FORD FLTM AK 110-1-2000 QUANTITATIVE ANALYSIS OF CARBONATES (AS CO2) IN CLEANERS.pdf

1、 FORD LABORATORY TEST METHOD AK 110-01 Date Action Revisions 2000 08 31 Revised Editorial no technical change A. Cockman 2000 03 23 Editorial no technical change A. Cockman 1992 06 03 Printed copies are uncontrolled Page 1 of 4 Copyright 2000, Ford Global Technologies, Inc. QUANTITATIVE ANALYSIS OF

2、CARBONATES (AS CO2) IN CLEANERS Application This test method is used to determine the percent carbonates in cleaners by the gas evolution method. The procedure is intended to be a simplified version of the applicable ASTM stand ard (e.g., D 501 or D 800) as well as being more appropriate for dealing

3、 with the many formulations of cleaners that are commonly encountered in plant operations. Apparatus Required Alkalimeter Heating Mantel Buret 50 mL Boiling Beads Flasks 300 mL and 500 mL Materials Required Hydrochloric Acid Concentrated; Reagent grade; CAUTION: Corrosive Sodium Hydroxide Reagent gr

4、ade; CAUTION: Corrosive Barium Chloride Reagent grade; CAUTION: Poisonous Sulfuric Acid Concentrated; Reagent grade; CAUTION : Corrosive Distilled or Deionized Water 10 ppm max total dissolved solids (ASTM D 1888) FORD LABORATORY TEST METHOD AK 110-01 Page 2 of 4 Copyright 2000, Ford Global Technolo

5、gies, Inc. Solutions Required Note: The following solutions must be free from CO 2 Sodium Hydroxide Solution 0.5 N Sulfuric Acid Solution 1:1 concentration Hydrochloric Acid Solution 0.5 N Phenolphthalein Indicator Dissolve 0.2 g in 50 mL of ethyl alcohol and add 50 mL of distilled water Barium Chlo

6、ride Solution 10 % concentration 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 otherwi

7、se specified. Procedure Gas Evolution Method (Alkalimeter) 1. Take a 0.5 to 1.0 g aliquot of the prepared 1 % solution of cleaner into the 300 mL distilling flask of the alkalimeter. 2. Add distilled water to make a volume of approximately 150 mL. 3. Buret 25 mL of 0.5 N sodium hydroxide into a 500

8、mL receiving flask and 10 m L into a 300 mL receiving flask. 4. Dilute the receiving flasks with distilled water to a volume of approximately 100 mL. FORD LABORATORY TEST METHOD AK 110-01 Page 3 of 4 Copyright 2000, Ford Global Technologies, Inc. 5. Assemble the apparatus using appropriate rubber an

9、d glass tubing, required stoppers and a vacuum line. The glass tube in the f irst receiving flask is a gas dispersion type with a fritted disc. It is preferred that ground glass joints be used instead of rubber stoppers. 6. Turn on the water in the condenser. 7. Turn on the vacuum line. 8. Add 30 mL

10、 of 1:1 sulfuric acid into th e bulb of the distilling apparatus (alkalimeter). 9. Allow the sulfuric acid to enter the distilling flask gradually until all of it has been added. The petcock is used to adjust the rate of flow. Shut petcock when all acid has been introduced. 10. Swi rl flask to dispe

11、rse the acid. 11. Heat the distillation flask to boiling. Note: Bumping may occur; use of boiling beads is recommended. The heating rate must be gradual to minimize this effect. 12. Adjust rate of flow using the vacuum line so that bub bling is uniform and kept at a minimum. 13. Boil for 20 minutes.

12、 14. Shut off heat. 15. Continue purging distillation flask for an additional 30 to 40 minutes. 16. Release pressure in the receiving flask by breaking the seal at the stopper so that ther e will be no backup of sodium hydroxide into the distilling flask. 17. Shut off vacuum line. 18. Rinse condense

13、r into first receiving flask with distilled water. 19. While disassembling, rinse glass tubing with distilled water. FORD LABORATORY TEST METHOD AK 110-01 Page 4 of 4 Copyright 2000, Ford Global Technologies, Inc. 20. Add 25 mL and 10 m L of neutral 10 % barium chloride solution respectively into ea

14、ch receiving flask. 21. Add 5 drops of phenolphthalein indicator to each flask. 22. Titrate with 0.5 N hydrochloric acid solution. Solution turns from pink to colorless in each flask. Note: The second receiving flask is normally used for a backup in case the CO 2 is not all absorbed in the first rec

15、eiving flask. 23. Calculate the % of CO 2 % CO 2 = (mL 0.5 N NaOH - mL 0.5 N HCL) x 0.011 x 100 weight of sample Chemicals, materials, par ts, 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.