Accurate determination method for high-temperature decomposition products of humic acid organic matters
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A technology of high temperature decomposition and determination method, which is used in measurement devices, material separation, material analysis, etc., and can solve problems such as difficulty in continuous start-up operation, limitation of water vapor detection, and complex water vapor composition.
Inactive Publication Date: 2017-02-22
CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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[0003] Ion chromatography is a traditional detection method born in the mid-1970s. It is an important branch of high performance liquid chromatography. It is currently the main detection method for the detection of anion and cation compound content. It has important applications and has become a powerful tool to study and deal with corrosion problems of power equipment. However, the application of conventional analytical ion chromatography in actual power plant operation has many defects. First, the flow rate of conventional analytical ion chromatography is very large, so it is difficult to do Continuous start-up operation requires a large volume of samples, which limits the large-scale water vapor detection. Secondly, for the current thermal system, the water vapor composition has become relatively complex, and the pyrolysis products of humic acid organic compounds also have low molecular weight. For organic acids and inorganic anions, for these complex samples, because there are large differences in the affinity of different types of ions to common ion chromatography column stationary phases, it is difficult to find a suitable eluent type and concentration to separate them, which is likely to cause detection errors , therefore, it is necessary to improve the method on the original conventional analytical ion chromatography method
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example 1
[0016] Example 1: Detection of water vapor samples in an in-service power plant
[0017] 1. Instruments and Reagents
[0018] The instrument used in the experiment is an ion chromatograph, the anion separation column and the protective housing are all supporting common chromatographic columns, a conductivity detector, and a sampler.
[0019] Sodium formate, sodium acetate, sodium fluoride, sodium chloride, sodium sulfate, sodium phosphate, sodium nitrate, potassium tetraborate, the above-mentioned drugs are all analytically pure, and the eluent K is configured 2 B 4 o 7 solution (gradient concentration eluent), the standard stock solution of each anion series is 1000µg / L, and the above seven standard stock solutions and eluents are all prepared with ultrapure water with a resistivity of 18.25MΏ·cm, all stored Store in a polyethylene bottle at 0-4°C.
[0020] 2. Standard liquid configuration and instrument calibration
[0021] According to the concentration range of the sa...
example 2
[0029] Example 2: Accurate determination of humic acid pyrolysis products at different concentrations
[0030] Repeat the operation steps of the above example 1, select instruments and reagents, calibrate the instruments and configure standard liquids, perform chromatography on the humic acid pyrolysis solution at different concentrations, and use gradient elution procedures to obtain the product content results of humic acid decomposition at different concentrations As shown in Table 3 below, the change trend diagram is as follows image 3 As shown, among them, the decomposition concentration gradient of humic acid is set to 0µg / L, 1500µg / L, 3500µg / L, 5500µg / L, 7500µg / L respectively.
[0031] The accurate determination example of the pyrolysis products of humic acid under different concentrations shows that the accurate determination method of a kind of humic acid organic matter pyrolysis products involved in the present invention has applicability and repeatable measurement....
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Abstract
The invention discloses an accurate determination method for high-temperature decomposition products of humic acid organic matters. Specifically, the high-temperature decomposition products of the humic acid organic matters in a water-gas system of a heat-engine plant are accurately analyzed and detected by virtue of an ion chromatography leacheate gradient program and mainly include low-molecule organic acid and inorganic anions. The accurate determination method specifically comprises the steps of filtering humic acid organic matter high-temperature decomposition liquid by virtue of a 0.45-micron millipore filter membrane, concentrating sample volume, and injecting the decomposition liquid into a quantitative feeding sample of an ion chromatograph. Detection conditions of the ion chromatography leacheate gradient program are as follows: the temperatures of an anion analytical column and a protection column are 30+ / -0.1 DEG C, leacheate is a K2B4O7 solution, the flow speed of the leacheate during the gradient leaching is controlled at 1.00mL / min, the current of a suppressor is contained at 60mA, and the sample volume is 500 microliters. By virtue of the analysis method of the invention, the standard deviation is the least when the detection limit of each ion is the lowest; the analysis method is suitable for rapidly and accurately detecting the high-temperature decomposition products of the humic acid organic matters in the water-gas system the heat-engine plant.
Description
technical field [0001] The invention relates to an accurate determination method for high-temperature decomposition products of humic acid organic substances, in particular to an accurate analysis and detection method for high-temperature decomposition products of humic acid organic substances in a water vapor system of a thermal power plant by using an ion chromatography eluent gradient program method. Background technique [0002] With the rapid development of the power industry, "heating transformation of condensing steam turbines" is also rapidly popularized. In order to meet the heat supply of the unit, the amount of make-up water has also increased, and the organic matter brought into the make-up water has also increased significantly, and organic compounds such as humic acid It is a main representative of organic matter. In the thermal power system of thermal power generation, humic acid organic matter decomposes under high temperature and high pressure environment, an...
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 朱志平王娜娜田龙标杨磊
Owner CHANGSHA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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