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
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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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