FORD FLTM AK 108-1-2000 QUANTITATIVE ANALYSIS OF COMBINED AND FREE AMMONIA IN AMMONIUM SALTS IN CLEANERS.pdf

1、 FORD LABORATORY TEST METHOD AK 108-01 Date Action Revisions 2000 08 31 Revised Editorial no technical change A. Cockman 2000 03 23 Editorial no technical change A. Cockman 1991 09 24 Printed copies are uncontrolled Page 1 of 3 Copyright 2000, Ford Global Technologies, Inc. QUANTITATIVE ANALYSIS OF

2、COMBINED AND FREE AMMONIA IN AMMONIUM SALTS IN CLEANERS Application This test method is used to determine the percent of combined and free ammonia in ammonium salts found in cleaners. The procedure is intended to be a simplifie d version of the applicable ASTM standard (e.g., D 501 or D 800) as well

3、 as being more appropriate for dealing with the many formulations of cleaners that are commonly encountered in plant operations. Apparatus Required Hot Plate Distillation Apparatus Distilling Flask 1,000 mL; similar to a Kjeldahl or a boiling flask with ground glass joints. Buret 50 mL Flask 500 mL

4、Boiling Chips The above apparatus is available from any reputable laboratory equipment supply house. Materials Required Distilled or Deionized Water 10 ppm max total dissolved solids (ASTM D 1888) Hydrochloric Acid Concentrated, Reagent grade; CAUTION: Corrosive FORD LABORATORY TEST METHOD AK 108-01

5、 Page 2 of 3 Copyright 2000, Ford Global Technologies, Inc. Sodium Hydroxide Reagent grade; CAUTION: Corrosive Red Litmus Paper Solutions Required Sodium Hydroxide Solutions - 50 % concentration - 0.5 N - Refer to FLTM AZ 102 - 01 Methyl Red Indicator Refer to FLTM AZ 102 - 01 Conditioning and Test

6、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 I. Combined Ammonia 1. Take a 1

7、 to 2 g aliquot of the prepared 1 % solution in a 1 000 mL distilling flask. 2. Add 250 mL of distilled water to the Kjeldahl flask. 3. Add boiling chips to this flask. 4. Buret 40 mL of 0.5 N hydrochloric acid into a 500 mL receiving flask. 5. Add five drops of methyl red indicator to this receivin

8、g flask. 6. Connect the rece iving flask to the condenser, making sure that the glass outlet tube is immersed in the acid solution. 7. Add 50 mL of a 50 % sodium hydroxide solution to the distilling flask. Note: Be sure that the sodium hydroxide does not come in contact with the gr ound glass joints

9、. 8. Immediately connect the distilling flask to the water condenser which has ground glass joints by means of a glass connecting arm which is also equipped with ground glass joints. FORD LABORATORY TEST METHOD AK 108-01 Page 3 of 3 Copyright 2000, Ford Global Technologies, Inc. 9. Swirl contents of

10、 the distilling flask. 10. Heat the contents of the flask. 11. After 200 mL of distillate has been collected in the receiving flask, check for completeness of the test by opening the tube in the connecting arm of the distilling flask and test for ammonia with moist red litmus paper. 1 2. When comple

11、te, remove the heat and receiving flask. 13. After disassembly, wash the condenser and collecting tube with distilled water into the receiving flask. 14. Titrate the recovered distillate with 0.5 N sodium hydroxide. 15. Calculate the % of NH 3 % NH 3 = (mL 0.5 N HCl - mL 0.5 N NaOH) x 0.008515 x 100

12、 weight of sample Note: Organic - bearing nitrogen compounds may interfere with this determination. I. Free Ammonia 1. Take 20 to 50 g of the sample as received. 2. All steps in Method I are repeated with the exception that caustic soda addition is omitted in this determination. (Steps 2 through 15, omitting step 7). Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is respo nsible for determining proper use and handling in its facilities.