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
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Embodiment 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 that enters the factory and crush it step by step through a 13mm sieve, take 2kg of sieved coke and soak it in water to prepare the coke sample; stir the sample evenly, weigh the sample according to Table 1 and place it in a 3000ml beaker, Add 1000ml deionized water, stir well and let it stand for more than 3 hours;
[0031] (2) Stir and mix the coke soaking solution, and then use slow quantitative filter paper to filter the soaked coke soaking solution to ensure that there are no visible particles in the filtrate;
[0032] (3) Get filtrate in the volumetric flask of 50ml, constant volume, add concentration again and be 50% nitric acid solution 1ml, mix to obtain the first mixed solution, promptly obtain the part metal ion solution in the coke to be measured.
Embodiment 2
[0034] A kind of detection method of calcium, magnesium content in coke, comprises the following steps: step (1)-(3) is identical with embodiment 1, also comprises the steps:
[0035] Take 1.0g of filter residue and dry it at low temperature, place it in a porcelain crucible, put it into a muffle furnace, and burn it at 400°C for 1.5h, 480°C for 2h, and finally at 550°C for 1.5h 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 10mL of hydrofluoric acid, 5.0mL of aqua regia and 1.5mL of perchloric acid in sequence, and slowly raise the temperature to 280°C on the electric heating plate. After the fumes of perchloric acid are exhausted, lower the temperature, add 1ml of nitric acid solution with a concentration of 50% to extract the sample, cool to room temperature, transfer the solution into a 50mL polytetrafluoroethylene volumet...
Embodiment 3
[0037] The contents of calcium and magnesium ions in the first mixed solution and the second mixed solution were respectively detected by EDTA titration.
[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 by 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 coke cannot be detected at present.
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