Estudio propanil

STUDY No. 01/04

PROPANIL TECHNICAL

FIVE BATCH ANALYSIS

AUTHOR

A. Castro A., Ph. C.
J. Díaz T., Ph. C.

PERFORMING LABORATORY

PROFICOL ANDINA B.V. SUCURSAL COLOMBIA
Quality Control Laboratory
Barranquilla - Colombia

August 2004

I. INTRODUCTION

Objective

The purpose of this study was to verify the chemical composition of Propanil Technical manufactured atPROFICOL ANDINA B.V. SUCURSAL COLOMBIA and to provide updated chromatograms for Propanil, 3,4 - Dichloroaniline and 3, 3´, 4, 4´- Tetrachloroazobenzene (TCAB).

This study is based on the Report No. 01 – 01, “Propanil Technical – Five lots Analysis and method validation performed by AGAN Chemical Manufacturers, Ltd” in March, 2001.

STUDY PERSONNEL

Study Director: Alejandro de CastroA.
Pharmacist Chemical

Analysts: José Díaz T. Ph. C.
Jorge Yaber Ph. C.

DATE OF COMPLETION: August 9, 2004

II. MATERIALS AND METHODS

MATERIALS

TEST SUBSTANCE
Five lots of Propanil Technical manufactured at PROFICOL ANDINA B.V. SUCURSAL COLOMBIA.

| ||
|BATCH No. |DATE OF MANUFACTURING |
| | |
|PP04030080 |March/2004|
| | |
|PP04040162 |April/2004 |
| ||
|PP04050200 |May/2004 |
| | |
|PP04060268 |June/2004|
| | |
|PP04070322 |July/2004 |

COMPOUNDS.

Propanil:
N – (3,4-Dichlorophenyl)propionamide (CAS)
3´, 4´- Dichloropropionanilide (IUPAC)
C9H9Cl2NO
MW 218.08

3, 4- Dichloroaniline (DCA)
C6H5Cl2N
MW 162.02

3, 3´, 4 , 4´- Tetrachloroazobenzene (IUPAC)
C12H16Cl4N2
MW 320.01

METHODS

PROPANIL CONTENT
Principle
The determination of Propanil in Propanil Technical was done by GC equipped with FID detector, using Benzil Benzoate (BB) 1 % in Acetone as Internal Standard.Sample and standard solutions were prepared similarly: Propanil standard (30 mg) and 2 mL solution BB (1 % in Acetone) were dissolved in 25 mL Methanol RG.

Equipment
1. GC system: Hewlett Packard 4890 – 5890 series II, equipped with detector FID and FPD.
2. Column: HP-17 50 % Phenyl Metil Siloxane.
3. Analytical Balance: Mettler AE-200
4. PC Dell and Software ASTERIK.

Reactive1. Methanol RG
2. Acetone
3. Propanil Std. Analytical (98.6 %)
4. Propanil Technical (98.5 %)
5. Benzil Benzoate (BB) Internal Std. (99%)
6. Solution Benzil Benzoate (BB) Internal Std.1% in Acetone (Sol BB)

Procedure
Chromatographic Conditions:
Oven temp = 210 ºC
Injector temp = 270 ºC
Detector temp = 300ºC
Flow N2 = 10.0 mL/min
Split = 3.0 mL/min
Purge = 3.0...