SY/T 5161-2002 Determination of metal elements in rocks by atomic absorption spectrometry
Some standard content:
ICS 75.010
Registration number: 10424—2002
Petroleum and natural gas industry standard of the People's Republic of China SY/T 51612002
Replaces SY/T5161--87bzxz.net
Determination of some metal elements in rocks by atomic absorptionspectrometry
Published on 2002-05-28
State Economic and Trade Commission
Implementation on 2002-08-01
Normative reference documents
Instruments and equipment
Reagents and materials
Sample processing
Analysis conditions and environment
Preparation of sample solution
Sample determination
Analysis precision
SY/T 51612002
SY/T5161—2002
This standard is a revision of SY/T5161—87 "Method for determination of metal elements in rocks by atomic absorption spectrometry". Compared with SY/T5161—87, this standard has the following changes: the text is more standardized;
adopts the format and expression method of GB/I'1.1—2000: proposes that the national standard solution must be used;
uses repeatability and reproducibility R to express precision; adds instrument tide source;
adds environmental protection clauses.
This standard will replace SY/T5161—87 from the date of implementation. This standard is proposed and managed by the Petroleum Geological Exploration Professional Standardization Committee: Drafting unit of this standard: Experimental Center of Exploration and Development Research Institute of China Shishan Natural Gas Co., Ltd. The drafting organizations of this standard include: Exploration and Development Research Institute of Xinjiang Oilfield Company of China National Petroleum Corporation, Research Institute of South China Sea West of China National Offshore Oil Corporation, Exploration and Development Research Institute of Qianhe Oilfield Company of China National Petroleum Corporation, and Bohai Oil Research Institute of China National Offshore Oil Corporation. The main drafters of this standard include: You Jianchang, Zhang Dijia, Gan Huitong, and Yu Rongguang. 1 Scope
Method for determination of metallic elements in rocks by atomic absorption spectroscopy
SY/T S161—2002
This standard specifies the method for determination of metallic elements (K, Na, Ca, Mg, Fc, Li, Sr, Ni, Cu, Zn, and Mn) in rocks by atomic absorption flame spectrometry, as well as sample pretreatment, analysis conditions, and sample analysis precision. This standard is applicable to the analysis of metallic elements in rocks. 2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For all references with dates, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties reaching an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used: For all references without dates, the latest versions are applicable to this standard CFH/T6379-1986 Precision of test methods Repeatability and reproducibility of standard test methods are determined through laboratory tests 3 Principle
The principle of atomic absorption analysis is that when the characteristic spectrum of the element to be measured radiated by the light source passes through the vapor of the sample, the ground state atoms of the element to be measured in the vapor selectively absorb it. Under certain conditions, the degree of absorption is proportional to the number of ground state atoms. The content of each element in the sample can be measured by measuring the degree of absorption of the radiation through the spectroscopic system and the detector. After the sample is dissolved, it is made into a test solution, and the test is carried out according to the analytical conditions of each element to be tested: 4 Instruments and equipment
4.1 Atomic absorption spectrometer.
4.2 Air cathode lamp.
4.3 Acetylene gas: purity not less than 97%:
4.4 Oil-free air compressor
4.5 Analytical balance: sensitivity is 0.1mg
4.6 Constant temperature drying oven: maximum temperature not less than 200t4.7 Muffle furnace: maximum temperature not less than 1000℃: 4.8 Adjustable electric heating plate (or sand bath): 1000W-3000W4.9 Voltage stabilizer.
Polytetrafluoroethylene.
Volume flasks of different specifications
4.12Pipette of different specifications
4.13Polyethylene plastic bottle: 50mml, 500ml., glass and plastic vessels are soaked in nitric acid solution with V (HV:H2O) = 1:1 or hydrochloric acid with V (HCI:HO) = 1:1 overnight, then rinsed with deionized water, dried and set aside. 5 Reagents and materials
5.1 Hydrochloric acid: high-grade pure.
5.2 Nitric acid: high-grade pure,
SY/T 5161-2002
5.3 Perfluoric acid: high-grade pure,
5.4 Hydrofluoric acid: high-grade pure,
5.5 Calcium chloride: analytically pure.
5.6 Strontium chloride: analytically pure.
5.7 Sodium oxide: analytically pure.
5.8 Preparation of solution: Accurately weigh 12.67g of saturated chloride and place it in a 1(HhriL beaker, add 50ml of deionized water to dissolve, transfer to a 100ml volumetric flask, dilute to the mark, shake well, this solution contains 100mg/mL, 5.9 Preparation of strontium solution: Accurately weigh 30.42g of strontium fluoride and place it in a 250mL beaker, add 50mL of deionized water to dissolve, transfer to a 100ml volumetric flask, dilute to the mark, shake well, this solution contains 100mg/mL strontium-. 5.10 Preparation of sodium solution: Accurately weigh 1!.73g of sodium oxide and place it in a 250hL beaker, slowly add V (HCl:H0) = 1:1 hydrochloric acid until the solution is transparent, cool it down and transfer it to a [00mL volumetric flask, dilute it to the mark with deionized water, shake it, and this solution contains 100rng/mLLu
5.11 Experimental water: deionized water (conductivity ≤0.1mS/m). 5.12 All standard stock solutions and working curve standard solutions of the metal elements to be tested must be prepared using national standard solutions. The preparation of the working curve standard solution shall not be less than 4 points, and the corresponding concentration of ionizer or release agent in Table 1 shall be added to each working curve standard solution.
5.13 The prepared standard stock solution has a shelf life of six months and should be stored at low temperature and away from light. 5.14 All prepared T. The validity period of the curve standard solution is "5d. 5.15 All discarded reagents, acids and alkalis should be placed in plastic barrels with red labels and should be handled in accordance with environmental protection regulations. 6 Sample handling
6.1 Samples with surface contamination should be cleaned before preparation. 6.2 The sample should be crushed to a particle size less than 0.[49mm. The sample should be dried in an oven at 105℃~110℃ for 1h~2h, then placed in a dryer and cooled to room temperature for use.
6.3 Samples with a high organic content should be placed in a porcelain pot with a constant weight and burned at 600℃-650℃ for 1h, and the loss on ignition should be calculated.
7 Analysis conditions and environment
7.1 For different types of instruments, the analysis conditions can be selected according to the instrument manual. 7.2 The modifiers and concentrations of each element are shown in Table 1nTable 1 Modifiers and concentrations
Modifiers and concentrations
Strontium==1mg/mL
Absolute mg/ml.
Strontium lng/nL
Strontium ≥3mg/ml.
3mg/ml
Direct determination
Direct determination
Table 1 (continued)
Note: Arsenic can be replaced by potassium or sodium, and the amount used should not be less than 2mg/m. 7.3 Environment:
7.3.1 Temperature: 10℃-30℃.
7.3.2 Relative humidity: meet the requirements of the instrument. 8 Preparation of sample solution
SY/T 5161-260:02
Corrector and concentration
Indirect determination
Direct determination
Direct determination
Oxide ≥3mg/ml.
8.1 Weigh 0.5g sample on a calibrated analytical balance, accurate to 0.0001g, put it in a polytetrafluoroethylene pot, and moisten the sample with a small amount of deionized water. Add 7mL~8mL of perchloric acid, dissolve on a hot plate below 250℃, heat to nearly ten, remove, cool slightly, add 6trl~7ml of hydrofluoric acid, continue heating, and evaporate to dryness. Remove the crucible, rinse the cup wall with a small amount of deionized water, add 1mL of perchloric acid, and heat until there is no white perchloric acid smoke. If the sample is completely dissolved, add appropriate amount of hydrofluoric acid and perchloric acid to make the sample completely dissolved, then evaporate and add V (HCl.H,O) = 1:1 2mL of hydrochloric acid, add a small amount of deionized water, and heat until the solution is transparent. After cooling, dilute to a 50mL volumetric flask.
8.2 The preparation method of rock standard and blank sample solutions is the same as 8.1, and is carried out at the same time as the sample solution preparation. 9 Determination of samples
9.1 Start the instrument; after the instrument is stable, start measuring under the selected instrument analysis conditions. 9.2 Measure the absorbance of the blank sample drop, measure the absorbance of the working standard solution series, and draw a standard curve by computer. 9.3 Measure each solution at least twice, record the stable readings, and take the average value. 9.4 Measure the rock standard solution. If the measured value meets the standard value of the rock standard and is within the uncertainty range, the sample can be measured. Otherwise, it should be repeated according to the requirements of Chapter 8.
9.5 According to the analysis conditions of each element to be measured, measure each element to be measured in the sample solution in turn. If the sample needs to be diluted, the dilution factor shall not be greater than 50g
10 Calculation
Use formula (1) to calculate the content of each element:
n×106
Where:
The mass fraction of the element, expressed as white fraction:Q
The element content of the solution being tested, in micrograms per milliliter (/nL):-the volume of the sample solution, in millimeters (rml.);K-the dilution factor of the sample solution;
SY/T 5161—2002
The mass of the sample, in grams (name) (If there is a loss on ignition, it should be converted into the original sample weight). 11 Analytical precision11
The repeatability and reproducibility of the analytical test results for each metal element shall comply with the following provisions: Repeatability r and reproducibility R shall be calculated in accordance with GB/16379—1986. If the difference between two single test results exceeds the corresponding repeatability or reproducibility value, the two test results are considered suspicious.
11.1 Conduct more than two tests in the same laboratory: If two groups of tests are conducted in the same laboratory space under repeatability conditions, the critical difference between the average values with a probability of 95% is expressed as Y2-YlrN2m
Where:
n—the number of tests conducted in the first group:
Y1—the average value of the first group of test results: n2—the number of tests conducted in the second group; Y2—the average value of the first group of test results. 22
11.2 Two laboratories each conduct more than : tests: If the first laboratory conducts n, tests, and the average value is,, and the first laboratory conducts n2 tests, and the average value is Y2, then:-
11.3 The repeatability and reproducibility R of each element analyzed by this method are shown in Table 2, Table 3, and Table 4. Table 2 Repeatability and reproducibility K of atomic absorption analysis results of 11 kinds of golden eagle elements in mudstone
Precision
Repeatability and reproducibility R of atomic absorption analysis results of 11 kinds of metal elements in sandstone
1) This precision was determined in the test conducted by 5 laboratories on : water samples in 2001. 4
Precision
SY/T5161--2002
Repeatability and reproducibility R of atomic absorption analysis results of 11 kinds of metal elements in limestone
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