CN104451620A - Method for preparing silver plating PEEK tube for in-tube solid phase microextraction - Google Patents
Method for preparing silver plating PEEK tube for in-tube solid phase microextraction Download PDFInfo
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- CN104451620A CN104451620A CN201410604925.7A CN201410604925A CN104451620A CN 104451620 A CN104451620 A CN 104451620A CN 201410604925 A CN201410604925 A CN 201410604925A CN 104451620 A CN104451620 A CN 104451620A
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Abstract
The invention discloses a method for preparing a silver plating PEEK tube for in-tube solid phase microextraction, and in particular relates to modification of a silver plating layer with a micrometer structure to the inner wall of the PEEK tube by utilizing chemical silver plating reaction. The new method is characterized in that the PEEK tube which is low in cost, easily available and high in mechanical strength and is conveniently connected with a high performance liquid chromatograph is used as a carrier, the silver plating layer serving as an extraction coating is prepared on the inner wall of the PEEK tube by utilizing a chemical plating method having the advantages of compactness, uniform thickness, high stability and the like of the plating layer. An in-tube solid phase microextraction coating material prepared by the method has the advantages of high selectivity, stable extraction performance, strong enrichment capacity, long service life, simplicity and convenience in preparation method, low cost and the like, can be used for performing on-line enrichment analysis on trace target analytes in samples such as food, environment, medicines, biochemistry and the like under the combination of a liquid chromatogram process, and is high in utilization potentiality.
Description
Technical field
The present invention relates to a kind of on PEEK inside pipe wall chemical silvering prepare the technology of In-tube SPME coating.
Background technology
Solid-phase microextraction comes across nineteen nineties, it is a kind of novel Sample Pretreatment Technique, because it is with low cost, accumulation ability is strong, analysis speed is fast, easy and simple to handle and be convenient to the advantage such as on-the site analysis and Instrument crosslinking, be widely used in the enrichment analysis of trace components in the samples such as food, environment, medicine and biochemistry.Solid-phase microextraction material is divided into solid-phase micro-extraction fibre and the large class of In-tube SPME pipe two according to its form, normal and the gas-chromatography coupling of solid-phase micro-extraction fibre, although highly sensitive detection can be realized, but find that off-line operation exists larger personal errors in actual applications, the bad control of desorption process, also can be not thorough because of each desorption, causes memory effect, Interference Detection, and be difficult to the detection meeting thermolability and difficult volatility target analytes.Solid-phase micro-extraction fibre and liquid chromatography coupling can analyze thermolability and difficult volatility target analytes, but need expensive special purpose interface, and are difficult to realize on-line coupling.In-tube SPME easily and liquid chromatography coupling realize on-line preconcentration analysis, overcome above-mentioned shortcoming, make the extraction of sample, desorb, sample introduction realize automatization, substantially increase efficiency, reduce experimental error, improve analysis circulation ratio.In-tube SPME commonly uses the quartz capillary that inwall modifies extraction coating, and because quartz capillary bad mechanical strength causes its work-ing life short, in extraction process and elution process, withstand voltage properties is poor, greatly limit the development of In-tube SPME.
PEEK pipe is that one has high temperature resistant, high performance thermoplastic special engineering plastic pipe, commonly use now it as liquid chromatography pipeline, because it is easily connected with liquid chromatography, high pressure resistant, antifatigue, chemical stability are good, and be easy to cutting, make PEEK pipe be a kind of good In-tube SPME carrier.But himself is almost without extracting power, and chemically stable smooth inner wall is difficult to utilize common extraction coated material to carry out chemically modified.Therefore, the application of PEEK pipe in In-tube SPME is restricted.The current relative maturity of electroless plating technology, covering power or covering power all show well, and to shape relative complex, the relatively strict carrier to be plated of dimensional requirement all can be suitable for.Have plated layer compact, thickness evenly, the plurality of advantages such as good stability.Utilize the method for chemical silvering uniformly the silver of micrometer structure firmly can be deposited on capillary tube inner wall.The chemical stability of silver is good, and have optionally absorption property, especially the silver coating of micrometer structure shows stronger hydrophobicity, optionally can adsorb apolar substance.Utilize this chemical property, the extraction to nonpolar pollutent can be applied to.Prepare silvering as extraction coated material by means of chemical silvering technology at PEEK inside pipe wall, obtain silver-plated PEEK pipe for In-tube SPME, realize the on-line preconcentration analysis of the nonpolar pollutents such as polycyclic aromatic hydrocarbons with liquid chromatography coupling.
Summary of the invention
The object of the present invention is to provide the technology of preparing of a kind of silver-plated PEEK pipe of In-tube SPME.The present invention is based on electroless plating technology, use PEEK pipe as carrier, the silvering of densification is deposited on PEEK pipe internal surface, obtain solid-phase microextraction pipe, preparation process is specific as follows:
Get the PEEK pipe of suitable length and internal diameter, use dilute hydrochloric acid, water, washed with methanol to remove the impurity of internal surface successively, inject chemical silvering reaction soln, silver plating reaction solution is mixed by silver ammino solution and potassium sodium tartrate solution, react complete, use water, washed with methanol successively, after nitrogen dries up, heat aging, repeats chemical silvering process to obtain the silvering of suitable thickness.
The present invention exists
oneplanting in the preparation of In-tube SPME with silver-plated PEEK pipe adopts the length of PEEK pipe to be 20-60 centimetre, and internal diameter is 0.1-0.5 millimeter.
The present invention exists
oneplanting in the preparation of In-tube SPME with silver-plated PEEK pipe adopts the mol ratio of silver-colored ammonium ion and Seignette salt in chemical silvering reaction soln to be 1:1-3, the mass percentage of Seignette salt is 10-20 %, the rise time of silvering is 3-10 hour, and temperature of reaction is 5-35 DEG C.
The present invention exists
oneplant the stability adopting aging raising silvering in the preparation of In-tube SPME with silver-plated PEEK pipe, aging temperature is 50-100 DEG C, and digestion time is 0.5-5 hour, and weathering process is carried out under nitrogen protection.
The present invention exists
oneplant in the preparation of In-tube SPME with silver-plated PEEK pipe and adopt chemical silvering number of times in PEEK pipe to be 1-5 time, obtain the silvering of suitable thickness.
The present invention exists
oneplant In-tube SPME silver coating in the preparation of silver-plated PEEK pipe as extraction coating, PEEK pipe has the following advantages as the solid-phase microextraction material of carrier:
(1) PEEK pipe is as carrier, can bear higher pressure, and be conveniently connected with high performance liquid chromatograph, low price, reduces experimental cost.
(2) silvering of micrometer structure can the extraction hydrophobicity target analytes of highly selective as extraction coating.
(3) preparation method is easy, with low cost, preparation circulation ratio is high.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of silver-plated PEEK pipe.
Embodiment
In order to understand the present invention better, be described by example:
embodiment 1: the preparation of the silver-plated PEEK pipe of 20 cm long 0.1 millimeter internal diameter
To get length be 20 centimetres and internal diameter is the PEEK pipe of 0.1 millimeter, use dilute hydrochloric acid successively, water, washed with methanol is to remove the impurity of internal surface, inject the chemical silvering reaction soln mixed by silver ammino solution and potassium sodium tartrate solution, the mol ratio of silver ammonium ion and Seignette salt is 1:1, the mass percentage of Seignette salt is 20 %, controlling temperature of reaction is 20 DEG C, react after 3 hours, use water successively, washed with methanol, after nitrogen dries up, 50 DEG C of heat agings 0.5 hour in nitrogen protection environment, chemical silvering number of times is 1 time, obtain the silvering of suitable thickness.The scanning electron microscope (SEM) photograph of the silvering of preparation as shown in Figure 1.
embodiment 2: the preparation of the silver-plated PEEK pipe of 30 cm long 0.18 millimeter internal diameter
To get length be 30 centimetres and internal diameter is the PEEK pipe of 0.18 millimeter, use dilute hydrochloric acid successively, water, washed with methanol is to remove the impurity of internal surface, inject the chemical silvering reaction soln mixed by silver ammino solution and potassium sodium tartrate solution, the mol ratio of silver ammonium ion and Seignette salt is 1:2, the mass percentage of Seignette salt is 15 %, controlling temperature of reaction is 25 DEG C, react after 6 hours, use water successively, washed with methanol, after nitrogen dries up, 70 DEG C of heat agings 2.5 hours in nitrogen protection environment, chemical silvering number of times is 2 times, obtain the silvering of suitable thickness.
embodiment 3: the preparation of the silver-plated PEEK pipe of 50 cm long 0.25 millimeter internal diameter
To get length be 50 centimetres and internal diameter is the PEEK pipe of 0.25 millimeter, use dilute hydrochloric acid successively, water, washed with methanol is to remove the impurity of internal surface, inject the chemical silvering reaction soln mixed by silver ammino solution and potassium sodium tartrate solution, the mol ratio of silver ammonium ion and Seignette salt is 1:1.8, the mass percentage of Seignette salt is 10 %, controlling temperature of reaction is 30 DEG C, react after 9 hours, use water successively, washed with methanol, after nitrogen dries up, 80 DEG C of heat agings 4 hours in nitrogen protection environment, chemical silvering number of times is 4 times, obtain the silvering of suitable thickness.
Claims (5)
1. the In-tube SPME preparation method of silver-plated PEEK pipe, it is characterized in that the PEEK pipe getting suitable length and internal diameter, use dilute hydrochloric acid, water, washed with methanol to remove the impurity of internal surface successively, inject chemical silvering reaction soln, silver plating reaction solution is mixed by silver ammino solution and potassium sodium tartrate solution, reacts complete, use water, washed with methanol successively, after nitrogen dries up, heat aging, repeats chemical silvering process to obtain the silvering of suitable thickness.
2. the method for claim 1, it is characterized in that the length of PEEK pipe is 20-60 centimetre, internal diameter is 0.1-0.5 millimeter.
3. the method for claim 1, it is characterized in that the mol ratio of silver-colored ammonium ion and Seignette salt in chemical silvering reaction soln is 1:1-3, the mass percentage of Seignette salt is 10-20 %, and the rise time of silvering is 3-10 hour, and temperature of reaction is 5-35 DEG C.
4. the method for claim 1, is characterized in that the stability of aging raising silvering, and aging temperature is 50-100 DEG C, and digestion time is 0.5-5 hour, and weathering process is carried out under nitrogen protection.
5. the method for claim 1, is characterized in that in PEEK pipe, chemical silvering number of times is 1-5 time, obtains the silvering of suitable thickness.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410604925.7A CN104451620A (en) | 2014-11-03 | 2014-11-03 | Method for preparing silver plating PEEK tube for in-tube solid phase microextraction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410604925.7A CN104451620A (en) | 2014-11-03 | 2014-11-03 | Method for preparing silver plating PEEK tube for in-tube solid phase microextraction |
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| CN104451620A true CN104451620A (en) | 2015-03-25 |
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| CN201410604925.7A Pending CN104451620A (en) | 2014-11-03 | 2014-11-03 | Method for preparing silver plating PEEK tube for in-tube solid phase microextraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126727A (en) * | 2017-07-11 | 2017-09-05 | 福州大学 | A kind of nano grain of silver immobilization SPME integral post |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2563590Y (en) * | 2002-09-03 | 2003-07-30 | 周桂耀 | Horizontal rotary type silver/silver iodide hollow optic fibre coating device |
| WO2004047981A1 (en) * | 2002-11-25 | 2004-06-10 | Varian, Inc. | Irregularly-shaped macroporous copolymer particles and methods of using same |
| CN101041897A (en) * | 2007-04-29 | 2007-09-26 | 南京工业大学 | Chemical plating method for tubular porous material loaded metal film |
-
2014
- 2014-11-03 CN CN201410604925.7A patent/CN104451620A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2563590Y (en) * | 2002-09-03 | 2003-07-30 | 周桂耀 | Horizontal rotary type silver/silver iodide hollow optic fibre coating device |
| WO2004047981A1 (en) * | 2002-11-25 | 2004-06-10 | Varian, Inc. | Irregularly-shaped macroporous copolymer particles and methods of using same |
| CN101041897A (en) * | 2007-04-29 | 2007-09-26 | 南京工业大学 | Chemical plating method for tubular porous material loaded metal film |
Non-Patent Citations (2)
| Title |
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| WENPENG ZHANG ET.AL.: "Mussel inspired polydopamine functionalized poly(ether ether ketone) tube for online solid-phase microextraction–high performance liquid chromatography and its application in analysis of protoberberine alkaloids in rat plasma", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 武汉大学主编: "《分析化学.下册（第五版）》", 31 December 2007, 高等教育出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107126727A (en) * | 2017-07-11 | 2017-09-05 | 福州大学 | A kind of nano grain of silver immobilization SPME integral post |
| CN107126727B (en) * | 2017-07-11 | 2023-02-21 | 福州大学 | Silver nanoparticle immobilized solid-phase microextraction monolithic column |
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Application publication date: 20150325 |