KS M 0027-2008 General rules for analytical methods in gas chromatography mass spectrometry《气相色谱法 质量分析通则》.pdf

1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS M 0027 KS M 0027:2008 2008 12 19 http:/www.kats.go.krKS M 0027:2008 : ( ) ( ) ()MPT ( ) : (http:/www.standard.go.kr) ： ： 1983 10 20 ： 2008 12 19 2008-0927 ： ： ( 025097301) (http:/www.kats.go.kr). 10 5 , . KS M 0027:2008 General rules for analytical metho

2、ds in gas chromatography mass spectrometry 1 , . ( .) . 2 . . ( ) . KS M 0001, KS M 0025, KS M 0031, 3 . . 3.1 (gas chromatograph mass spectrometer, ： GC/MS) 3.2 (gas chromatography mass spectrometry, ： GC/MS) (GC/MS) . 3.1 GC/MS . 3.3 (magnetic field type) / (m/z) 3.4 KS M 0027:2008 2 3.5 3.6 (quad

3、rapole type) / (m/z) 3.7 (total ion detection or total ion monitoring, ： TID TIM) . 3.8 (total ion chromatogram) (TID) 3.9 (selected ion detection or selected ion monitoring, ： SID SIM) . 3.10 (mass fragmentography, ： MF) (SID) . . 3.11 (mass chromatography, ： MC) , . . 3.12 (reconstructed ion chrom

4、atogram, ： RIC) 3.13 2 (secondary electron multiplier, ： SEM) 2 3.14 (electron accelerating voltage) 3.15 (ion accelerating voltage) KS M 0027:2008 3 3.16 (ionization energy) , 3.17 (emission current) 3.18 (repeller electrode) 3.19 (lens electrode) 3.20 (electron ionization, ： EI) . 3.21 (chemical i

5、onization, ： CI) . 3.22 (reagent gas) (CI) 3.23 (reactant ion) (CI) 3.24 (field ionization) . 3.25 (atomic mass unit, ： u) , 12C 1/12 1 3.26 (milli mass unit, ： mu) 1 u 1/1 000 3.27 (mass number) (u) KS M 0027:2008 4 3.28 / (mass-to-charge ratio, ： m/z) (u) 3.29 / (m/z) . / (m/z) , . . 3.30 (backgro

6、und) 3.31 (molecular ion, ： M, M) 3.32 (rearrangement ion) 3.33 (fragmention) 3.34 (adduct ion) 3.35 (base peak) . . 3.36 3.37 3.38 (capillary column) 3.39 KS M 0027:2008 5 3.40 , 4 (GC/MS) , . / (m/z) , . 5 5.1 1 , . . 1 ( ) 5.2 a) f) . a) , , , . . b) (septum) , , . KS M 0027:2008 6 c) . d) , ( 35

7、0 ) (1 20 /min ) , . 150 0.5 . e) . . f) . . 5.3 , , . . , 2 . a) 1 b) 2 c) 2 ( ) 5.4 a) f) . KS M 0027:2008 7 a) , , , , . . (EI)1), (CI)2), (FI)3) 3 . 3 . A D G B E H C F I 2 ( ) b) / (m/z) 2 . 1) (collector) 2 . . 4 5 . 2) 4 4) , 6 . 1) (EI) 10 eV . , . 2) (CI) ( CH4) 0.1 kPa ( CH3, C2H5) . (M1)

8、. 3) (FI) , . . 4) 5 10 mm, 10 20 cm . . C D E F G H I A B KS M 0027:2008 8 A D B E C F 3 ( ) a) A E B F C G D 4 ( ) C E F B A G FEDC ABDKS M 0027:2008 9 b) A E B F C G D 5 ( )( ) A D B E C F 5 ( ) c) , 103 107 2 (SEM)5), (TID) 6) . , (collector slit) . . a) (TID) , (TID) (beam monitor)7) / (m/z) 5)

9、 . 6) 2 . 7) , (He) (back ground) (24.6 eV) . E F G DC A B EF DCB A KS M 0027:2008 10 ( )8) . b) (SlD) , / (m/z) ( ), . , / (m/z) , . c) , , 2 (SEM) . / (m/z) . d) , (oscillograph) . . . e) 1) 4) . . 1) , , , . 2) . , . 3) 2 (SEM) , (gain) . 4) , . f) (1.310 4 1.310 5Pa) , , , . , . 5.5 5.5.1 (DS) ,

10、 , , , , , , CRT, , . 5.5.2 , (probe), , . 8) , . KS M 0027:2008 11 5.5.3 , ( ) , . 6 6.1 . a) ( 15 30 ), ( 70 % ) , b) . c) , . d) . e) , 5 % , . f) , . g) . h) , , , ( , ) . i) . 6.2 9) . a) . 1) . 2) . 3) . 4) , , 10), , (FI) , , . 5) , , . 6) , , , , . b) . c) 99.8 % . (CI) 99 % , . 9) . 10) . K

11、S M 0027:2008 12 d) . 1) (m/z) . , . (perfluorokerosene ： PFK) (perfluorotributylamine ：PFTBA) , 1 2 . KS M 0027:2008 13 1 (PFK) (u) (u) 69 CF368.995 207 L 455 C11F17454.972 837 74 C3F273.996 804 467 C12F17466.972 837 81 C2F380.995 207 469 C9F19468.969 642 93 C3F392.995 207 481 C10F19480.969 642 100

12、 C2F499.993 609 M 193 C11F19492.969 642 105 C4F3104.995 207 505 C12F19504.969 642 117 C5F3116.995 207 517 C13F19516.969 642 119 C2F5118.992 011 L 519 C10F21518.966 446 131 C3F5130.992 011 L 531 C11F21530.966 446 143 C4F5142.992 011 543 C12F21542.966 446 155 C5F5154.992 011 555 C13F21554.966 446 167

13、C6F5166.992 011 567 C14F21566.966 446 169 C3F7168.988 815 L 569 C11F23568.963 251 181 C4F7180.988 815 L 581 C12F23580.963 251 193 C5F7192.988 815 593 C13F23592.963 251 205 C6F7204.988 815 605 C14F23604.963 251 217 C7F7216.988 815 617 C15F23616.963 251 219 C4F9218.985 620 M 619 C12F25618.960 055 231

14、C5F9230.985 620 M 631 C13F25630.960 055 243 C6F9242.985 620 643 C14F25642.960 055 255 C7F9254.985 620 655 C15F25654.960 055 267 C8F9266.985 620 667 C16F25666.960 055 269 C5F11268.982 424 681 C14F27680.956 859 281 C6F11280.982 424 M 693 C15F27692.956 859 293 C7F11292.982 424 705 C16F27704.956 859 305

15、 C8F11304.982 424 717 C17F27716.956 859 317 C9F11316.982 424 731 C15F29730.953 664 319 C6F13318.979 229 743 C16F29742.953 664 331 C7F13330.979 229 755 C17F29754.953 664 343 C8F13342.979 229 767 C18F29766.953 664 355 C9F13354.979 229 781 C16F31780.950 468 367 C10F13366.979 229 793 C17F31792.950 468 3

16、69 C7F15368.976 033 805 C18F31804.950 468 381 C8F15380.976 033 817 C19F31816.950 468 393 C9F15392.976 033 831 C17F33830.947 273 405 C10F15404.976 033 843 C18F33842.947 273 417 C11F15416.976 033 855 C19F33854.947 273 419 C8F17418.972 837 867 C20F33866.947 273 431 C9F17430.972 837 443 C10F17442.972 83

17、7 L： 10 % , M： 510 %, ： 5 % KS M 0027:2008 14 2 (PFTBA) (u) (u) 69 CF368.995 2 L( ) 219 C4F9218.985 6 L 100 C2F499.993 6 264 C5F10N 263.987 1 M 114 C2F4N 113.996 7 414 C8F16N 413.977 5 119 C2F5118.992 0 M 502 C9F20N 501.971 1 131 C3F5130.992 0 L 614 C12F24N 613.964 7 169 C3F7168.988 8 181 C4F7180.988 8 L： 10 % , m： 510 %, ： 5 % 2) . 10 % , 1 5 % . 3 10 % 11). 3) . . (R) 7 10 % (valley), . a) 10 % (valley) b) MMR= WWMMR= R M M W W 6 4) , 11) ( , , , , ) .