FORD FLTM AK 117-1-2001 QUANTITATIVE ANALYSIS OF SOLVENT CONTENT OF CLEANERS.pdf

1、 FORD LABORATORY TEST METHOD AK 117-01 Date Action Revisions 2001 01 22 Revised Editorial no technical change A. Cockman 1990 04 26 Printed copies are uncontrolled Page 1 of 4 Copyright 2001, Ford Global Technologies, Inc. QUANTITATIVE ANALYSIS OF SOLVENT CONTENT OF CLEANERS Application This test me

2、thod is used to determine the percent solvent in a cleaner. The procedure is intended to be a simplified version of the applicable ASTM Standard (e.g. D 501 or D 800) as well as being more appropriate for dealing with the many formulations of cleaners that are commonly encountered in plant operation

3、s. Apparatus Required Analytical Balance Precision +/- 0.1 mg Distillation Flask Reflux Condenser Solvent Collection Trap Refer to ASTM D 322 Pycnometer Hot Plate Glass Beads or Pumice Stone Graduated Cylinder 250 mL The above apparatus is available from any reputable laboratory equipment supply hou

4、se. Materials Required Distilled or Deionized Water 20 micromhos/cm at 25 C maximum conductivity (ASTM D 1125) FORD LABORATORY TEST METHOD AK 117-01 Page 2 of 4 Copyright 2001, Ford Global Technologies, Inc. Potassium Carbonate Reagent grade Strontium Chloride or Silicone CAUTION: Strontium chloride

5、 is toxic. Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere of 23 +/- 2 C and 50 +/- 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure

6、Method 1 - For Water-immiscible solvents 1. Add a 10 g sample of the material to a distillation flask. 2. Add 200 mL of distilled water to the flask. 3. Assemble the apparatus which consists of: (a) Distillation flask (b) Reflux condenser (c) Solvent collection trap similar to ASTM D 322. This trap

7、serves to collect and measure the solvent and return the water to the distilling flask. 4. Starting with the solution at 23 +/- 2 C, heat the distillation flask so that the refluxing starts 10 minutes after heat has been applied. 5. Take a reading of the amount collected in the trap 2 h from the sta

8、rt of refluxing. 6. Make additional readings at the end of each subsequent 1 h period until the analysis is complete, that is, when the volume of solvent does not increase by more than 0.1 mL in any 2 consecutive 1 h periods. 7. Discontinue heating. 8. When the analysis is complete, allow the distil

9、late to stand for at least 1 h until it settles clear and cools to 23 +/- 2 C. FORD LABORATORY TEST METHOD AK 117-01 Page 3 of 4 Copyright 2001, Ford Global Technologies, Inc. 9. Read the volume of the solvent in the trap. 10. Immediately after reading, carefully remove the solvent with a pipet and

10、determine the specific gravity in a pycnometer (ASTM D 891, Method C). 11. Calculate % by weight of solvent. % Solvent = mL recovered x specific gravity x 100 Weight of sample Note: A. If alcohol or other volatile compounds that are soluble in water and solvents are present, incomplete solvent conte

11、nt will be obtained. B. Bumping may occur. C. Foaming may occur. To minimize and help prevent the possibility of foaming and bumping, add sufficient strontium chloride or silicone (3 to 5 g will usually suffice) to prevent foaming and a few glass beads or pumice stone to prevent bumping. If water so

12、luble compounds are present, the test procedure must be modified as indicated in Method II. Method II - For water-immiscible and water soluble solvents 1. Apparatus in Method I, except change the collecting trap to a 250 mL graduated cylinder. 2. Collect 90 % of the volatiles including the water in

13、the graduated cylinder. 3. Salt out the collection of solvent and water with powdered potassium carbonate. 4. Sufficient potassium carbonate must be added to have an excess of the powder in the graduated cylinder. 5. Allow to cool to 23 +/- 2 C. 6. Read the volume collected. 7. Carefully remove the

14、solvent with a pipet and determine the specific gravity. FORD LABORATORY TEST METHOD AK 117-01 Page 4 of 4 Copyright 2001, Ford Global Technologies, Inc. 8. Calculate % by weight of solvent. % Solvent = mL recovered x specific gravity x 100 weight of sample (g) Note: Infrared spectra should be used to identify the types of solvents that might be present. This is applicable to both methods. Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.