Method for detecting trace metal elements in coke and application thereof

A technology of trace metal elements and detection methods, which is applied in the field of chemical analysis, can solve problems such as lack of detection methods, abnormal furnace conditions, and impact on coke quality, and achieve the effects of meeting acceptance requirements, improving accuracy, and strong operability

Active Publication Date: 2020-01-10
YANGCHUN NEW STEEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also a lack of detection methods for trace metal elements in coke in the industry, and in the coking plant, due to desulfurization waste liquid, residual ammonia water in the coking process, denitrification waste liquid, scaling washing water of power generation boilers, biochemical dephenolization water, etc. directly enter the coke quenching pool , participate in the water coke quenching operation, the complex process leads to the final coke containing a variety of metal elements, which affects the quality of the coke
Most of the detection technologies for coke in the prior art only focus on the detection of soluble metal ions on the surface of coke, but do not propose an accurate and quantitative detection technology for the total content of specific trace metal elements in coke
[0003] Coke is widely used as sme

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028] Example 1

[0029] A sample pretreatment method for the determination of trace metal elements in coke, comprising the following steps:

[0030] (1) Take the coke sample from the factory and crush it step by step and pass it through a 13mm sieve, take 2kg of sieved coke and soak in water to prepare a coke sample; stir the sample evenly, weigh the sample according to Table 1 and place it in a 3000ml beaker, respectively. Add 1000ml of deionized water, stir well and let stand for more than 3 hours;

[0031] (2) Stir and mix the coke soaking liquid, and then filter the soaked coke soaking liquid with slow quantitative filter paper to ensure that there is no visible particulate matter in the filtrate;

[0032] (3) Take the filtrate into a 50ml volumetric flask, set the volume, add 1ml of nitric acid solution with a concentration of 50%, and mix to obtain the first mixed solution, that is, to obtain part of the metal ion solution in the coke to be tested.

Example Embodiment

[0033] Example 2

[0034] A method for detecting calcium and magnesium content in coke, comprising the following steps: Steps (1)-(3) are identical to those in Embodiment 1, and further comprise the following steps:

[0035] Take 1.0g of filter residue after drying at low temperature, put it in a porcelain crucible, put it in a muffle furnace, and burn it at 400 °C for 1.5 hours, 480 °C for 2 hours, and finally 550 °C for 1.5 hours according to the set heating program. ". After the heating program is over, take it out and place it at room temperature, transfer it to a tetrafluoroethylene beaker with a small amount of water, add 10 mL of hydrofluoric acid, 5.0 mL of aqua regia and 1.5 mL of perchloric acid in sequence, and slowly raise it to 280°C on a hot plate at low temperature, After the perchloric acid is completely smoked, lower the temperature, add 1 ml of nitric acid solution with a concentration of 50% to extract the sample, cool to room temperature, transfer the solu...

Example Embodiment

[0036] Example 3

[0037] EDTA titration was used to detect the calcium and magnesium ion contents in the first mixed solution and the second mixed solution respectively.

[0038] The above technical scheme prepares a representative coke sample, soaks it in deionized water for several hours, prepares a solution to be tested, and uses GB / T 15452-2009 "Determination of Calcium and Magnesium Ions in Industrial Circulating Cooling Water EDTA Titration Method" to measure The content of calcium and magnesium in the solution to be tested solves the technical problem that the content of adsorbed calcium and magnesium in the coke cannot be detected at present.

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PUM

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Abstract

The invention discloses an extraction method of trace metal elements in coke and an application. The extraction method comprises the following steps: taking coke to prepare a sample, uniformly stirring the sample, weighing the sample, putting the sample into a beaker, adding deionized water, performing uniform stirring, and standing for a plurality of hours; filtering the soaked coke soak solutionto ensure that no visible particulate matters exist in the filtrate; adding the filtrate into a volumetric flask, fixing the volume, adding a nitric acid solution, and performing uniform mixing to obtain a first to-be-detected solution; and drying the filter residues, performing ashing, carrying out mixed acid digestion treatment to obtain a second to-be-detected solution; and finally, respectively measuring the content of the target metal element by adopting an EDTA method and an inductively coupled plasma atomic emission spectrometry. The method can extract the metal elements in the coke, has the advantages of simple steps, short time consumption and high extraction efficiency, and can eliminate experiment interference by adopting deionized water.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a detection method and application of trace metal elements in coke. Background technique [0002] Most of the domestic long-process iron and steel complexes are equipped with coking plants. Generally, a large proportion or even all of them use self-produced coke, and the quality is relatively stable and controllable. The problem of trace metal elements in coke has attracted enough attention. There is also a lack of detection methods for trace metal elements in coke in the industry, and in the coking plant, due to desulfurization waste liquid, residual ammonia water in the coking process, denitrification waste liquid, scaling washing water of power generation boilers, biochemical dephenolization water, etc. directly enter the coke quenching pool , Participate in water coke quenching operations, the complex process leads to the final coke containing a variety of metal el...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/73G01N1/28G01N1/44
CPCG01N1/28G01N1/44G01N21/73G01N31/16
Inventor 樊尧桂程祥刘林刚郑呈祥周小盛刘涛
Owner YANGCHUN NEW STEEL CO LTD
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