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Kit and detection method for determining ammonia nitrogen in sample by ion chromatography post-column derivatization method

An ion chromatographic column and derivatization technology, which is applied in the field of detection of ammonia nitrogen content in water quality, can solve the problems of long time consumption, insufficient sensitivity, incomplete color development of the solution, etc.

Pending Publication Date: 2021-09-14
赵永刚 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The sensitivity is not high enough: the detection limit cannot meet the needs of some samples. When the water sample volume is 50mL and a 20mm cuvette is used, the detection limit of this method is 0.025mg / L
[0007] (2) There are interference factors: if the sample itself is colored, it will also absorb light at 420nm, which will cause serious interference; different ion concentrations, salinity, etc. will interfere with the test
[0008] (3) It takes a long time: experiments show that the color development of the solution is not complete before the reaction time is 10 minutes; the color is relatively stable after 10-30 minutes; the color tends to deepen after 30-45 minutes; the color gradually fades after 45-90 minutes

Method used

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  • Kit and detection method for determining ammonia nitrogen in sample by ion chromatography post-column derivatization method
  • Kit and detection method for determining ammonia nitrogen in sample by ion chromatography post-column derivatization method
  • Kit and detection method for determining ammonia nitrogen in sample by ion chromatography post-column derivatization method

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Embodiment 1

[0034] Example 1: A kit for post-column derivatization of ion chromatography for detecting ammonia nitrogen content in a sample

[0035] (1) The potassium salt or sodium salt system of mineral acid+mineral acid as mobile phase is preferably the potassium salt or sodium salt of hydrochloric acid+hydrochloric acid, followed by the potassium salt or sodium salt of sulfuric acid+sulfuric acid, the potassium salt of nitric acid+nitric acid or Sodium salt, the concentration of hydrochloric acid + potassium salt or sodium salt of hydrochloric acid is 30-100mmoL / L+1-20mmoL / L, the concentration of sulfuric acid+potassium or sodium salt of sulfuric acid is 30-100mmoL / L+1-20mmoL / L, the system concentration of nitric acid+potassium or sodium salt of nitric acid is 30~100mmoL / L+1~20mmoL / L.

[0036] (2) The chromatographic column used to fill the cation exchange resin containing sulfonic acid or carboxylic acid groups is to graft sulfonic acid groups or carboxylic acid groups on polystyren...

Embodiment 2

[0038] Embodiment 2: The kit of the present invention is applied in the post-column derivatization method of ion chromatography for measuring sample ammonia, specifically comprising the following steps:

[0039] First filter the aqueous solution of the sample containing ammonia nitrogen to be tested, then inject the solution, separate and elute through a cation exchange chromatography column, and then undergo the mixed reaction of salicylate, sodium nitroferricyanide and hypochlorite in sequence Heating produces a blue compound which has the strongest absorption at a wavelength of 660nm. The heating temperature is 30-100°C; when the cation exchange column is separated and eluted, the flow rate of the mobile phase pump is 1-4mL / min; min; the sodium nitroferricyanide is added to the heater through the infusion pump to react, and the flow rate of the infusion pump is 0.1-0.8mL / min; the hypochlorite ion is added to the heater through the infusion pump to react, and the infusion T...

Embodiment 3

[0040] Embodiment 3: the application of kit in measuring 1ppm ammonia, ammonium ion standard solution

[0041] Kits for ion chromatography post-column derivatization for the detection of ammonia nitrogen content in samples:

[0042] (1) 30mmol / L sodium chloride+1mmol / L hydrochloric acid as mobile phase

[0043] (2) A chromatographic column for packing cation exchange resins containing sulfonic acid or carboxylic acid groups, with a particle size of 5 microns and a group density of 1 mmol / g.

[0044] (3) Derivative reagent: 100mmol / L sodium salicylate, 1mmol / L sodium nitroferricyanide, sodium hypochlorite with 0.5% available chlorine content.

[0045]Specific implementation steps:

[0046] (1) Use 100mg / L ammonia nitrogen standard solution and dilute it with deionized water to a standard solution with a concentration of 1mg / L.

[0047] (2) Take 2ml of the solution and filter it with a 0.45μm membrane filter.

[0048] (3) filtrate is transferred to the autosampler of HPLC, a...

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Abstract

The invention discloses an ion chromatography post-column derivatization kit for detecting ammonia nitrogen content in a sample and a detection method. The detection method is combined with the kit and has the advantages of simple and rapid pretreatment, low detection limit, strong anti-interference capability and simple operation. The specific method comprises the following steps of firstly filtering a to-be-detected sample aqueous solution, then feeding the solution into a sample, separating and eluting through a cation exchange chromatographic column, heating and reacting with salicylate and hypochlorous acid ions under an alkaline condition in the presence of sodium nitroferricyanide to generate a blue compound, and enabling the product to have relatively strong absorption under a certain wavelength. Therefore, the ammonia nitrogen content is detected.

Description

technical field [0001] The invention relates to a detection technology for ammonia nitrogen content in water quality, in particular to a kit for detecting ammonia nitrogen by an ion chromatographic post-column derivatization method and a method for detecting ammonia nitrogen content in a sample in combination with the kit. Background technique [0002] Ammonia nitrogen in water can be converted into nitrite under certain conditions. If consumed for a long time, nitrite in water will combine with protein to form nitrosamine, which is a strong carcinogen and extremely harmful to human health. [0003] The main harmful effect of ammonia nitrogen on aquatic organisms is free ammonia, which is more than ten times more toxic than ammonium salt, and increases with the increase of alkalinity. The toxicity of ammonia nitrogen is closely related to the pH value and water temperature of the pool water. In general, the higher the pH value and water temperature, the stronger the toxicity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/96G01N30/06G01N30/14
CPCG01N30/96G01N30/06G01N30/14
Inventor 宋兴伟胡玲赵永刚
Owner 赵永刚
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