1、 FORD LABORATORY TEST METHOD AK 114-01 Date Action Revisions 2001 01 22 Revised Editorial no technical change A. Cockman 2000 03 23 Revised Editorial no technical change A. Cockman 1991 09 24 Printed copies are uncontrolled Page 1 of 3 Copyright 2001, Ford Global Technologies, Inc. QUANTITATIVE ANAL
2、YSIS OF SULFATES IN CLEANERS Application This test method is used to determine the percent sulfates 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 cl
3、eaners that are commonly encountered in plant operations. Apparatus Required Analytical Balance Precision +/- 0.1 mg. Muffle Furnace Must be capable of maintaining 800 +/- 10 C. Steam Bath Hot Plate Desiccator With desiccant. Platinum Crucible Buret or Pipet Beaker 400 mL Funnel Suitable for use wit
4、h filter paper. The above apparatus is available from any reputable laboratory equipment supply house. FORD LABORATORY TEST METHOD AK 114-01 Page 2 of 3 Copyright 2001, Ford Global Technologies, Inc. Materials Required Hydrochloric Acid Concentrated; Reagent grade; CAUTION: Corrosive. Hydrofluoric A
5、cid Concentrated; Reagent grade; CAUTION: EXTREMELY CORROSIVE - SPECIAL HANDLING PRECAUTIONS MUST BE EMPLOYED. Barium Chloride Reagent grade; CAUTION: Poisonous. Distilled or Deionized Water 10 ppm max total dissolved solids (ASTM D 1888). Filter Paper Must be suitable for fine precipitates. Solutio
6、ns Required Hydrochloric Acid Solution 1:1 Barium Chloride Solution 10 % concentration (with distilled water). 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 th
7、an 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure 1. Take a 0.5 to 1.0 g aliquot of the prepared 1 % solution of cleaner in a 400 mL beaker. 2. Dilute to 200 mL with distilled water. 3. Add 10 mL of 1:1 hydrochloric acid. Make sure that an excess of
8、acid has been added. FORD LABORATORY TEST METHOD AK 114-01 Page 3 of 3 Copyright 2001, Ford Global Technologies, Inc. 4. Heat to boiling. 5. Add a 10 % solution of barium chloride in a fine stream from a buret or pipet at the rate of 10 mL in 2 to 10 minutes. The reagent is added in slight excess of
9、 that required to react with the sulfate radical. (Ten mL of 10 % BaCl2 solution will precipitate about 0.13 g of sulfur.) 6. The beaker is placed on a steam bath and the precipitate allowed to settle for at least one h. The solution is filtered through a fine grade of filter paper. Since the precip
10、itate frequently passes through the filter, it is advisable always to pass the solution through the same filter a second time. The precipitate is washed for at least 10 times with hot distilled water then dried and ignited gently with a burner for 30 minutes in a tared crucible, followed by ignition
11、 in a muffle furnace. (Blasting is not necessary, nor desirable.) The white barium sulfate is cooled in a desiccator and then weighed. The sulfur-bearing compounds so determined are calculated as SO4 based on the weight of sample used. The precipitate is usually ignited at 800 C for one h, cooled in
12、 a desiccator and weighed. Note: A. A final volume of 350 mL with 0.8 g of precipitate under the above conditions has been proven to be highly satisfactory. The presence of KNO3 and probably any nitrate is objectionable. B. Siliceous-bearing matter may also be precipitated with the above method. The
13、 barium sulfate should be purified by using a platinum crucible and HF to remove the SiO2. Factors to use for calculations: (1) Wt BaSO 4 x 0.41158 x 100 = % SO4 (2) % SO4 x 1.4789 = % Na2SO4 (3) % SO4 x 1.8141 = % of K2SO4 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.
