FORD FLTM AK 103-02-2001 QUANTITATIVE ANALYSIS OF NITRITE (AS NO2) IN CLEANERS《清洁剂中亚硝酸盐(如二氧化氮)的定量分析》.pdf
《FORD FLTM AK 103-02-2001 QUANTITATIVE ANALYSIS OF NITRITE (AS NO2) IN CLEANERS《清洁剂中亚硝酸盐(如二氧化氮)的定量分析》.pdf》由会员分享,可在线阅读,更多相关《FORD FLTM AK 103-02-2001 QUANTITATIVE ANALYSIS OF NITRITE (AS NO2) IN CLEANERS《清洁剂中亚硝酸盐(如二氧化氮)的定量分析》.pdf(8页珍藏版)》请在麦多课文档分享上搜索。
1、 FORD LABORATORY TEST METHOD AK 103-02 Date Action Revisions 2001 01 22 Revised Editorial no technical change A. Cockman 2000 03 22 Revised Editorial no technical change A. Cockman 1990 02 14 Printed copies are uncontrolled Page 1 of 8 Copyright 2001, Ford Global Technologies, Inc. QUANTITATIVE ANAL
2、YSIS OF NITRITE (AS NO2) IN CLEANERS Application This method describes two test procedures for determining the percent nitrite in a cleaner. The procedures are: distillation method by conversion to NH3 (preferred) and the permanganate method. Apparatus Required Analytical Balance - Having a precisio
3、n of +/- 0.1 mg Hot Plate Distillation Apparatus Titration Apparatus Kjeldahl Distillation Flask - 500 mL Erlenmeyer Flask - 500 mL Graduated Cylinder - 100 mL Materials Required Mossy Zinc Reagent grade Ferrous Sulfate Reagent grade Sodium Hydroxide Reagent grade. CAUTION: Corrosive Distilled or De
4、ionized Water 10 ppm max total dissolved solids (ASTM D 1888) FORD LABORATORY TEST METHOD AK 103-02 Page 2 of 8 Copyright 2001, Ford Global Technologies, Inc. Kerosene, Silicone or Strontium Chloride Refer to Note “A“ in the Procedure. CAUTION: Kerosene has a low flash point; strontium chloride is t
5、oxic. Potassium Permanganate Reagent grade. CAUTION: Dangerous fire and explosion hazard. Solutions Required Hydrochloric Acid Solution - 0.5 N Sodium Hydroxide Solution - 30 % cone and 0.5 N Methyl Red Refer to FLTM AZ 102-01 Potassium Permanganate - 0.1 N (KMnO4) Ferrous Sulfate - 0.1 N (FeSO4) Su
6、lfuric Acid - 50 % 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. Pr
7、ocedure for Distillation Method The Distillation Method by Conversion to NH3 is preferred. 1. Place a 0.5 to 1.0 g aliquot of the prepared 1 % solution of cleaner into a 500 mL Kjeldahl distillation flask. 2. A receiving flask containing methyl red indicator and 25 mL of 0.5 N HCl must be in place p
8、rior to starting the distillation. 3. The end of the delivery tube must be immersed in the HCl solution during the distillation. 4. Dilute the sample in the distilling flask to 250 mL with distilled water. 5. Add to this 5.0 g of mossy zinc and 2.0 g of ferrous sulfate. FORD LABORATORY TEST METHOD A
9、K 103-02 Page 3 of 8 Copyright 2001, Ford Global Technologies, Inc. 6. Add 50 mL of a 30 % sodium hydroxide solution being careful not to touch the sides or lip of the flask. 7. Agitate this mixture by swirling. 8. Distillation should then be made for 3/4 to 1 hour until approximately half of the vo
10、lume of liquid in the distilling flask has been recovered in the receiving flask. 9. Wash the condenser and tube with distilled water into the receiving flask. 10. Titrate the excess 0.5 N HCl with 0.5 N NaOH. 11. Calculate the amount of NO2 as follows: % NO2 = A - B x 0.023 x 100 C Where: A = mL of
11、 0.5 N HCl B = mL of 0.5 N NaOH C = Weight of sample, grams Note “A“: On occasion, excessive foaming may take place. Addition of kerosene, silicone or strontium chloride to the distillation flask normally suppresses this foaming tendency. General Notes on the Distillation Method Nitrite, nitrate, am
12、monia and ammonium are quantitatively detected by this method. If two or more of these species are present, the result must be interpreted as total nitrogen. This may be useful information, since the contribution from ammonia, ammonium and nitrite can be determined by alternate methods. Some organic
13、 compounds also partly distill or give off ammonia on distillation with strong alkali. Mono, di-, and tri- ethanolamine, EDTA and other nitrogen-bearing compounds will contribute to the result but not in a quantitative manner. The presence of these nitrogen-bearing compounds is therefore undesirable
14、. For samples containing a low concentration of nitrite, better accuracy can be obtained by analyzing a larger sample. If the observed titration is less than 0.5 mL, the distillation must be repeated with a larger sample. This is necessary to ensure that nitrite is actually present in the sample bei
15、ng analyzed. FORD LABORATORY TEST METHOD AK 103-02 Page 4 of 8 Copyright 2001, Ford Global Technologies, Inc. General Information for the Distillation Method 1. In the basic solution, ferrous sulfate quantitatively reduces nitrite to ammonia in the presence of zinc. The ammonia is distilled into a r
16、eceiving flask containing standard 0.5 N HCl and neutralized. The excess HCl is titrated with standard 0.5 N NaOH. 2. The amount of nitrite in the sample, expressed as % NO2, is calculated as follows: % NO2 = (mL of 0.5 N HCl used to neutralize the NH 3) x 0.023 x 100 weight of sample (grams) 3. The
17、 mathematical factor in the formula is obtained as follows: 0.023 = 0.5 mol HCl x L x mol NH 3 x mol NO 2 x 46.0 g NO 2 L 1000 mL mol HCl mol NH3 mol NO2 4. The method also quantitatively reduces nitrate to ammonia and can be used as an alternative to FLTM AK 113-01. If nitrate is the only nitrogen
18、species present, the amount of nitrate, expressed as % NO3 can be calculated by substituting 0.031 for 0.023 in the formula. Procedure for the Permanganate Method 1. Place a 0.5 to 1.0 g aliquot of the prepared 1 % solution in a 500 mL Erlenmeyer flask. 2. Add distilled water to obtain a total volum
19、e of 200 mL. 3. Add 10 mL of 1:1 sulfuric acid. 4. Add potassium permanganate until a pink color persists. 5. To a fresh sample identical in size to the preliminary sample of material, add this amount of potassium permanganate plus 10 mL excess. 6. Then add 10 mL of 1:1 sulfuric acid. 7. Titrate the
20、 excess of permanganate with ferrous sulfate solution until the pink color is gone. 8. Add a slight excess of ferrous sulfate. 9. Titrate again with permanganate until one drop of permanganate makes a pink color persist. FORD LABORATORY TEST METHOD AK 103-02 Page 5 of 8 Copyright 2001, Ford Global T
21、echnologies, Inc. 10. Record the total volume of permanganate solution used. 11. Record the total volume of ferrous sulfate solution used. 12. Calculate the percent of nitrite as % NaNO2 by the following: % NaNO2 = A - B x 0.003451 x 100 C Where: A = mL of 0.1 N KMnO4 used B = mL of 0.1 N FeSO4 used
22、 C = Weight of sample, grams % NO2 = % NaNO 2 1.5 General Notes for the Permanganate Method Other materials oxidizable by potassium permanganate must be absent. For samples containing a low concentration of nitrite, better accuracy can be obtained by analyzing a larger sample. Glassware may be stain
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