Method for detecting nitrate, nitrite and sulfite in brine purified by lime flue gas method

A technology of lime flue gas and nitrite, applied in the field of chemical analysis, can solve the problems that the accurate detection of nitrate, nitrite and sulfite cannot be realized, and achieve the effect of inhibiting the oxidation of sulfurous acid

Active Publication Date: 2020-04-24
CHINASALT JINTAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, this method cannot realize the accurate detection of trace nitrate, nitrite and sulfite in brine

Method used

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  • Method for detecting nitrate, nitrite and sulfite in brine purified by lime flue gas method
  • Method for detecting nitrate, nitrite and sulfite in brine purified by lime flue gas method
  • Method for detecting nitrate, nitrite and sulfite in brine purified by lime flue gas method

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Embodiment 1

[0031] To draw a mixed standard curve of nitrate, nitrite and sulfite ions, accurately weigh 27.4168g of anhydrous sodium nitrate, 1.4997g of anhydrous sodium nitrite and 1.5742g of anhydrous sodium sulfate in the same beaker , the mixture was diluted to a 1000ml volumetric flask and prepared as a mixed standard stock solution. Use 0.02mg / L formaldehyde solution to dilute the mixed standard stock solution, and prepare a series of nitrate concentrations of 0.2mg / L, 0.4mg / L, 1mg / L, 2mg / L, 4mg / L, 8mg / L after serial dilution Mix the standard solution; the concentrations of nitrite and sulfurous acid are 0.02mg / L, 0.04mg / L, 0.1mg / L, 0.2mg / L, 0.4mg / L, 0.8mg / L. The ion chromatography parameter is eluent 3.0mmol / LNa 2 CO 3 and 1.2mmol / L NaHCO 3 , Eluent flow rate 0.7mL / min, suppressor regeneration solution: 92mmol / LH 2 SO 4 , ultrapure water; the detector conductance 861 type IonPacAS5 separation column and the ultraviolet 844 type IonPacAS4 separation column are synchronously de...

Embodiment 2

[0035] Firstly, the ion chromatography conductivity 861 detector was used to detect the SO in the sample to be detected after pretreatment. 4 2- The content is measured to ensure that SO 4 2- The content is less than 110.0mg / L, which solves the problem of SO in the detection of sulfite ion content by ion chromatography ultraviolet 844 4 2- ion effects.

[0036] Table 2 Comparison of detection limits of ions to be measured

[0037]

[0038] Ion chromatography conductance 861 type IonPacAS5 separation column and ultraviolet 844 type IonPacAS4 separation column are used for synchronous detection. The ion chromatography ultraviolet 844 type has high sensitivity for the detection of nitrite, nitrate and sulfite ions, with a resolution of > 5.0 and a peak shape. Symmetry factor ≥ 0.90, its ion chromatography detection limit NO 2 - : 0.002mg / L, NO 2 - : 0.002mg / L, SO 3 2- : 0.02mg / L; while it has an inhibitory effect on the detection of chloride ions and sulfate ions, i...

Embodiment 3

[0040] The content of nitrate, nitrite and sulfite ions in the brine after purification by lime flue gas method is low, on the order of mg / kg or ug / kg, and the tailing of the chloride ion peak will affect the sub- Nitrate, nitrate and sulfite ion detection, see appendix figure 2 .

[0041] Lime flue gas purified brine, its main components are NaCl: 280-305g / L, Ca 2+ : 0~10ppm, Mg 2+ : 0~5ppm, SO 4 2- : 8~12g / L, CO 3 2- : 0.2~0.8g / L, OH - : 0.05~0.1g / L, among which the pH of brine after lime flue gas purification: 9.5~11, the interference of calcium and magnesium cations on ion chromatography detection has been removed, and sulfite is not easy to be oxidized in this alkaline brine, Add mercury salt to remove chloride ion interference, n(Hg):n(Cl)=1:3.5-1:4, use 0.02mg / L formaldehyde solution to dilute 200-400 times, and the relative standard deviation of the ions is ≤1.0% ; Filtrate with a 0.22 μm organic microporous membrane to prepare the solution to be tested, and u...

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Abstract

The invention belongs to the technical field of chemical analysis, and particularly relates to a method for detecting nitrate, nitrite and sulfite in brine purified by a lime flue gas method. The method comprises the following steps of adding a dechlorination aid into a brine sample, and removing chloride ion interference by adopting trace rapid pretreatment; and detecting nitrate, nitrite and sulfite at the same time by adopting cooperative detection of conductivity 861 type and ultraviolet 844 type detectors. In the method, contents of nitrate, nitrite and sulfite in brine can be accuratelyand quickly detected, and influence of impurity gases NOX and SO2 in a flue gas on quality of the brine can be reflected in time. Problems that detection of nitrite, nitrate and sulfite ions is affected due to trailing of chloride ion peaks in the brine purified through a lime flue gas method and the sulfite is difficult to accurately detect due to a low peak separation degree with sulfate radicals are solved, and the problems that a high-salt-content sample is easy to crystallization, a detection instrument is blocked, and a detection result is affected are solved too.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, and in particular relates to a method for detecting nitrate, nitrite and sulfite in water containing ions such as calcium, magnesium, iron and sulfate. In particular, it relates to a method for detecting nitrate, nitrite and sulfite in brine after lime flue gas purification. Background technique [0002] Lime flue gas brine purification process, the main component of flue gas is N 2 , O 2 , NO X , SO X , CO 2 、H 2 O, dust, heat, directly discharged into the atmosphere will cause pollution to the environment, desulfurization and denitrification purification treatment is required, the lime flue gas brine purification process makes full use of CO in the flue gas 2 Applied to brine purification. To study and analyze the migration route, removal and impact of impurity ions in flue gas on the quality of salt, but its content is low, on the order of mg / kg or ug / kg, and general detection...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/64G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N30/64G01N2030/027G01N2030/645
Inventor 冷翠婷赵营峰陈留平朱旭初刘凯郝剑波李焕孙桀谢兴胜
Owner CHINASALT JINTAN
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