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Metal heteroatom zeolite molecular sieve fenton method sample pretreatment method

A zeolite molecular sieve and sample pretreatment technology, applied in the field of functional materials, can solve the problems of non-reusable catalysts, easy precipitation of active iron ions, harsh pH value requirements, etc., and achieve the effect of fast and easy operation, easy operation and efficient treatment

Inactive Publication Date: 2016-05-04
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is worth pointing out that there are "bottleneck" problems such as free active iron ions in the corresponding reaction medium are easy to precipitate, the catalyst cannot be reused, and the pH value of the sample reaction medium is harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] This embodiment relates to a sample pretreatment method of Fe-ZSM-5 zeolite molecular sieve Fenton method with different proportions, and the method includes the following steps:

[0033] The synthetic method of step one.Fe-ZSM-5 (1%Fe content) zeolite molecular sieve: with Na 2 SiO 3 9H 2 O is the silicon source, tetrapropylene ammonium bromide (TPABr) is the template, Fe 2 (SO 4 ) 3 9H 2 O is an iron source. Fe 2 (SO 4 ) 3 9H 2 O stirred and dissolved in H 2 SO 4 solution, and then slowly dropwise added the pre-dissolved Na 2 SiO 3 9H 2 O solution, after fully stirring, add tetrapropylene ammonium bromide (TPABr) in a metered ratio, and fully stir evenly; the molar ratio of the final obtained precursor is: 60Na 2 O:5Fe 2 o 3 :60SiO2 2:2080H 2 O:2TPABr:50H 2 SO 4 ; The resulting precursor gel was sealed and reacted at 180°C for 96h, cooled to room temperature, filtered, washed until the pH of the filtrate was 7, and dried at 1°C·min -1 The tempera...

Embodiment 2

[0039] This embodiment relates to a sample pretreatment method of Fe-ZSM-5 zeolite molecular sieve Fenton method with different proportions, and the method includes the following steps:

[0040] The synthetic method of step 1.Fe-ZSM-5 (6%Fe content) zeolite molecular sieve: with Na 2 SiO 3 9H 2 O is the silicon source, tetrapropylene ammonium bromide (TPABr) is the template, Fe 2 (SO 4 ) 3 9H 2 O is an iron source. Fe 2 (SO 4 ) 3 9H 2 O stirred and dissolved in H 2 SO 4 solution, and then slowly dropwise added the pre-dissolved Na 2 SiO 3 9H 2 O solution, after fully stirring, add tetrapropenyl ammonium bromide (TPABr) in a metered ratio, and fully stir evenly. The molar ratio of the final precursor is: 30Na 2 O:5Fe 2 o 3 :30SiO2 2 :1040H 2 O:TPABr:25H 2 SO 4 . The resulting precursor gel was sealed and reacted at 180°C for 96h, cooled to room temperature, filtered, washed until the pH of the filtrate was 7, and dried at 1°C·min -1 The temperature was p...

Embodiment 3

[0046] This embodiment relates to a sample pretreatment method of Fe-ZSM-5 zeolite molecular sieve Fenton method with different proportions, and the method includes the following steps:

[0047] The synthetic method of step one.Fe-ZSM-5 (10%Fe content) zeolite molecular sieve: with Na 2 SiO 3 9H 2 O is the silicon source, tetrapropylene ammonium bromide (TPABr) is the template, Fe 2 (SO 4 ) 3 9H 2 O is an iron source. Fe 2 (SO 4 ) 3 9H 2 O stirred and dissolved in H 2 SO 4 solution, and then slowly dropwise added the pre-dissolved Na 2 SiO 3 9H 2 O solution, after fully stirring, add tetrapropenyl ammonium bromide (TPABr) in a metered ratio, and fully stir evenly. The molar ratio of the final precursor is: 60Na 2 O:25Fe 2 o 3 :60SiO2 2 :2080H 2 O:2TPABr:50H 2 SO 4 . The resulting precursor gel was sealed and reacted at 180°C for 96h, cooled to room temperature, filtered, washed until the pH of the filtrate was 7, and dried at 1°C·min -1 The temperature ...

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Abstract

The invention discloses a Fenton-method sample pretreatment method for metal-heteroatom zeolite molecular sieves. The method comprises the steps of synthesizing metal-heteroatom ZSM-5 zeolite molecular sieves; adding the metal-heteroatom ZSM-5 zeolite molecular sieves into centrifugal tubes, and adding a biological sample solution and a H2O2 solution; transferring the centrifugal tubes into a thermostatic waterbath, inserting ultrasonic reactor probes to the certain depth below a liquid surface, and stopping after reacting for certain time; taking out the centrifugal tubes, centrifuging, transferring and taking supernate, and waiting to be tested; according to maximum absorbencies which are measured by an ultraviolet visible spectrophotometer before and after the protein reaction, combining a gel electrophoresis technology and Image-Lab software to perform quantitative analysis and measurement. By the aid of the method, complex actual samples, such as blood and protein solutions, are decomposed in advance in an efficient, fast, pollution-free and simple mode, so that requirements of fields such as subsequent instrumental analysis and testing can be met.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and relates to a sample pretreatment method of metal heteroatom zeolite molecular sieve Fenton method. Background technique [0002] Actual biological samples (such as whole blood, dairy products, etc.) have a complex background composition and a high proportion of organic matter such as protein, which cannot directly meet the testing needs of analytical instruments such as atomic spectroscopy, and effective sample pretreatment is necessary. The traditional wet digestion sample pretreatment technology consumes a large amount of strong corrosive acid and alkali reagents in the process, which may affect the health of experimental operators and does not conform to the modern "green laboratory" concept. [0003] Using the Fenton reaction to decompose organic matter has the advantages of high efficiency, the reaction is carried out at room temperature, the operation is safe, and the reage...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 徐芳王晶莹张闻中曾曾王德举
Owner SHANGHAI JIAOTONG UNIV