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1.11.2025 · also written as Batch- NO-50 · BYK 9076 · B. NO - 50B · B. NO - 50A · Batch - NO-50 · 50 · 50B · 50 A

Aim

Handwritten lab-note for a BYK 9076 analogue batch (9076 Exp 48-60 series): Step-I phosphate ester of the polyol with P2O5, Step-II acylate/acrylate intermediate from SP-18 (or Lupasol G-20) with 2-ethyl hexyl acrylate/acylate, Step-III neutralisation of the phosphate ester with the acylate intermediate.

Observations

Step-I: Clear mass, No particles Step-II: Slowly from a... (OCR incomplete) 50B: Clear Mass, No foam, No turbidity 50A: Clear yellowish Mass, Clear Uniform Mass, Slight Turbidity Step I: Clear mass, No particles, HV - 52.5, mono - 23.5, Dioctyl - 53.2, Free Acid - 0.1. Step II: Slowly from a... (text cut off). Step III (50B): Clear Mass, No foam, No turbidity, AV - 44.14, Amine - 47. Step III (50A): Clear Uniform Mass, Slight Turbidity, AV - 48.7, Amine - 31.08. Charged LUB 1010 301 gm. Feed of P205 - 15.82 Over 10-12 Clear mass., No particles. Charged SP-18. Feed of 2-Ethyl hexyl Acylate / 2 hrs. Slowly from a... Charged - Acylate Intermediate 20g Feed of phosphate Ester 80g / 10-12 min Clear Mass / No foam, No turbidity Charged Acylate, Feed of DMS (1:1) over 15 min. Clear yellowish Mass Feed of phosphate Ester 30 min Clear Uniform Mass, Slight Turbidity. Expt Table remarks: Clear mass no particles; Mono-23.5 / Di- 53.2/ Free acid-0.1; P-1.71 %; Feed of phosphate ester; IV-26.1 @ 5.5 hrs; Stirrer well , clear transparent mass; Yellowish clear transparent mass; B.No-50 A; 1.5 hr clear yellowish mass; 3 hr/ Clear uniform mass Slight turbidity; Tested on Black & violet pigment Resolubility less while other parameters nearby

Procedure summary

Step-I: Charged LUB 1010 (301 gm) at RT-50/N2, fed P2O5 (15.82 gm) over 10-12 min, held 2.5 hrs at 75-78°C/N2. Step-II: Charged SP-18 (30 gm) at 78-81°C/N2, fed 2-Ethyl hexyl Acylate over 2 hrs at 78-80°C/N2, held 5.5 hrs. Batch 50B: Charged Acylate Intermediate (20 gm) at 55-57°C/N2, fed phosphate ester (80 gm) over 10-12 min, held 2.5 hrs. Batch 50A: Charged Acylate (15%) + DMS (1:1) (1%) at 55-58°C/N2, fed phosphate ester (85%) over 30 min at 55-62°C/N2, held 3 hrs. Step I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis. Step III: Neutralization (Batch 50B) and Variant with DMS (Batch 50A).

Raw materials

Material	Qty	Mol. wt.	Moles	Role
Vicaspin - LUB 1010, Ble-Eo-PD, MW-900, HV-62.3 ×3	301 gm	900	0.3344	reactant
P2O5 ×3	15.82 gm	141.94	0.111	reactant
Epamine SP-18 ×3	30 gm			reactant
2-Ethyl hexyl Acylate ×3	70 gm	184.27	701.	reactant
DMS (1:1) ×2	1% %			-
Phosphate Ester (CPT) (B. NO - 50B)	80 gm			reactant
Acylate Intermediate Step-II (B. NO - 50B)	20 gm			reactant
Acylate - Step-I) (B. NO - 50A)				reactant
DMS (1:1) (B. NO - 50A)				reactant
Phosphate Ester Step-II (B. NO - 50A)				reactant

Reaction conditions (optimized)

atmosphere: N2other: Step-I: RT-50 to 75-78°C; Step-II: 78-81°C; 50B: 55-57°C; 50A: 55-75°C; Step I: RT-50 to 75-78°C; Step II: 78-81 to 78-80°C; Step III (50B): 55-57°C; Step III (50A): 55-58 to 58-62°C

Process

Step

Conditions

Charged

What happened

Results

Step 1

Phosphate Ester

28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf

atmosphere: N2

Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 301 g (MW 900, 0.3344 mol)

P2O5 15.82 g (MW 141.94 [journal cell: 141.44], 0.111 mol)

Clear mass no particles [Table remark]

Step-by-step (4 entries)

Time (h)	Temp (°C)	Atm	What happened
0.5	RT-50	N2	Changed LUB 16/0 Notes
			Feed of P2O5-15-82; 30 g/m²; OVR2 10-12 Notes
2.5	75-78	N2	Clear mates; No particles Notes
0.2	45		Table

acid_value 52.5mono 23.5Brokers 53.2free_acid 0.1P 2.14 %

Step 2

Step-II Acrylate Intermediate

28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf

atmosphere: N2

Epomine SP-018 30 g

2-ethylhexyl Acrylate 70 g (MW 184.27)

Step-by-step (4 entries)

Time (h)	Temp (°C)	Atm	What happened
0.5	78-31	N2	Changed SP-18 Notes
2	78-80	N2	Fixed of 2ethyl Notes
5.5	78-80	N2	Hexyl Acrylate /2 hrs Notes
0.2	80		Table

mono 23.5di 53.2free_acid 0.1

Step 3

(sp-III) Neutralisation / B.No- 50B

28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf

atmosphere: N2

Phosphate Ester (CP/P) 20 [Notes; journal cells '20, 201']

B.No- 50B Step - 1 Product Phosphate ester 0.8 [Table]

'5.5' [Table, stray value outside the fixed columns, role unknown]

Stirrer well, clear transparent mass [Table remark]

Yellowish clear transparent mass [Table remark]

Journal p6 log continues as a flat hold: times 4.5 h to 180.5 h, all 55-57/N2, observation cell repeating '- 8h' at every 1-hour interval; no measurements recorded in that span [Notes]

Step-by-step (6 entries)

Time (h)	Temp (°C)	Atm	What happened
0.5	55-57	N2	Changed - Acetate Tumor Notes
0.5	55-57	N2	- No Tumor Notes
2.5	55-57	N2	AV - 4h/1h Notes
3.5	55-57	N2	AV - 4h/1h Notes
	79-81		Table
3.5			Feed of phosphate ester Table

P 1.71 %acid_value 44.14amine_value 47.1iodine_value 4.9SAP 84.29HV 58.5iodine_value 26.1

Step 4

B.No-50 A

28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf

atmosphere:

i) Acrylate (15%) 37.5 g

ii) DMS (1%) 2.52 g

iii) Phosphate ester- (85%) 212.5 g

B.No-50 A [Table remark]

Tested on Black & violet pigment - Resolubility less while other parameters nearby [Table remark]

Step-by-step (5 entries)

Time (h)	Temp (°C)	What happened
0.2	65-70	Table
		Feed of DMS over 15 min Table
1.5	70-75	clear yellowish mass Table
0.5	55-62	feed of RM-III Table
3	58-62	Clear uniform mass Slight turbidity Table

acid_value 48.7amine_value 31.08iodine_value 4.58SAP 88.4HV 45.5

Step 1 — Phosphate Ester curated · 2 sources

atmosphere: N2

Charged Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900 301 g (MW 900, 0.3344 mol)P2O5 15.82 g (MW 141.94 [journal cell: 141.44], 0.111 mol)

acid_value 52.5 mono 23.5 Brokers 53.2 free_acid 0.1 P 2.14 %

Clear mass no particles [Table remark]

Step-by-step (4 entries)

Time (h)	Temp (°C)	Atmosphere	What happened
0.5	RT-50	N2	Changed LUB 16/0	Notes
			Feed of P2O5-15-82; 30 g/m²; OVR2 10-12	Notes
2.5	75-78	N2	Clear mates; No particles	Notes
0.2	45			Table

View each source separately (28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf)

as recorded in 28112025 9076 Expt Table 2025.xls:

time_h: 0.2temperature: 45

Charged: i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO HV-62.3/ MW-900

acid_value 2.14 %

Step-by-step (1 entry)

Time (h)	Temp (°C)	Atmosphere	What happened
0.2	45		react

Clear mass no particles

as recorded in 9076 Exp 48-60_1.pdf:

Step 2 — Step-II Acrylate Intermediate curated · 2 sources

atmosphere: N2

Charged Epomine SP-018 30 g2-ethylhexyl Acrylate 70 g (MW 184.27)

mono 23.5 di 53.2 free_acid 0.1

Step-by-step (4 entries)

Time (h)	Temp (°C)	Atmosphere	What happened
0.5	78-31	N2	Changed SP-18	Notes
2	78-80	N2	Fixed of 2ethyl	Notes
5.5	78-80	N2	Hexyl Acrylate /2 hrs	Notes
0.2	80			Table

View each source separately (28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf)

as recorded in 28112025 9076 Expt Table 2025.xls:

time_h: 0.2temperature: 80

Charged: i) Epomine SP- 018

free_acid 0.1

Step-by-step (1 entry)

Time (h)	Temp (°C)	Atmosphere	What happened
0.2	80		react

as recorded in 9076 Exp 48-60_1.pdf:

Step 3 — (sp-III) Neutralisation / B.No- 50B curated · 2 sources

atmosphere: N2

Charged Phosphate Ester (CP/P) 20 [Notes; journal cells '20, 201']B.No- 50B Step - 1 Product Phosphate ester 0.8 [Table]'5.5' [Table, stray value outside the fixed columns, role unknown]

P 1.71 % acid_value 44.14 amine_value 47.1 iodine_value 4.9 SAP 84.29 HV 58.5 iodine_value 26.1

Stirrer well, clear transparent mass [Table remark]

Yellowish clear transparent mass [Table remark]

Journal p6 log continues as a flat hold: times 4.5 h to 180.5 h, all 55-57/N2, observation cell repeating '- 8h' at every 1-hour interval; no measurements recorded in that span [Notes]

Step-by-step (6 entries)

Time (h)	Temp (°C)	Atmosphere	What happened
0.5	55-57	N2	Changed - Acetate Tumor	Notes
0.5	55-57	N2	- No Tumor	Notes
2.5	55-57	N2	AV - 4h/1h	Notes
3.5	55-57	N2	AV - 4h/1h	Notes
	79-81			Table
3.5			Feed of phosphate ester	Table

View each source separately (28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf)

as recorded in 28112025 9076 Expt Table 2025.xls:

temperature: 79-81

Charged: B.No- 50B Step - 1 Product Phosphate ester · 5.5

phosphorus 1.71 % acid_value 44.14 amine 47.1 iodine_value 4.9 saponification_value 84.29 viscosity_HV 58.5 iodine_value 26.1

Step-by-step (2 entries)

Time (h)	Temp (°C)	Atmosphere	What happened
	79-81		react
3.5	79-81		feed phosphate ester

Stirrer well , clear transparent mass; Yellowish clear transparent mass

as recorded in 9076 Exp 48-60_1.pdf:

Step 4 — B.No-50 A curated · 2 sources

atmosphere:

Charged i) Acrylate (15%) 37.5 gii) DMS (1%) 2.52 giii) Phosphate ester- (85%) 212.5 g

acid_value 48.7 amine_value 31.08 iodine_value 4.58 SAP 88.4 HV 45.5

B.No-50 A [Table remark]

Tested on Black & violet pigment - Resolubility less while other parameters nearby [Table remark]

Step-by-step (5 entries)

Time (h)	Temp (°C)	What happened
0.2	65-70		Table
		Feed of DMS over 15 min	Table
1.5	70-75	clear yellowish mass	Table
0.5	55-62	feed of RM-III	Table
3	58-62	Clear uniform mass Slight turbidity	Table

View each source separately (28112025 9076 Expt Table 2025.xls · 9076 Exp 48-60_1.pdf)

as recorded in 28112025 9076 Expt Table 2025.xls:

time_h: 0.2 / 1.5 / 0.5 / 3temperature: 65-70 / 70-75 / 55-62 / 58-62

Charged: i) Acrylate (15%) · ii) DMS (1%) · iii) Phosphate ester- (85%)

acid_value 48.7 amine 31.08 iodine_value 4.58 saponification_value 88.4 viscosity_HV 45.5

Step-by-step (5 entries)

Time (h)	Temp (°C)	What happened
0.2	65-70	react
		feed DMS
1.5	70-75	react
0.5	55-62	feed
3	58-62	react

B.No-50 A; Tested on Black & violet pigment Resolubility less while other parameters nearby

as recorded in 9076 Exp 48-60_1.pdf:

Sample unspecified sample

HV 52.5

mono 23.5

Dioctyl 53.2

Free Acid 0.1

AV 44.14

Amine 47

AV 48.7

Amine 31.08

HV - 52.5

mono - 23.5

Dioctyl - 53.2

Free Acid - 0.1

AV - 44.14

Amine - 47

AV - 48.7

Amine - 31.08

Where this record comes from

9076 Exp 48-60_1.pdf — handwritten notebook (primary source) · linked by a person

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 (33 fields) — for auditors

4 extraction fragments · merged 2026-08-25 · 1 human-validated fields

Fix a wrong or missing extraction side-by-side with the original: qwen-extract--9076-Exp-48-60-1--batch-50 qwen-extract--9076-exp-48-60-1--batch-50 qwen-extract--9076-exp-48-60_1--batch-no-50 expt-block--50

Field	Source	Extractor	Conf.
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aim	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	high
conditions.atmosphere	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	high
materials[0]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[1]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[2]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[3]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[4]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
samples[0]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	high
procedure_summary	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
observations	28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '50'	qwen-tasks/extract-expt-block.md@unversioned	high
materials[5]	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
materials[6]	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
materials[7]	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
materials[8]	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
materials[9]	9076 Exp 48-60_1.pdf Page 5-6	qwen-tasks/extract-fragment.md@direct-v1	high
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materials[12]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[13]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[14]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[15]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[16]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[17]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
materials[18]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
process_steps[0]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
process_steps[1]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
process_steps[2]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
process_steps[3]	9076 Exp 48-60_1.pdf pages 6-7	qwen-tasks/extract-fragment.md@unversioned	medium
process_steps[4]	28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '50'	qwen-tasks/extract-expt-block.md@unversioned	high
process_steps[5]	28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '50'	qwen-tasks/extract-expt-block.md@unversioned	high
process_steps[6]	28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '50'	qwen-tasks/extract-expt-block.md@unversioned	high
process_steps[7]	28112025 9076 Expt Table 2025.xls sheet 9076_Experiments, batch block '50'	qwen-tasks/extract-expt-block.md@unversioned	high

Raw record JSON

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      },
      "process_steps[4]": {
        "source_file": "docs/Project Expt Report/28112025  9076 Expt Table 2025.xls",
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        "locator": "sheet 9076_Experiments, batch block '50'",
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        "locator": "sheet 9076_Experiments, batch block '50'",
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      }
    },
    "last_merged": "2026-08-25"
  },
  "documents": [
    {
      "file": "pdf/9076 Data for Raven POC project/Handwritten  notes/9076 Exp 48-60_1.pdf",
      "role": "handwritten_notes",
      "link_basis": "human link (exp-9076-050)",
      "link_status": "user-confirmed"
    },
    {
      "file": "docs/Project Expt Report/28112025  9076 Expt Table 2025.xls",
      "role": "summary_table",
      "link_basis": "alias match: 50",
      "link_status": "rule"
    }
  ],
  "validation": {
    "validated_fields": {
      "date": {
        "validated_by": "FOIL review",
        "date": "2026-08-25"
      }
    },
    "corrections_applied": [
      "corr-0050"
    ]
  },
  "date": "1.11.2025",
  "aim": "Handwritten lab-note for a BYK 9076 analogue batch (9076 Exp 48-60 series): Step-I phosphate ester of the polyol with P2O5, Step-II acylate/acrylate intermediate from SP-18 (or Lupasol G-20) with 2-ethyl hexyl acrylate/acylate, Step-III neutralisation of the phosphate ester with the acylate intermediate.",
  "conditions": {
    "atmosphere": "N2",
    "other": "Step-I: RT-50 to 75-78°C; Step-II: 78-81°C; 50B: 55-57°C; 50A: 55-75°C; Step I: RT-50 to 75-78°C; Step II: 78-81 to 78-80°C; Step III (50B): 55-57°C; Step III (50A): 55-58 to 58-62°C"
  },
  "materials": [
    {
      "name": "Vicaspin - LUB 1010",
      "quantity": "301",
      "unit": "gm",
      "role": "unknown",
      "molecular_wt": "900",
      "moles": "0.3344",
      "notes": "Ble-Eo-PD, HV-62.3",
      "role_verbatim": "polyol"
    },
    {
      "name": "P2O5",
      "quantity": "15.82",
      "unit": "gm",
      "role": "unknown",
      "molecular_wt": "141.94",
      "moles": "0.111",
      "role_verbatim": "phosphorylating agent"
    },
    {
      "name": "Epamine SP-18",
      "quantity": "30",
      "unit": "gm",
      "role": "unknown",
      "role_verbatim": "amine"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "70",
      "unit": "gm",
      "role": "unknown",
      "molecular_wt": "184.27",
      "role_verbatim": "acylating agent"
    },
    {
      "name": "DMS (1:1)",
      "quantity": "1%",
      "unit": "%",
      "role": "unknown",
      "role_verbatim": "co-solvent (Batch 50A)"
    },
    {
      "name": "Vicaspin - LUB 1010",
      "quantity": "301",
      "unit": "gm",
      "role": "reactant",
      "notes": "Ble-Eo-PD / MW-900, HV-62.3"
    },
    {
      "name": "P205",
      "quantity": "15.82",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "Epamine SP-18",
      "quantity": "30",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "70",
      "unit": "gm",
      "role": "reactant"
    },
    {
      "name": "DMS (1:1)",
      "quantity": "1",
      "unit": "%",
      "role": "unknown",
      "notes": "Used in Batch 50A",
      "role_verbatim": "additive"
    },
    {
      "name": "Vicaspin - LUB 1010, Ble-Eo-PD, MW-900, HV-62.3",
      "quantity": "301",
      "unit": "gm",
      "molecular_weight": "900",
      "moles": "0.3344",
      "role": "reactant"
    },
    {
      "name": "P205",
      "quantity": "15.82",
      "unit": "gm",
      "molecular_weight": "141.94",
      "moles": "0.111",
      "role": "reactant"
    },
    {
      "name": "Epamine SP-18",
      "quantity": "30",
      "unit": "gm",
      "percentage": "301.",
      "role": "reactant"
    },
    {
      "name": "2-Ethyl hexyl Acylate",
      "quantity": "70",
      "unit": "gm",
      "molecular_weight": "184.27",
      "moles": "701.",
      "role": "reactant"
    },
    {
      "name": "Phosphate Ester (CPT) (B. NO - 50B)",
      "quantity": "80",
      "unit": "gm",
      "percentage": "80%",
      "role": "reactant"
    },
    {
      "name": "Acylate Intermediate Step-II (B. NO - 50B)",
      "quantity": "20",
      "unit": "gm",
      "percentage": "20%",
      "role": "reactant"
    },
    {
      "name": "Acylate - Step-I) (B. NO - 50A)",
      "percentage": "15%",
      "role": "reactant"
    },
    {
      "name": "DMS (1:1) (B. NO - 50A)",
      "percentage": "1%",
      "role": "reactant"
    },
    {
      "name": "Phosphate Ester Step-II (B. NO - 50A)",
      "percentage": "85%",
      "role": "reactant"
    }
  ],
  "samples": [
    {
      "alias": "Batch-50",
      "analytical": [
        {
          "technique": "HV",
          "value": "52.5"
        },
        {
          "technique": "mono",
          "value": "23.5"
        },
        {
          "technique": "Dioctyl",
          "value": "53.2"
        },
        {
          "technique": "Free Acid",
          "value": "0.1"
        },
        {
          "technique": "AV",
          "value": "44.14"
        },
        {
          "technique": "Amine",
          "value": "47"
        },
        {
          "technique": "AV",
          "value": "48.7"
        },
        {
          "technique": "Amine",
          "value": "31.08"
        },
        {
          "verbatim": "HV - 52.5"
        },
        {
          "verbatim": "mono - 23.5"
        },
        {
          "verbatim": "Dioctyl - 53.2"
        },
        {
          "verbatim": "Free Acid - 0.1"
        },
        {
          "verbatim": "AV - 44.14"
        },
        {
          "verbatim": "Amine - 47"
        },
        {
          "verbatim": "AV - 48.7"
        },
        {
          "verbatim": "Amine - 31.08"
        }
      ],
      "sample_id": "unspecified sample"
    }
  ],
  "procedure_summary": "Step-I: Charged LUB 1010 (301 gm) at RT-50/N2, fed P2O5 (15.82 gm) over 10-12 min, held 2.5 hrs at 75-78°C/N2. Step-II: Charged SP-18 (30 gm) at 78-81°C/N2, fed 2-Ethyl hexyl Acylate over 2 hrs at 78-80°C/N2, held 5.5 hrs. Batch 50B: Charged Acylate Intermediate (20 gm) at 55-57°C/N2, fed phosphate ester (80 gm) over 10-12 min, held 2.5 hrs. Batch 50A: Charged Acylate (15%) + DMS (1:1) (1%) at 55-58°C/N2, fed phosphate ester (85%) over 30 min at 55-62°C/N2, held 3 hrs.\n\nStep I: Phosphate ester synthesis. Step II: Acylate intermediate synthesis. Step III: Neutralization (Batch 50B) and Variant with DMS (Batch 50A).",
  "observations": "Step-I: Clear mass, No particles\nStep-II: Slowly from a... (OCR incomplete)\n50B: Clear Mass, No foam, No turbidity\n50A: Clear yellowish Mass, Clear Uniform Mass, Slight Turbidity\n\nStep I: Clear mass, No particles, HV - 52.5, mono - 23.5, Dioctyl - 53.2, Free Acid - 0.1.\nStep II: Slowly from a... (text cut off).\nStep III (50B): Clear Mass, No foam, No turbidity, AV - 44.14, Amine - 47.\nStep III (50A): Clear Uniform Mass, Slight Turbidity, AV - 48.7, Amine - 31.08.\n\nCharged LUB 1010 301 gm. Feed of P205 - 15.82 Over 10-12\nClear mass., No particles.\nCharged SP-18.\nFeed of 2-Ethyl hexyl Acylate / 2 hrs.\nSlowly from a...\nCharged - Acylate Intermediate 20g\nFeed of phosphate Ester 80g / 10-12 min\nClear Mass / No foam, No turbidity\nCharged Acylate, Feed of DMS (1:1) over 15 min.\nClear yellowish Mass\nFeed of phosphate Ester 30 min\nClear Uniform Mass, Slight Turbidity.\n\nExpt Table remarks: Clear mass no particles; Mono-23.5 / Di- 53.2/ Free acid-0.1; P-1.71 %; Feed of phosphate ester; IV-26.1  @ 5.5 hrs; Stirrer well , clear \ntransparent mass; Yellowish clear \ntransparent mass; B.No-50 A; 1.5 hr clear yellowish mass; 3 hr/ Clear uniform mass\nSlight turbidity; Tested on Black & violet pigment \nResolubility less while other parameters nearby",
  "process_steps": [
    {
      "name": "Step-I Phosphate Ester",
      "process": [
        {
          "time": "0.5",
          "temperature": "RT-50 / N2",
          "observation": "Charged LUB 1010 301 gm. Feed of P205 - 15.82 Over 10-12"
        },
        {
          "time": "2.5",
          "temperature": "75-78 / N2 -",
          "observation": "Clear mass., No particles."
        }
      ],
      "measurements": [
        {
          "verbatim": "HV - 52.5"
        },
        {
          "verbatim": "mono - 23.5"
        },
        {
          "verbatim": "Dioctyl - 53.2"
        },
        {
          "verbatim": "Free Acid - 0.1"
        }
      ],
      "step": 1,
      "materials": {}
    },
    {
      "name": "Step-II Acylate Intermediate",
      "process": [
        {
          "time": "0.5",
          "temperature": "78-81 / N2",
          "observation": "Charged SP-18."
        },
        {
          "time": "2 hrs",
          "temperature": "78-80 / N2",
          "observation": "Feed of 2-Ethyl hexyl Acylate / 2 hrs."
        },
        {
          "time": "5.5 hrs",
          "temperature": "78-80 / N2",
          "observation": "Slowly from a..."
        }
      ],
      "step": 2,
      "materials": {}
    },
    {
      "name": "Step-III Neutralisation (B. NO - 50B)",
      "process": [
        {
          "time": "0.5",
          "temperature": "55-57 / N2",
          "observation": "Charged - Acylate Intermediate 20g"
        },
        {
          "time": "0.5",
          "temperature": "55-57 / N2",
          "observation": "Feed of phosphate Ester 80g / 10-12 min"
        },
        {
          "time": "2.5",
          "temperature": "55-57 / N2",
          "observation": "Clear Mass / No foam, No turbidity"
        }
      ],
      "measurements": [
        {
          "verbatim": "AV - 44.14"
        },
        {
          "verbatim": "Amine - 47"
        }
      ],
      "step": 3,
      "materials": {}
    },
    {
      "name": "B. NO - 50A",
      "process": [
        {
          "time": "0.5",
          "temperature": "55-58 / N2, 65-70",
          "observation": "Charged Acylate, Feed of DMS (1:1) over 15 min."
        },
        {
          "time": "1.5 hrs",
          "temperature": "70-75 / N2",
          "observation": "Clear yellowish Mass"
        },
        {
          "time": "0.5 hrs.",
          "temperature": "55-62 / N2",
          "observation": "Feed of phosphate Ester 30 min"
        },
        {
          "time": "3 hrs.",
          "temperature": "58-62 / N2",
          "observation": "Clear Uniform Mass, Slight Turbidity."
        }
      ],
      "measurements": [
        {
          "verbatim": "AV - 48.7"
        },
        {
          "verbatim": "Amine - 31.08"
        }
      ],
      "step": 4
    },
    {
      "step": 1,
      "materials": [
        {
          "name": "i) Vicaspin LUB 1010 (R225100845) Bu- EO-PO\nHV-62.3/ MW-900",
          "quantity_g": 301,
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "time_h": "0.2",
          "action": "react",
          "verbatim": "45 °C, 0.2 h",
          "temperature": "45"
        }
      ],
      "conditions": {
        "time_h": "0.2",
        "temperature": "45"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "2.14",
          "unit": "%",
          "verbatim": "P-2.14%"
        }
      ],
      "remarks": "Clear mass no particles"
    },
    {
      "step": 2,
      "materials": [
        {
          "name": "i)  Epomine SP- 018",
          "quantity_g": 30,
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "time_h": "0.2",
          "action": "react",
          "verbatim": "80 °C, 0.2 h",
          "temperature": "80"
        }
      ],
      "conditions": {
        "time_h": "0.2",
        "temperature": "80"
      },
      "results": [
        {
          "parameter": "unlabelled",
          "value": "23.5",
          "verbatim": "Mono-23.5"
        },
        {
          "parameter": "unlabelled",
          "value": "53.2",
          "verbatim": "Di- 53.2"
        },
        {
          "parameter": "free_acid",
          "value": "0.1",
          "verbatim": "Free acid-0.1"
        }
      ],
      "remarks": ""
    },
    {
      "step": 3,
      "materials": [
        {
          "name": "B.No- 50B\nStep - 1 Product\nPhosphate ester",
          "quantity_g": 0.8,
          "role": "intermediate"
        },
        {
          "name": "5.5",
          "role": "unknown",
          "note": "Stray value outside the fixed columns, kept verbatim; role unknown"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "action": "react",
          "verbatim": "79-81",
          "temperature": "79-81"
        },
        {
          "seq": 2,
          "time_h": "3.5",
          "action": "feed phosphate ester",
          "verbatim": "3.5, Feed of phosphate ester"
        }
      ],
      "conditions": {
        "temperature": "79-81"
      },
      "results": [
        {
          "parameter": "phosphorus",
          "value": "1.71",
          "unit": "%",
          "verbatim": "P-1.71 %"
        },
        {
          "parameter": "acid_value",
          "value": "44.14",
          "verbatim": "AV-44.14"
        },
        {
          "parameter": "amine",
          "value": "47.1",
          "verbatim": "Amine-47.1"
        },
        {
          "parameter": "iodine_value",
          "value": "4.9",
          "verbatim": "IV-4.9"
        },
        {
          "parameter": "saponification_value",
          "value": "84.29",
          "verbatim": "SAP-84.29"
        },
        {
          "parameter": "viscosity_HV",
          "value": "58.5",
          "verbatim": "HV-58.5"
        },
        {
          "parameter": "iodine_value",
          "value": "26.1",
          "verbatim": "IV-26.1  @ 5.5 hrs",
          "note": "time-point reading at 5.5 hrs, kept as stray reading"
        }
      ],
      "remarks": "Stirrer well , clear \ntransparent mass; Yellowish clear \ntransparent mass"
    },
    {
      "step": 4,
      "materials": [
        {
          "name": "i) Acrylate (15%)",
          "quantity_g": 37.5,
          "role": "reactant"
        },
        {
          "name": "ii) DMS (1%)",
          "quantity_g": 2.52,
          "role": "reactant"
        },
        {
          "name": "iii)   Phosphate ester- (85%)",
          "quantity_g": 212.5,
          "role": "reactant"
        }
      ],
      "procedure": [
        {
          "seq": 1,
          "time_h": "0.2",
          "action": "react",
          "verbatim": "65-70, 0.2",
          "temperature": "65-70"
        },
        {
          "seq": 2,
          "action": "feed DMS",
          "verbatim": "Feed over 15 min"
        },
        {
          "seq": 3,
          "time_h": "1.5",
          "action": "react",
          "verbatim": "70-75, 1.5 hr clear yellowish mass",
          "temperature": "70-75"
        },
        {
          "seq": 4,
          "time_h": "0.5",
          "action": "feed",
          "verbatim": "55-62, 0.5 hr feed of RM-III",
          "temperature": "55-62"
        },
        {
          "seq": 5,
          "time_h": "3",
          "action": "react",
          "verbatim": "58-62, 3 hr/ Clear uniform mass Slight turbidity",
          "temperature": "58-62"
        }
      ],
      "conditions": {
        "time_h": "0.2 / 1.5 / 0.5 / 3",
        "temperature": "65-70 / 70-75 / 55-62 / 58-62"
      },
      "results": [
        {
          "parameter": "acid_value",
          "value": "48.7",
          "verbatim": "AV-48.7"
        },
        {
          "parameter": "amine",
          "value": "31.08",
          "verbatim": "amine-31.08"
        },
        {
          "parameter": "iodine_value",
          "value": "4.58",
          "verbatim": "IV-4.58"
        },
        {
          "parameter": "saponification_value",
          "value": "88.4",
          "verbatim": "SAP-88.4"
        },
        {
          "parameter": "viscosity_HV",
          "value": "45.5",
          "verbatim": "HV-45.5"
        }
      ],
      "remarks": "B.No-50 A; Tested on Black & violet pigment \nResolubility less while other parameters nearby"
    }
  ]
}