SY/T 5116-1997 Determination of Total Organic Carbon in Sedimentary RocksSY/T5116-1997 Standard download decompression password: www.bzxz.net

ICS75.180.99.
Preparation number: 1147—1998
Petroleum and natural gas industry standard of the People's Republic of ChinaSY/T 5116-1997
The determination of total organic carbon in sedimentary rock
1997--12-31 Issued
China National Petroleum Corporation
1998-07-01Implementation
SY/T 5116-1997
2 Instrumental determination method
3 Dry combustion gravimetric method
Quality requirements
SY/T 5116-1997
This standard is a revision of SY5116-86 "Analysis Method of Organic Carbon in Rocks" according to the revision plan of petroleum and natural gas standards issued by China National Petroleum Corporation in 1997. Through revision, the adopted determination method can adapt to the rapid development of domestic petroleum geological experimental technology and international technical exchanges as soon as possible. This standard removes Chapter 2 "Non-aqueous titration method" and Chapter 3 "Dry burning volumetric method" of the original standard, and adds a chapter "Dry burning weight method". In view of the different instrument models of various units, the instrument model is no longer specified in Chapter 2 "Instrument determination method" of this standard. From the date of entry into force, this standard will replace SY5116-86 at the same time. This standard is proposed and managed by the Petroleum Geological Exploration Professional Standard Promotion Committee. The responsible drafting unit of this standard is: Experimental Center of Petroleum Exploration and Development Research Institute. The participating drafting unit of this standard is: Petroleum Geology Central Laboratory of the Ministry of Geology and Mineral Resources. The main drafters of this standard are Xu Guanjun and Hu Wen. 1 Scope Standard of the People's Republic of China for the petroleum and natural gas industry Determination of total organic carbon in sedimentary rock SY/ T 5116--1997 Replaces SY 5116-86 The determination of total organic carbon in sedimentary rock This standard specifies two methods for the determination of total organic carbon in sedimentary rock: instrumental determination method and dry burning weight method. This standard is applicable to the determination of total organic carbon in sedimentary rock, modern sediment and coal. 2 Instrumental determination method 2.1 Principle Use dilute hydrochloric acid to remove inorganic carbon in the sample: then burn it in a high-temperature oxygen flow to convert the total organic carbon into carbon dioxide, and then detect the total organic carbon content with an infrared detector. 2.2 Instruments and equipment
Carbon-sulfur measuring instrument;
Special porcelain cube for carbon-sulfur analysis: diameter 25mm, quotient 25mm, burned at 900℃ for 2h before use; b)
Analytical balance: sensitivity 0.1mg:
Muffle furnace: heating temperature greater than 900℃;
Controllable temperature electric heating plate or water bath:
Oven;
Vacuum pump;
h)'Filter;
Crumb rack.
2.3 Reagents and materials
Hydrochloric acid solution: prepare anhydrous magnesium perfluorite (analytical grade) with analytical grade hydrochloric acid at a ratio of 1:7 (volume ratio);
Alkali asbestos:
Glass fiber;
Desulfurized cotton;
Platinum silica gel;
Iron spray flux: C0.002%S<0.002%
Tungsten particle flux: C<0.001%, S<0.0005%, standard steel samples with various carbon contents of 0.35~0.83mm in particle size;
Oxygen: purity of 99.99%;
k) Compressed air or fluorine gas (oil-free and water-free). 2.4 Analysis steps
2.4.1 Sample preparation
Grind the sample to a particle size of less than 0.2 mm. The amount of ground sample should generally not be less than 4 g. 2.4.2 Sample weighing
Approved by China National Petroleum Corporation on December 31, 1997 and implemented on July 1, 1998
SY/ T 5116-1997
According to the sample type, weigh 0.01-1.00 g of sample, accurate to 0.0001 g. 2.4.3 Sample dissolution
Slowly add excess hydrochloric acid solution to the container containing the sample [preparation method see a) in 2.3) Place on a hot plate, control the temperature at 60-80°C, and dissolve the sample for more than 2 hours until the reaction is complete. During the dissolution process, ensure that the sample does not splash out, otherwise it should be redone. 2.4.4 Transfer
Transfer the dissolved sample to the crucible placed on the suction filter, wash the residual acid solution with steam water, and place it on the crucible rack in order. 2.4.5 Drying
Place the sample crucible in an oven at 70-80℃ and dry it for later use. 2.4.6 Start-up measurement
2.4.6.1 Check the efficiency of each absorbent [b]~e] in 2.3. 2.4.6.2 Start-up stabilization: The stabilization time is carried out according to the instrument manual. 2.4.6.3 Turn on the gas: Connect the oxygen flow and control the pressure to 0.25MPa. 2.4.6.4 System inspection: After the instrument is stable, proceed according to the instrument manual. 2.4.6.5 Instrument calibration: Select three standard samples with high, medium and low carbon contents according to the sample type for measurement, and determine the correction factor with the standard sample with high carbon content. The results of the three standard samples should all meet the standard error requirements, otherwise the correction coefficient should be adjusted and recalibrated. 2.4.6.6 Blank test: Take an empty crucible treated with acid and add about 1.0g of iron filings [2.3 g] and about 1.0g of tungsten particles [2.3 h)]. The measured carbon content should not be greater than 0.01%.
2.4.6.7 Sample determination: Add about 1.0g of iron filings [2.3 g] and about 1.0g of tungsten particles [2.3 h)] to the dried sample crucible (2.4.5), and put it in the induction furnace, and then enter the sample mass. Press the analysis key to measure the sample. The measurement results are automatically printed. The combustion chamber should be cleaned and the standard sample detection instrument should be inserted every 20 samples. If the standard sample measurement result exceeds the error range, the instrument should be recalibrated according to 2.4.6.5.
2.4.7, Turn off the instrument
According to the instrument operation manual.
3 Dry burning weight method
3.1 Principle
Use dilute hydrochloric acid to remove inorganic carbon in the sample, then burn it in a high oxygen flow, and the generated carbon dioxide is absorbed by alkali asbestos. The total organic carbon content is calculated based on the increment of alkali asbestos. 3.2 Apparatus and equipment
a) Total organic carbon determination apparatus (see Figure 1); b) Balance: sensitivity is 0.01 mg;
c) Porcelain boat.
3.3 Reagents
a) Hydrochloric acid solution: same as a) in 2.3);
Alkali asbestos: particle size is 0.45~0.55mm
Acid washed asbestos: analytical grade, burn at 900~1000℃ for 2h, cool; 9)
Anhydrous magnesium perchlorate (analytical grade);
Anhydrous calcium fluoride (analytical grade);
Hydrogen peroxide: 3%, prepare with 10mL 30% peroxide and add 90mL water;
Concentrated sulfuric acid: analytical grade;
Silver nitrate solution: 10%, 10g silver nitrate is dissolved in 100mL water; h)
Sodium hydroxide solution: 40%. 40g sodium hydroxide is dissolved in 1001mL water. i
3.4 ​​Analysis steps
3.4.1 Sample preparation
Same as 2,4. 1.
3.4.2 Sample weighing
SY/ T 51161997
Weigh 0.01~1.00g of sample according to the sample type, accurate to 0.0001g, and place it in a 100mL beaker. 3.4.3 Sample dissolution
Add 40~50mL of 10% hydrochloric acid [a in 3.3] to the beaker containing the sample, place it on a hot plate and heat it to a slight boil for 20min. 1- oxygen cylinder: 2- safety bottle, 3- gas washing bottle (containing 40% sodium hydroxide); 4- drying tower (containing anhydrous calcium chloride); 5- tubular combustion furnace and quartz tube: 6- sulfur absorption bottle (containing 3% hydrogen peroxide); 7- potassium ball (containing 10% silver nitrate); 8- potassium ball (containing concentrated sulfuric acid); 9- large U-shaped tube [containing anhydrous perchloric acid; 10, 11 weighing U-shaped tubes with 2/3 tubes of caustic soda minus asbestos at the inlet end and 13 tubes of anhydrous magnesium perchlorate at the outlet end) 12- U-shaped tube (containing reagents alternately with 10 and 11, in the opposite direction) Figure 1 Schematic diagram of the device for determining total organic carbon by dry burning weight method 3.4.4 Transfer
Filter the solution with acid-washed asbestos in a triangular funnel and wash with hot steam water until there is no fluorine. The residue and acid-washed asbestos are all transferred to the porcelain boat.
3.4.5 Drying
Place the porcelain boat in an oven at 70-80℃ for drying. 3.4.6 Constant weight (mass) weighing U-shaped tube
Before testing each batch of samples, place the weighing U-shaped tube in the sample measuring device system and ventilate to constant weight (mass). The difference between two consecutive weighings should not exceed 0.4mg.
3.4.7 Burning
3.4.7.1 Raise the temperature of the tube furnace to 1000-1100℃, pass oxygen, and control the flow rate at 1-2 bubbles/second. 3.4.7.2 Check whether the system has leaks and drive out the air in the system: connect the U-shaped tube that has been constant weight (mass). 3.4.7.3 Send the porcelain boat containing the sample into the quartz tube of the tube furnace. Pass oxygen, open the pistons of the two U-shaped tubes, push the porcelain boat into the high temperature zone after 1 to 2 minutes, continue burning for 10 minutes, and close the pistons of the two U-shaped tubes. 3.4.7.4 Gently wipe the weighing U-shaped tube with silk cloth, put it in the dryer, and weigh it after 2 to 3 minutes. 3.4.7.5 Replace the other two U-shaped tubes with constant weight (mass), analyze the next sample, or close the oxygen valve to end the analysis. 3.4.8 Determination of blank value
While measuring the sample, two blank values ​​must be determined according to steps 3.4.3 to 3.4.7. 3.5 Calculation
The total organic carbon content of the measured sample is calculated according to the following formula; where:
SY/ T 5116-1997
C= (4- B)× 0.2727 × 100%
- Determine the total organic carbon content of the sample;
Weigh the U-tube increment, g
- Determine the blank value, g
- Determine the mass and name of the sample;
Quality requirements
Mass fraction of carbon in carbon dioxide
Each batch of sample analysis must have 10% parallel samples. The results of parallel sample determination should comply with the provisions of Table 1: Table 1 Parallel sample determination results
Total organic carbon content range
>0.10 ～0.30
>0.30～0.,50
>0.50～1.00
1.00～~3.00
Relative deviation is calculated as follows:
Absolute deviation is calculated as follows
Where:
d-relative deviation;
Absolute deviation;
First measurement result;bzxz.net
Second measurement result
Relative deviation
X,- X,
×100%
Absolute deviation
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