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GB/T 18606-2017 English PDF (GBT18606-2017)

GB/T 18606-2017 English PDF (GBT18606-2017)

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GB/T 18606-2017: The test method for biomarkers in sediment and crude oil by GC-MS

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.
GB/T 18606-2017
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 75.040
E 21
Replacing GB/T 18606-2001
The test method for biomarkers in
sediment and crude oil by GC-MS
ISSUED ON. MAY 12, 2017
IMPLEMENTED ON. DECEMBER 1, 2017
Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the PEOPLE Republic of China;
Standardization Administration of the PEOPLE Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Methodological principle ... 5
4 Equipment and materials ... 5
5 Analytical procedure ... 6
6 Quality requirements ... 13
Appendix A (Informative) Compound structure and nomenclature ... 15
Appendix B (Informative) Mass chromatogram ... 19
References ... 24
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
4.1 Gas chromatography-mass spectrometer. A gas chromatograph with
programmed temperature rising function and a mass spectrometer and data processing system with an EI ion source and a maximum scanning mass of not less than 650amu.
4.2 Gas chromatographic column. The stationary phase is 5% benzyl siloxane 5.3.2 Perfluorotributylamine is tuned to the normal operating state. The ratio of each ion peak after tuning should be appropriate. If it is required to comply with spectral library retrieval, the ion peak of m/z 69 shall be tuned to 100%; the ion peak of m/z 219 shall be tuned to less than or equal to 80%, and greater than or equal to 40%; the ion peak of m/z 502 shall be tuned to greater than or equal to 2%, and less than or equal to 5%.
5.3.3 SET the analysis conditions for samples.
5.3.4 After the blank and internal management samples have passed the test, the saturated hydrocarbons and aromatic hydrocarbons are dissolved in n- hexane or dichloromethane prior to sample determination.
5.3.5 CARRY out data processing.
5.4 Analysis report
5.4.1 Mass chromatogram
At least the following spectrograms shall be extracted from the analysis report. a) Saturated hydrocarbons include.
1) Tricyclic terpane and hopane m/z 191 mass chromatogram, as shown in
Figure B.1;
2) Sterane m/z 217 mass chromatogram, as shown in Figure B.2;
3) Bicyclic sesquiterpene m/z 123 mass chromatogram, as shown in Figure B.3.
b) Aromatic hydrocarbons include.
1) Naphthalene series compounds m/z 128; 142; 156; 170; 184; 198 mass
chromatograms, as shown in Figure B.4;
2) Phenanthrene series compounds m/z 178; 192; 206; 220; 234 mass
chromatograms, as shown in Figure B.5;
3) Fluoranthene, perylene and pyrene series compounds m/z 202; 216; 228; 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.
5.4.2 Qualitative results
SEE Appendix A for the nomenclature of saturated hydrocarbon and aromatic hydrocarbon. For the qualitative results of saturated hydrocarbon, SEE
Appendix B for related spectrograms as well as Table 1 (tricyclic terpane and Table 3 -- Identification table for bicyclic sesquiterpene compounds in m/z 123 mass chromatogram
Peak No. Molecular formula Molecular weight Compound name
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 8??(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 8??(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, 17??(H)-22, 29, 30 trisnorhopane; 17??(H), 21??(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, 5??(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, 18??(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
5??(H), 14??(H), 17??(H)-C27 sterane (20R) ??????-C27 sterane (20R)
24-methyl-5??(H), 14??(H), 17??(H)-C28 sterane (20S) ??????-C28 sterane (20S) 24-ethyl-5??(H), 14??(H), 17??(H)-C29 sterane (20R) ??????-C29 sterane (20R)
4-methyl, 24-ethyl-5??(H), 14??(H), 17??(H)-C30 sterane (20R) ??????-C30 4-methyl sterane (20R) 17??(H)-C27 trisnorhopane Tm
17??(H), 21??(H)-C29 hopane (normoretane) ????-C29 normoretane
17??(H), 21??(H)-C30 hopane ????-C30 hopane
17??(H), 21??(H)-C31 hopane (22R) ????-C31 hopane (22R)

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