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Method for detecting nitrite ions based on ratio-type colorimetry

A nitrite ion, ratio-based technology, applied in the field of analytical chemistry, can solve the problems of expensive detection equipment, complex detection method operation, high cost of detection reagents, etc., and achieve the effect of low detection cost, simple operation and rapid detection

Active Publication Date: 2021-08-31
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1) Some detection methods are relatively complicated to operate, and the detection equipment is relatively expensive;
[0010] (2) Some detection reagents are relatively expensive and require high storage conditions

Method used

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  • Method for detecting nitrite ions based on ratio-type colorimetry
  • Method for detecting nitrite ions based on ratio-type colorimetry
  • Method for detecting nitrite ions based on ratio-type colorimetry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Add 0.0187mmol Fe 2 (SO 4 ) 3 with 0.373mmol MnSO 4 ·H 2 O dissolved in 0.3g PVP, 10mL LC 2 h 5 OH, 10mL deionized water mixed solution, ultrasonic 15min, after stirring for 10min, 10mL20mM K 3 [Fe(CN) 6 ] slowly added dropwise to Fe 2 (SO4) 3 with MnSO 4 ·H 2 In the mixed solution of O, continue to stir at room temperature for 1 h, then centrifuge the mixture at a speed of 8000 r / min, wash with ethanol and deionized water for 3 times, and finally freeze-dry to obtain Mn / Fe PBA;

[0046] (2) Dissolve 0.1g of Mn / Fe PBA in the above step (1) in 15mL of deionized water, add 10mL of 6mM TGA and stir at room temperature for 3h after ultrasonication for 20min, then centrifuge the mixture at a speed of 8000r / min, and then use Wash with ethanol and deionized water three times each, and finally freeze-dry to obtain hollow Mn / Fe PBA;

[0047] (3) Take an appropriate amount of hollow Mn / Fe PBA in step (2) and heat it in a tube furnace at 2.0°C min -1 Raise the tem...

Embodiment 2

[0052] (1) 0.048mmol Fe 2 (SO 4 ) 3 with 0.373mmol MnSO 4 ·H 2 O dissolved in 0.6g PVP, 20mL LC 2 h 5 OH, 20mL deionized water mixed solution, ultrasonic 15min, after stirring for 10min, 20mL 20mM K 3 [Fe(CN) 6 ] Slowly added dropwise to Fe 2 (SO4) 3 with MnSO 4 ·H 2 In the mixed solution of O, continue to stir at room temperature for 1 h, then centrifuge the mixture at a speed of 8000 r / min, wash with ethanol and deionized water for 3 times, and finally freeze-dry to obtain Mn / Fe PBA;

[0053] (2) Dissolve 0.1g of Mn / Fe PBA in the above step (1) in 25mL of deionized water, add 15mL of 6mM TGA after ultrasonication for 20min and stir at room temperature for 6h, then centrifuge the mixture at a speed of 8000r / min, and then use Wash with ethanol and deionized water three times each, and finally freeze-dry to obtain hollow Mn / Fe PBA;

[0054] (3) Take an appropriate amount of hollow Mn / Fe PBA in step (2) and heat it in a tube furnace at 2.0°C min -1 Raise the tempera...

Embodiment 3

[0059] (1) 0.187mmol Fe 2 (SO 4 ) 3 with 0.373mmol MnSO 4 ·H 2 O dissolved in 0.9g PVP, 30mLLC 2 h 5 OH, 30mL deionized water mixed solution, ultrasonic 15min, after stirring for 10min, 30mL 20mM K 3 [Fe(CN) 6 ] slowly added dropwise to Fe 2 (SO4) 3 with MnSO 4 ·H 2 In the mixed solution of O, after continuing to stir at room temperature for 1 h, the mixture was centrifuged at a speed of 8000 r / min, washed with ethanol and deionized water for 3 times, and finally freeze-dried to obtain Mn / Fe PBA;

[0060] (2) Dissolve 0.1g of Mn / Fe PBA in the above step (1) in 35mL of deionized water, add 20mL of 6mM TGA after ultrasonication for 20min and stir at room temperature for 9h, then centrifuge the mixture at a speed of 8000r / min, and then use Wash with ethanol and deionized water three times each, and finally freeze-dry to obtain hollow Mn / Fe PBA;

[0061] (3) Take an appropriate amount of hollow Mn / Fe PBA in step (2) and heat it in a tube furnace at 2.0°C min -1 Raise ...

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Abstract

The invention belongs to the technical field of analytical chemistry, and relates to a method for detecting nitrite ions based on ratio type colorimetry. The method comprises the following steps: sequentially adding 25 [mu] L of 1 mg / mL hollow MnFeO suspension, 30 [mu] L of 5 mM TMB solution and 1440 [mu] L of 0.2 M acetate buffer solution into a 2 mL centrifugal tube, and uniformly mixing; respectively adding NO2 <-> with different concentrations, wherein the final concentrations of the NO2 <-> in the system are respectively 3.33 [mu] M, 6.67 [mu] M, 10 [mu] M, 13.33 [mu] M, 20 [mu] M, 33.33 [mu] M, 50 [mu] M, 66.67 [mu] M, 83.33 [mu] M, 100 [mu] M, 120 [mu] M and 133.33 [mu] M; measuring an absorption spectrum by using an ultraviolet-visible absorption spectrophotometer, and drawing a standard working curve; and measuring an absorption spectrum of a to-be-measured NO2<->sample, and comparing the absorption spectrum with the standard working curve to obtain the NO2<-> concentration of the sample. According to the invention, the oxidation product TMBox of the hollow MnFeO + TMB system and the nitrite are subjected to a diazotization reaction so as to achieve the indirect detection of the nitrite, the detection process conditions are mild, the detection limit is as low as 0.2 [mu] M, and the detection of the nitrite in the food can be achieved.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, relates to a method for detecting nitrite, in particular to a method for detecting nitrite ion based on ratio type colorimetry. Background technique [0002] Nitrite contains nitrite (NO 2 - ) industrial salt is also a common food additive, and the dosage must be strictly controlled when used, otherwise it will cause nitrite poisoning, cause various injuries to the human body, and produce various diseases. For example, when too much nitrite enters the human body, it can oxidize the normal hemoglobin in the blood into methemoglobin, causing the hemoglobin to lose its oxygen-carrying capacity, leading to tissue hypoxia and expanding peripheral blood vessels; under the action of gastric acid, nitrite can It reacts with secondary amines, tertiary amines and amides in food to generate strong carcinogen nitrosamines, which induce gastric cancer and esophageal cancer. In addition, nitros...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78G01N21/31G01N21/33
CPCG01N21/78G01N21/31G01N21/33G01N2021/775
Inventor 牛湘衡汪梦珠刘朋朱恒佳刘邦祥
Owner JIANGSU UNIV
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