An accurate determination method for pyrolysis products of humic acid organic matter
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A technology of pyrolysis and determination method, which is applied in the direction of measuring devices, material separation, and analysis of materials, and can solve problems such as detection errors, separation, and large eluent flow rates
Inactive Publication Date: 2018-12-14
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, an anion separation column and a protection column are commonly used 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 drugs are of analytical grade, and the eluent K is prepared 2 B 4 O 7 Solution (gradient concentration eluent), the series of standard stock solutions of each anion are 1000µg / L, 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. Configuration of standard liquid and instrument calibration
[0021] According to the concentration range of the sample to be tested and ...
example 2
[0029] Example 2: Precise determination of humic acid pyrolysis products at different concentrations
[0030] Repeat the operation steps of above-mentioned example 1, select instruments and reagents, calibrate instruments and configure standard use liquid, carry out chromatography on humic acid pyrolysis solution under different concentrations, adopt gradient elution procedure, obtain the product content results under different concentrations of humic acid decomposition As shown in Table 3 below, the change trend graph 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] Examples of accurate determination of humic acid pyrolysis products at different concentrations illustrate that the method for accurate measurement of humic acid-based organic matter pyrolysis products involved in the present invention has popularization and applicability, and can be r...
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Abstract
The invention discloses an accurate determination method for pyrolysis products of humic acid organic matter, specifically an ion chromatography eluent gradient program method for precise analysis and detection of humic acid organic matter pyrolysis products in the water vapor system of a thermal power plant. The pyrolysis products of humic acid organic matter are mainly low-molecular organic acids and corrosive inorganic anions. The specific steps are as follows: filter the humic acid organic matter pyrolysis liquid through a 0.45 μm microporous membrane, concentrate the sample volume, and inject it into an ion chromatograph In the quantitative sampling loop; the detection conditions of the ion chromatography eluent gradient program method are: the column temperature of the anion analysis column and the guard column is 30 ° C ± 0.1 ° C, the eluent is K2B4O7 solution, gradient elution, leaching The flow rate of the washing solution was controlled at 1.00mL / min, the current of the suppressor was controlled at 60mA, and the injection volume was 500µL. The analysis method of the present invention has the smallest standard deviation on the premise that the detection limit of each ion is the lowest, and is suitable for rapid and accurate detection of humic acid organic matter pyrolysis products in a water vapor system of a thermal power plant.
Description
technical field [0001] The invention relates to a method for accurate determination of high-temperature decomposition products of humic acid organic compounds, in particular to an accurate analysis and detection of the high-temperature decomposition products of humic acid organic compounds in a water vapor system of a thermal power plant by using an ion chromatography eluent gradient procedure method. Background technique [0002] With the rapid development of the power industry, the "condensing steam turbine heating transformation" has also been rapidly popularized. In order to meet the heating requirements of the unit, the amount of make-up water has also increased, and the organic matter brought in by the make-up water has also increased significantly, while the humic acid organic matter It is a main representative of organic matter. In thermal power generation systems, humic acid organic matter decomposes under high temperature and high pressure environment, resulting in ...
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Patent Type & Authority Patents(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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