Page No. 1/2 FC-PF-229 PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD Sr. No. in Scope NABL / NON NABL Flow Chart for Analysis of 2, 4-D Sodium Salt Date of Analysis Sl. No. 1. 2 2.1 3. 3.1 3.2 4. 4.1 Step Sample No. Name of Sample Sample Description Preparation of NaOH Standard solution (0.1 N): Weigh 4 g of NaOH and dissolve in water to give 1 L solution. Note the Serial No. of Balance log book 4.2 Standardization of 0.1N NaOH Solution: Weigh 0.42-0.45 g GR grade Potassium Hydrogen Phthalate (KHP) in a 250 mL conical flask. Note the Serial No. of Balance log book 4.3 Dissolve in 50-70 mL of water 4.4 Add Phenolphthalein indicator. 4.5 Titrate with 0.1N NaOH solution taken in a burette slowly with continuous stirring from colourless to faint pink colour. Titre value for standardization is 4.6 5. 5.1 5.1.1 5.1.2 5.1.3 5.1.4 5.1.5 5.1.6 5.1.7 5.1.8 5.1.9 Executed By Execution Procedure Preparation of Sample Solution Weigh Accurately about 1 g of Sample in a 100 mL beaker. Note the Serial No. of balance log book. Dissolve the Sample in about 10 mL distilled Water. Transfer it quantitatively to a 250 mL separating funnel using minimum quantity of water. Acidify the solution with about 1.5 mL of hydrochloric acid (1:1) using methyl orange indicator. Extract the aqueous phase with three successive portions of 25 ml diethyl ether. Combine ether extracts from all the three separating funnels into one separating funnel, quantitatively. Then wash the ether layer with distilled water (25 mL) until the ether solution is free of chloride ions. (Test for complete removal of chlorides with 0.1 N AgNO3). Transfer the ether solution to a 250 ml beaker and evaporate the ether on water bath to dryness. R1 R2 g g g g mL g mL g Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad Flow Chart for analysis of 2,4-D Sodium Document No. : FC-PF-229 Document Name : Salt Revision No. : 02 Issue Date : 11/07/2013 Revision Date : 26/03/2014 Next Revision Date : 26/03/2016 Prepared By Checked By Approved & Issued By Mrs. T. Sridevi (Assistant Scientific Officer) Mr. C.V. Rao (Technical Manager) Dr Abhay Ekbote (Director PM & Quality Manager) Page No. 2/2 FC-PF-229 PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD 5.1.10 Dissolve the residue in 80 mL of neutral alcohol and titrate with 0.1 N sodium hydroxide solution using bromo thymol blue indicator to green colour Endpoint. 5.1.11 Titre value for sample is mL mL 6. Calculation: Wt. of KHP X 1000 Normality of NaOH (N) = ---------------------------------------------------Volume of NaOH consumed X 204.22 V X N X 22.1 Acid (2,4-D) Content, = ----------------------percent by mass M V = Volume of NaOH required for sample N = Normality of NaOH M = Weight of sample taken for analysis Result: Sl. No. Name of test 1. Result (2,4-D) Acid Content Unit Method of Analysis % IS 1488 : 1989 (Reaffirmed 2009) Remark / Reference : Name Analyzed by Dated signature Name Checked by Dated signature Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad Flow Chart for analysis of 2,4-D Sodium Document No. : FC-PF-229 Document Name : Salt Revision No. : 02 Issue Date : 11/07/2013 Revision Date : 26/03/2014 Next Revision Date : 26/03/2016 Prepared By Checked By Approved & Issued By Mrs. T. Sridevi (Assistant Scientific Officer) Mr. C.V. Rao (Technical Manager) Dr Abhay Ekbote (Director PM & Quality Manager)