GB/T 18606-2017The test method for biomarkers in sediment and crude oil by GC-MS (English PDF)

Foreword

This Standard was drafted in accordance with the provisions of GB/T 1.1-2009.

This Standard is the substitute for GB/T 18606-2001 The Test Method for

Biomarkers in Sediment and Crude Oil by GC-MS. Compared with GB/T 18606-

2001, the major technical changes are as follows.

— The identification of the bicyclic sesquiterpene compound m/z 123 and

the illustration of its mass chromatogram were added (SEE 5.4);

— The identification of the naphthalene series compounds m/z 128; 142;

156; 170; 184; 198 and the illustration of their mass chromatograms were

added (SEE 5.4);

— The identification of the phenanthrene series compounds m/z 178; 192;

206; 220; 234 and the illustration of their mass chromatograms were

added (SEE 5.4);

— The identification of the fluoranthene, perylene and pyrene series

compounds m/z 202; 216; 228; 252 and the illustration of their mass

chromatograms were added (SEE 5.4);

— The identification of the biphenyl and dibenzofuran series compounds

m/z 154; 168; 182 and the illustration of their mass chromatograms were

added (SEE 5.4);

— The identification of the dibenzothiophene and benzo-naphthylthiophene

series compounds m/z 184; 198; 234 and the illustration of their mass

chromatograms were added (SEE 5.4);

— The identification of the fluorene series compounds m/z 166; 180 and the

illustration of their mass chromatograms were added (SEE 5.4);

— The quality chromatogram of the original standard was modified (SEE

Appendix B).

This Standard was proposed by China National Petroleum Corporation.

This Standard shall be under the jurisdiction of the National Technical

Committee for Standardization of Petroleum and Gas (SAC/TC 355).

Drafting organizations of this Standard. Research Institute of Petroleum

Exploration & Development, China National Petroleum Corporation; Wuxi

Institute of Petroleum Geology, Research Institute of Petroleum Exploration &

Development, China National Petroleum Corporation; College of Earth

Environment and Water Resources, Yangtze University; Research Institute of

The test method for biomarkers in

sediment and crude oil by GC-MS

1 Scope

This Standard specifies the GC-MS identification method and quality

requirements for saturated hydrocarbon and aromatic hydrocarbon component

biomarkers in sediment and crude oil.

This Standard is applicable to the analysis and identification of biomarker

compounds of saturated hydrocarbon and aromatic hydrocarbon components

in sediment and crude oil.

2 Normative references

The following documents are essential to the application of this document. For

dated references, only the editions with the dates indicated are applicable to

this document. For undated references, only the latest editions (including all the

amendments) are applicable to this document.

GB/T 6379.1-2004 Accuracy (trueness and precision) of measurement

methods and results - Part 1. General principles and definitions

3 Methodological principle

The saturated hydrocarbon and aromatic hydrocarbon components prepared

from the sediment and crude oil are separated by gas chromatography and

detected by mass spectrometry. After being processed by the data processing

system, the desired total ion chromatogram, mass chromatogram, and mass

spectrum are obtained.

4 Equipment and materials

252 mass chromatograms, as shown in Figure B.6;

4) Biphenyl and dibenzofuran series compounds m/z 154; 168; 182 mass

chromatograms, as shown in Figure B.7;

5) Fluorene series compounds m/z 166; 180 mass chromatograms, as

shown in Figure B.8.

1 C14H26 194 Bicyclic sesquiterpene (C14)

2 C14H26 194 Bicyclic sesquiterpene (C14)

3 C15H28 208 Bicyclic sesquiterpene (C15)

4 C15H28 208 Bicyclic sesquiterpene (C15)

5 C15H28 208 8beta(H)-drimane (C15)

6 C15H28 208 Bicyclic sesquiterpene (C15)

7 C16H30 222 Bicyclic sesquiterpene (C16)

8 C16H30 222 Bicyclic sesquiterpene (C16)

9 C16H30 222 Bicyclic sesquiterpene (C16)

10 C16H30 222 8beta(H)-homodrimane (C16)

Table 4 -- Identification table for compounds in the mass chromatogram

of aromatic hydrocarbons

Peak

No.

Mass

chromatogram

(m/z)

Molecular

formula

Molecular

weight Compound name

1 128 C10H8 128 Naphthalene

2 142 C11H10 142 2-methylnaphthalene

3 142 C11H10 142 1-methylnaphthalene

4 156 C12H12 156 2-ethylnaphthalene

5 156 C12H12 156 1-ethylnaphthalene

6 156 C12H12 156 2, 6-dimethylnaphthalene + 2, 7-dimethylnaphthalene

7 156 C12H12 156 1, 3-dimethylnaphthalene + 1, 7-dimethylnaphthalene

8 156 C12H12 156 1, 6-dimethylnaphthalene

9 156 C12H12 156 1, 4-dimethylnaphthalene + 2, 3-dimethylnaphthalene

10 156 C12H12 156 1, 5-dimethylnaphthalene

11 156 C12H12 156 1, 2-dimethylnaphthalene

12 170 C13H14 170 1, 3, 7-trimethylnaphthalene

13 170 C13H14 170 1, 3, 6-trimethylnaphthalene

14 170 C13H14 170 1, 3, 5-trimethylnaphthalene + 1, 4, 6-trimethylnaphthalene

15 170 C13H14 170 2, 3, 6-trimethylnaphthalene

16 170 C13H14 170 1, 2, 7-trimethylnaphthalene + 1, 6, 7-trimethylnaphthalene

17 170 C13H14 170 2, 3, 5-trimethylnaphthalene

18 170 C13H14 170 1, 2, 4-trimethylnaphthalene

19 170 C13H14 170 1, 2, 5-trimethylnaphthalene

20 170 C13H14 170 1, 2, 3-trimethylnaphthalene

52 206 C16H14 206 2, 3-dimethylphenanthrene

53 206 C16H14 206 1, 9 + 4, 9 + 4, 10-dimethylphenanthrene

54 206 C16H14 206 1, 8-dimethylphenanthrene

55 206 C16H14 206 1, 2-dimethylphenanthrene

56 234 C18H18 234 Retene

57 234 C16H10S 234 Benzo [b] naphthalene [2, 1-d] thiophenol

58 234 C16H10S 234 Benzo [b] naphthalene [1, 2-d] thiophenol

59 234 C16H10S 234 Benzo [b] naphthalene [2, 3-d] thiophenol

60 202 C16H10 202 Fluoranthene

61 202 C16H10 202 Pyrene

62 216 C17H12 216 Benzo [a] fluorene

63 216 C17H12 216 Benzo [b] fluorene + 4-methylpyrene

64 216 C17H12 216 2-methylpyrene

65 216 C17H12 216 1-methylpyrene

66 216 C17H12 216 Methyl fluoranthene

67 228 C18H12 228 Benzo [c] anthracene

68 228 C18H12 228 Benzo [a] anthracene

69 228 C18H12 228 Chrysene

70 252 C20H12 252 Benzo [k] fluoranthene

71 252 C20H12 252 Benzo [e] pyrene

72 252 C20H12 252 Benzo [a] pyrene

73 252 C20H12 252 Perylene

74 154 C12H10 154 Biphenyl

75 168 C13H12 168 3-methyl biphenyl

76 168 C13H12 168 4-methyl biphenyl

77 168 C12H8O 168 Dibenzofuran

78 182 C14H14 182 3-ethyl biphenyl

79 182 C14H14 182 3, 5-dimethylbenzidine

80 182 C14H14 182 3, 3'-dimethylbenzidine

81 182 C14H14 182 4-ethyl biphenyl

82 182 C14H14 182 3, 4'-dimethylbenzidine

83 182 C14H14 182 4, 4'-dimethylbenzidine

84 182 C13H10O 182 Methyl dibenzofuran

85 182 C13H10O 182 Methyl dibenzofuran

86 182 C13H10O 182 Methyl dibenzofuran

87 166 C13H10 166 Fluorene

88 180 C14H12 180 2-Methyl fluorene

89 180 C14H12 180 1-Methyl fluorene

3) Steranes shall be named for configurations at carbon positions 5, 8, 9,

10, 13, 14, 17, and 20. However, since some of these configurations are

stable and some cannot be changed by hydrogen exchange, regular

sterane only needs to be labeled as the configurations at carbon

positions 5, 14, 17 and 20, and diasterane only needs to be labeled as

the configurations at carbon positions 13, 17 and 20.

4) The nomenclature of hopane only needs to indicate the configurations at

carbon positions 17, 21, and 22.

5) Carbon loss and carbon addition. "nor-" for carbon loss, "homo-" for

carbon addition, and "nor-" or "homo-" group rankings are indicated by

Arabic numerals. For instance, 17alpha(H)-22, 29, 30 trisnorhopane; 17alpha(H),

21beta(H)-30 homohopane (22R). In case of ring carbon loss or carbon

addition, English capital letters A, B, C... shall be added before "nor-" or

"hemo-" to mark the indicated ring. For instance, 5alpha(H)-A-norcholestane.

6) Ring opening. Steroid and terpene rings are separated by "(seco-)", and

the position of broken bonds is indicated by Arabic numerals. For

instance, 8, 14-seco-hopane.

7) In hopane, the methyl group shifts from C-18 to C-17. The methyl group

at the C-18 position is replaced by H, which is denoted by "neo-". For

instance, 18alpha(H)-30 norneohopane (C29Ts).

d) Abbreviation

In order to facilitate geological applications, steranes and terpanes can be used

as abbreviations commonly used at home and abroad. The principle is to omit

the Arabic numerals for the chiral carbon position of the ring and the hydrogen,

and to name them according to the number of carbon atoms contained, as

shown in Table A.1.

Table A.1 -- Abbreviations of sterane and terpane compounds

Chemical nomenclature Abbreviation

5alpha(H), 14alpha(H), 17alpha(H)-C27 sterane (20R) alphaalphaalpha-C27 sterane (20R)

24-methyl-5alpha(H), 14beta(H), 17beta(H)-C28 sterane (20S) alphabetabeta-C28 sterane (20S)

24-ethyl-5alpha(H), 14alpha(H), 17alpha(H)-C29 sterane (20R) alphaalphaalpha-C29 sterane (20R)

4-methyl, 24-ethyl-5alpha(H), 14alpha(H), 17alpha(H)-C30 sterane (20R) alphaalphaalpha-C30 4-methyl sterane (20R)

17alpha(H)-C27 trisnorhopane Tm

17beta(H), 21alpha(H)-C29 hopane (normoretane) betaalpha-C29 normoretane

17alpha(H), 21beta(H)-C30 hopane alphabeta-C30 hopane

17alpha(H), 21beta(H)-C31 hopane (22R) alphabeta-C31 hopane (22R)

......