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Preparation method and application of fluorescent test strip for trace water analysis in organic reagents

A technology of organic reagents and test strips, which is applied in the field of preparation of fluorescent test strips for trace water analysis in organic reagents. It can solve the problems of long measurement time, high environmental requirements, and poor accuracy, and achieves intuitive quantitative methods and portable detection systems. , the effect of short detection time

Active Publication Date: 2020-11-06
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The co-distillation method is to co-distill the oil sample with the same volume of solvent such as toluene, and the trace moisture in the oil is taken out by the toluene. The volume ratio of the latter to the original sample is the trace moisture content of the sample. The measurement error of this method is Larger, only suitable for the determination of constant and trace moisture; Karl Fischer method is used as a method for the determination of trace moisture in common oils, and its titration solution involves the use of iodine, sulfur dioxide, pyridine, methanol and other substances, which are prone to side reactions. , the naked eye judges the end point is not sensitive, and the reproducibility is poor. . Most of the Fischer reagents are toxic, poor in accuracy, and take a long time to measure. Although gas chromatography is easy to operate and is suitable for the determination of a large number of samples, the instrument is large, expensive, time-consuming, and requires high environmental requirements, which is not conducive to on-site detection and Product Process Control

Method used

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  • Preparation method and application of fluorescent test strip for trace water analysis in organic reagents
  • Preparation method and application of fluorescent test strip for trace water analysis in organic reagents
  • Preparation method and application of fluorescent test strip for trace water analysis in organic reagents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Disperse QG in absolute ethanol for pretreatment, centrifugally purify and dry, add 5.0 mg QG in 30 mL DMF, and ultrasonically disperse;

[0044] (2) Add 0.20 g MA to the QG after ultrasonic dispersion in step (1) while stirring, and add 0.20 g 2-aminoterephthalic acid after stirring for 10 minutes;

[0045] (3) Add 2.0 mL of 25% glutaraldehyde to the solution prepared in step (2) and stir for 15 minutes, then add 0.1 g of zinc nitrate while stirring;

[0046] (4) Slowly drop 1.0 mL of triethylamine into the solution prepared in step (3), stir for 120 minutes, centrifuge, and wash with DMF;

[0047] (5) Disperse the precipitate obtained in step (4) in CH 2 Cl 2 Medium, aging for 24 hours;

[0048] (6) After centrifuging the precipitate obtained after aging in step (5), collect the product and dry it in a vacuum oven at 120°C for 12 h to obtain a QG-loaded MOF composite;

[0049] (7) Dip the test strip into the ethanol solution of the QG-loaded MOF nanocomposite ...

Embodiment 2

[0051] (1) Disperse QG in absolute ethanol for pretreatment, centrifugally purify and dry, add 5.0 mg QG in 30 mL DMF, and ultrasonically disperse;

[0052] (2) Add 0.2523 g of MA to the QG after ultrasonic dispersion in step (1) while stirring, and add 0.15 g of 2-aminoterephthalic acid after stirring for 10 minutes;

[0053] (3) Add 2.0 mL of 25% glutaraldehyde to the solution prepared in step (2) and stir for 15 minutes, then add 1.20 g of zinc nitrate while stirring;

[0054] (4) Slowly drop 1.0 mL of triethylamine into the solution prepared in step (3), stir for 120 minutes, centrifuge, and wash with DMF;

[0055] (5) Disperse the precipitate obtained in step (4) in CH 2 Cl 2 Medium, aging for 24 hours;

[0056] (6) After centrifuging the precipitate obtained after aging in step (5), collect the product and dry it in a vacuum oven at 120°C for 12 h to obtain a QG-loaded MOF composite;

[0057] (7) Dip the test strip into the ethanol solution of the QG-loaded MOF nanoc...

Embodiment 3

[0059] (1) Disperse QG in absolute ethanol for pretreatment, centrifugally purify and dry, add 5.0 mg QG in 30 mL DMF, and ultrasonically disperse;

[0060] (2) Add 0.2523 g MA to the QG after ultrasonic dispersion in step (1) while stirring, and add 0.3623 g 2-aminoterephthalic acid after stirring for 10 minutes;

[0061] (3) Add 2.0 mL of 25% glutaraldehyde to the solution prepared in step (2) and stir for 15 minutes, then add 1.50 g of zinc nitrate while stirring;

[0062] (4) Slowly drop 1.0 mL of triethylamine into the solution prepared in step (3), stir for 120 minutes, centrifuge, and wash with DMF;

[0063] (5) Disperse the precipitate prepared in step (4) in CH 2 Cl 2 Medium, aging for 24 hours;

[0064] (6) After centrifuging the precipitate obtained after aging in step (5), collect the product and dry it in a vacuum oven at 120°C for 12 h to obtain a QG-loaded MOF composite;

[0065] (7) Dip the test strip into the ethanol solution of the QG-loaded MOF nanocompo...

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Abstract

The invention belongs to the field of energy chemical industry detection, and particularly relates to a preparation method and application of a trace water analysis fluorescent test strip in an organic reagent. The preparation method of the fluorescent test strip comprises the following steps that (1) glutaraldehyde is used for covalently combining melamine with QG, and 2-aminoterephthalic acid and zinc nitrate are added in sequence for coordination to form MOFs; (2) the MOFs is subjected to triethylamine precipitation, DMF washing and drying to obtain a nanocomposite; and (3) the nanocomposite is loaded on the test strip to prepare a water sensitive fluorescent test strip. When the test strip is used for detecting trace water in the organic reagent, the operation is simple, the detectiontime is short, the sensitivity is high and a detection system is portable, the test strips is suitable for rapid, sensitive, automatic, micro-quantization and field-appliable rapid measurement of trace water in organic reagent samples such as ethanol, aviation gasoline and DMF, and the test results are consistent with the quantitative results of a classical Karl Fischer method.

Description

technical field [0001] The invention belongs to the field of energy and chemical industry detection, and in particular relates to a preparation method and application of a fluorescent test strip for analyzing trace amounts of water in organic reagents. Background technique [0002] Water is a very important resource in nature. But it may exist as a pollutant and harmful impurity in many solvents, pharmaceuticals, foods or chemicals. For example, trace amounts of water in organic chemical reactions may have a great influence on the reaction process, and even determine the product, yield and selectivity of the reaction. Therefore, it is of great significance to quantitatively determine the content of trace moisture in organic reagents. Another example is aviation gasoline. For the safe operation of the aircraft, the gasoline should not contain water. Under severe flight conditions, the water in aviation gasoline will not only reduce the utilization rate of fuel, but also fr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
CPCG01N21/6402
Inventor 王桦蔡园园华玥刘欢陈丽君吕晓霞李帅
Owner QUFU NORMAL UNIV
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