Simultaneous online analysis method for nitrite and nitrate in water sample and test sample treatment device thereof

一种亚硝酸盐、硝酸盐的技术，应用在通过观察对化学指示剂的影响进行材料分析、测量装置、分析材料等方向，能够解决分析成本增大、同时性低、干扰准确性等问题，达到抗盐度干扰能力强、降低分析成本、良好精密度的效果

Inactive Publication Date: 2014-06-04
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(1) The deficiencies of ion chromatography are reflected in: the ion chromatography is a high-pressure ion chromatography, using a high-pressure pump, so the instrument is inconvenient to carry, which is not conducive to on-site determination; using conductivity detection, so nitrite and nitrate pass through the anion After separation, the chromatographic column must pass through the suppressor or suppressor column and then enter the detection channel. The suppressor or suppressor column is expensive, resulting in high analysis costs. In addition, regular regeneration is required, and the operation is cumbersome; the service life of the anion chromatographic column is short, resulting in analysis Increased cost; the sensitivity of nitrite and nitrate detection is not high enough, the minimum detection limit of nitrite is about 3 μg / L (calculated as N), and the minimum detection limit of nitrate is about 2 μg / L (calculated as N meter); the ability to resist the interference of chloride ions is poor, so it cannot be used for the detection of nitrite and nitrate in seawater
(2) Salinity will interfere with the accuracy of the flow injection method for the determination of nitrite and nitrate, and the flow injection method has low simultaneity in the determination of nitrite and nitrate, and the operation is cumbersome. , it is necessary to manually adjust the instrument to measure nitrate; (3) The sensitivity of UV spectrophotometry is not high enough and the salinity will interfere with the determination of nitrite and nitrate

Method used

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  • Simultaneous online analysis method for nitrite and nitrate in water sample and test sample treatment device thereof
  • Simultaneous online analysis method for nitrite and nitrate in water sample and test sample treatment device thereof
  • Simultaneous online analysis method for nitrite and nitrate in water sample and test sample treatment device thereof

Examples

Experimental program
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Embodiment 1

[0057] Embodiment 1: prepare low pressure anion exchange resin

[0058] This embodiment prepares low-pressure anion exchange resin, and the process steps are as follows:

[0059] (1) With styrene and divinyl benzene as raw materials and benzoyl peroxide as a catalyst, the quality of styrene: the quality of divinyl benzene: the quality of benzoyl peroxide=600:60:1; , divinylbenzene and benzoyl peroxide are put into a reaction vessel, and the polymerization reaction is carried out at normal pressure and 90° C. to generate styrene-divinylbenzene spherical copolymer beads, and the reaction time is 15 hours;

[0060] (2) Place the styrene-divinylbenzene spherical copolymer beads prepared in step (1) in a reaction vessel, first chloromethylate them with chloromethyl ether, and then aminate them with trimethylamine to obtain The anion-exchange resin beads; the addition of the chloromethyl ether should make the quality of the styrene-divinylbenzene spherical copolymer beads and the v...

Embodiment 2

[0061] Embodiment 2: reduction column structure

[0062] In this embodiment, the inner diameter of the reduction column is 3mm, the column length is 40mm, and its structure is as follows figure 1 As shown, the reduction column is mainly composed of a column body, a filter membrane 7-4 installed at the liquid inlet and outlet ends of the column body, and a column packing 7-3 filled in the inner cavity of the column body; the column body includes a column tube 7-2, a plug 7 -5. The fixed sleeve 7-1 and the conduit 7-6, the plug is located on the outside of the filter membrane and a central hole is provided on it for the insertion of the catheter, and the fixed sleeve is located at the junction of the plug and the column tube for fixing the plug fixed on the column tube; the filter membrane 7-4 is made of nylon silk, and is installed between the two ends of the column tube and the plug; the column tube 7-2 is made of glass, and the column packing 7-3 is filled with Copper-plated...

Embodiment 3

[0065] Example 3: The first sample processing device

[0066] In this embodiment, the structural diagram of the sample processing device is shown in figure 2 , including a low-pressure pump 1, a six-way sampling valve 2, a mixer 6, a reactor 8, a sample container 11, an eluent container 12, a chromogenic liquid container 13, a waste liquid container 14, a sampling loop 10, and a low-pressure anion The separation column 3 and the reduction column 7; the reactor 8 is a coil structure, which is made of a polytetrafluoroethylene tube with a length of 3.0m and an inner diameter of 0.5mm. The inner diameter of the low-pressure anion separation column 3 is 5mm, and the column length It is 40mm, and its column filler is prepared by embodiment 1, and reduction column 7 is the reduction column described in embodiment 2, and the working pressure of low-pressure pump 1 is 2~3×10 5 Pa; combination of components:

[0067]The sample container 11 communicates with a liquid inlet of the six...

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Abstract

The invention provides a simultaneous online analysis method for nitrite and nitrate in a water sample and a test sample treatment device thereof. The test sample treatment device has two structures, and mainly comprises a low-pressure pump, a six-way sample feeding valve, a mixer, a reactor, a sample container, an eluent container, a color developing solution container, a waste liquid container, a low-pressure anion separation column and a reduction column. An analysis instrument comprising the test sample treatment device and a testing device is used in the method. The method comprises the following steps: 1. setting the analysis instrument in a sample feeding state for surveying and mapping a base line; 2. converting the analysis instrument into a spectrogram of nitrite and nitrate in an analysis state surveying and mapping test sample; 3. replacing a test sample by using a series of standard samples with known nitrite and nitrate concentrations, repeating the steps 1 and 2 to respectively obtain corresponding standard sample spectrograms, drawing a working curve by using a concentration of a standard sample as a horizontal coordinate and a peak height of a standard sample spectrogram as a longitudinal coordinate; and 4. substituting a peak height value of the test sample spectrogram in a regression equation of the working curve, and figuring out nitrite and nitrate concentrations in the test sample.

Description

technical field [0001] The invention belongs to the field of analysis of nitrate and nitrite in water samples, and in particular relates to a simultaneous online analysis and analysis method of nitrate and nitrite and a sample processing device thereof. Background technique [0002] Nitrite is a general-purpose chemical reagent widely used in food industry, dye industry, and inhibition of water corruption. Nitrite can effectively inhibit the growth and reproduction of botulinum toxin, prevent botulinum toxin poisoning, and make the food after adding nitrite have good color. However, after nitrite is absorbed by the human body, normal hemoglobin can be converted into methemoglobin and then lose its oxygen-carrying function, and the secondary amines in the human or animal body can be combined with it and converted into strong carcinogen nitrosamines, thereby inducing cancer. The adult poisoning dose of nitrite is 0.3-0.5g, and the lethal dose is 1-3g. The Food and Agricultur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78G01N1/28
CPCG01N33/188
Inventor 张新申李楠蒋小萍
Owner SICHUAN UNIV
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