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Application of rare earth element complex in detection of trace nitrite in mineral water

A technology of rare earth elements and nitrite, applied in the field of analysis, can solve the problems of long reaction time and achieve the effects of high selectivity, wide detection range and high sensitivity

Active Publication Date: 2020-07-14
延吉海关综合技术服务中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this method, the buffer system of rare earth element complexes and nitrite ions mix and react for a long time, which takes 50-60 minutes. Therefore, it is necessary to broaden the range of rare earth element complexes for rapid detection of nitrite ions.

Method used

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  • Application of rare earth element complex in detection of trace nitrite in mineral water
  • Application of rare earth element complex in detection of trace nitrite in mineral water
  • Application of rare earth element complex in detection of trace nitrite in mineral water

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation of the rare earth element complex of embodiment 1, formula (I) (according to figure 1 Synthetic route shown):

[0029] 1. Synthesis of dimethyl pyridine-2,6-dicarboxylate

[0030] Dissolve pyridine-2,6-dicarboxylic acid (4g, 24mmol) in 50mL methanol, 2 SO 4 Under the condition of existence, the reaction was refluxed for 6h. After stopping the reaction, spin out the solvent, add 45 mL of water to the residue, and extract with ethyl acetate. The combined ethyl acetate was washed twice with water. Na 2 SO 4 After drying and concentrating, the target product was obtained with a yield of 91.5%.

[0031] 2. Synthesis of dimethyl 4-hydroxymethylpyridine-2,6-dicarboxylate

[0032] Dissolve 5.0g (22.45mmol) of dimethyl pyridine-2,6-dicarboxylate in a mixed solution of 30.6mL of 30% sulfuric acid and 38.3mL of methanol, stir at a medium speed, and then add 20.8mL of it dropwise at the same speed 30%H 2 0 2 And containing 7.8g (51mmol) FeS0 4 Saturated ...

Embodiment 2

[0046] Embodiment 2, the mensuration of nitrite ion

[0047] 1. Working curve making:

[0048] In order to determine the sensitivity of the detection method of the present invention to the detection of nitrite ions, adopt the above-mentioned detection method and conditions, add different concentrations of nitrite ion solutions (6.8 × 10 -2 μmol / L~2μmol / L), after shaking well, record the fluorescence emission peak intensity at 493nm at 280nm as excitation wavelength respectively. From this, the working curve diagram is obtained, such as image 3 shown. The linear equation is I=-330.4X-1331.5, I is the fluorescence intensity of the mixed system, X is the lg value of the concentration of nitrite ion, and the linear correlation coefficient R 2 is 0.993, and the linear range is 6.8×10 -2 μmol / L~2μmol / L, the nitrite ion concentration in this range can be calculated by the equation to get the accurate value.

[0049] 2. Sample determination:

[0050] Take a 3mL cuvette, add 2.7...

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Abstract

The invention belongs to the technical field of analysis, discloses an application of a rare earth element complex in detection of trace nitrite in mineral water, and discloses a new method for detecting trace nitrite in mineral water by using the rare earth element complex. The specific method comprises the following steps: adding 2.7 mL of a buffer system of a rare earth element complex into mineral water, uniformly mixing, detecting a fluorescence emission peak at 493nm by using 280nm as an excitation wavelength, and detecting nitrite ions according to the change of a fluorescence signal incombination with a working curve. The luminescent complex disclosed by the invention is not interfered by other ions in mineral water, and has the characteristics of high selectivity, convenience inoperation and high accuracy.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to the application of a rare earth element complex in detecting trace amounts of nitrite in mineral water. Background technique [0002] With the continuous improvement of people's living standards, drinking natural mineral water (hereinafter referred to as mineral water) has entered thousands of households, and the production scale and sales volume of mineral water are constantly expanding. Inspection work is also becoming more frequent. Mineral water was formed after a long history, so there should be no nitrite in mineral water. However, in actual work, it often occurs that the content of nitrite exceeds the national standard, especially in source water, sometimes the content of nitrite is too low to be detected, which affects the quality and reputation of mineral water. [0003] Nitrite exists widely in the water environment. After eating, under the action of gast...

Claims

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Application Information

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IPC IPC(8): G01N21/64
CPCG01N21/6428G01N21/643G01N2021/6432
Inventor 南京熙周鑫王娟毕程程赵嘉靓吴学张恩旭于文
Owner 延吉海关综合技术服务中心
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