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Test method for sulfur isotope of source rock, oil, natural gas and water
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SY/T 7774-2024: (Sulfur isotope determination methods for source rocks, petroleum, natural gas and water)
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/SYT7774-2024
SY
PETROLEUM AND NATURAL GAS INDUSTRY STANDARD
ICS 75-010
CCS E 11
Test method for sulfur isotope of source rock, oil, natural gas
and water
Issued on: SEPTEMBER 24, 2024
Implemented on: MARCH 24, 2025
Issued by. National Energy Administration
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Terms and definitions... 4
4 Reagents and materials... 4
5 Instruments and equipment... 5
6 Sample pretreatment... 5
7 Sulfur isotope determination... 7
8 Precision... 8
Test method for sulfur isotope of source rock, oil, natural gas
and water
1 Scope
This document describes the sample pretreatment and test method for sulfur isotope of
source rocks, oil, natural gas, and water.
This document applies to the determination for sulfur isotope of source rocks, oil,
natural gas, and water.
2 Normative references
This document has no normative references.
3 Terms and definitions
This document does not contain any terms or definitions that need to be defined.
4 Reagents and materials
4.1 Chromium trichloride. analytically pure.
4.2 Hydrochloric acid. mass fraction is 36%~38%.
4.3 Arsenic-free zinc powder. purity is greater than 99.99%; particle size is 5µm~10µm.
4.4 Silver nitrate. analytically pure.
4.5 Barium chloride. analytically pure.
4.6 Nitrogen. purity is greater than 99.99%.
4.7 Helium. purity is greater than 99.99%.
4.8 Oxygen. purity is greater than 99.99%.
4.9 Sulfur dioxide. purity is greater than 99.99%.
4.10 Silver sulfide standard sample.
4.11 Centrifuge tube.
4.12 Polytetrafluoroethylene (PTFE) tubing.
4.13 Flat-bottomed flask.
4.14 Erlenmeyer flasks. 250 mL, 500 mL, with two-hole rubber stoppers.
4.15 Condenser.
4.16 pH test paper.
4.17 Filter membrane. cellulose acetate membrane; pore size is 0.45 µm.
4.18 Filter paper. qualitative rapid filter paper.
5 Instruments and equipment
5.1 Isotope mass spectrometer. equipped with a continuous flow interface, it can be
connected to an elemental analyzer.
5.2 Elemental analyzer. high-temperature nitriding furnace with a maximum
temperature rise of not less than 1200°C.
5.3 Electromagnetic heating stirrer. the maximum temperature rise is not less than
100°C; the rotation speed is not less than 1200 r/min.
5.4 Drying oven. the maximum temperature is not less than 120°C.
5.5 Centrifuge. the rotation speed is not less than 2000 r/min.
5.6 Analytical balance. the sensitivity is 0.1 mg.
6 Sample pretreatment
6.1 Pyrite in source rocks transforms into silver sulfide
6.1.1 Weigh at least 40 g of source rock sample. Grind to a particle size no larger than
0.18 mm. Dry in an oven at 100°C for 1 h.
6.1.2 Add 50 mL of silver nitrate solution to the conical flask.
6.1.3 Insert one hole of the two-hole rubber stopper into a PTFE tube filled with
nitrogen. Insert the other hole into a condenser tube. Connect the top of the condenser
tube to a PTFE tube and immerse it in a silver nitrate solution.
6.1.4 Place the dried source rock sample into a flat-bottomed flask. Then add 400 mL
of 1 mol/L chromium trichloride solution.
6.1.5 Fit the flat-bottomed flask with a two-hole rubber stopper. Open the nitrogen valve.
Adjust the nitrogen flow rate until the silver nitrate solution produces a uniform
bubbling rate of 1 bubble/s ~ 3 bubbles/s.
6.1.6 The flat-bottomed flask is placed on an electromagnetic stirrer. Heated to 100°C,
it is rotated at 1200 r/mm. The silver nitrate solution reacts with pyrite to produce
hydrogen sulfide. The reaction time is no less than 2 h.
6.1.7 Filter the solution in the conical flask using filter paper. Filter the silver sulfide
onto the filter paper. Wash the silver sulfide with deionized water until the test paper
shows neutral. Collect the resulting silver sulfide.
6.1.8 Place the silver sulfide in an oven and dry at a temperature not lower than 100°C
for 2 h. Store away from light.
6.2 Removal of pyrite from kerogen
6.2.1 Use X-ray diffraction (XRD) to analyze and measure the content of pyrite in
kerogen.
6.2.2 If the pyrite content in kerogen is less than 0.5% (mass fraction), sulfur isotope
analysis can be performed directly.
6.2.3 If the pyrite content in the kerogen is greater than or equal to 0.5% (mass fraction),
the pyrite shall be removed using method 6.1.
6.2.4 Dry the kerogen that has been through pyrite removal in an oven at 100°C for 12
h.
6.3 Conversion of hydrogen sulfide in natural gas into silver sulfide
6.3.1 If the volume percentage of hydrogen sulfide in natural gas is less than or equal
to 0.1%, the hydrogen sulfide in the natural gas shall be converted into silver sulfide.
6.3.2 Add 300 mL of silver nitrate solution to a two-hole rubber-stoppered conical flask.
6.3.3 One hole of the rubber stopper is inserted into a PTFE tube. One end of the PTFE
tube is connected to a natural gas cylinder via a stainless-steel pressure reducing valve.
The other end is immersed in a silver nitrate solution. The other hole of the rubber
stopper is inserted into the PTFE tube, and the system is vented in a fume hood.
6.3.4 Adjust the natural gas flow rate until the silver nitrate solution produces a uniform
bubbling rate of 1 bubble/s ~ 3 bubbles/s. Allow the silver nitrate solution to react with
the hydrogen sulfide in the natural gas for at least 10 min.
6.3.5 Filter the silver sulfide. Rinse with deionized water until neutral. After air drying,
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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