SY/T 5118-1995 Determination of chloroform bitumen in rocks - Fat extractor method SY/T5118-1995 standard download decompression password: www.bzxz.net

Petroleum and Natural Gas Industry Standard of the People's Republic of China SY/T 5118 -- 1995
Determination of Chloroform Bitumen in Rocks
Fat Extractor Method
Published on December 25, 1995
China National Petroleum Corporation
Implemented on June 30, 1996
Cited Standards
Method Summary
Reagents and Materials
Instruments and Equipment
Analysis Procedures
Calculation and Expression of Analysis Results
Quality Requirements
Chloroform Bitumen Analysis in Rocks is a basic data for the evaluation of source rocks and has been used as a conventional indicator of source rocks. With the rapid development of organic geochemical analysis and identification technology, modern instruments have been widely used, and new methods for extracting soluble organic matter in rock samples have also been introduced. In order to adapt to the new development of petroleum geological experimental technology in the 1990s and fully consider the alignment with international general standards, SY5118-86 "Extraction Determination Method of Chloroform-Injured Asphalt in Rocks" was revised. The main change is to change the name of the original standard to "Determination of Chloroform-Injured Asphalt in Rocks by Fat Extractor Method" to clarify that when using various new rapid extractors, the quality requirements specified in the revised standard must be met; and the inappropriate parts are modified to improve the practicality, scientificity and advancement of the standard. This standard will replace SY5118-86 from the date of entry into force. This standard is proposed and managed by the Petroleum Geological Exploration Professional Standardization Committee. The drafting units of this standard are: Exploration and Development Research Institute of North China Petroleum Administration Bureau, and Experimental Center of Petroleum Exploration and Development Scientific Research Institute. The main drafters of this standard are Zhang Mingwen, Li Hailing, Mou Luwen, Guo Yongyin, Qian Zhihao, Hui Yingzu, Cong Aifen. 1 Scope
Petroleum and Natural Gas Industry Standard of the People's Republic of China Determination of Chloroform Asphalt in Rocks
Fat Extractor Method
This standard specifies the determination method and quality requirements for nitrogen asphalt in rocks using a fat extractor. This standard is applicable to the determination of samples with a chloroform asphalt content of less than (.0040%) in rocks. 2 Reference Standards
SY/T 5118-—1995
Replaces SY 5118---86
The following standards contain clauses that constitute the clauses of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised. All parties using this standard shall discuss the possibility of using the latest version of the following standards. SY/T602894 Top-day sampling and results requirements for well testing 3 Method Summary
This method mainly relies on the solubility of chloroform on small asphalt substances in rocks, and uses fat extraction Extraction is performed using an extractor, and the content of asphalt is determined by the mass method.
4 Reagents and materials
4.1 Chlorine: analytical grade, dehydrated, distilled, no acidic reaction - chromatographic inspection qualified. 4.2 Acetone: analytical grade.
4.3 Ethanol: analytical grade.
4.4 Calcium chloride: analytical grade.
Hydrochloric acid analytical grade.
4.6 Copper sheet: The copper content should be greater than 99%: Treat with one of the following methods before use : 1. Activate with dilute hydrochloric acid (volume ratio of 1:3), and rinse with water, ethanol or acetone, and chloroform respectively; use fine sandpaper to remove surface oxides, and rinse with chloroform. 4.7 Sample packaging: Extract with chloroform until no fluorescence before use. 5. Instruments and equipment
5.1 Fat extractor (b0UmL, 1000ml). 5.2 Electric constant temperature water bath or electric heating jacket.
5.3 Fluorescent lamp.
5.4 Weighing bottle.
5.5 Sample crusher.
5.6 Sampling test sieve.
Approved by China National Petroleum Corporation on December 25, 1995 and implemented on June 30, 1996
6 Samples
6.1 Check samples
Check according to the notice.
6.2 Purify samples
If there are stains on the surface of the sample, purify it. 6.3 Dry samples
SY/T 5118—1995
The sample should be dried at 40~45℃ for more than 4 hours before crushing. 6.4 Crushed samples
After drying, all samples should be crushed to a particle size of less than 0.18mm at a temperature not exceeding 50℃ and kept dry. 6.5 Storage and packaging of samples
The storage and packaging of selected samples shall comply with the relevant provisions of 5.9.1 and 5.9.6 of SY/T6028-94. 7 Analysis steps
7.1 Packaging samples|| tt||Weigh the crushed sample (100~200g for mudstone and limestone: 5~50g for coal and oil shale) and put it into the extracted filter paper tube. The height of the paper tube should be lower than the height of the siphon tube:
7.2 Extraction
7.2.1 Put the wrapped sample into the sample chamber of the extractor, add several copper sheets and chloroform for desulfurization in the bottom bottle, and the amount of chloroform added should be 1/2~2/3 of the capacity of the bottom bottle. The time for the solution to reflux once should not exceed 30min. 7.2.2 Calculate the effective extraction time from the first solution reflux: 48h for limestone: 721 for mudstone, 100h for coal sample. Samples with high soluble organic matter content that are difficult to extract should be replaced with fluoroform and then extracted for 24h. 7.2.3 During the extraction process, attention should be paid to replenishing chloroform to prevent the extract from oxidizing and deteriorating due to insufficient solution in the bottom bottle. 7.2.4 If the pins are found to turn black during the extraction process, they should be dried again until they do not change color. 7.3 Concentrated extractbzxZ.net
Put the extract into a conical flask and recover the solvent in an electric constant temperature water bath at a distillation rate of no more than 120 drops/min. 3-5ml of concentrated solution is filtered and transferred to a weighing bottle that has been well filtered. The utensils, filter paper and cotton used in the whole process are washed with chloroform until they do not fluoresce.
7.4 Discharging solvent and weighing
7.4.1 The solvent in the weighing bottle is evaporated to nearly zero at no more than 40℃, and the pins are placed in a desiccator. 7.4.2 All weighing bottles are placed in a drying oven and kept at 40℃ for 30 minutes before being taken out. Put it in the desiccator and cool it in the room for 30 minutes before weighing. The difference between the two weighings of the empty weighing bottle should not be greater than 0.0002g: the difference between the two weighings of the weighing bottle filled with chloroform asphalt should not be greater than 0.0010g:
8 Calculation and expression of analysis results
The analysis results are calculated according to formula (1)
where: X-...Chloroform asphalt content,%;
G)-weight of the weighing bottle + g;
G--weight of chloroform asphalt in the weighing bottle·g:m sample mass·g.
The result should be rounded to four decimal places.
X=G- G,
9 Quality requirements
SY/1 5118--1995
9.1 Precision 5%~10% of the samples to be analyzed shall be sampled for parallel inspection to test the analysis quality. Table 1 gives the standard for the allowable double difference of the sample analysis results.
Table "Comparison table of allowable double difference range of parallel sample analysis Chloroform bitumen content range
40. 5000 ~ 0. 1000
≤0. 1000 -~ 0. 0500
Allowed double difference
Chloroform bitumen content range
0. 0300 -- 0. 0100
Allowed double difference
9.2 Other extraction instruments can be used as long as they are consistent with the fat extractor and meet the quality requirements specified in this standard.%
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