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GB/T 18606-2017 PDF English


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GB/T 18606-2017: PDF in English (GBT 18606-2017)

GB/T 18606-2017 GB NATIONAL STANDARD OF THE PEOPLE’S 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’s Republic of China; Standardization Administration of the People’s 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 8β(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 8β(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, 17α(H)-22, 29, 30 trisnorhopane; 17α(H), 21β(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, 5α(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, 18α(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 5α(H), 14α(H), 17α(H)-C27 sterane (20R) ααα-C27 sterane (20R) 24-methyl-5α(H), 14β(H), 17β(H)-C28 sterane (20S) αββ-C28 sterane (20S) 24-ethyl-5α(H), 14α(H), 17α(H)-C29 sterane (20R) ααα-C29 sterane (20R) 4-methyl, 24-ethyl-5α(H), 14α(H), 17α(H)-C30 sterane (20R) ααα-C30 4-methyl sterane (20R) 17α(H)-C27 trisnorhopane Tm 17β(H), 21α(H)-C29 hopane (normoretane) βα-C29 normoretane 17α(H), 21β(H)-C30 hopane αβ-C30 hopane 17α(H), 21β(H)-C31 hopane (22R) αβ-C31 hopane (22R) ......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.