | 0.077 | reactant | |
| 3 | Epomine SP-018 ×3 | Nippon | 30 gms | 100 | reactant | ||
| 4 | 2 ethyl hexyl acrylate ×4 | 70 gms | 100 | 184.27 | 7 | reactant | |
| Micropin LUB 1010 Bu-Eo-PO | 208 gm | 900 | 0.2311 | - | |||
| Phosphate Ester (Step-I) | 87 gm | reactant | |||||
| Acylate Intermediate (Step-II) | 13 gm | reactant |
Reaction conditions (optimized)
atmosphere: N2other: Step-I: RT-50 to 77-80°C; Step-II: 75-79°C; Neutralisation: 55-58°C; Step I: RT-50 to 77-80°C; Step II: 75-79 to 77-79°C; Step III: 55-58 to 55-57°C
Process
| Step | Conditions | Charged | What happened | Results | ||||||||||||||||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
|
Step 1
Step-I) Phosphate Ester
28112025 9076 Expt Table 2025.xls · LBN 49.pdf · 9076 Exp 48-60_1.pdf
|
temperature: 58-75 °Catmosphere: N2time: 5 hrs |
Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 (Viswaat) 208 gms (MW 900, 0.2311 mol) P2O5 (Commercial) 10.93 gms (MW 141.94, 0.077 mol)
|
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 (4 entries)
|
acid_value 51.87mono 22.56di 48.93bi 48free_acid 1.096P 2.14 % | ||||||||||||||||||||||||
|
Step 2
Step-II) Acrylate Intermediate
28112025 9076 Expt Table 2025.xls · LBN 49.pdf · 9076 Exp 48-60_1.pdf · 9076 Exp 48-60_1.pdf
|
temperature: 78-82 °Catmosphere: N2time: 6.5 hrs |
Epomine SP-018 (Nippon) 30 gms (100 %) 2 ethyl hexyl acrylate 70 gms (100 %, MW 184.27)
|
Step 2) Acrylate intermediate - RBF with Epomine SP- 018 heated to 78-81 deg C under N2 atmosphere. Slowly feed of 2-ethyl hexyl acrylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. Cool to RT. [ELN]
Step-by-step (5 entries)
|
Appearance yellowish clearacid_value 0.45iodine_value 26.1 | ||||||||||||||||||||||||
|
Step 3
Step-III) Neutralisation
28112025 9076 Expt Table 2025.xls · LBN 49.pdf
|
temperature: 56-61 °Catmosphere: N2time: 3.5 hrs |
Phosphate Ester (Step-I product) 87 g = 87 % [ELN, Notes; Table: 0.87] Acrylate Intermediate (Step-II product) 13 g = 13 % [ELN, Notes]
|
Step 3) Neutralization - RBF with acrylate intermediate of step-2) (13%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) (87%) Phosphate ester into it over 30 min and continue 1ue for 3 hrs. Cool to RT and filter through Nylon Mesh. [ELN]
Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments [ELN remarks] Table batch-block remarks (block-level, not tied to a step): '0.5,Feed of phosphate ester'; 'IV-26.1 @ 5.5 hrs'; 'Stirrer well , clear transparent mass'
Step-by-step (2 entries)
|
acid_value 46.5HV 49.4SAP 61.98amine_value 20.2iodine_value 2.58P 1.86 %mono 22.56di 48.93free_acid 1.096 |
Critical parameters — measured vs target
| Parameter | Target | Measured |
|---|---|---|
| aminev | 30.1 | 20.2 |
| av | 43.2 | 46.5 |
Sample S 9076 #49
result
Violet 23 (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 30 sec | 29 sec |
| Gloss | 52.7 | 57.6 |
| 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)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 31 sec | 30 sec |
| Gloss | 6.7 | 8.2 |
| 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)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 37 sec | 35 sec |
| Gloss | 24.7 | 26.6 |
| Colour Strength | 1 | 1 |
| Resolubility | 5 | 4 |
| Transparency | Eq to Std | Ref as Std |
APP DATA- BYK 9076 equivalent.xlsx
result
Blue (NC-PU ink)
| Parameter | This sample | Standard (BYK 9076 Standard) |
|---|---|---|
| Viscosity | 33 sec | 32 sec |
| Gloss | 40.3 | 39.5 |
| Colour Strength | 1 | 1 |
| Resolubility | 4 | 4 |
| Transparency | Eq to std | Ref as Std |
APP DATA- BYK 9076 equivalent.xlsx
Sample unspecified sample
AV
46.5
Amine
20.2
HV
51.87
mono
22.56
di
48
Free Acid
1.096
HV - 51.87
mono - 22.56 / di - 48
Free Acid - 1.096
AV - 46.5
Amine - 20.2
Where this record comes from
LBN 49.pdf
— lab journal (primary source) · linked by a person
APP DATA- BYK 9076 equivalent.xlsx
— application testing
9076 Exp 48-60_1.pdf
— handwritten notebook (primary source) · linked by a person
28112025 9076 Expt Table 2025.xls
— researcher summary (cross-check)
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Field-by-field provenance (37 fields) — for auditors
6 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-49--lbn-48
app-data--S 9076 #49
qwen-extract--9076-Exp-48-60-1--batch-49
qwen-extract--9076-exp-48-60-1--batch-49
qwen-extract--9076-exp-48-60_1--batch-no-49
expt-block--49
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},
"materials[16]": {
"source_file": "pdf/9076 Data for Raven POC project/Handwritten notes/9076 Exp 48-60_1.pdf",
"extractor": "qwen-tasks/extract-fragment.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "pages 4-5",
"confidence": "medium",
"human_checked": true
},
"process_steps[3]": {
"source_file": "pdf/9076 Data for Raven POC project/Handwritten notes/9076 Exp 48-60_1.pdf",
"extractor": "qwen-tasks/extract-fragment.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "pages 4-5",
"confidence": "medium",
"human_checked": true
},
"process_steps[4]": {
"source_file": "pdf/9076 Data for Raven POC project/Handwritten notes/9076 Exp 48-60_1.pdf",
"extractor": "qwen-tasks/extract-fragment.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "pages 4-5",
"confidence": "medium",
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},
"process_steps[5]": {
"source_file": "pdf/9076 Data for Raven POC project/Handwritten notes/9076 Exp 48-60_1.pdf",
"extractor": "qwen-tasks/extract-fragment.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "pages 4-5",
"confidence": "medium",
"human_checked": true
},
"process_steps[6]": {
"source_file": "docs/Project Expt Report/28112025 9076 Expt Table 2025.xls",
"extractor": "qwen-tasks/extract-expt-block.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "sheet 9076_Experiments, batch block '49'",
"confidence": "medium",
"human_checked": true
},
"process_steps[7]": {
"source_file": "docs/Project Expt Report/28112025 9076 Expt Table 2025.xls",
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"source_file": "docs/Project Expt Report/28112025 9076 Expt Table 2025.xls",
"extractor": "qwen-tasks/extract-expt-block.md",
"extractor_version": "unversioned",
"extracted_date": "",
"locator": "sheet 9076_Experiments, batch block '49'",
"confidence": "medium",
"human_checked": true
}
},
"last_merged": "2026-08-25"
},
"documents": [
{
"file": "pdf/9076 Data for Raven POC project/Old ELN/LBN 49.pdf",
"role": "eln_report",
"link_basis": "human link (exp-9076-049)",
"link_status": "user-confirmed"
},
{
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx",
"role": "application_test",
"link_basis": "alias match: S 9076 #49",
"link_status": "rule"
},
{
"file": "pdf/9076 Data for Raven POC project/Handwritten notes/9076 Exp 48-60_1.pdf",
"role": "handwritten_notes",
"link_basis": "human link (exp-9076-049)",
"link_status": "user-confirmed"
},
{
"file": "docs/Project Expt Report/28112025 9076 Expt Table 2025.xls",
"role": "summary_table",
"link_basis": "alias match: 49",
"link_status": "rule"
}
],
"validation": {
"validated_fields": {
"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[8].conditions.time_h": {
"validated_by": "Claude direct analysis (Rishi-authorized 2026-08-21)",
"date": "2026-08-21"
},
"outcome.status": {
"validated_by": "FOIL review",
"date": "2026-08-21"
},
"aim": {
"validated_by": "FOIL review",
"date": "2026-08-25"
}
},
"corrections_applied": [
"corr-0010",
"corr-0032",
"corr-0033",
"corr-0034",
"corr-0035",
"corr-0036",
"corr-0042",
"corr-0044",
"corr-0045",
"corr-0049"
]
},
"aim": "Prepare phosphate ester, acrylate intermediate, and neutralised product (BYK-9076 equivalent)",
"conclusion": "Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments",
"conditions": {
"atmosphere": "N2",
"other": "Step-I: RT-50 to 77-80°C; Step-II: 75-79°C; Neutralisation: 55-58°C; Step I: RT-50 to 77-80°C; Step II: 75-79 to 77-79°C; Step III: 55-58 to 55-57°C"
},
"materials": [
{
"sr_no": "1",
"name": "Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900",
"source": "Viswaat",
"quantity": "208",
"unit": "gms",
"molecular_wt": "900",
"moles": "0.2311"
},
{
"sr_no": "2",
"name": "P2O5",
"source": "Commercial",
"quantity": "10.93",
"unit": "gms",
"molecular_wt": "141.94",
"moles": "0.077"
},
{
"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"
},
{
"name": "Micropin LUB 1010 Bu-Eo-PO",
"quantity": "208",
"unit": "gm",
"role": "unknown",
"molecular_wt": "900",
"moles": "0.2311",
"notes": "HV-62.3",
"role_verbatim": "polyol"
},
{
"name": "P2O5",
"quantity": "10.93",
"unit": "gm",
"role": "unknown",
"molecular_wt": "141.94",
"moles": "0.077",
"role_verbatim": "phosphorylating agent"
},
{
"name": "Epimine SP-18",
"quantity": "30",
"unit": "gm",
"role": "unknown",
"role_verbatim": "amine"
},
{
"name": "2-ethyl hexyl Acrylate",
"quantity": "70",
"unit": "gm",
"role": "unknown",
"molecular_wt": "184.27",
"role_verbatim": "acylating agent"
},
{
"name": "Micropin LUB 1010",
"quantity": "208",
"unit": "gm",
"role": "reactant",
"notes": "Bu-Eo-PO, HV - 62.3, MW. 900"
},
{
"name": "P205",
"quantity": "10.93",
"unit": "gm",
"role": "reactant"
},
{
"name": "Epimine SP-18",
"quantity": "30",
"unit": "gm",
"role": "reactant"
},
{
"name": "2-ethyl hexyl Acrylate",
"quantity": "70",
"unit": "gm",
"role": "reactant"
},
{
"name": "Micropin LUB 1010, Bu-Eo-PO, HV - 62.3, MW. 900",
"quantity": "208",
"unit": "gm",
"molecular_weight": "900",
"moles": "0.2311",
"role": "reactant"
},
{
"name": "P205",
"quantity": "10.93",
"unit": "gm",
"molecular_weight": "141.94",
"moles": "0.077",
"role": "reactant"
},
{
"name": "2-ethyl hexyl Acrylate",
"quantity": "70",
"unit": "gm",
"molecular_weight": "184.27",
"moles": "7",
"role": "reactant"
},
{
"name": "Phosphate Ester (Step-I)",
"quantity": "87",
"unit": "gm",
"percentage": "87.",
"role": "reactant"
},
{
"name": "Acylate Intermediate (Step-II)",
"quantity": "13",
"unit": "gm",
"percentage": "13.1.",
"role": "reactant"
}
],
"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-51.87"
}
],
"remarks": "Mono-22.56 / Di- 48.93/ Free acid-1.096",
"results": [
{
"parameter": "AV",
"value": "51.87",
"verbatim": "AV-51.87"
},
{
"parameter": "Mono",
"value": "22.56",
"verbatim": "Mono-22.56"
},
{
"parameter": "Di",
"value": "48.93",
"verbatim": "Di- 48.93"
},
{
"parameter": "Free acid",
"value": "1.096",
"verbatim": "Free acid-1.096"
}
]
},
{
"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 acrylate over 2 hrs and continue reaction for 5 hrs. Monitoring of reaction done by IV. IV-26.1 @ 5.5 hrs Cool to RT"
}
],
"remarks": "Appearance- yellowish clear AV-0.45 IV-26.1 @ 5.5 hrs",
"results": [
{
"parameter": "Appearance",
"value": "yellowish clear",
"verbatim": "Appearance- yellowish clear"
},
{
"parameter": "AV",
"value": "0.45",
"verbatim": "AV-0.45"
},
{
"parameter": "IV",
"value": "26.1",
"verbatim": "IV-26.1 @ 5.5 hrs"
}
]
},
{
"step": "3",
"time_hrs": "3.5",
"temp_c": "56-61",
"pressure": "N2",
"procedure": [
{
"action": "Step 3) Neutralization - RBF with acrylate intermediate of step-2) (13%) heated to 56 deg C under N2 atmosphere. Slowly feed of step-1) (87%) Phosphate ester into it over 30 min and continue 1ue for 3 hrs. Cool to RT and filter through Nylon Mesh."
}
],
"remarks": "AV-46.5/ HV-49.4/SAP-61.98 /Amine-20.2/ IV-2.58 Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments",
"results": [
{
"parameter": "AV",
"value": "46.5",
"verbatim": "AV-46.5"
},
{
"parameter": "HV",
"value": "49.4",
"verbatim": "HV-49.4"
},
{
"parameter": "SAP",
"value": "61.98",
"verbatim": "SAP-61.98"
},
{
"parameter": "Amine",
"value": "20.2",
"verbatim": "Amine-20.2"
},
{
"parameter": "IV",
"value": "2.58",
"verbatim": "IV-2.58"
}
]
},
{
"name": "Step-I phosphate ester",
"process": [
{
"time": "0.5",
"temperature": "RT-50 / N2",
"observation": "Charged LUB 1010-"
},
{
"time": "1.5",
"temperature": "50-75-77 / N2",
"observation": "Feed of P205 / 10, Dispersion of P205"
},
{
"time": "1.5",
"temperature": "77-80 / N2",
"observation": "No - Particles., Clear mass., No Turbidity, HV - 51.87, mono - 22.56 / di - 48, Free Acid - 1.096"
}
],
"measurements": [
{
"verbatim": "HV - 51.87"
},
{
"verbatim": "mono - 22.56 / di - 48"
},
{
"verbatim": "Free Acid - 1.096"
}
],
"step": 1
},
{
"name": "Step-II Acrylate Intermediate",
"process": [
{
"time": "0.5",
"temperature": "75-79 / N2",
"observation": "Charged SP-18"
},
{
"time": "2hrs.",
"temperature": "75-79 / N2",
"observation": "feed of 2ethyl hexyl Acrylate / 2hr"
},
{
"time": "5.5 hrs.",
"temperature": "77-79 / N2",
"observation": "Clear"
}
],
"step": 2,
"materials": {}
},
{
"name": "Step-II Neutralisation (printed heading; follows Step-II)",
"process": [
{
"time": "0.5",
"temperature": "55-58 / N2",
"observation": "Acylate Intermediate 13 gm"
},
{
"time": "1.5",
"temperature": "55-57 / N2",
"observation": "Feed of phosphate Ester over"
},
{
"time": "1.5",
"temperature": "55-57 / N2",
"observation": "clear transparent Mass."
},
{
"observation": "AV - 46.5, Amine - 20.2"
}
],
"measurements": [
{
"verbatim": "AV - 46.5"
},
{
"verbatim": "Amine - 20.2"
}
],
"step": 2
},
{
"step": 1,
"materials": [
{
"name": "i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO\nHV-62.3/ MW-900",
"qty_g": "208",
"role": "reactant",
"verbatim": "i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO\nHV-62.3/ MW-900"
}
],
"procedure": [],
"conditions": {
"temperature": "45",
"time_h": "0.2"
},
"results": [
{
"parameter": "unlabelled",
"value": "P-2.14%",
"verbatim": "P-2.14%",
"note": "A.V. column, Step 1; likely phosphorus content of the Step 1 reactant (Vicaspin phosphate), parameter not explicit in the cell."
}
]
},
{
"step": 2,
"materials": [
{
"name": "i) Epomine SP- 018",
"qty_g": "30",
"role": "reactant",
"verbatim": "i) Epomine SP- 018"
}
],
"procedure": [],
"conditions": {
"temperature": "80",
"time_h": "0.2"
},
"results": [],
"note": "Sheet cell layout has Temp/Time columns holding 0.2 and 80; interpreted as 0.2 h at 80 oC. Values copied verbatim from the printed Temp oC and Time (h) cells, mapping is an interpretation (confidence medium)."
},
{
"step": 3,
"materials": [
{
"name": "Step - 1 Product\nPhosphate ester",
"qty_g": "0.87",
"role": "intermediate",
"verbatim": "Step - 1 Product\nPhosphate ester"
}
],
"procedure": [],
"conditions": {
"time_h": "3.5"
},
"results": [
{
"parameter": "unlabelled",
"value": "P-1.86 %",
"verbatim": "P-1.86 %",
"note": "Printed in the Step 3 Temp oC column; appears to be a phosphorus result, not a temperature (layout shift in this row). Confidence medium."
},
{
"parameter": "unlabelled",
"value": "AV-46.5/ HV-49.4/SAP-61.98\n/Amine-20.2/ IV-2.58",
"verbatim": "AV-46.5/ HV-49.4/SAP-61.98\n/Amine-20.2/ IV-2.58",
"note": "Printed in the Step 3 Time (h) column; multi-parameter analysis line (acid value, HV, SAP, amine value, iodine value), kept whole to avoid mis-splitting."
},
{
"parameter": "unlabelled",
"value": "Mono-22.56 / Di- 48.93/ Free acid-1.096",
"verbatim": "Mono-22.56 / Di- 48.93/ Free acid-1.096",
"note": "Printed in the Step 3 Vac/N2 column; mono/di/free-acid distribution analysis."
}
],
"note": "Step 3 condition cells are occupied by analysis results rather than temperature/time/atmosphere; no reaction conditions are printed for Step 3 (confidence low for the missing conditions)."
}
],
"critical_parameters": [
{
"parameter": "aminev",
"reference_value": "30.1",
"value": "20.2"
},
{
"parameter": "av",
"reference_value": "43.2",
"value": "46.5"
}
],
"procedure_summary": "Three-step synthesis: (1) Phosphate ester - Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/MW-900 heated to 50 deg C, P2O5 added under N2, digested 3 hrs at 70-75 deg C, cooled to RT. (2) Acrylate intermediate - Epomine SP-018 heated to 78-81 deg C under N2, 2-ethyl hexyl acrylate fed over 2 hrs, reaction continued 5 hrs, monitored by IV, cooled to RT. (3) Neutralization - acrylate intermediate of step 2 (13%) heated to 56 deg C under N2, phosphate ester of step 1 (87%) fed over 30 min, continued 3 hrs, cooled to RT, filtered through Nylon Mesh.\n\nStep-I: Charged LUB 1010 (208 gm) at RT-50/N2, fed P2O5 over 1.5 hrs at 50-77°C/N2, held 1.5 hrs at 77-80°C/N2. Step-II: Charged SP-18 (30 gm) at 75-79°C/N2, fed 2-ethyl hexyl Acrylate over 2 hrs, held 5.5 hrs at 77-79°C/N2. Neutralisation: Charged Acylate Intermediate (13 gm) at 55-58°C/N2, fed phosphate ester (87 gm) over 1.5 hrs at 55-57°C/N2.\n\nStep I: Phosphate ester synthesis. Step II: Acrylate intermediate synthesis. Step III: Neutralization.",
"observations": "Appearance of acrylate intermediate: yellowish clear\nTested over pigment Black, Blue, Violet-23/27 etc - all having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments\n\nStep-I: No Particles, Clear mass, No Turbidity\nStep-II: Clear\nNeutralisation: clear transparent Mass\n\nStep I: No - Particles, Clear mass, No Turbidity, HV - 51.87, mono - 22.56, di - 48, Free Acid - 1.096.\nStep II: Clear.\nStep III: AV - 46.5, Amine - 20.2.\n\nCharged LUB 1010-\nFeed of P205 / 10, Dispersion of P205\nNo - Particles., Clear mass., No Turbidity, HV - 51.87, mono - 22.56 / di - 48, Free Acid - 1.096\nCharged SP-18\nfeed of 2ethyl hexyl Acrylate / 2hr\nClear\nAcylate Intermediate 13 gm\nFeed of phosphate Ester over\nclear transparent Mass.\nAV - 46.5, Amine - 20.2\n\nExpt Table remarks: 0.5,Feed of phosphate ester\nExpt Table remarks: IV-26.1 @ 5.5 hrs\nExpt Table remarks: Stirrer well , clear \ntransparent mass",
"outcome": {
"status": "ok",
"basis": "Tested over pigment Black, Blue, Violet-23/27 etc All having matching resolubility in black, blue & violet 27 while slight reduced in gloss found in all pigments",
"citation": "LBN 49.pdf, page 2"
},
"samples": [
{
"sample_id": "S 9076 #49",
"application_tests": [
{
"test": "Violet 23",
"system": "NC-PU ink",
"conditions": "trial 03.11.2025",
"result": "Viscosity: 30 sec; Gloss: 52.7; Colour Strength: 98-99.00%; Resolubility: 3; Transparency: Opaque",
"vs_reference": "BYK 9076 Standard — Viscosity: 29 sec; Gloss: 57.6; 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 03.11.2025",
"result": "Viscosity: 31 sec; Gloss: 6.7; Colour Strength: 1; Resolubility: 4; Transparency: Eq to Std",
"vs_reference": "BYK 9076 Standard — Viscosity: 30 sec; Gloss: 8.2; 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 03.11.2025",
"result": "Viscosity: 37 sec; Gloss: 24.7; Colour Strength: 1; Resolubility: 5; Transparency: Eq to Std",
"vs_reference": "BYK 9076 Standard — Viscosity: 35 sec; Gloss: 26.6; 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 03.11.2025",
"result": "Viscosity: 33 sec; Gloss: 40.3; Colour Strength: 1; Resolubility: 4; Transparency: Eq to std",
"vs_reference": "BYK 9076 Standard — Viscosity: 32 sec; Gloss: 39.5; Colour Strength: 1; Resolubility: 4; Transparency: Ref as Std",
"file": "docs/Application data Summary/APP DATA- BYK 9076 equivalent.xlsx"
}
]
},
{
"alias": "Batch-49",
"analytical": [
{
"technique": "AV",
"value": "46.5"
},
{
"technique": "Amine",
"value": "20.2"
},
{
"technique": "HV",
"value": "51.87"
},
{
"technique": "mono",
"value": "22.56"
},
{
"technique": "di",
"value": "48"
},
{
"technique": "Free Acid",
"value": "1.096"
},
{
"verbatim": "HV - 51.87"
},
{
"verbatim": "mono - 22.56 / di - 48"
},
{
"verbatim": "Free Acid - 1.096"
},
{
"verbatim": "AV - 46.5"
},
{
"verbatim": "Amine - 20.2"
}
],
"sample_id": "unspecified sample"
}
],
"date": "1/11/25"
}