KS M 2418-2006 Standard test method for instrumental determination of carbon hydrogen and nitrogen in petroleum products and lubricants《石油产品和润滑剂的、碳、氢、氮的仪器分析试验方法》.pdf

1、 ?G?G?G?GG?G?G?G ?G?G?G G?G?G ?G?G G?G ?G 2006 5 2 KS M 2418 p* N*(*00ly J$;KS M 2418： 2006 M 2418： 2006 ( ) ( ) LG SK( ) ( ) ( ) ： ： 2006 5 2 2006 0186 ： ： ( ) ( 02 509 7271 3) . 7 5 , . ICS 75.080； 75.100 KS , M 2418： 2006Standard test method for instrumental determination of carbon, hydrogen, and

2、 nitrogen in petroleum products and lubricants 1. 1.1 , . , . 1.2 , , , . 75 87 %, 9 16 % 0.1 2 % . 1.3 , , , 0.75 % 2 . 1.4 , . 1.5 , % . , . 2. . . KS M 2001： 2000 ASTM D 4177 ASTM D 6299 3. 3.1 , . , ( ) . . 3.2 . . 3.2.1 ( ) , 3.2.2 3.3 , . . 3.3.1 M 2418： 2006 2 3.3.2 ( ) 3.3.3 ( ) 3.3.4 3.3.5

3、 (sulfurous and sulfuric acids) . 3.4 . 3.4.1 A (1)(2) , 2 . NOx N2 (train), CO2 NaOH, H2O (magnesium perchlorate) . , , CO2 H2O . 3.4.2 B (2)(3) (3.4.1 , ) CO2, N2 (mixing chamber) , . . . , . 3.4.3 C(2)(4) , NOx N2 . N2, CO2 H2O . . 3.5 , . 3.5.1 3.5.2 ( ) 3.5.3 3.6 . 4. 4.1 , ASTM . 4.2 , . CHN

4、 4.3 . . . . . 5. 5.1 . 5.2 . M 2418： 2006 3 5.2.1 , ( ) . , , . 5.2.2 . 5.2.2.1 (sulfur oxyacid) ( ). 5.2.2.2 ( ). 5.2.3 . 5.2.4 ( ) ( ) . 5.2.2 . 5.2.5 ( ) . . 5.2.5.1 (linear response) . 5.2.5.2 . 5.2.6 ( ) . 5.2.7 , . 5.3 , . 5.3.1 (tin capsules) , . 5.3.2 (ceramic crucibles) 5.3.3 (copper caps

5、ules) 5.3.4 (tin plugs) 5.3.5 (tin boats) 5.3.6 (copper plugs) 5.3.7 (aluminum capsules) 5.3.8 (combustion tubes) 5.3.9 (adsorption tubes) 5.3.10 (nickel capsules) 5.3.11 (reduction tubes) 5.4 0.000 01 g . 5.5 M 2418： 2006 4 1 CHN a,b ( %) ( %) ( %) (acetanilide) C8H9NO 71.09 6.71 10.36 (atropine) C

6、17H23NO370.56 8.01 4.84 (benzoic acid) C7H6O268.84 4.95 2,4 C12H14N4O451.79 5.07 20.14 (cyclohexanone 2,4 dinitrophenylhydrazone) (cystine) C6H12N2O4S229.99 5.03 11.66 (diphenyl) C12H1093.46 6.54 EDTA C10H16N2O841.10 5.52 9.59 (imidazol) C3H4N252.92 5.92 41.15 (nicotinic acid) C6H5NO258.53 4.09 11.3

7、8 (stearic acid) C18H36O275.99 12.76 (succinamide) C4H8N2O241.37 6.94 24.13 (sucrose) C12H22O1142.10 6.48 (sulphanilamide) C6H8N2O2S 41.84 4.68 16.27 (triethanol amine) C6H15NO348.30 10.13 9.39 a (Merk Index), 10 , & , , , 1983 b Aldrich, Alpha, Kodak (NIST) . 6.1 . 6. 6.1 . , . . 6.2 3.4.1 3.4.3 1

8、 6.3 6.3.1 (99.998 %) 6.3.2 (99.995 %) 6.3.3 , (pneumatic valve) 6.3.4 6.4 ( ) 5.2.2 5.2.3 . . . 6.4.1 A (1)(2) 6.4.1.1 (sodium hydroxide coated silica) 6.4.1.2 (quartz wool) 6.4.1.3 (magnesium perchlorate) 6.4.1.4 (copper turnings) 6.4.1.5 (coated calcium oxid e)( ) M 2418： 2006 5 6.4.1.6 (nitroge

9、n catalyst) 6.4.1.7 (magnesium oxide) (2)(5) 6.4.2 B (2)(3) 6.4.2.1 EA 1000 (2)(6) 6.4.2.2 MgO (silver tungstate) 6.4.2.3 (silver vanadate) 6.4.2.4 6.4.2.5 (silver gauze) 6.4.2.6 (copper oxide) (7) 6.4.2.7 (tungstic oxide) 6.4.2.8 (cobalt oxide) 6.4.2.9 (copper powder) 6.4.2.10 (sodium hydroxide coa

10、ted silica) 6.4.2.11 (alumina) 6.4.2.12 6.4.2.13 (platinum gauze) 6.4.3 C(2)(4) 6.4.3.1 6.4.3.2 (chromic oxid e)( ) 6.4.3.3 (silver coated cobalt oxide) 6.4.3.4 ( ) 6.4.3.5 6.4.3.6 (molecular Sieve) 3A 1/16 (1.6 mm) . 6.4.3.7 6.4.3.8 (chromosorb) (8), 6.4.3.9 (grain) (1) Leco CHN 600 Leco Corporatio

11、n , 3000 Lakeview Ave., St. Joseph, MI 49085 . (2) ASTM . . (3) Perkin Elmer 240C, 2400 CEC 240XA 440 Perkin Elmer Corporation , Main Ave,. Norwalk, CT 06856 . (4) Carlo Erba 1106, 1108 1500 Carlo Erba Strumentazione Strada Rivoltana, 20090 Rodano, Milan, Italy . (5) Leco Com aid Leco Corporation ,

12、3000 Lakeview Ave., St. Joseph, MI 49085 . (6) Perkin Elmer EA 1000 Perkin Elmer Corporation , Main Ave,. Norwalk, CT 06856 . (7) Perkin Elmer Cuprox Perkin Elmer Corporation , Main Ave,. Norwalk, CT 06856 . M 2418： 2006 6 (8) Carlo Erba Strumentazione Carlo Erba Strumentazione Strada Rivoltana, 200

13、90 Rodano, Milan, Italy . 6.5 . 12. . 7. , 7.1 KS M 2001 . 7.2 . 7.2.1 5 . 7.2.2 9. . 8. 8.1 ( ) . 8.2 1 . . 8.3 / ( ) . . . 50 300 . . 8.3.1 A (1)(2) 8.3.1.1 1 ( ) 5 cm . 1 . 2 ( ) 3.1 cm . (furnace reagent) 6.3 cm . 11.9 cm . 8.3.1.2 . N 8.8 cm . N 13.8 cm . 8.3.2 B (2)(3) 8.3.2.1 10 30 900 EA 100

14、0(3)(6) . . . 2.5 cm . EA 1000(3)(6) 5 cm . 2.5 cm . . 1 1.2 cm . (vial receptacle) 1.2 cm . 8.3.2.2 . 1 . . 23.8 cm . 1.2 cm 1 M 2418： 2006 7 . . 8.3.3 C(2)(4) 8.3.3.1 2 mm . 50 mm . 10 mm . 120 mm . 10 mm . O . 8.3.3.2 5 mm . . 10 mm . O . 8.3.3.3 10 mm . 3A 1/16(1.6 mm) (2)(6) . 10 mm . . 8.3.3.4

15、 10 mm . 50 mm . (2)(5) . 50 mm . 10 mm . . 9. 9.1 A (1)(2) 9.1.1 KS M 2001 50 200 mg 1 mg . . 9.1.1.1 . 9.1.1.2 (7) . . . 9.1.2 9.1.2.1 , 2 950 , 1 950 750 53 9.1.2.2 40 psi . 9.1.2.3 . 400 cm3/min( ) 70 cm3/min( ) 7 dm3/min 6 dm3/min 9.1.3 2 4 , 5 . 10 %, 1 % . 9.1.4 . (one point) . 9.1.5 (calibra

16、nt) . 1 % M 2418： 2006 8 . 9.1.6 . (matix) . 9.2 B(2)(3) 9.2.1 KS M 2001 2 4 mg 0.02 mg (vial) . 1/2 . 1/3 . 9.2.2 . 975 640 80 84 137.9 kPa 110.3 kPa , 413.7 kPa 9.2.3 2 4 . . . 9.2.4 (K) , (detection counts) . , / . 9.2.5 , . 9.3 C (2)(4) 9.3.1 KS M 2001 5 mg 0.02 mg . . 9.3.2 (8) 30 mg . 9.3.3 .

17、1 020 650 60 100 (filament) 190 420 20 70 70 2 9.3.4 . 100 kPa 20 cm3/min 200 kPa 40 cm3/min 80 cm3/min M 2418： 2006 9 60 cm3/min 500 kPa 3.5 kg/cm29.3.5 . 1 2 1 2 3 (linear regression calculation) 3 6 . . 9.3.6 . . 10 ( ). 1992 , 3 . . 13. 1992 . 10. 10.1 , . DCFEBA= (1) A： , ( %) B： , . C： , . D： (mg) E： (mg) F： , ( %) 10.2 . 11. 11.1 , % . 12. 12.1 (6.10) . 12.1.1 / . 12.1.2 / X1 / . 13. 13.1