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A kind of determination method of ammonium ion content in fly ash

A technology of ammonium ion and determination method, which is applied in the direction of measurement device, material separation, instrument, etc., can solve the problems of high airtightness requirements of collection device, irritating formaldehyde solution, and many preparations before experiment, etc., and achieves widening determination method , Optimize the separation degree, the effect of simple operation steps

Active Publication Date: 2021-05-07
KZJ NEW MATERIALS GROUP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The formaldehyde titration method uses the combination of formaldehyde solution and ammonium root to realize the determination of ammonia by using the color difference of the indicator within a specific range. When this method is used for determination, the free acid in the solution must be removed first. The existence of free acid will affect the test results. accuracy, and the formaldehyde solution is more irritating, which is harmful to the human body; the distillation titration method is a method of distilling first, and then titrating. This method requires more preparations before the experiment, and the operation steps are cumbersome and time-consuming. Long; CN107300601A discloses a kind of assay method of fly ash ammonium ion content, dissolves fly ash sample with distilled water, with formaldehyde solution and ammonium ion effect, is equivalent to the acid of ammonium salt content with alkali titration, and then calculates the ammonium ion content content, what this invention adopts is the formaldehyde titration method, there are certain deficiencies, such as free acid may affect the accuracy of test results, formaldehyde can produce certain harm to human body etc.; In the method, the released ammonia is collected in a closed collection device, and the absorbance of the absorption liquid is measured after color development to calculate the release amount of ammonia. This method takes a long time to collect and requires a high airtightness of the collection device.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1.1 Instruments and reagents

[0032] Metrohm China Co., Ltd. Metrohm 883 ion chromatography system; CS20 cation exchange column; CG20 analytical guard column; CSRS300 cation suppressor; Mettler Toledo Instruments (Shanghai) Co., Ltd. electronic analytical balance; NH 4 Cl (standard substance); sulfurous acid (analytical pure); nitric acid (analytical pure); perchloric acid (analytical pure); citric acid (analytical pure); formic acid (analytical pure); acetic acid (analytical pure); Analytical pure); laboratory water is ultrapure water; the samples used are fly ash samples 1#, 2#, 3#, purchased from a company

[0033] 1.2 Sample pretreatment

[0034] Accurately weigh 0.5002 g of fly ash sample 1#, add 10 mL of 10 mmol / L sulfurous acid into a 50 mL small beaker, oscillate on an ultrasonic oscillator for 10 min, and then add it to a 10 mL centrifuge tube to Centrifuge at a speed of 2000r / min for 10min, take the supernatant and pass it through a 0.22μm water phase filte...

Embodiment 2

[0044] 1.2 Sample pretreatment

[0045] Accurately weigh 0.7500g of fly ash sample 2#, add 15mL of 15mmol / L nitric acid into a 50mL small beaker, oscillate on an ultrasonic oscillator for 15min, then add it to a 10mL centrifuge tube, Centrifuge for 15 minutes at a speed of 1 / min, take the supernatant and pass through a 0.22 μm water phase filter membrane to obtain the sample to be tested;

[0046] 1.4 Fly ash sample test

[0047] The chromatographic conditions are: CS20 cation exchange column, 4×250mm, CG20 analytical guard column, 4×50mm, CSRS300 cation suppressor, the suppressor current is 50mA, the column temperature is 40°C, the injection volume is 20μL, and the eluent is prepared by Prepared from sulfamic acid solution and acetonitrile solution, the sample was analyzed by gradient elution, and the gradient elution procedure is as follows:

[0048] 0~5min, the concentration of sulfamic acid is 0.005mol / L, the concentration of acetonitrile solution is 10%,

[0049] 6~15m...

Embodiment 3

[0053] 1.2 Sample pretreatment

[0054] Accurately weigh 1.0012g of fly ash sample 3#, add 20mL of 20mmol / L perchloric acid into a 50mL small beaker, oscillate on an ultrasonic oscillator for 20min, and then add it to a 10mL centrifuge tube. Centrifuge at a speed of 4000r / min for 20min, take the supernatant and pass through a 0.22μm water phase filter membrane to obtain the sample to be tested;

[0055] 1.4 Fly ash sample test

[0056] The chromatographic conditions are: CS20 cation exchange column, 4×250mm, CG20 analytical guard column, 4x50mm, CSRS300 cation suppressor, the suppressor current is 50mA, the column temperature is 50°C, the injection volume is 30μL, and the eluent is It is prepared from sulfamic acid solution and acetonitrile solution, and the sample is analyzed by gradient elution. The gradient elution procedure is as follows:

[0057] 0~5min, the concentration of sulfamic acid is 0.005mol / L, the concentration of acetonitrile solution is 10%,

[0058] 6~15mi...

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PUM

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Abstract

The invention discloses a method for determining the content of ammonium ion in fly ash. The method comprises the following steps: (1) pretreatment of the fly ash sample to be tested; (2) drawing of a standard working curve; (3) ion chromatography analysis and result calculation. The invention adopts inorganic acid solution or organic acid solution to dissolve the fly ash sample, and through ultrasonic oscillation, centrifugation, filtration, etc., all the ammonia in the fly ash exists in the form of ammonium salt, the dissolution is complete, the operation steps are simple and fast, and the improvement is improved. Analyze test efficiency. The present invention uses an ion chromatograph to test the content of ammonium ions in the pretreated fly ash, which effectively avoids the influence of other ions on the interference of the test results, improves the accuracy of the method, and has small measurement errors and high precision. high merit.

Description

technical field [0001] The invention belongs to the technical field of building material detection, and in particular relates to a method for measuring ammonium ion content in fly ash. Background technique [0002] Fly ash is one of the solid wastes discharged from power plants and has been widely used in the field of building materials in recent years. The increase in construction projects and the maturity of fly ash application technology make the market demand for fly ash more and more, and then there is a situation that the supply of fly ash is in short supply. As a secondary product of power plants, fly ash is mostly treated as waste raw material, so it is difficult to guarantee the quality of fly ash. The secondary processing of fly ash may also introduce unknown impurities. In the process of mixing concrete mixed with fly ash, there will be an irritating and unpleasant smell. Sometimes the concrete after pouring will bubble. After hardening, the concrete Hollows wil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 李格丽方云辉林艳梅林添兴郭元强
Owner KZJ NEW MATERIALS GROUP CO LTD
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