Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample

A nitrite ion and cation chromatography technology, applied in the field of automatic online analysis of trace amounts of NH4+ and NO2- in water samples, can solve the problems of easy contamination of chromatographic columns, slow analysis speed, consumables, etc. Contamination and anti-interference ability, reduce analysis cost, prolong the effect of life

Inactive Publication Date: 2017-04-26
SICHUAN UNIV
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Problems solved by technology

[0003] Currently, ion chromatography analyzes NH in water samples 4 + and NO 2 - When using high-pressure ion chromatography, the two ions need to be sampled separately and detected separately, that is, an anion chromatographic column and a supporting anion elution system are usually used, and the conductivity detection is used to analyze the NO 2 - , using a cation chromatographic column and a matching cation elution system to separate and detect NH 4 + , unable to achieve NH 4 + and NO 2 - Simultaneous analysis of
Existing analysis of NH in water samples 4 + and NO 2 - The current ion chromatography method has the following disadvantages: separate sampling and separate detection have the disadvantages of slow analysis speed and low analysis efficiency; high pressure ion chromatography adopts high pressure operation, the price of high pressure ion chromatography is high, and the supporting chromatographic column is consumable products, whose price is generally 10,000 to 20,000 yuan / piece, so the analysis cost of this method is extremely high, and it is difficult to popularize and apply; at the same time, the column packing of the chromatographic column used in high-pressure ion chromatography is a thin-shell ion resin. The exchange capacity is very low, only 0.01-0.02mmol / g. When analyzing wastewater with complex components such as tannery wastewater, the chromatographic column is easily polluted, resulting in shortened service life of the chromatographic column and reduced anti-interference ability of the analysis system. Therefore, it is difficult to popularize and apply in the tannery wastewater analysis industry

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  • Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample
  • Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample
  • Low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in water sample

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Embodiment 1

[0038] In the present embodiment, investigate the column packing composition of low-pressure cation exchange column to measure NH to the method for the present invention 4 + with NO 2 - Impact.

[0039] 1. Preparation containing NH 4 + and NO 2 - standard sample

[0040] NH 4 + Standard stock solution (1000mg / L): bake ammonium sulfate at 110°C for 1 hour, then place in a desiccator to cool to room temperature, weigh 0.4716g of dry ammonium sulfate, transfer it into a 100mL volumetric flask, and dilute to the mark with deionized water , shake well, and store in a refrigerator at 4°C, it can be stored stably for six months. When using, measure an appropriate amount and dilute with deionized water to the desired concentration.

[0041] NO 2 - Standard stock solution (1000mg / L): bake sodium nitrite at 110°C for 1 hour, place it in a desiccator and cool it to room temperature, weigh 0.4929g of dry sodium nitrite, transfer it into a 100mL volumetric flask, and dilute it...

Embodiment 2

[0061] The present embodiment tests the standard sample, to investigate the precision of the method of the present invention, the steps are as follows:

[0062] 1. Preparation containing NH 4 + with NO 2 - standard sample

[0063] NH 4 + Standard stock solution (1000mg / L): bake ammonium sulfate at 110°C for 1 hour, then place in a desiccator to cool to room temperature, weigh 0.4716g of dry ammonium sulfate, transfer it into a 100mL volumetric flask, and dilute to the mark with deionized water , shake well, and store in a refrigerator at 4°C, it can be stored stably for six months. When using, measure an appropriate amount and dilute with deionized water to the desired concentration.

[0064] NO 2 - Standard stock solution (1000mg / L): bake sodium nitrite at 110°C for 1 hour, place it in a desiccator and cool it to room temperature, weigh 0.4929g of dry sodium nitrite, transfer it into a 100mL volumetric flask, and dilute it with deionized water to Mark the line, shak...

Embodiment 3

[0080] In the present embodiment, the standard working curve is drawn, and the steps are as follows:

[0081] 1. Preparation of standard samples

[0082] (1) NH 4 + Standard stock solution (1000mg / L): bake ammonium sulfate at 110°C for 1 hour, then place in a desiccator to cool to room temperature, weigh 0.4716g of dry ammonium sulfate, transfer it into a 100mL volumetric flask, and dilute to the mark with deionized water , shake well, and store in a refrigerator at 4°C, it can be stored stably for six months. When using, measure an appropriate amount and dilute with deionized water to the desired concentration.

[0083] (2)NO 2 - Standard stock solution (1000mg / L): bake sodium nitrite at 110°C for 1 hour, place it in a desiccator and cool it to room temperature, weigh 0.4929g of dry sodium nitrite, transfer it into a 100mL volumetric flask, and dilute it with deionized water to Mark the line, shake well, store in a brown bottle, and store in a refrigerator at 4°C in the...

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Abstract

The invention provides a low-pressure anion-cation chromatographic-spectrophotometric method for simultaneous online automatic analysis of trace ammonium ions and nitrite ions in a water sample; the method employs analytical apparatuses, such as a low-pressure pump, a sample injection valve, a sample injection ring, a low-pressure anion exchange column, a low-pressure cation exchange column, an oxidation reactor, a color rendering reactor, an optical flow cell, an optical detector, a computer processing system, a first mixer and a second mixer, and comprises the steps of (1) drawing a baseline; (2) drawing a spectrum of NH4+ and NO2- in a sample; (3) drawing a standard working curve; (4) calculating the concentrations of NH4+ and NO2- to be detected in the sample according to peak height values of the spectrum of NH4+ and NO2- and a regression equation of the standard working curve. It is the first time for the method to provide simultaneous online analysis for trace NH4+ and NO2- in a water sample by the joint use of low-pressure ion chromatography and spectrophotometry, and the method has the advantages of low analytical cost and high analytical efficiency.

Description

technical field [0001] The invention belongs to NH 4 + with NO 2 - The field of detection and analysis, especially involving trace amounts of NH in water samples 4 + and NO 2 - Simultaneous online automatic analysis method. Background technique [0002] Nitrogen-containing compounds will not only pollute water quality, but also be extremely harmful to human health. NH 4 + , NO 2 - and NO 3 - Through the oxidation, nitrification and denitrification of microorganisms, they can be transformed into each other. NH 4 + Oxidation will significantly reduce the concentration of dissolved oxygen in the water, resulting in a decline in water quality, leading to a sharp increase in photosynthetic microorganisms, and eutrophication of the water. High concentration of NH 4 + May affect the permeability of aquatic organisms and may cause acute ammonia poisoning and even death. NH 4 + It is not only a factor affecting the sensory water quality, but also an important co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/20G01N30/14G01N21/31G01N21/78B01D15/22B01D15/26B01D15/36
CPCB01D15/22B01D15/265B01D15/361G01N21/31G01N21/78G01N30/02G01N30/14G01N30/20G01N2030/143G01N2030/146G01N2030/201
Inventor 张新申赵正喜莫珊高跃昕
Owner SICHUAN UNIV
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