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Sheet · 28112025 9076 Expt Table 2025.converted_sheet_9076_Experiments.csv — rows 2–151 of 400 · cited row highlighted


Batch No	Step 1							Step 2						Step 3					Remarks
	Raw Materials		Reaction Conditions			Results		Raw Materials		Reaction Conditions			Results	Raw Materials		Reaction Conditions
	Name	Qty (g)	Temp. oC	Time (h)	Vac / N2	A.V.	Other	Name	Qty (g)	Temp. oC	Time (h)	Vac / N2	A.V.	Name	Qty (g)	Temp. oC	Time (h)	Vac / N2
1	STD BYK 9076
2	MPEG-350	300	35\n55\n75\n\n	0.15\n0.5\n1-2 \n\n	N2	41	During feeding of P-RM found slight exotherm Very fine yellow tincture found ,\n slight grip in viscosity found,	Step 1- Product	152	35\n55\n60	0.15\n1\n2	N2	AV- 40, \nAmine value- 45						For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5
	Phosphorous pentaoxide	9.9						Lupasol G-20 WF	11
							Initially found brownish dots with exotherm later on changed to pale yellow.\nIn Final product added -EHA/ Toluene/ Methoxy propyl acetate 3.33% each( by weight %)												For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5
3	MPEG-350	150	35	0.15
	Tripropylene glycol mono-butyl ether	150	55	1	N2	55		Step- 1 product	152	40	0.5	N2	AV-48\n
	Phosphorous pentaoxide	13.2	60	2				Lupasol G-20 WF	13.8	65	2		Amine value-42
							During feeding found slight exotherm ,\nVery fine yellow tincture found , slight grip in viscosity found
4	Vicasurf -1010	250	40	0.15				Step- 1 product	150	45	0.5	N2	AV-53
	Butanol- 2 EO-2PO	50	55	0.5	N2	53		Lupasol G-20 WF	13.5	65	2.5		Amine value-42
	Phosphorous pentaoxide	15	75	1 hr-2 hr
							During feeding found slight exotherm ,\nslight grip in viscosity with distinct turbidity( Not like sunflower oil)												For Carbon black pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink removal Batch 2=3<4<5
5	Vicasurf -1010	300	40	0.15				Step- 1 product	152	40	0.5	N2	AV-38
	Phosphorous pentaoxide	10.2	55	0.5	N2	38		Lupasol G-20 WF	7.5	70	2		Amine value- 19
			75	1 hr-2 hr
							Exotherm found while feed , moderate viscosity
6	Vicasurf -1010	150	40	0.5				Step- 1 product	170	40	0.5	N2	AV-38
	Butanol- 2 EO-2PO	150	80	3.5	N2	42		Lupasol G-20 WF	7.8	70	3		Amine value- 19
	Phosphorous pentaoxide	10.6
																			For Carbon black/ Red/ White pigment-Gloss, Tinting strength, Shade good \nhaving adhesion dots while cleaning Ink
7	Vicasurf -1010	200	40	0.5	N2	19		Step- 1 product	200	45	0.5	N2	AV-19
	Phosphorous pentaoxide	5.2	75	3			Slight exotherm while feeding ,\nAppearance- viscous good flow, found particles	Lupasol G-20 WF - 2EO- 2 PO	9.6	70	3		Amine value- 42
							Found exotherm and and slight turbidity!
8	Vicasurf -1010	300	40	0.5				Step- 1 product	300	40	0.5	N2	AV-35
	Phosphorous pentaoxide	10.5	75	3	N2	36.5		Lupasol G-20 WF	7.5	75	3		Amine value- 14

9- I	Batch -8 Step-II	95	45	2
	5% Polymer (Bondex - Jeson polymer emulsion - Upon water removal)	5	50	1	N2	AV-40.5\nAmine value-13	Viscous transparent mass, less flowability\n than reference sample. AV-40.5
9- II	Batch -8 Step-II	90	45	2	N2														Tested on Red pigment found\n better result than earlier and very finely inferior than standard(5% less) while other parameters gloss, tinting sterngth good.
	5% Polymer (Bondex - Jeson polymer emulsion - Upon water removal)	10	50	1	N2	AV- 39.2\nAmine value-12.1	more Viscous less transparent mass, very less flowability than reference sample.\nAV-39.2\nadded -EHA/ Toluene/ Methoxy propyl acetate 3.33% each( by weight %)
10	Vicasurf -1010 (HV-115-120)	230	60	1			Clear reaction mass, \nno charing/residue in mass	Epomine SP- 018	105	68	2			Step 1- product -80	248 gm %	60	0.5		Initial feed of Step 10 B slowly\n found clear transparent mass ( still 20%) then slowly\n increased turbidity. Upon total feed reaction mass became viscous non flowable yellowish white mass.\nAV-55
	Polyphosphpric acid	15.2	75	3	N2	183		2 ethyl hexyl acrylate	245	78	4	N2	257	Step-2 Product -20%	62 gm %	62	3
																			Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product.
11	Vicasurf -1010 (HV-115-120)	300	40	0.15				Epomine SP- 018	105	68	2\n			Step- 1 product (80)	160	60	1		AV-36.7
	Phosphorous pentaoxide	10.5	55	0.5	N2	38		2 ethyl hexyl acrylate	245	78	4	N2	257	Step - 2 Product (20)	40	65	3	N2	Amine value- 37
			75	1 hr- 2 hr

12	Butanol EO - ( Unitop- 25.05.23)	184	60	1				Epomine SP- 018	105	68	2\n			Step- 1 product (80)	160	60	1		AV-38.9
	Polyphosphpric acid	15.2	62	3	N2	99		2 ethyl hexyl acrylate	245	78	4	N2	215	Step - 2 Product (20)	40	65	3	N2	Amine value-36

13	Butanol EO - 150 gm ( Unitop- Dated 25.05.23)	150	70	1				Epomine SP- 018	105	68	2		Amine-215	Step- 1 product (80)	160	60	1		AV-32
	Phosphorous pentaoxide	4.4	75	3	N2	34		2 ethyl hexyl acrylate	245	78	4	N2		Step - 2 Product (20)	40	65	3	N2	Amine value-33

14	Vicasurf 1010 (HV-115-120)	300	60	1				Epomine SP- 018	105	68	2		Amine-224	Step- 1 product (80)	160	60	1		Tested sample and found good results likely resolubility/ tinting strenghth/ gloss etc. with respect to reference product.\nAV-37.6 \nAmine- 35.3
	Phosphorous pentaoxide	9.5	80	4	N2	33		2 ethyl hexyl acrylate	245	78	4	N2		Step - 2 Product (20)	40			N2

15	Vicasurf 1010 (HV-115-120)	970	60	1				Epomine SP- 018	129.5	68	2			Step- 1 product (80)	200	65	1
	Phosphorous pentaoxide	35.45	80	3	N2	38.3		2 ethyl hexyl acrylate	302.16 \n(0.001 % Hydroquinone)	78	5	N2	Amine 209	Step - 2 Product (20)	800	75	2	N2	AV-34.2

16	Vicasurf 1010 (HV-115-120)	970	55	1				Epomine SP- 018	129.5	68	2			Step- 1 product (80)	200	65	1		While feeding of acrylate stirring off for 2 min, more viscous ,
	Phosphorous pentaoxide	34.2	80	3	N2	37.8		2 ethyl hexyl acrylate	302.16	78-80	8	N2	Amine-210	Step - 2 Product (20)	800	75	2	N2	Application test slightly\n inferior to reference product.\nAV-36.7\n Amine-34.8

17	Vicasurf 1010 (HV-115-120)	450	65	2 hrs	N2	AV-44\n		Epomine SP- 018	60	75	2 hrs		amine - 263/	Step- 1 product (78)	78	60	2 hrs		AV-41.5/ SAP- 80
	Polyphosphoric acid	16.18	75	3.5 hrs		Final AV-48 \nSAP-81/ HV-120		2 ethyl hexyl acrylate	140	80	4.5 hrs	N2	SAP- 197/\n HV-170/IV-42	Step - 2 Product (20)	20	65	5 hrs	N2	IV-12/HV-136.5/ \nAmine value-42.195

18	Butanol EO/PO BEP-55 (110 gm HV-88) Unitop RM	110	60	1 hrs		47		Step-1 Product	110	58	1 hr		AV-37
	Phosphorous pentaoxide	2.53	65	4 hrs	N2			Lupasol G-20 WF	5.2	61	3 hr	N2	Amine value-29/

19	Vicasurf 1010 (HV-115-120)	300	40	0.15				Step-1 Product	50
	Phosphorous pentaoxide	10.5	55	0.5				Lupasol G-20 WF	2	55	2		Amine-35
			75	2 hrs	N2	38		LLP ( Liquid paraffin ) 0.2 gm	0.2			N2	AV-32

20	Butanol EO - PO\nHV-56	226	45	0.7										Step- 1 product (80)	160	60	6	N2	AV-35.6\nAmine-14
	Phosphorous pentaoxide	8.24	68-75	4.5	N2	37		Epomine SP- 018	90	80-82	6			Step - 2 Product (20)	40
								2 ethyl hexyl acrylate	210	80-83	2	N2	Amine-259
																			Amine-40.56
																			AV-42.56
21	Butanol EO - PO - 300 gm (Sunshield)\nHV-56	300	40	1				Epomine SP- 018	90	80-82	6			Step- 1 product (80)	160	60	605		Strength/gloss for \nC black good/ Resolubility issue
	Phosphorous pentaoxide	13.7	65-75	4.5	N2	AV-46.86		2 ethyl hexyl acrylate	210	80-83	2	N2	256	Step - 2 Product (20)	40			N2
								Iodine Value	Time
								70	2
								37.2	5.5

	Solvent Blend
	LBN 21A) LBN 21 +3% AMP
	LBN 21B) LBN 21 +2% IPA
	LBN 21 C) LBN21 A + 2% mix xylene

	Solvent Blend
	LBN 21D) LBN 21 +4% mix xylene
	LBN 21E) LBN 21D +1% MIBK
	LBN 21F) LBN 21 +2% ethyl cellosolve


22	BEP (1450) - (Esteem indusry)	150	50	0.5				Step- 1 product	157				43.7
	Phosphorous pentaoxide	7.09	70-75	5	N2	42		Epoimine SP-018 -	4.9 gm	60	4.5	N2

	Solvent Blend
	LBN 22 A) LBN 22 + 2 ethyl hexyl acrylate 3% + Xylene 1.44 % + MPA 0.6%+2 ethyl hexanol - 1.4 %
23
	Sun Surfol R-1400- \nHV-56	1010	45-50	0.5				Epomine SP- 018	90	75-81	2			Step- 1 product (80)	800				Strength/gloss for \nC black good/ Resolubility issue\ni) With 3% MPA solvent and ii) without solvent
	Phosphorous pentaoxide	47.16	70-75	4.5	N2	49.5		2 ethyl hexyl acrylate	210	78-82	6	N2	AV-1.1/ Amine 256\n/IV-37.2	Step - 2 Product (20)	200	60	4	N2
								Iodine value	Time										AV-42.67/amine-39.8/HV-55.32\n/SAP-63.5/IV-7.22
								49	4
								37.2	5.5

24A	Sun Surfol R-1400- \nHV-56	1010	45-50	0.5				Epomine SP- 018	90	77-81	2			Step- 1 product (85)	106.25	60	4		Pigment Green- Strength / Gloss inferior\nPigment Black & Red- All properties good.
	Phosphorous pentaoxide	47.16	70-75	4.5	N2	49.5		2 ethyl hexyl acrylate	210	78-82	6	N2	AV-1.1/ Amine 256\n/IV-37.2	Step - 2 Product (15)	18.75			N2	AV-53/Amine-29.5/\n HV-65/SAP-85.9/IV-6.5
									Iodine value	Time
									49	4
									37.2	5.5

24B	Sun Surfol R-1400- HV-56	112	45-50	0.5				Epomine SP- 018	90	77-81	2			Step- 1 product (85)	106.25
	Phosphorous pentaoxide	4.5	70-75	4.5	N2	46.34		2 ethyl hexyl acrylate	210	78-82	6	N2	AV-0.3/\n Amine 260/IV-34.5	Step - 2 Product (15)	18.75	60	4	N2	Pigment Green- Strength / Gloss inferior\nPigment Black, Red, Violet, Blue - All properties good.
								Iodine value	Time										AV-37.97/\nAmine-27.8/HV-83/IV-5.
								62.2	2
								46.5	4
								35.6	5

24 C	Sun Surfol R-1400- HV-58	450	45-50	0.5		AV- 39.8	Yellowish floable liq AV adjusted to 39.8\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.8)	Epomine SP- 018	90	74-82	2			Step- 1 product (85)	170	58-60	Feed 20 min		Pigment Black, Red, Green, Blue - All properties good
	Phosphorous pentaoxide	22.03	70-75	4.5	N2		Phosphate ester- Mono- 12/ Di- 75/\nFree acid- 0.3	2 ethyl hexyl acrylate	210	78-82	6	N2	AV- 0.2 \n / Amine - 265 \n /IV-34.5	Step - 2 Product (15)	30	60	4	N2	Pigment Green/ Violet - Strength / Gloss inferior
									Iodine value	Time									AV- 35.56 \n /Amine-29.79
									62.2	2
									46.5	4
									35.6	5


24 CR	Sun Surfol R-1400- HV-58	850	45-50	0.5			Yellowish floable liq AV adjusted to 39.8\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.8)	Epomine SP- 018	90	74-82	2			Step- 1 product (85)	483		feed 25 min		Pigment Black, Red, Orange, \nyellow, white Blue - All properties good
	Phosphorous pentaoxide	39.5	70-75	4.5	N2	39.8	Phosphate ester- Mono- 12/ Di- 75/\nFree acid- 0.3	2 ethyl hexyl acrylate	210	78-82	6	N2	AV- 0.2 \n / Amine -265/ IV-34.5	Step - 2 Product (15)	85.23	60	4	N2	AV- 35.43 \n /Amine-31.1
									Iodine value	Time
									35.6	5

24 CR2	Sun Surfol R-1400- HV-58	1700	45-50	0.5				Epomine SP- 018	150	74-82	2			Step- 1 product (85)	1700	55-58	35 min
	Phosphorous pentaoxide	68.77	70-75	4.5	N2	39.7	Yellowish floable liq AV adjusted to 39.7\n(180 gmAV-46.6+37.3 gm R-1400 to AV-39.7)	2 ethyl hexyl acrylate	350	78-82	6	N2	AV- 0.2 \n / Amine -255 \n /IV-34	Step - 2 Product (15)	300	58-60	4	N2	AV- 35.25 \n /Amine-30.9
								Iodine value	Time
							Phosphate ester- Mono- 08/ Di- 81/\nFree acid- 0.25	70	2
								56	4
								35	5.5

25- I	Sun Surfol R-1400- HV-56	160	35	0.5			Phosphate ester- Mono- 9.7/ Di-40.16/\nFree acid- 0.29	Epomine SP- 018	150	74-82	2			Step- 1 product (80)	80	60	Feed 2 hrs
	Polyphosphoric acid \n(AV-46 matching)	5.714	55-60	4.5	N2	46		2 ethyl hexyl acrylate	350	78-82	6	N2	AV- 0.2 \n / Amine -255 \n /IV-34	Step - 2 Product (20)	20	60	4	N2	Found turbid mass/non uniform
									Iodine value	Time
									70	2
									56	4
									35	5.5

25-II	Sun Surfol R-1400- HV-56	150	40	0.5				Epomine SP- 018	150	74-82	2			Step- 1 product (80)	80	60	Feed 2 hrs		AV-98.65
	Polyphosphoric acid \n(Quantity as per patent)	12.39	55-60	4.5	N2	115		2 ethyl hexyl acrylate	350	78-82	6	N2	AV- 0.2 \n / Amine -255 \n /IV-34	Step - 2 Product (20)	20	60	4	N2	Amine -32.18\nIR PPA/P2O5 matching (mailed)
								Iodine value	Time										after 2 hr found turbid mass/non uniform
								70	2
								56	4
								35	5.5

25-A	Sun Surfol R-1400- HV-56	100	40	0.5				Epomine SP- 018	150	74-82	2			Step- 1 product (80)	80	60	Feed 2 hrs
	PPA:P2O5 (20:80)	1.071 \ngm :1.98gm	55-60	4.5	N2	45.75	Phosphate ester- Mono- 14.5/ Di-61.37/\nFree acid- 0.42	2 ethyl hexyl acrylate	350	78-82	6	N2	AV- 0.2 \n / Amine -255 \n /IV-34	Step - 2 Product (20)	20	60	4	N2	After 2 hr feed slight turbidity /yellowish flowable liq
								Iodine value	Time										AV-37.69\nAmine-40.72
								70	2

Extracted values

… checked

Cited: sheet 9076_Experiments, batch block '37 A', csv rows 5-11 (highlighted). Compare with the original on the left. Press Enter to OK the highlighted value, or click OK / fix on any value. Experiment: exp-9076-037A

Process steps medium check every value

Step

Charged

What happened

Results

Step 1

temperature ramp 54 / 56 / 68 / 55 / 55 / 75 (N2) / 55 / 75 (N2) atmosphere N2 time_h 0.5 h / 1 h / 1.5 h / 10 min / 5 min / 1.5 hr / 10 min / 1.5 hrs

i) Surfol R-1400 HV-59 (R-53/07032024) · 250

role reactant · verbatim i) Surfol R-1400 HV-59 (R-53/07032024), 250

ii) PolyPhosphoric acid ( 102 %) · 4.201

role reactant · verbatim ii) PolyPhosphoric acid ( 102 %), 4.201

ii) Phosphorous pentaoxide · 3.44

role reactant · verbatim ii) Phosphorous pentaoxide, 3.44

#	Time	Temp	What happened
1	0.5	54	verbatim 54 / 0.5
2	1	56	verbatim 56 / 1
3	1.5	68	verbatim 68 / 1.5
4	10 min	55 deg	verbatim 55 deg / 10 min
5	5 min	55 deg	verbatim 55 deg / 5 min
6	1.5 hr	75 deg N2	verbatim 75 deg N2 / 1.5 hr
7	10 min	55 deg	verbatim 55 deg / 10 min
8	1.5 hrs	75 deg N2	verbatim 75 deg N2 / 1.5 hrs

acid_value 40.25

verbatim AV-40.25

Step 2

temperature 68-70, 68-72, 68-72 atmosphere N2 time_h 0.15 h, 1.15 hr feed, 3.5 h

i) Epomine SP- 018 · 60

role reactant · verbatim i) Epomine SP- 018, 60gm

ii) Toluene · 190 ml

role solvent · verbatim ii) Toluene, 190 ml

iii) AIBN catalyst · 0.4

role catalyst · verbatim iii) AIBN catalyst, 0.4 gm

iv) 2 ethyl hexyl acrylate · 140

role reactant · verbatim iv) 2 ethyl hexyl acrylate, 140 gm

v) AIBN catalyst · 0.64

role catalyst · verbatim v) AIBN catalyst, 0.64 gm

#	Time	Temp	What happened
1	0.15	68-70	note Stirrer well and disperse amine · verbatim 68-70 / 0.15 / Stirrer well and disperse amine
2	1.15 hr feed	68-72	note Feed; N2 · verbatim 68-72 / 1.15 hr feed / Feed / N2
3	3.5	68-72	note Initially turbid; After 1 hr clear mass; N2 · verbatim 68-72 / 3.5 / Initially turbid After 1 hr clear mass / N2

iodine_value 13.2

verbatim IV-13.2

Step 3

temperature 56-57 deg, 56-57, 56-59 deg, RT atmosphere N2 time_h 10 min, 35 min, 2 hr

Step - 1 Product · 160

pct 80% · role intermediate · verbatim Step - 1 Product, 160 (80%)

Step - 2 Product · 40

pct 20% · role intermediate · verbatim Step - 2 Product ,40 (20%)

Step- I RM

role reactant · verbatim Step- I RM, 56-57 deg, Stirrer 10 min/N2

Feed RM Step-2

role reactant · verbatim Feed RM Step-2, 56-57 , 35 min slowly

#	Time	Temp	What happened
1	10 min	56-57 deg	note Stirrer 10 min/N2 · verbatim 56-57 deg / Stirrer 10 min/N2
2	35 min	56-57	note 35 min slowly; Feed RM Step-2 · verbatim 56-57 , 35 min slowly
3	2 hr	56-59 deg	note 2 hr/ N2 · verbatim 56-59 deg, 2 hr/ N2
4		RT	note Cool to RT · verbatim Cool to RT

—

[
  {
    "conditions": {
      "atmosphere": "N2",
      "temperature": "ramp 54 / 56 / 68 / 55 / 55 / 75 (N2) / 55 / 75 (N2)",
      "time_h": "0.5 h / 1 h / 1.5 h / 10 min / 5 min / 1.5 hr / 10 min / 1.5 hrs"
    },
    "materials": [
      {
        "name": "i) Surfol R-1400 HV-59  (R-53/07032024)",
        "qty_g": "250",
        "role": "reactant",
        "verbatim": "i) Surfol R-1400 HV-59  (R-53/07032024), 250"
      },
      {
        "name": "ii) PolyPhosphoric acid ( 102 %)",
        "qty_g": "4.201",
        "role": "reactant",
        "verbatim": "ii) PolyPhosphoric acid ( 102 %), 4.201"
      },
      {
        "name": "ii) Phosphorous pentaoxide",
        "qty_g": "3.44",
        "role": "reactant",
        "verbatim": "ii) Phosphorous pentaoxide, 3.44"
      }
    ],
    "procedure": [
      {
        "seq": 1,
        "temperature": "54",
        "time_h": "0.5",
        "verbatim": "54 / 0.5"
      },
      {
        "seq": 2,
        "temperature": "56",
        "time_h": "1",
        "verbatim": "56 / 1"
      },
      {
        "seq": 3,
        "temperature": "68",
        "time_h": "1.5",
        "verbatim": "68 / 1.5"
      },
      {
        "seq": 4,
        "temperature": "55 deg",
        "time_h": "10 min",
        "verbatim": "55 deg / 10 min"
      },
      {
        "seq": 5,
        "temperature": "55 deg",
        "time_h": "5 min",
        "verbatim": "55 deg / 5 min"
      },
      {
        "seq": 6,
        "temperature": "75 deg N2",
        "time_h": "1.5 hr",
        "verbatim": "75 deg N2 / 1.5 hr"
      },
      {
        "seq": 7,
        "temperature": "55 deg",
        "time_h": "10 min",
        "verbatim": "55 deg / 10 min"
      },
      {
        "seq": 8,
        "temperature": "75 deg N2",
        "time_h": "1.5 hrs",
        "verbatim": "75 deg N2 / 1.5 hrs"
      }
    ],
    "remarks": "",
    "results": [
      {
        "parameter": "acid_value",
        "value": "40.25",
        "verbatim": "AV-40.25"
      }
    ],
    "step": 1
  },
  {
    "conditions": {
      "atmosphere": "N2",
      "temperature": "68-70, 68-72, 68-72",
      "time_h": "0.15 h, 1.15 hr feed, 3.5 h"
    },
    "materials": [
      {
        "name": "i)  Epomine SP- 018",
        "qty_g": "60",
        "role": "reactant",
        "verbatim": "i)  Epomine SP- 018, 60gm"
      },
      {
        "name": "ii) Toluene",
        "qty_g": "190 ml",
        "role": "solvent",
        "verbatim": "ii) Toluene, 190 ml"
      },
      {
        "name": "iii) AIBN catalyst",
        "qty_g": "0.4",
        "role": "catalyst",
        "verbatim": "iii) AIBN catalyst, 0.4 gm"
      },
      {
        "name": "iv)   2 ethyl hexyl acrylate",
        "qty_g": "140",
        "role": "reactant",
        "verbatim": "iv)   2 ethyl hexyl acrylate, 140 gm"
      },
      {
        "name": "v)  AIBN catalyst",
        "qty_g": "0.64",
        "role": "catalyst",
        "verbatim": "v)  AIBN catalyst, 0.64 gm"
      }
    ],
    "procedure": [
      {
        "note": "Stirrer well and disperse amine",
        "seq": 1,
        "temperature": "68-70",
        "time_h": "0.15",
        "verbatim": "68-70 / 0.15 / Stirrer well and disperse amine"
      },
      {
        "note": "Feed; N2",
        "seq": 2,
        "temperature": "68-72",
        "time_h": "1.15 hr feed",
        "verbatim": "68-72 / 1.15 hr feed / Feed / N2"
      },
      {
        "note": "Initially turbid; After 1 hr clear mass; N2",
        "seq": 3,
        "temperature": "68-72",
        "time_h": "3.5",
        "verbatim": "68-72 / 3.5 / Initially turbid After 1 hr clear mass / N2"
      }
    ],
    "remarks": "",
    "results": [
      {
        "parameter": "iodine_value",
        "value": "13.2",
        "verbatim": "IV-13.2"
      }
    ],
    "step": 2
  },
  {
    "conditions": {
      "atmosphere": "N2",
      "temperature": "56-57 deg, 56-57, 56-59 deg, RT",
      "time_h": "10 min, 35 min, 2 hr"
    },
    "materials": [
      {
        "name": "Step - 1 Product",
        "pct": "80%",
        "qty_g": "160",
        "role": "intermediate",
        "verbatim": "Step - 1 Product, 160 (80%)"
      },
      {
        "name": "Step -  2 Product",
        "pct": "20%",
        "qty_g": "40",
        "role": "intermediate",
        "verbatim": "Step -  2 Product ,40 (20%)"
      },
      {
        "name": "Step- I RM",
        "role": "reactant",
        "verbatim": "Step- I RM, 56-57 deg, Stirrer 10 min/N2"
      },
      {
        "name": "Feed RM Step-2",
        "role": "reactant",
        "verbatim": "Feed RM Step-2, 56-57 , 35 min slowly"
      }
    ],
    "procedure": [
      {
        "note": "Stirrer 10 min/N2",
        "seq": 1,
        "temperature": "56-57 deg",
        "time_h": "10 min",
        "verbatim": "56-57 deg / Stirrer 10 min/N2"
      },
      {
        "note": "35 min slowly; Feed RM Step-2",
        "seq": 2,
        "temperature": "56-57",
        "time_h": "35 min",
        "verbatim": "56-57 , 35 min slowly"
      },
      {
        "note": "2 hr/ N2",
        "seq": 3,
        "temperature": "56-59 deg",
        "time_h": "2 hr",
        "verbatim": "56-59 deg, 2 hr/ N2"
      },
      {
        "note": "Cool to RT",
        "seq": 4,
        "temperature": "RT",
        "verbatim": "Cool to RT"
      }
    ],
    "remarks": "",
    "results": [],
    "step": 3
  }
]

observations medium check against source

Expt Table remarks: Stirrer well and disperse amine; Feed; Initially turbid After 1 hr clear mass; PPA feed; P2O5 added; Clear mass; Clear brownish tint; IV-13.2; AV-; Stirrer; Cool to RT Clear yellowish transparent mass

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History (1)

Action	Field	Value	Date
verify			2026-08-20

Raw fragment JSON

{
  "fragment_id": "expt-block--37a",
  "source_file": "docs/Project Expt Report/28112025  9076 Expt Table 2025.xls",
  "derived_from": "ocr/28112025  9076 Expt Table 2025.converted/28112025  9076 Expt Table 2025.converted_sheet_9076_Experiments.csv",
  "locator": "sheet 9076_Experiments, batch block '37 A', csv rows 5-11",
  "extractor": "qwen-tasks/extract-expt-block.md",
  "target_aliases": [
    "37 A"
  ],
  "document_role": "summary_table",
  "payload": {
    "record_type": "synthesis",
    "process_steps": [
      {
        "step": 1,
        "materials": [
          {
            "name": "i) Surfol R-1400 HV-59  (R-53/07032024)",
            "qty_g": "250",
            "role": "reactant",
            "verbatim": "i) Surfol R-1400 HV-59  (R-53/07032024), 250"
          },
          {
            "name": "ii) PolyPhosphoric acid ( 102 %)",
            "qty_g": "4.201",
            "role": "reactant",
            "verbatim": "ii) PolyPhosphoric acid ( 102 %), 4.201"
          },
          {
            "name": "ii) Phosphorous pentaoxide",
            "qty_g": "3.44",
            "role": "reactant",
            "verbatim": "ii) Phosphorous pentaoxide, 3.44"
          }
        ],
        "procedure": [
          {
            "seq": 1,
            "time_h": "0.5",
            "verbatim": "54 / 0.5",
            "temperature": "54"
          },
          {
            "seq": 2,
            "time_h": "1",
            "verbatim": "56 / 1",
            "temperature": "56"
          },
          {
            "seq": 3,
            "time_h": "1.5",
            "verbatim": "68 / 1.5",
            "temperature": "68"
          },
          {
            "seq": 4,
            "time_h": "10 min",
            "verbatim": "55 deg / 10 min",
            "temperature": "55 deg"
          },
          {
            "seq": 5,
            "time_h": "5 min",
            "verbatim": "55 deg / 5 min",
            "temperature": "55 deg"
          },
          {
            "seq": 6,
            "time_h": "1.5 hr",
            "verbatim": "75 deg N2 / 1.5 hr",
            "temperature": "75 deg N2"
          },
          {
            "seq": 7,
            "time_h": "10 min",
            "verbatim": "55 deg / 10 min",
            "temperature": "55 deg"
          },
          {
            "seq": 8,
            "time_h": "1.5 hrs",
            "verbatim": "75 deg N2 / 1.5 hrs",
            "temperature": "75 deg N2"
          }
        ],
        "conditions": {
          "temperature": "ramp 54 / 56 / 68 / 55 / 55 / 75 (N2) / 55 / 75 (N2)",
          "atmosphere": "N2",
          "time_h": "0.5 h / 1 h / 1.5 h / 10 min / 5 min / 1.5 hr / 10 min / 1.5 hrs"
        },
        "results": [
          {
            "parameter": "acid_value",
            "value": "40.25",
            "verbatim": "AV-40.25"
          }
        ],
        "remarks": ""
      },
      {
        "step": 2,
        "materials": [
          {
            "name": "i)  Epomine SP- 018",
            "qty_g": "60",
            "role": "reactant",
            "verbatim": "i)  Epomine SP- 018, 60gm"
          },
          {
            "name": "ii) Toluene",
            "qty_g": "190 ml",
            "role": "solvent",
            "verbatim": "ii) Toluene, 190 ml"
          },
          {
            "name": "iii) AIBN catalyst",
            "qty_g": "0.4",
            "role": "catalyst",
            "verbatim": "iii) AIBN catalyst, 0.4 gm"
          },
          {
            "name": "iv)   2 ethyl hexyl acrylate",
            "qty_g": "140",
            "role": "reactant",
            "verbatim": "iv)   2 ethyl hexyl acrylate, 140 gm"
          },
          {
            "name": "v)  AIBN catalyst",
            "qty_g": "0.64",
            "role": "catalyst",
            "verbatim": "v)  AIBN catalyst, 0.64 gm"
          }
        ],
        "procedure": [
          {
            "seq": 1,
            "time_h": "0.15",
            "note": "Stirrer well and disperse amine",
            "verbatim": "68-70 / 0.15 / Stirrer well and disperse amine",
            "temperature": "68-70"
          },
          {
            "seq": 2,
            "time_h": "1.15 hr feed",
            "note": "Feed; N2",
            "verbatim": "68-72 / 1.15 hr feed / Feed / N2",
            "temperature": "68-72"
          },
          {
            "seq": 3,
            "time_h": "3.5",
            "note": "Initially turbid; After 1 hr clear mass; N2",
            "verbatim": "68-72 / 3.5 / Initially turbid After 1 hr clear mass / N2",
            "temperature": "68-72"
          }
        ],
        "conditions": {
          "temperature": "68-70, 68-72, 68-72",
          "atmosphere": "N2",
          "time_h": "0.15 h, 1.15 hr feed, 3.5 h"
        },
        "results": [
          {
            "parameter": "iodine_value",
            "value": "13.2",
            "verbatim": "IV-13.2"
          }
        ],
        "remarks": ""
      },
      {
        "step": 3,
        "materials": [
          {
            "name": "Step - 1 Product",
            "qty_g": "160",
            "pct": "80%",
            "role": "intermediate",
            "verbatim": "Step - 1 Product, 160 (80%)"
          },
          {
            "name": "Step -  2 Product",
            "qty_g": "40",
            "pct": "20%",
            "role": "intermediate",
            "verbatim": "Step -  2 Product ,40 (20%)"
          },
          {
            "name": "Step- I RM",
            "role": "reactant",
            "verbatim": "Step- I RM, 56-57 deg, Stirrer 10 min/N2"
          },
          {
            "name": "Feed RM Step-2",
            "role": "reactant",
            "verbatim": "Feed RM Step-2, 56-57 , 35 min slowly"
          }
        ],
        "procedure": [
          {
            "seq": 1,
            "time_h": "10 min",
            "note": "Stirrer 10 min/N2",
            "verbatim": "56-57 deg / Stirrer 10 min/N2",
            "temperature": "56-57 deg"
          },
          {
            "seq": 2,
            "time_h": "35 min",
            "note": "35 min slowly; Feed RM Step-2",
            "verbatim": "56-57 , 35 min slowly",
            "temperature": "56-57"
          },
          {
            "seq": 3,
            "time_h": "2 hr",
            "note": "2 hr/ N2",
            "verbatim": "56-59 deg, 2 hr/ N2",
            "temperature": "56-59 deg"
          },
          {
            "seq": 4,
            "note": "Cool to RT",
            "verbatim": "Cool to RT",
            "temperature": "RT"
          }
        ],
        "conditions": {
          "temperature": "56-57 deg, 56-57, 56-59 deg, RT",
          "atmosphere": "N2",
          "time_h": "10 min, 35 min, 2 hr"
        },
        "results": [],
        "remarks": ""
      }
    ],
    "observations": "Expt Table remarks: Stirrer well and disperse amine; Feed; Initially turbid After 1 hr clear mass; PPA feed; P2O5 added; Clear mass; Clear brownish tint; IV-13.2; AV-; Stirrer; Cool to RT Clear yellowish transparent mass"
  },
  "field_confidence": {
    "record_type": "medium",
    "process_steps": "medium",
    "observations": "medium"
  }
}