Chapter 2 General Analytical Operations and Information.pdf.pdf
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1、SECTION 100 Pesticide Analytical Manual Vol. I 2001 Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) Table of Contents pagedate 201:Percentage Fat, Water, and Sugars in Foods 02: Grains201-21/94 09: Dairy201-31/94 12: Cheese201-31/94 13: Ice Cream, etc.201-41/94 14: Milk Products201-51/94 15: Eggs
2、 and Egg Products201-51/94 16: Fish201-51/94 17: Meat and Poultry201-71/94 20: Fruits201-81/94 21: Fruit Products201-91/94 22: Vine Fruits (Melons) and Products201-101/94 23: Nuts, Edible Seeds, and Products201-111/94 Chapter 1 Regulatory Operations Chapter 2 General Analytical Operations and Inform
3、ation Chapter 3 Multiclass MRMs Chapter 5 GLC Chapter 4 Selective MRMs Chapter 6 HPLC Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) 2002 SECTION 100Pesticide Analytical Manual Vol. I pagedate 24: Beans, Peas, Corn, and Fruiting Vegetables201-111/94 25: Vegetables and Products201-141/94 28: Spic
4、es, Flavors, and Salts201-151/94 36: Sweeteners (Nutritive)201-161/94 38: Soups201-161/94 40: Baby Foods201-161/94 202:Basic Analytical Techniques 202 A:Introduction202-11/94 202 B:Column Chromatography202-11/94 Terminology202-11/94 Recommended Operating Procedure202-21/94 Common Problems202-21/94 2
5、02 C:Solvent Evaporation202-41/94 Kuderna-Danish Concentrators202-41/94 Rotary Evaporator202-61/94 Rotary Evaporator with Circulating202-71/94 Chilled Liquid Turbo-Vap202-81/94 Common Problems202-81/94 References202-81/94 203:Equipment and Procedures for Comminuting Samples 203 A:Equipment203-11/94
6、Blenders and Homogenizers203-11/94 Choppers and Food Processors203-11/94 Grinders203-21/94 Mills203-21/94 203 B:Procedures for Specific Commodities203-21/94 Crabs and Crayfish203-21/94 Eggs203-31/94 Fish203-31/94 Fruits and Vegetables203-31/94 Hays, Straws, and Dry, Low Fat203-31/94 Feed Ingredients
7、 Oilseeds203-41/94 Dry Products (Pasta, Dry Beans, Grains, etc.)203-41/94 References203-41/94 204:Special Reagent Preparation 204 A:Introduction204-11/94 204 B:PAM I Conventions for Reagents204-11/94 204 C:General Tests for Reagent Purity204-11/94 Test for Substances Causing Determinative204-11/94 S
8、tep Interference SECTION 100 Pesticide Analytical Manual Vol. I 2003 Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) pagedate Test for Substances Causing Pesticide204-21/94 Degradation 204 D:Tests and Purification Processes for204-21/94 Specific Reagents Acetonitrile204-21/94 Ethyl Ether204-21/94
9、 Glass Wool204-21/94 Sodium Sulfate204-31/94 Florisil204-31/94 Lauric acid test204-41/94 Elution test204-59/96 205:Reference Standards 205 A:Sources205-11/94 205 B:Equipment and Solvents205-11/94 Equipment205-11/94 Solvents205-21/94 205 C:Storage205-21/94 205 D:Purity205-21/94 205 E:Standard Solutio
10、ns205-31/94 Definitions205-31/94 Protocols for Preparing Standard Solutions205-31/94 205 F:Safety205-41/94 205 G:Disposal of Reference Standards and Solutions205-41/94 206:Quality Assurance and Quality Control 206 A:General Principles206-11/94 206 B:QA Program Plan206-21/94 Quality Control Points206
11、-21/94 Quality of Equipment206-21/94 Quality of Standards and Reagents206-21/94 Environmental Control/Facility206-31/94 Quality of Analytical Work206-31/94 Quality of Analytical Documentation206-31/94 Audits206-41/94 Sample Accountability206-41/94 Quality of Administrative Systems206-41/94 206 C:SOP
12、s206-41/94 206 D:Bibliography206-61/94 207:Safety 207 A:Introduction207-11/94 207 B:Laws and Regulations Related to Safety207-11/94 207 C:Material Safety Data Sheets207-21/94 207 D:Development of a Chemical Hygiene Plan207-31/94 Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) 2004 SECTION 100Pest
13、icide Analytical Manual Vol. I pagedate 207 E:Responsibilities of the Individual Chemist207-51/94 207 F:Role of Training207-61/94 207 G:Bibliography207-61/94 Government or Organizational Materials207-61/94 Other Publications207-71/94 208:Hazardous Waste Disposal 208 A:Identification of Waste208-11/9
14、4 Waste Specifically Excluded208-11/94 Chemicals Listed in 40 CFR 261.30208-11/94 Subpart D Chemicals Exhibiting Hazardous Waste208-21/94 Characteristics Hazardous Waste Mixtures208-31/94 208 B:Categorization of Waste Generator208-31/94 208 C:Obtaining Appropriate ID Numbers208-31/94 208 D:Waste Col
15、lection and Storage Procedures208-41/94 208 E:Arrangement for Waste Disposal208-41/94 208 F:Additional Management Requirements208-41/94 208 G:Bibliography208-51/94 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92)2011 Product CodeCommodity% Fat% Water% Sugars SECTION 201Pesticide Analytical Manual V
16、ol. I 201: PERCENTAGE FAT, WATER, AND SUGARS IN FOODS Methods in Chapters 3 and 4 are usually designated as applicable to either fatty (2%) or nonfatty (65 C.) Hold receiving flask with spring test tube holder, and place tip into steam. Position tip of receiving flask carefully to avoid “bumping” of
17、 solvent as it boils. Allow to boil until volume is slightly less than desired. Allow apparatus to cool and fluid to drain into receiving flask before removing column. Minimum attainable volume is about 0.2-0.4 mL. SECTION 202Pesticide Analytical Manual Vol. I Transmittal No. 94-1 (1/94) Form FDA 29
18、05a (6/92)2026 Rotary Evaporator Vacuum and heat combine to reduce the quantity of solvent in a rotary evapora- tor. Solution in a round-bottom (r-b) flask is simultaneously rotated and heated by a water bath, while a vacuum pulled from the end of a condenser increases the rate of evaporation. Solve
19、nt evaporated from the solution is collected in a second flask attached to condenser. Application. Evaporation of solvent using rotary evaporation is recommended for heat-labile residues, because temperature of the water bath used is much lower than that of a steam bath. Vacuum withdrawal of vapors,
20、 combined with water bath temperature of about 30 C, adequately removes solvents such as methylene chlo- ride (b.p. 40.5 C) without damaging analytes. Evaporation in a rotary evaporator is more rapid than in a K-D, but is limited to only one solution at a time. Equipment. 1) r-b flasks of appropriat
21、e volume. Flask that contains solution being evapo- rated has ground glass joint; flask that collects condensate has ball-and- socket joint. 2) rotary evaporator, including condenser and variable speed motor that rotates shaft to which r-b flask is attached. Use of glass trap connected to shaft betw
22、een motor and r-b flask is recommended to protect motor. Electronically controlled motor for constant torque is preferred to main- tain constant rotation throughout evaporation. Variable transformer for controlling speed is recommended only for evaporator with AC/DC motor; use of variable transforme
23、r on evaporator with AC motor will result in burning out evaporator motor. 3) constant temperature water bath 4) vacuum pump 5) needle valve to control vacuum, positioned between condenser and pump. Controlling vacuum with stopcock-type valve on condenser is also possible but is less precise than ne
24、edle valve and requires more analyst attention. Use of vacuum gauge (preferred) or manometer is also recommended. 6) (optional) additional traps between condenser and vacuum pump, to protect pump from effects of corrosive vapors. Refrigerated condensation traps and/or chemical traps that collect vap
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