1、 FORD LABORATORY TEST METHOD AS 001-01 Date Action Revisions 2001 01 31 Revised Editorial no technical change A. Cockman 2000 04 25 Editorial no technical change A. Cockman 1992 05 01 Printed copies are uncontrolled Page 1 of 3 Copyright 2001, Ford Global Technologies, Inc. TEST FOR DICYCLOHEXYLAMMO
2、NIUM NITRITE Application This procedure is used to determine the amount of volatile corrosion inhibitor in treated papers. It should only be used for papers which have dicyclohexylammonium nitrite as the single corrosion inhibitor in the paper. Apparatus Required Photelometer or Spectrophotometer Th
3、e Photelometer or Spectrophotometer used in this test shall have a transmission band at 540 Mu with maximum band width of 60 Mu. Solutions Required Hydrochloric Acid (1:1) Dilute 25 mL of HCl Sp. Gr. 1.18 with an equal volume of distilled water. Sulfanilamide Solution - 0.2 % Weigh 1.0 g of the reag
4、ent, Eastman No. 4378, dissolve in distilled water and dilute to 500 mL. Store in a dark bottle and renew the solution every two months. N-1 Naphthylethylenediamine Dihydrochloride - 0.1 % Solution Weigh 1.0 g of the reagent, Eastman No. 4835, dissolve in distilled water and dilute to 1000 mL. Store
5、 in a dark bottle and renew the solution every two months. Standard Sodium Nitrite Solution Dissolve 1.0000 g of CP NaNO2 in distilled water and dilute to 1000 mL in a volumetric flask and mix thoroughly. Dilute 10 mL of this solution to 1000 mL with distilled water and mix thoroughly. Each mL of th
6、e resulting dilute standard solution contains 10 micrograms (0.010 milligrams) of sodium nitrite equivalent to 33 micrograms of dicyclohexylammonium nitrite. This solution should be stored in a dark bottle and made fresh every two months. FORD LABORATORY TEST METHOD AS 001-01 Page 2 of 3 Copyright 2
7、001, Ford Global Technologies, Inc. Standardization Prepare a curve on graph paper plotting the Photelometer reading vs. dicyclohexylammonium nitrite as follows: Introduce 1, 2, 3, 4 and 5 mL of the dilute sodium nitrite solution into separate 50 mL volumetric flasks and proceed with development of
8、the color as directed in the procedure for analysis, starting with Step 4. To another 50 mL flask add the reagents alone starting with Step 4 of the procedure. This solution will contain no nitrite but will be used as a blank on the reagents. Measure the absorption of each solution and subtract the
9、reading of the blank from those of the other standards. Plot these corrected readings against the number of micrograms of dicyclohexylammonium nitrite (3.3 times sodium nitrite values). Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlle
10、d 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 1. Cut an accurately measured 1 inch square piece of coated carrier into strips 1/8 x 1/2 inch (approx.) and place in a 500 m
11、L volumetric flask. 2. Fill the flask to the mark with distilled water, stopper and shake well. Allow to stand for 20 - 30 minutes with occasional agitation. Note: Dicyclohexylammonium nitrite is completely extracted for most treated carriers within 20 or 30 minutes with less time required for paper
12、 than for cardboard or laminated materials. In some cases where the dicyclohexylammonium nitrite has been occluded, a supplementary analysis should be made several hours later to determine completeness of extraction. 3. Place approximately 15 mL of distilled water in a 50 mL volumetric flask and pip
13、ette a 5 mL aliquot of the above extract into this flask. 4. Add 1 mL of dilute HCl (1:1). FORD LABORATORY TEST METHOD AS 001-01 Page 3 of 3 Copyright 2001, Ford Global Technologies, Inc. 5. Add 5 mL of sulfanilamide solution. 6. Allow solution to stand a minimum of five minutes with intermittent ag
14、itation. 7. Add 1 mL of N-1 naphthalethylenediamine solution. 8. Allow to stand at least ten minutes with intermittent agitation. 9. Fill to volume, shake well, transfer to a cell of the Photelometer or Spectrophotometer and measure the absorbency of the resulting colored solution. 10. Convert the P
15、hotelometer readings to micrograms of dicyclohexylammonium nitrite by means of the standardization curve. Convert further to grams per square foot coating on the carrier by multiplying by 0.0144. 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.
