Method for determining glutaraldehyde in water based on metal organic framework material composite substrate surface enhanced Raman spectroscopy

A surface-enhanced Raman, metal-organic framework technology, applied in the field of chemical detection, can solve the problems of complex structure, difficult synthesis, and complicated operation of fluorescent probes

Inactive Publication Date: 2021-04-23
GUANGXI UNIV FOR NATITIES
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Problems solved by technology

Among them, the spectral analysis method has the advantages of fast speed and low analysis cost. However, most of the existing spectral analysis techniques can only detect high levels of glutaraldehyde in disinfectants, and the sensitivity is not enough.
Chromatography requires complex processing procedures such as derivation, extraction, desorption, and separation; fluorescence probes have complex structures, long synthetic routes, difficult synthesis, and complicated operations

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  • Method for determining glutaraldehyde in water based on metal organic framework material composite substrate surface enhanced Raman spectroscopy
  • Method for determining glutaraldehyde in water based on metal organic framework material composite substrate surface enhanced Raman spectroscopy
  • Method for determining glutaraldehyde in water based on metal organic framework material composite substrate surface enhanced Raman spectroscopy

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preparation example Construction

[0040] The present invention provides gold doped MIL-101(Cr). In the present invention, the preparation method of the gold-doped MIL-101(Cr) preferably comprises: dispersing MIL-101(Cr) in an aqueous solution of chloroauric acid, then mixing it with sodium citrate, and performing a redox reaction to obtain Gold doped MIL-101(Cr).

[0041] In the present invention, preferably, MIL-101 (Cr) is dispersed in an aqueous chloroauric acid solution to obtain an aqueous dispersion of MIL-101 (Cr) and chloroauric acid.

[0042] In the present invention, there is no special limitation on the dispersion operation of the MIL-101(Cr), and the operation of solid-liquid dispersion well-known to those skilled in the art can be used. In the present invention, the dispersion of MIL-101(Cr) preferably includes ultrasonication and stirring performed in sequence. In the present invention, there is no special limitation on the power of the ultrasound, and the conventional ultrasound power of those...

Embodiment 1

[0087] (1) Provide gold-doped MIL-101(Cr) (hereinafter referred to as Au@MIL-101)

[0088] ① Preparation of MIL-101(Cr) by hydrothermal method:

[0089] 1.1620g terephthalic acid, 2.8000g Cr(NO 3 ) 3 9H 2 O, 33.6g of ultrapure water, 0.4166mL of 40% hydrofluoric acid (0.4909g in mass) were homogenized by ultrasound, and then hydrothermally reacted at 220°C for 8 hours in a 50mL closed reactor. After cooling the hydrothermal product to room temperature, centrifuge at 3000rpm for 3min to obtain the crude product; then reflux the obtained crude product in ethanol at 80°C for 5h, and after cooling to room temperature, centrifuge at 3000rpm for 3min to obtain the preliminary Purified crude product; reflux the preliminary purified crude product in 200mL of 30mM ammonium fluoride solution at 60°C for 10h to obtain further purified crude product; After centrifugation for 3 minutes, the centrifuged solid was washed with ultrapure water at 60°C to remove ammonium fluoride, dried in ...

Embodiment 2

[0103] Repeat the method of embodiment 1, difference with embodiment 1 is as follows:

[0104] (1) Take eight 2mL centrifuge tubes in step (3), and add 30 μL of Au@MIL-101 / PATP with a concentration of 10 g / L, 2 μL of glacial acetic acid with a concentration of 4 mol / L and 30 μL of Glutaraldehyde solution.

[0105] (2) The medical wastewater sample was used as the sample solution to be tested.

[0106] Then read 1078cm with the Raman spectrum of the solution to be tested -1 with 1621cm -1 The ratio of the peak height of the absorption peak at 1078 / I 1621 , obtain the concentration C of glutaraldehyde in the sample solution to be tested according to the working curve that embodiment 1 step (3) draws 样 , and then according to the formula ω=C 样 × M × 1000, calculate the content ω of glutaraldehyde in medical wastewater, and measure 5 sets of parallel data of the solution to be tested. The calculation results are shown in Table 1.

[0107] Embodiment 1~2 test solution laser...

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Abstract

The invention relates to the technical field of chemical detection, and provides a method for determining glutaraldehyde in water based on metal organic framework material composite substrate surface enhanced Raman spectroscopy. According to the method, glutaraldehyde reacts with PATP under the weak acid condition to generate Schiff base, then a solution obtained through the reaction is subjected to laser Raman testing to obtain a Raman spectrum for generating the Schiff base, and the content of glutaraldehyde in water can be rapidly determined according to the linear relation between the SERS spectrum peak value and the glutaraldehyde concentration. Experimental results show that the method provided by the invention has the advantages that the glutaraldehyde detection limit is as low as 3.5*10<-8> mol / L, the detection limit is relatively low, and the sensitivity is relatively high; moreover, in the presence of interfering substances, the influence on the detection result is relatively small, and the selectivity on glutaraldehyde detection is relatively good.

Description

technical field [0001] The invention relates to the technical field of chemical detection, in particular to a method for measuring glutaraldehyde in water based on surface-enhanced Raman spectroscopy of metal-organic framework material composite substrates. Background technique [0002] Glutaraldehyde (GA) can be used as processing aids, preservatives, disinfectants, tanning agents, wood adhesives, drugs and polymer synthesis raw materials in the food industry, and is widely used in food processing, biomedicine, and oil exploration. , tanning industry and pharmaceutical science and other fields. GA has a certain degree of harm to various organisms, and is usually discharged into the environment through wastewater in the form of an aqueous solution. It is acutely toxic to aquatic organisms (especially algae) and has long-term effects on aquatic organisms. It is also harmful to the health of humans and other animals. make an impact. The increasing concern for human health an...

Claims

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Application Information

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IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 严军徐阳李营营马纯晶朱伟伟
Owner GUANGXI UNIV FOR NATITIES
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