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Name of molecule

Study Title /Project Name


Sponsor
Original Manufacturer
Study Director
Study Personnel
Test facility Management
Sample Received Date
Batch No.
Mfg. Date
Expiry Date
Laboratory Code
Study Initiated date/Date of
analysis started
Study Completion date
Report date
Study Code Number
Report Code Number

Test Facility

Sponsor Address/Customer
Name and address

Name of A.I.
Thiamethoxam
DBP

Sr. No.
1
2
4
3
5
6
7
8
9

Method No.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

Taken Weight
mg
1

Prep
mg
32.2

Pr
mg
35.7

Pr
mg
35.6

Pr
mg
35.7

Pr
mg
35.6
Pr
mg
35.7

Pr
mg
35.6
Pr
mg
35.7

Pr
mg
35.6
Boscalid
Analytical Test Report on Fenazaquin 18.3 % w/w SC (200 SC)
M/s UPL Limited, Mumbai
M/s UPL Limited, Mumbai
Mr. Iqbal Shaikh, M,Sc.
Mr. Sandeep Jagtap, M.Sc.
Kedar Deobhankar, Ph.D.
3/29/2017
BOS/R2/S1/086
11/25/2016
11/24/2018
C/1595/1
09 May 2017
07 November 2017
10 November 2017
RLS/TS/242/10/16/0011426
RLS/TS/242/10/16/0011426/2
Ross Lifescience Private Limited, Plot No. 96, Sector No. 10, PCNTDA, Bhosari, Pune -
411026, Maharashtra, India.
M/s UPL Limited., UPL House, 610 B/2, Bandra Village, Off Western Express Highway,
Bandra (East), Mumbai 400 051

Nature of Test Item


Insecticide
Internal standard

Parameter Name
Description
a.i. content, percent by mass
Moisture content, percent by mass
pH (1% solution in water)
Material insoluble in acetone, percent by mass
Acidity (as H2SO4), percent by mass
Alkalinity (as NaOH), percent by mass
Melting Point ,°C
Ash content ,percent by mass

METHODS
DESCRIPTION
ACTIVE CONTENT (WITH IS)-BY HPLC
ACTIVE CONTENT (WITH IS)-BY GC
ACTIVE CONTENT (WITHOUT IS)-BY HPLC
ACTIVE CONTENT (WITHOUT IS) BY GC
MOISTURE (WATER) CONTENT BY IS
MOISTURE (WATER) CONTENT BY CIPAC
pH CONTENT
MATERIAL INSOLUBLE IN ACETONE
ACIDITY (as H2SO4)
ALKALINITY (as NaOH)
MELTING POINT
ASH CONTENT
Container Condition
IMPURITY CONTENT BY GC

Preparation
Internal standard
mg
1

Preparation of Standard Solution


mg
32.2

Sample
Preparation of Sample solution: 1
gm
35.7

Preparation of Sample solution: 2


gm
35.6

Sample
Preparation of Sample solution: 1
gm
35.7

Preparation of Sample solution: 2


gm
35.6
Preparation of Sample solution: 3
gm
35.7

Preparation of Sample solution: 4


gm
35.6
Preparation of Sample solution: 5
gm
35.7

Preparation of Sample solution: 6


gm
35.6
GLP
Nature of Test Item Insecticide
Fungicide
Herbicide GLP

ASS guidelines CIPAC MT 46.3


Sathiyanarayanan,S. Ph.D.
NABL

DSIR

CIB&RC

GI/019

Purity
99.80
98.00 gm Volumetric flask
1 100

Specification Observation
White solid powder White solid powder
Min. 95.00 97.52
Max. 1.00 0.52
4.00-6.50 5.20 (This yellow marking
Max. 0.50 0.20 value should be linked
to Averarage or mean
Max. 0.50 0.25 average value of
respective tests)
Max. 0.50 0.15
121-125 123
Max. 2.00 1.02

Method No.
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
3.9
3.10
3.11
3.12
3.13
3.14
3.15

Preparation
Internal standard
Internal concentration Volumetric falsk Diluent IS
DDB 100 Acetonitrile 0

ation of Standard Solution


Internal concentration Volumetric falsk Diluent Dilution
DDB 100 Acetonitrile 5

Sample
ration of Sample solution: 1
Internal concentration Volumetric falsk Diluent Dilution
DDB 100 Acetonitrile 5

ration of Sample solution: 2


Internal concentration Volumetric falsk Diluent Dilution
100 Acetonitrile 5

Sample
ration of Sample solution: 1
Internal concentration Volumetric falsk Diluent Dilution
Internal concentration 100 Acetonitrile 5

ration of Sample solution: 2


Internal concentration Volumetric falsk Diluent Dilution
100 Acetonitrile 5
ration of Sample solution: 3
Internal concentration Volumetric falsk Diluent Dilution
0 100 Acetonitrile 5

ration of Sample solution: 4


Internal concentration Volumetric falsk Diluent Dilution
100 Acetonitrile 5
ration of Sample solution: 5
Internal concentration Volumetric falsk Diluent Dilution
0 100 Acetonitrile 5

ration of Sample solution: 6


Internal concentration Volumetric falsk Diluent Dilution
100 Acetonitrile 5
Test Facility Page No. 23

Before 17 April 2017 Nil GLP


17 April 2017 17 April 2020 GLP certified (Chemistry including 5 batch analyses, and

12 February 2013 11 February 2015 ISO/IEC-17025-2005 accredited (NABL) - Chemical (Certific


12 February 2015 23 September 2015 Nil
24 September 2015 23 September 2017 ISO/IEC-17025-2005 accredited (NABL) - Chemical (Certific
24 September 2017 05 December 2017 Nil
06 December 2017 05 December 2019 ISO/IEC-17025-2005 accredited (NABL) - Chemical and Bio

31 October 2011 31 March 2014 DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2


01 April 2014 31 March 2017
DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2
01 April 2017 26 June 2017 Nil
27 June 2017 31 March 2020 DSIR- recognized “in-house’ laboratory (TU/IV-RD/3310/2

25 June 2015 18 May 2017 Approved by CIB&RC for registration data generation- as per

19 May 2017 18 May 2019 Approved by CIB&RC for registration data generation- as per

For all dates Sponsored by Science and Technology Park promoted by NS

EXPERIMENTAL DETAILS
Nature of Study Container Content Compatibility
Date of initiation of study
Period of study proposed 28 days
Control container Glass
Type of container for study

Pack Container
MS Drum IS 2552 -1989

MS Drum IS 2552 -1989


LDPE Pouches IS 2508-1984
HDPE bottles IS 9754 - 1981
Fiber bord Drum IS 7601 - 1983
Aluminium Container IS 9445 - 1980
HDPE Woven Sack IS 8069- 1989
Pet Bottels IS 13123 - 2000
Steel Drum IS 1783 (1) - 1993
Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50

Volumetric falsk
50
Volumetric falsk
50

Volumetric falsk
50
ng 5 batch analyses, and ecotoxicology)-GLP/C-098/2017-Valid -16-April 2020

NABL) - Chemical (Certificate No. T-2446) and Biological (Certificate No. T-2447) valid till 11-February-2015

NABL) - Chemical (Certificate No. T-2446) and Biological (Certificate No. T-2447) valid till 23-September-2017

NABL) - Chemical and Biological (Certificate No. TC-6633) valid till 05-December-2019

atory (TU/IV-RD/3310/2011). Valid till 31-March-2013

atory (TU/IV-RD/3310/2014). Valid till 31-March-2017

atory (TU/IV-RD/3310/2017). Valid till 31-March-2020

on data generation- as per 356th RC Meeting held on 25th June 2015 (valid till May-2017)

on data generation- as per 375th RC Meeting held on 19th May 2017 (valid till April-2019)

ogy Park promoted by NSTEDB- Govt of India and University of Pune (License no-Gl/019)
015

2017
MATERIALS
CHEMICALS AND REAGENTS
Sr. No. Reagent /Chemicals
1 Acetonitrile (HPLC grade)
2 Methanol (HPLC grade)
3 Water (HPLC grade)
4 Distilled Water
5 Dried Methanol
6 Dried Acetone
7 Orthosphoric Acid (HPLC grade)
8 Acetone (HPLC grade)
9 Karl Fischer Reagents
10 0.05 Sodium Hydroxide solution
11 Methyl red indicator solution
12 Acetic Acid (HPLC grade)
13 Acetic Anhydride (AR grade)
14 Toluene (HPLC grade)
15 Hexane (HPLC grade)
16 Ethyl Acetate ((AR grade)
17 Methylene Chloride (AR grade)
18 Tetrahydrofuran (HPLC grade)
19 0.05Potassium Hydroxide
20 0.05 Hydrochloric acid solution
21 Formic Acid (HPLC grade)
22 Crystal Violet Indicator solution
23 0.1 N Silver nitrate solution
24 0.1 N Anmonium thiocyanate solution
25
26
27
28
29
30

LIST OF INSTR
Sr .No. Instruments /Apparatus Make
1 HPLC Shimadzu
2 GC Agilent (7820 A)
3 Analytical Balance M/s. Contech India
4 Standard Lab Glasswares A Class
5 Karl fisher Autotitrator M/s. Metrohm
6 Microliter Syringe 0-50 µl Capacity
7 pH meter Eutech
8 Meling point/Boiling point apparatus Veego
9 Sonicator Upper India Scientific
10 Water Bath Met lab
11 Hot air Oven Met lab
12 Sintered Glass Filtering crucible porocity No.3 Borocilicate
13 250 ml Erlenmeyer flask Borocilicate
14 FT IR Agilent
15 UV -Visible Spectrophotometer Shimadzu
16 LCMS -MS Waters
17 GCMS Agilent
18 NMR Bruker

BY HPLC
Chromatographic conditions:
Instrument
Column
Detection wavelength
Flow rate
Temperature
Injection volume
Mobile phase
Diluent
Run time
Gradient Program

Gradient Program
Time in minutes A

BY GC
Chromatographic conditions:
Instrument
Column
Temperatures
Column oven (Isothermal)

Temperature Program

Injector
Detector
Carrier Gas
Nitrogen
Hydrogen
Air
Column Flow
Split ratio
Injection volume
Diluent
Retention time (Approx.

Run Time
LIST OF INSTRUMENTS AND APPARATUS
Model
UV-1800 Series
Acquity- H Class with Xevo TQD Mass Detector Acquity
5977 E -MSD , 7820 A-GC

B
Software Detector
LC Solution software PDA
Ezchrome Elite /Open lab software FID
UVprobe2.52
Masslynx.4.1
Open lab 2.2
Desiccator
Mechanical Shaker
Stability Chamber Newtronics
4 RESULTS

4.1. DESCRIPTION
White solid powder

Method
4.2. ACTIVE CONTENT (WITH IS)-BY HPLC 3.2
Table - 1 : Calculation results - Active content

Weight of Weight of Area of Active in the Area of Active in the Area of IS in the
standard sample standard solution sample solution standard solution
Replicates

mg mg
M1 M2 A1 A2 A3
0 Day
S1R1 32.2 35.7 17437785 17448562 6674256
S1R2 32.2 35.7 17437785 17562531 6674256
S2R1 32.2 35.6 17463281 17495842 6676954
S2R2 32.2 35.6 17463281 17452654 6676954
0 Day
S1 32.2 35.7 17437785 17448562 6674256
S2 32.2 35.7 17437785 17562531 6674256
S3 32.2 35.6 17463281 17495842 6676954
S4 32.2 35.6 17463281 17452654 6676954
S5 32.2 35.7 17463281 17495842 6676954
S6 32.2 35.7 17463281 17452654 6676954

Table - 1 : Calculation results - Active content


Weight of Weight of Area of Active in the Area of Active in the Area of IS in the
standard sample standard solution sample solution standard solution
Replicates

mg mg
M1 M2 A1 A2 A3
28 Day
S1R1 35.6 17437785 17448562 6674256
S1R2 35.6 0 17437785 17562531 6674256
S2R1 35.6 mg 17463281 17495842 6676954
S2R2 35.6 mg 17463281 17452654 6676954
28 Day
S1 35.6 35.6 17437785 17448562 6674256
S2 35.6 35.6 17437785 17562531 6674256
S3 35.6 0.0 17463281 17495842 6676954
S4 35.6 0.0 17463281 17452654 6676954
S5 35.6 0.0 17463281 17495842 6676954
S6 35.6 0.0 17463281 17452654 6676954

4.3 ACTIVE CONTENT (WITH IS)-BY GC 3.3


Table - 2 : Calculation results - Active content

Weight of Weight of Area of Active in the Area of Active in the Area of IS in the
standard sample standard solution sample solution standard solution
Replicates

mg mg
M1 M2 A1 A2 A3
0 Day
S1R1 32.2 35.7 17437785 17448562 6674256
S1R2 32.2 35.7 17437785 17562531 6674256
S2R1 32.2 35.6 17463281 17495842 6676954
S2R2 32.2 35.6 17463281 17452654 6676954
0 Day
S1 32.2 35.2 17437785 17448562 6674256
S2 32.2 35.7 17437785 17562531 6674256
S3 32.2 35.8 17463281 17495842 6676954
S4 32.2 35.2 17463281 17495842 6676954
S5 32.2 35.7 17463281 17452654 6676954
S6 32.2 35.2 17463281 17452655 6676954

Table - 2 : Calculation results - Active content

Weight of Weight of Area of Active in the Area of Active in the Area of IS in the
standard sample standard solution sample solution standard solution
Replicates

mg mg
M1 M2 A1 A2 A3
28 Day
S1R1 35.6 35.7 17437785 17448562 6674256
S1R2 35.6 35.7 17437785 17562531 6674256
S2R1 35.6 35.8 17463281 17495842 6676954
S2R2 35.6 35.8 17463281 17452654 6676954
28 Day
S1 35.6 35.2 17437785 17448562 6674256
S2 35.6 35.1 17437785 17562531 6674256
S3 35.6 35.7 17463281 17495842 6676954
S4 35.6 35.8 17463281 17495842 6676954
S5 35.6 35.9 17463281 17452654 6676954
S6 35.6 35.4 17463281 17452655 6676954

Method
4.4 ACTIVE CONTENT (WITHOUT IS)-BY HPLC 3.4
3.5
Table - 2 : Calculation results - Active content
Area of Active in the Area of Active in the % Purity of
Weight of standard Weight of sample standard solution sample solution Standard
Replicates

mg mg
M1 M2 A1 A2 P
0 Day
S1R1 32.2 35.7 17437785 17448562 99.80
S1R2 32.2 35.7 17437785 17562531 99.80
S2R1 32.2 35.6 17463281 17495842 99.80
S2R2 32.2 35.6 17463281 17452654 99.80
0 Day
S1 32.2 35.7 17437785 17448562 99.80
S2 32.2 35.2 17437785 17562531 99.80
S3 32.2 35.1 17437785 17448562 99.80
S4 32.2 35.7 17437785 17562531 99.80
S5 32.2 35.8 17463281 17495842 99.80
S6 32.2 35.2 17463281 17452654 99.80

Table - 2 : Calculation results - Active content

Area of Active in the Area of Active in the % Purity of


Weight of standard Weight of sample standard solution sample solution Standard
Replicates

mg mg
M1 M2 A1 A2 P
28 Day
S1R1 35.6 37.6 17437785 17448562 0.00
S1R2 35.6 37.6 17437785 17562531 0.00
S2R1 35.6 37.4 17463281 17495842 0.00
S2R2 35.6 37.4 17463281 17452654 0.00
28 Day
S1 35.6 35.2 17437785 17448562 0.00
S2 35.6 35.7 17437785 17562531 0.00
S3 32.2 35.8 17437785 17448562 99.80
S4 32.2 35.6 17437785 17562531 99.80
S5 35.6 35.1 17463281 17495842 0.00
S6 35.6 35.2 17463281 17452654 0.00

4.5 ACTIVE CONTENT (WITHOUT IS) BY GC


Table - 2 : Calculation results - Active content

Area of Active in the Area of Active in the % Purity of


Weight of standard Weight of sample standard solution sample solution Standard
Replicates
mg mg
M1 M2 A1 A2 P
0 Day
S1R1 32.2 35.7 17437785 17448562 99.80
S1R2 32.2 35.7 17437785 17562531 99.80
S2R1 32.2 35.6 17463281 17495842 99.80
S2R2 32.2 35.6 17463281 17452654 99.80
0 Day
S1R1 32.2 35.3 17437785 17448562 99.8
S1R2 32.2 35.3 17437785 17562531 99.8
S1R1 32.2 35.7 17437785 17448562 99.80
S1R2 32.2 35.7 17437785 17562531 99.80
S2R1 32.2 35.6 17463281 17495842 99.80
S2R2 32.2 35.6 17463281 17452654 99.80

Table - 2 : Calculation results - Active content


Area of Active in the Area of Active in the % Purity of
Weight of standard Weight of sample standard solution sample solution Standard
Replicates

mg mg
M1 M2 A1 A2 P
28 Day
S1R1 35.6 36.4 17437785 17448562 99.80
S1R2 35.6 36.4 17437785 17562531 99.80
S2R1 35.6 35.7 17463281 17495842 99.80
S2R2 35.6 35.7 17463281 17452654 99.80
28 Day
S1R1 32.2 35.3 17437785 17448562 99.80
S1R2 32.2 35.3 17437785 17562531 99.80
S1R1 35.6 35.6 17437785 17448562 99.80
S1R2 35.6 35.6 17437785 17562531 99.80
S2R1 35.6 35.2 17463281 17495842 99.80
S2R2 35.6 35.2 17463281 17452654 99.80

Method
4.6 MOISTURE (WATER) CONTENT BY IS 3.6
Table-3 : Water equivalence factor

Water equivalence factor Mean Factor, T


Sr.No. Weight of water (mg) KF Reading (ml) (T) (mg/ml)

0 Day
1 10.3 2.01 5.1244
5.0999
2 10.2 2.00 5.1000 5.0999
3 10.1 1.99 5.0754

Table-3 : Water equivalence factor

Water equivalence factor Mean Factor, T


Sr.No. Weight of water (mg) KF Reading (ml) (T) (mg/ml)

28 Day
1 10.3 2.01 5.1244
2 10.2 2.00 5.1000 5.0999
3 10.1 1.99 5.0754

Method
4.7 MOISTURE (WATER) CONTENT BY CIPAC 3.7
Table-5 : Water equivalence factor
Water equivalence factor Mean Factor E (g/l)
Sr.No. Weight of water (gm) W KF Reading (ml) b (T)

0 Day
1 0.0395 7.81 5.0576
2 0.0391 7.80 5.0128 5.0256
3 0.0390 7.79 5.0064

Table-5 : Water equivalence factor

Water equivalence factor Mean Factor E (g/l)


Sr.No. Weight of water (gm) W KF Reading (ml) b (T)

28 Day
1 0.0395 7.81 5.0576
2 0.0391 7.80 5.0128 5.0256
3 0.0390 7.79 5.0064
Method
4.8. pH content 3.8
Table-7: pH results
Sample No. Sample weight in gm pH observed Avg. pH observed
0 Day Glass Container
1 1.0052 5.50
5.54
2 1.0063 5.58
0 Day
1 1.0052 5.50
2 1.0063 5.58
1 1.0052 5.50
5.54
2 1.0063 5.58
1 1.0052 5.50
2 1.0063 5.58

Table-7: pH results
Sample No. Sample weight in gm pH observed Avg. pH observed
28 Day Glass Container
1 1.0052 5.50
5.54
2 1.0063 5.58
28 Day
1 1.0052 5.50
2 1.0063 5.58
1 1.0052 5.50
5.54
2 1.0063 5.58
1 1.0052 5.50
2 1.0063 5.58
Method
4.9 Material insoluble in acetone 3.9
Table-8: Material insoluble in acetone content results

Weight of residue in Material insoluble in


Weight of sample in gm Weight of empty crucible Weight of crucible +
Sample No. acetone, percent by
(M) in gm residue in gm gm (m) mass

0 Day
1 10.0325 65.3521 65.3572 0.0051 0.05
2 10.0852 65.3248 65.3313 0.0065 0.06
0 Day
1 10.0325 65.3521 65.3572 0.0051 0.05
2 10.0852 65.3248 65.3313 0.0065 0.06
3 10.0325 65.3521 65.3572 0.0051 0.05
4 10.0852 65.3248 65.3313 0.0065 0.06
5 10.0325 65.3521 65.3572 0.0051 0.05
6 10.0852 65.3248 65.3313 0.0065 0.06

Table-8: Material insoluble in acetone content results

Weight of residue in Material insoluble in


Weight of sample in gm Weight of empty crucible Weight of crucible +
Sample No. acetone, percent by
(M) in gm residue in gm gm (m) mass

28 Day
1 10.0325 65.3521 65.3572 0.0051 0.05
2 10.0852 65.3248 65.3313 0.0065 0.06
28 Day
1 10.0325 65.3521 65.3572 0.0051 0.05
2 10.0852 65.3248 65.3313 0.0065 0.06
3 10.0325 65.3521 65.3572 0.0051 0.05
4 10.0852 65.3248 65.3313 0.0065 0.06
5 10.0325 65.3521 65.3572 0.0051 0.05
6 10.0852 65.3248 65.3313 0.0065 0.06

Method
4.10 ACIDITY (as H2SO4) 3.10
Table-9: Acidity content results

Normality of 0.05N
Mass of the sample taken for Titration reading(V) in
Sample No. Blank reading (v) in ml Difference in ml Sodium Hydroxide
test in gm (M) ml solution (N)

0 Day
1 10.0141 0.1 0.5 0.4 0.0501
2 10.1027 0.1 0.7 0.5 0.0501
0 Day
1 10.0141 0.1 0.5 0.4 0.0501
2 10.1027 0.1 0.7 0.5 0.0501
3 10.0141 0.1 0.5 0.4 0.0501
4 10.1027 0.1 0.7 0.5 0.0501
5 10.0141 0.1 0.5 0.4 0.0501
6 10.1027 0.1 0.7 0.5 0.0501

Table-9: Acidity content results


Normality of 0.05N
Mass of the sample taken for Titration reading(V) in
Sample No. Blank reading (v) in ml Difference in ml Sodium Hydroxide
test in gm (M) ml solution (N)
28 Day
1 10.0141 0.1 0.5 0.4 0.0501
2 10.1027 0.1 0.7 0.5 0.0501
28 Day
1 10.0141 0.1 0.5 0.4 0.0501
2 10.1027 0.1 0.7 0.5 0.0501
3 10.0141 0.1 0.5 0.4 0.0501
4 10.1027 0.1 0.7 0.5 0.0501
5 10.0141 0.1 0.5 0.4 0.0501
6 10.1027 0.1 0.7 0.5 0.0501

Method
4.11 Alkalinity (as NaOH) 3.11
Table-10: Alkalinity content results
Normality of 0.05N
Mass of the sample taken for Titration reading(V) in
Sample No. Blank reading (v) in ml Difference in ml Hydrochloric acid
test in gm (M) ml solution (N)
0 Day
1 10.0654 0.1 0.6 0.5 0.0505
2 10.0748 0.1 0.7 0.6 0.0505
0 Day
1 10.0654 0.1 0.6 0.5 0.0505
2 10.0748 0.1 0.7 0.6 0.0505
3 10.0654 0.1 0.6 0.5 0.0505
4 10.0748 0.1 0.7 0.6 0.0505
5 10.0654 0.1 0.6 0.5 0.0505
6 10.0748 0.1 0.7 0.6 0.0505

Table-10: Alkalinity content results


Normality of 0.05N
Mass of the sample taken for Titration reading(V) in
Sample No. Blank reading (v) in ml Difference in ml Hydrochloric acid
test in gm (M) ml solution (N)
0 Day
1 10.0654 0.1 0.6 0.5 0.0505
2 10.0748 0.1 0.7 0.6 0.0505
28 Day
1 10.0654 0.1 0.6 0.5 0.0505
2 10.0748 0.1 0.7 0.6 0.0505
3 10.0654 0.1 0.6 0.5 0.0505
4 10.0748 0.1 0.7 0.6 0.0505
5 10.0654 0.1 0.6 0.5 0.0505
6 10.0748 0.1 0.7 0.6 0.0505

Method
4.12 Melting Point 3.12
Table-11: Melting point results
Avg. Melting point
Sample No. Melting point observed °C observed °C
0 Day
1 105.0
105.5
2 106.0
0 Day
1 105.0
2 106.0
1 105.0
105.5
2 106.0
1 105.0
2 106.0

Table-11: Melting point results


Avg. Melting point
Sample No. Melting point observed °C observed °C
0 Day
1 105.0
105.5
2 106.0
0 Day
1 105.0

105.5
2 106.0
1 105.0
105.5
2 106.0
1 105.0
2 106.0

Method
4.13 Ash content 3.13
Table-12: Ash content results

Weight of silica crucible Weight of residue


Weight of empty silica
Sample No Weight of sample in gm (M) +cruccible after (M2-M1 ) in gm
crucible (M2) in gm + sample in gm ignition (M1) in gm

0 Day
1 1.0065 37.8546 38.8611 38.8752 1.0206
2 1.0087 37.8985 38.9072 38.9285 1.0300
0 Day
1 1.0065 37.8546 38.8611 38.8752 1.0206
2 1.0087 37.8985 38.9072 38.9285 1.0300
3 1.0065 37.8546 38.8611 38.8752 1.0206
4 1.0087 37.8985 38.9072 38.9285 1.0300
5 1.0065 37.8546 38.8611 38.8752 1.0206
6 1.0087 37.8985 38.9072 38.9285 1.0300

Table-12: Ash content results

Weight of silica crucible Weight of residue


Weight of empty silica
Sample No Weight of sample in gm (M) +cruccible after (M2-M1 ) in gm
crucible (M2) in gm + sample in gm ignition (M1) in gm
28 Day
1 1.0065 37.8546 38.8611 38.8752 1.0206
2 1.0087 37.8985 38.9072 38.9285 1.0300
28 Day
1 1.0065 37.8546 38.8611 38.8752 1.0206
2 1.0087 37.8985 38.9072 38.9285 1.0300
3 1.0065 37.8546 38.8611 38.8752 1.0206
4 1.0087 37.8985 38.9072 38.9285 1.0300
5 1.0065 37.8546 38.8611 38.8752 1.0206
6 1.0087 37.8985 38.9072 38.9285 1.0300

4.14 CONTAINER CONDITION

Specifications of the packing containers


Physical observation of
Sr. No Results Guidelines
Container

Material of construction of
1 LDPE liner bag IS : 8190 (part 1) : 1988
Primary pack

2 Capacity- 100 gm 100 gm 100 gm

Weight of empty LDPE Liner


3 4 gm 4 gm
bag in g

Container condition before and after storage


Testing of Container as per clause 12.4.2 of IS 2798:1998
Visible cracks Change in color Change in weight
Bag No.
Before storage After storage Before storage After storage Before storage
1 None None Transparent No change 104.2
2 None None Transparent No change 104.2
3 None None Transparent No change 104.2
4 None None Transparent No change 104.2
5 None None Transparent No change 104.2
6 None None Transparent No change 104.2

Glass – 0 Day
Obervations
Parameters
Sample-1 Sample - 2
Glass Container
Description White solid powder
ACTIVE
CONTENT Carfentrazone-ethyl content, 96.32 96.34
(WITH IS)-BY Percent by mass,
HPLC
ACTIVE
CONTENT Carfentrazone-ethyl content, 96.32 96.34
(WITH IS)-BY Percent by mass,
GC

ACTIVE
CONTENT Carfentrazone-ethyl content, 96.32 96.34
(WITHOUT IS)- Percent by mass,
BY HPLC

ACTIVE
CONTENT Carfentrazone-ethyl content, 96.32 96.34
(WITHOUT IS)- Percent by mass,
BY GC
Moisture Content, Percent by
BIS mass,
Moisture Content, Percent by
CIPAC mass,
Material insoluble in Acetone
Percent by mass,
pH of 1% aq. Solution
Material insoluble in Acetone
Percent by mass
Acidity (As,H2SO4), Percent by
mass
Alkalinity (As, NaOH), Percent
by mass
Melting Point (at 25 °C)

Ash content, Percent by mass

Container condition before and


after storage
MS Drum – 0 Day
Sample S1 Sample S2 Sample S3 Sample S4
Description Viscous yellow to orange color liquid
ACTIVE
CONTENT Carfentrazone-ethyl content, 96.37 96.38 96.42 96.25
(WITH IS)-BY Percent by mass,
HPLC

ACTIVE
CONTENT Carfentrazone-ethyl content, 0.05 0.04 0.05 0.05
(WITH IS)-BY Percent by mass,
GC

ACTIVE
CONTENT Carfentrazone-ethyl content, 0.22 0.21 0.22 0.22
(WITHOUT IS)- Percent by mass,
BY HPLC
ACTIVE
CONTENT Carfentrazone-ethyl content, 4.83 4.89 4.9 4.84
(WITHOUT IS)- Percent by mass,
BY GC

Moisture Content, Percent by


BIS mass,

Moisture Content, Percent by


CIPAC mass,

Material insoluble in Acetone


Percent by mass,
pH of 1% aq. Solution
Material insoluble in Acetone
Percent by mass
Acidity (As,H2SO4), Percent by
mass
Alkalinity (As, NaOH), Percent
by mass
Melting Point (at 25 °C)

Ash content, Percent by mass

Glass – 28 Day
Obervations
Parameters
Sample-1 Sample - 2
Glass Container
Description 0
Carfentrazone-ethyl content, 96.32 96.34
Percent by mass,
Carfentrazone-ethyl content, 96.32 96.34
Percent by mass,
Carfentrazone-ethyl content, 96.32 96.34
Percent by mass,
Carfentrazone-ethyl content, 96.32 96.34
Percent by mass,
Moisture Content, Percent by
mass,
Moisture Content, Percent by
mass,
Material insoluble in Acetone
Percent by mass,
pH of 1% aq. Solution
Material insoluble in Acetone
Percent by mass
Acidity (As,H2SO4), Percent by
mass
Alkalinity (As, NaOH), Percent
by mass
Melting Point (at 25 °C)
Ash content, Percent by mass

Container condition before and


after storage
MS Drum – 28 Day
Sample S1 Sample S2 Sample S3 Sample S4
Description Viscous yellow to orange color liquid
Carfentrazone-ethyl content, 96.37 96.38 96.42 96.25
Percent by mass,
Carfentrazone-ethyl content, 0.05 0.04 0.05 0.05
Percent by mass,
Carfentrazone-ethyl content, 0.22 0.21 0.22 0.22
Percent by mass,
Carfentrazone-ethyl content, 4.83 4.89 4.9 4.84
Percent by mass,
Moisture Content, Percent by
mass,
Moisture Content, Percent by
mass,
Material insoluble in Acetone
Percent by mass,
pH of 1% aq. Solution
Material insoluble in Acetone
Percent by mass
Acidity (As,H2SO4), Percent by
mass
Alkalinity (As, NaOH), Percent
by mass
Melting Point (at 25 °C)
Ash content, Percent by mass
nt

Active Content,
Area of IS in the % Purity of percent by
Avg. Active Content, Mean
sample solution Standard Avg. Active
mass Content, percent
percent by mass by mass

A4 P

6647512 99.80 90.43


90.61
6665284 99.80 90.78
90.58
6651247 99.80 90.79
90.55
6669282 99.80 90.32

6647512 99.80 90.43


6665284 99.80 90.78
6651247 99.80 90.79
90.49
6669282 99.80 90.32
6651247 99.80 90.53
6669282 99.80 90.06

nt
Active Content,
Area of IS in the % Purity of percent by
Avg. Active Content, Mean
sample solution Standard Avg. Active
mass Content, percent
percent by mass by mass

A4 P

6647512 99.80 #DIV/0!


#DIV/0!
6665284 99.80 #DIV/0!
#DIV/0!
6651247 99.80 #VALUE!
#VALUE!
6669282 99.80 #VALUE!

6647512 99.80 100.26


6665284 99.80 100.65
6651247 99.80 #DIV/0!
#DIV/0!
6669282 99.80 #DIV/0!
6651247 99.80 #DIV/0!
6669282 99.80 #DIV/0!

nt

Active Content,
Area of IS in the % Purity of percent by
Avg. Active Content, Mean
sample solution Standard Avg. Active
mass Content, percent
percent by mass by mass

A4 P

6647512 99.80 90.43


90.61
6665284 99.80 90.78
90.58
6651247 99.80 90.79
90.55
6669282 99.80 90.32
6647512 99.80 91.72
6665284 99.80 90.78
6651247 99.80 90.28
91.00
6651247 99.80 91.82
6669282 99.80 90.06
6669283 99.80 91.34

nt

Active Content,
Area of IS in the % Purity of percent by
Avg. Active Content, Mean
sample solution Standard Avg. Active
mass Content, percent
percent by mass by mass

A4 P

6647512 99.80 99.98


100.17
6665284 99.80 100.37
99.86
6651247 99.80 99.81
99.55
6669282 99.80 99.30

6647512 99.80 101.40


6665284 99.80 102.08
6651247 99.80 100.09
100.47
6651247 99.80 99.81
6669282 99.80 99.02
6669283 99.80 100.42
Active Content, Mean Avg.
percent by mass Avg. Active Content, Active Content,
percent by mass percent by
mass

99.80
95.23
90.66
92.78
90.44
90.33
90.21

90.07
91.95
91.09
90.99
91.69
89.93
91.24

Active Content, Mean Avg.


percent by mass Avg. Active Content, Active Content,
percent by mass percent by
mass

0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
0.00
91.09
30.46
91.69
0.00
0.00

Active Content, Mean Avg.


percent by mass Avg. Active Content, Active Content,
percent by mass percent by
mass

90.07
90.37
90.66
90.35
90.44
90.33
90.21

91.09
91.68
90.07
90.69
90.66
90.44
90.21
Active Content, Mean Avg.
percent by mass Avg. Active Content, Active Content,
percent by mass percent by
mass

97.67
97.99
98.30
98.78
99.71
99.58
99.46

91.09
91.68
99.86
97.52
100.51
101.12
100.87

Table-4 : Water content results

Water equivalent Weight of Moisture Average Moisture


of Karl Fischer Volume of the Karl
Sample No. Sample in g content ,percent content ,percent by
reagent (T) Fischer reagent (B)
(E) by mass mass
(mg/ml)

0 Day
1 5.0999 1.0050 0.21 0.11
0.12
0.12
2 5.0999 1.0256 0.25 0.12
0 Day
1 5.0999 1.0050 0.21 0.11
2 5.0999 1.0256 0.25 0.12
3 5.0999 1.0050 0.21 0.11
0.12
4 5.0999 1.0256 0.25 0.12
5 5.0999 1.0050 0.21 0.11
6 5.0999 1.0256 0.25 0.12

Table-4 : Water content results

Water equivalent Weight of Moisture Average Moisture


of Karl Fischer Volume of the Karl
Sample No. Sample in g content ,percent content ,percent by
reagent (T) Fischer reagent (B)
(E) by mass mass
(mg/ml)

28 Day
1 5.0999 1.0050 0.21 0.11
0.12
2 5.0999 1.0256 0.25 0.12
28 Day
1 5.0999 1.0050 0.21 0.11
2 5.0999 1.0256 0.25 0.12
3 0.0000 1.0050 0.21 0.00
0.04
4 0.0000 1.0256 0.25 0.00
5 0.0000 1.0050 0.21 0.00
6 0.0000 1.0256 0.25 0.00

Table-6: Water content results


Volume required for
Water equivalence mass of Avg. Moisture
the sample Moisture Moisture content, content
Sample No. of Karl Fischer sample taken ,percent
determination (ml) content,g/kg percent by mass
reagent (E) (g/l) (g) (w) by mass
(t)

0 Day
1 5.0256 5.0125 10.1 10.13 1.01
1.02
2 5.0256 5.0136 10.3 10.32 1.03
0 Day
1 5.0256 5.0125 10.1 10.13 1.01
2 5.0256 5.0136 10.3 10.32 1.03
3 5.0256 5.0125 10.1 10.13 1.01
1.02
4 5.0256 5.0136 10.3 10.32 1.03
5 5.0256 5.0125 10.1 10.13 1.01
6 5.0256 5.0136 10.3 10.32 1.03

Table-6: Water content results

Volume required for


Water equivalence mass of Avg. Moisture
the sample Moisture Moisture content, content
Sample No. of Karl Fischer sample taken determination ,percent
(ml) content ,g/kg percent by mass
reagent (E) (g/l) (g) (w) by mass
(t)

28 Day
1 5.0256 5.0125 10.1 10.13 1.01
1.02
2 5.0256 5.0136 10.3 10.32 1.03
28 Day
1 0.0000 5.0125 10.1 0.00 0.00
2 0.0000 5.0136 10.3 0.00 0.00
3 0.0000 5.0125 10.1 0.00 0.00
0.00
0.00
4 0.0000 5.0136 10.3 0.00 0.00
5 0.0000 5.0125 10.1 0.00 0.00
6 0.0000 5.0136 10.3 0.00 0.00
Avg. Material
insoluble in
acetone, percent
by mass

0.06

0.06

Avg. Material
insoluble in
acetone, percent
by mass

0.06

0.06
0.06

Acidity (as Avg. Acidity (as


H2SO4), percent H2SO4), percent by
by mass mass

0.02
0.02
0.02

0.02
0.02
0.02
0.02
0.02
0.02
0.02

Acidity (as Avg. Acidity (as


H2SO4), percent H2SO4), percent by
by mass mass

0.02
0.02
0.02

0.02

0.02
0.02
0.02
0.02
0.02
0.02
0.02

Alkalinity (as Avg.Alkalinity (as


NaOH), percent NaOH), percent by
by mass mass

0.02
0.02
0.02

0.02
0.02
0.02
0.02
0.02
0.02
0.02

Alkalinity (as Avg.Alkalinity (as


NaOH), percent NaOH), percent by
by mass mass

0.02
0.02
0.02

0.02

0.02
0.02
0.02
0.02
0.02
0.02
0.02
Ash content, Avg. Ash content,
percent by mass percent by mass

1.01
1.02
1.02

1.01
1.02
1.01
1.02
1.02
1.01
1.02

Ash content, Avg. Ash content,


percent by mass percent by mass
1.01
1.02
1.02

1.01
1.02
1.01
1.02
1.02
1.01
1.02

n weight (g) Change in shape


After storage Before storage After storage
104.3 Rectangular No change
104.2 Rectangular No change
104.4 Rectangular No change
104.2 Rectangular No change
104.3 Rectangular No change
104.5 Rectangular No change

Average

96.33

96.33

96.33

96.33
Sample S5 Sample S6 Average
d

96.2 96.23 96.31

0.04 0.05 0.05

0.22 0.21 0.22


4.9 4.83 4.87

0.00

0.00

0.00

0.00

0.00

0.00

0.00

0.00

0.00

Average

96.33
96.33

96.33

96.33

Sample S5 Sample S6 Average


d
96.2 96.23 96.31

0.04 0.05 0.05

0.22 0.21 0.22


4.9 4.83 4.87

0.00

0.00

0.00
0.00
0.00

0.00

0.00
0.00
0.00
Temperature
conditions inside the test chamber
Date Temperature (°C) % Humidity
12/1/2018 54.3 65.1
12/2/2018 54.6 65.9
12/3/2018 54.2 65.9
12/4/2018 54.7 65.8
12/5/2018 54.8 65.0
12/6/2018 54.8 65.5
12/7/2018 54.3 65.4
12/8/2018 54.2 65.1
12/9/2018 54.8 65.9
12/10/2018 54.1 65.1
12/11/2018 54.1 66.0
12/12/2018 54.4 65.1
12/13/2018 54.3 65.6
12/14/2018 54.2 65.4
12/15/2018 54.5 65.8
12/16/2018 54.7 65.1
12/17/2018 54.3 65.2
12/18/2018 54.9 65.5
12/19/2018 54.8 65.7
12/20/2018 54.7 65.6
12/21/2018 54.7 65.7
12/22/2018 54.5 65.8
12/23/2018 54.2 65.5
12/24/2018 54.8 65.0
12/25/2018 54.3 65.8
12/26/2018 54.5 65.7
12/27/2018 54.1 65.4
12/28/2018 54.7 65.7
0 DAY

${RST!D33} ${RST!H33}
S1R1 ,percent by mass = X X ${RST!J33} = ${RST!K33}
${RST!E33} ${RST!I33}

${RST!D34} ${RST!H34}
S1R2 ,percent by mass = X X ${RST!J34} = ${RST!K34}
${RST!E34} ${RST!I34}

Average Active content ,percent by = ${RST!K33} + ${RST!K34} / 2 = ${RST!L33}


mass

${RST!D35} ${RST!H35}
S2R1 ,percent by mass = X X ${RST!J35} = ${RST!K35}
${RST!E35} ${RST!I35}
${RST!D36} ${RST!H36}
S2R2 ,percent by mass = X X ${RST!J36} = ${RST!K36}
${RST!E36} ${RST!I36}

Average Active content ,percent by


= ${RST!K35} + ${RST!K36} / 2 = ${RST!L35}
mass

Mean Active content,percent by


= ${RST!K35} + ${RST!L35} / 2 = ${RST!M33}
mass
28 DAY

S1 , Active Content,percent by ${RST!D38} ${RST!H38}


= X X ${RST!J38} = ${RST!K38}
mass
${RST!E38} ${RST!I38}

S2 , Active Content,percent by ${RST!D39} ${RST!H39}


= X X ${RST!J39} = ${RST!K39}
mass ${RST!E39} ${RST!I39}

S3 , Active Content,percent by ${RST!D40} ${RST!H40}


= X X ${RST!J40} = ${RST!K40}
mass ${RST!E40} ${RST!I40}

S4 , Active Content,percent by ${RST!D41} ${RST!H41}


= X X ${RST!J41} = ${RST!K41}
mass ${RST!E41} ${RST!I41}

S5 , Active Content,percent by ${RST!D42} ${RST!H42}


= X X ${RST!J42} = ${RST!K42}
mass ${RST!E42} ${RST!I42}

S6 , Active Content,percent by ${RST!D43} ${RST!H43}


= X X ${RST!J43} = ${RST!K43}
mass ${RST!E43} ${RST!I43}

= ${RST!K38} + ${RST!K40} + ${RST!K41}


Mean Average Active content
,percent by mass = ${RST!L38}
+ ${RST!K42} + ${RST!K43} / 6
Calculation Formula:
W x 1000
Water equivalent of titration solution =
b
txE
Moisture content, g/kg =
w
Moisture content, g/
Moisture content, percent by mass =
10
Where,
W = mass of water taken for the calibration (g)
E = water equivalent of the titration solution (g/l)
b = Volume required for the calibration (ml)
t = Volume required for the sample determination (
w = mass of sample taken (g)
W x 1000
b
txE
w
Moisture content, g/kg
10

or the calibration (g)


e titration solution (g/l)
he calibration (ml)
he sample determination (ml)
(g)
Weight of water KF Reading (ml)
(mg)

${RST!D165}

${RST!D165}

${RST!D165}
Table-6: Wate

Water
equivalence of
Karl Fischer Sample No. Sample No.
reagent (E)
(g/l)

1 #REF!
2 #REF!

1 #REF!
2 #REF!
3 #REF!
4 #REF!
5 #REF!
6 #REF!
0 DAY

S1R1 ,percent ${RST!D91}


= X
by mass
${RST!E91}

S1R2 ,percent ${RST!D92}


= X
by mass
${RST!E92}

Average ActFve
content ,percent = ${RST!K52} +
by mass

S2R1 ,percent ${RST!D54}


= X
by mass
${RST!E54}

S2R2 ,percent ${RST!D55}


= X
by mass
${RST!E55}

Average ActFve
content ,percent = ${RST!K54} +
by mass

Mean ActFve
content, percent = ${RST!K52} +
by mass

28 DAY

S1 , ActFve ${RST!D38}
Content, percent = X
by mass
${RST!E38}

S2 , ActFve ${RST!D39}
Content, percent = X
by mass
${RST!E39}

S3 , ActFve ${RST!D40}
Content, percent = X
by mass
${RST!E40}

S4 , ActFve ${RST!D41}
Content, percent = X
by mass
${RST!E41}

S5 , ActFve ${RST!D42}
Content, percent = X
by mass
${RST!E42}

S6 , ActFve ${RST!D43}
Content, percent = X
by mass
${RST!E43}
Mean Average
ActFve = (${RST!K38} +
content ,percent
by mass
+ ${RST!K42} +

Weight of Sample (g)


Water Moisture
Mean Factor Volume of the Karl content,
equivalence Sample No. percent
mg/ml fisher reagent (B)
factor (T) (E) by mass

0 Day
RST!D165} 1 ${RST!K165} ${RST!L165} ${RST!M165}
2 ${RST!K165} ${RST!L166} ${RST!M166}
0 Day
1 ${RST!K165} ${RST!L165} ${RST!M165}
RST!D165}
${RST!G165} 2 ${RST!K165} ${RST!L166} ${RST!M166}
3 ${RST!K165} ${RST!L165} ${RST!M165}
4 ${RST!K165} ${RST!L166} ${RST!M166}
5 ${RST!K165} ${RST!L165} ${RST!M165}
RST!D165}
6 ${RST!K165} ${RST!L166} ${RST!M166}
Average ${RST!N165}
Table-6: Water content results

Volume Avg. Moisture


mass of required for Moisture Moisture content
sample taken the sample content content, percent ,percent by
(g) (w) determinatio ,g/kg by mass mass
n (ml) (t)

0 Day
5.0125 10.1 #REF! #REF!
#REF!
5.0136 10.3 #REF! #REF!
0 Day
5.0125 10.1 #REF! #REF!
5.0136 10.3 #REF! #REF!
5.0125 10.1 #REF! #REF!
#REF!
5.0136 10.3 #REF! #REF!
5.0125 10.1 #REF! #REF!
5.0136 10.3 #REF! #REF!
${RST!I91} = ${RST!K91}

${RST!I53} = ${RST!K53}

2 = ${RST!L52}

${RST!I54} = ${RST!K54}

${RST!I55} = ${RST!K55}

2 = ${RST!L54}

2 = ${RST!M33}

${RST!I38} = ${RST!K38}

${RST!I39} = ${RST!K39}

${RST!I40} = ${RST!K40}

${RST!I41} = ${RST!K41}

${RST!I42} = ${RST!K42}

${RST!I43} = ${RST!K43}
${RST!K41}

6 = ${RST!K43})