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Volume IV - 5.2 General Exercises

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Orientation and Training

Food and Drug Administration

DOCUMENT NO.:

IV-05
VERSION NO.: 1.3

Section 5 - Pesticides Analysis

EFFECTIVE DATE: 10/01/2003REVISED: 02/14/2013

5.2.1  Equipment, Supplies, and Reagents

A.  Objective

To familiarize the trainee with the pesticide residue laboratory and its equipment.

B.  Assignment

The trainer will discuss the location, care, and cleaning procedures for equipment found in the residue laboratory and will explain proper procedures to obtain, handle, and store needed reagents and solvents. The general organization of the PAM and its use will be reviewed. Reading and reference materials pertinent to pesticides will be provided.

C.  Reference

  1. U.S. Food & Drug Administration, Center for Food Safety and Applied Nutrition, Office of Plant, Dairy Foods and Beverages. Makovi, C. M. (Ed.), McMahon, B. M. (Ed Emerita). (1994). Pesticide Analytical Manual-multiresidue methods (3rd ed., Vol. I, Chaps. 1-Regulatory Operations and 2-General Analytical Operations and Information, updated October 1999). R.O.W. Sciences, Inc.

5.2.2  Standard Solutions

A.  Objective

To introduce the subject of pesticide standards: proper procedures for preparation, precautions during preparation and use, and problems associated with degradation. 

B.  Assignment

The trainer will explain the laboratory standard operating procedure (SOP) for preparing "stock" and "working" standard solutions, including documentation of standard solution preparation and comparison to previous standards. Proper storage of primary and working standards and associated problems, such as degradation or toxicity, will be discussed.

  1. Determine the proper handling of toxic compounds. 
  2. Read the references and answer the questions that follow. Use this procedure for all subsequent assignments. Optional assignments will be completed as needed by the trainee. 
  3. Determine procedures for ordering standards from EPA.

C.  References

  1. U.S. Food & Drug Administration, Center for Food Safety and Applied Nutrition, Office of Plant, Dairy Foods and Beverages. Makovi, C. M. (Ed.), McMahon, B. M. (Ed Emerita). (1994). Pesticide Analytical Manual Vol. I, section 205-Reference Standards, updated October 1999). R.O.W. Sciences, Inc.
  2. Laboratory Information Bulletin, LIB No. 633 and LIB No.1386.
  3. Hodgson, D. W., Thompson, J. F., Watson, R. R. (1982). Journal of Association of Official  Analytical Chemists, 65, 89-93; 94-102.

D.  Questions

  1. Which SOP is used in the laboratory to ensure primary standard purity and reliability?
  2. What constitutes a stock solution? A working solution?
  3. Which SOP is used to ensure reliability of stock and working solutions?
  4. What are the hazards associated with handling and storage of pesticide standards?
  5. What class of pesticides is particularly toxic by skin absorption as well as by inhalation and ingestion?
  6. Where can information such as chemical structure for EPA standards be found?
  7. In general, what would be a good solvent for organochlorine pesticides? For organophosphates? How would someone prepare a mixed standard containing both organochlorine and organophosphate pesticides?