CN103801275A - Preparation method of palladium coating solid-phase micro-extraction fiber - Google Patents
Preparation method of palladium coating solid-phase micro-extraction fiber Download PDFInfo
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- CN103801275A CN103801275A CN201410083682.7A CN201410083682A CN103801275A CN 103801275 A CN103801275 A CN 103801275A CN 201410083682 A CN201410083682 A CN 201410083682A CN 103801275 A CN103801275 A CN 103801275A
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Abstract
The invention discloses a preparation method of a palladium coating solid-phase micro-extraction fiber on a metal wire carrier, and in particular relates to a technology for modifying a palladium coating with a micron structure on a metal wire by using a replacement reaction. The new method is characterized in that a stainless steel wire or iron wire is selected as a carrier, one end the carrier is arranged in a palladium chloride hydrochloric acid solution, and by using the replacement reaction, the palladium coating with the micron structure is prepared on the surface of the metal wire. The solid-phase micro-extraction fiber prepared according to the invention has high mechanical strength, high thermal stability and chemical stability of the coating, excellent extraction performance and the like, can be used for the analysis and detection of hydrophobic targets with trace high boiling point in samples of food, environment and the like, and has preferable utilization potentiality.
Description
Technical field
The present invention relates to a kind of technology of utilizing wire carrier to prepare palladium coating solid phase micro-extraction fiber, belong to the technology of preparing of the core component solid-phase micro-extraction fibre in SPME field.
Background technology
SPME is the novel Sample Pretreatment Technique of one that development in recent years is got up, this technology centralized procurement sample, enrichment, extraction, sample introduction are in one, have that cost is low, analysis speed is fast, easy and simple to handle, analysis efficiency is high and be convenient to the advantage such as field assay and Instrument crosslinking, be widely used in the extractive analysis of trace object in food, environment, medicine and the sample such as biochemical.The core component of this technology is solid-phase micro-extraction fibre, and the development of high-performance solid-phase micro-extraction fibre is the forward position of solid phase micro-extraction technique development always.Solid-phase micro-extraction fibre is made up of carrier and extraction coating two parts, vitreous silica rod is the initial common carrier of solid-phase micro-extraction fibre, the shortcoming that has bad mechanical property very easily ruptures in operating process, causes service life of extracting fiber short and brought inconvenience for operating personnel.In order to improve the mechanical strength of solid-phase micro-extraction fibre, people start to prepare the solid-phase micro-extraction fibre of wire as carrier, have improved the convenience in mechanical strength and the use procedure of extracting fiber.
Aspect extraction coating, various types of materials is used to prepare solid-phase micro-extraction coating as organic polymer, inorganic nano material etc., some metals like gold, silver etc. are also used to extract coating, for organo-phobicity analyte extraction ability excellence, and show good heat endurance and chemical stability.The coating of Metal Palladium is modified at the metal substrate surface such as stainless steel, titanium can improve its acid and alkali resistance greatly, and the metal coating of micron, nanostructured is beneficial to the surface nature that obtains strong-hydrophobicity, can form stronger hydrophobic interaction with hydrophobic compound.Using wire as carrier, utilize displacement reaction, prepare the palladium coating solid phase micro-extraction fiber of micrometer structure, there is good heat endurance and chemical stability, with gas-chromatography coupling effectively enrichment analyze high boiling hydrophobic organic compound, as the environmental contaminants such as polycyclic aromatic hydrocarbon, plasticiser.
Summary of the invention
The object of the present invention is to provide a kind of technology of preparing palladium coating solid phase micro-extraction fiber in wire carrier.The present invention is based on displacement reaction and in wire carrier, generate palladium coating, obtain palladium coating solid phase micro-extraction fiber, preparation process is specific as follows:
Wire one end is placed in to palladium solution and reacts certain hour, form palladium coating in wire surface.
The wire adopting in the present invention is stainless steel wire, the iron wire of diameter 0.1-0.3 mm.
The hydrochloric acid solution that the palladium solution adopting in the present invention is palladium bichloride, palladium bichloride concentration is 0.5-3.0 g/L, concentration of hydrochloric acid is 0.05-3.0 mol/L.
In the present invention, wire one end being placed in to the palladium solution reaction time is 20-150 min, and reaction temperature is 0-50 ℃.
In the present invention, be 1-10 μ m at the thickness of wire surface formation palladium coating.
The prepared palladium coat metal wire solid-phase micro-extraction fibre of the present invention has the following advantages:
(1) wire can effectively improve the easily broken shortcoming of quartz fibre carrier as carrier, has improved the convenience in mechanical strength and the use procedure of extracting fiber.
(2) select palladium coating to obtain resistant to elevated temperatures solid-phase micro-extraction fibre, be beneficial to the enrichment analysis of higher boiling target analytes.
(3) select palladium coating to obtain the solid-phase micro-extraction fibre of high chemical stability, the life-span of greatly having improved extracting fiber.
(4) utilize displacement reaction to prepare the palladium coating solid phase micro-extraction fiber of micrometer structure in wire surface, preparation method is simple.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of palladium coating stainless steel wire solid-phase micro-extraction fibre.
The specific embodiment
In order to understand better the present invention, describe by example:
embodiment 1: the preparation of palladium coating stainless steel wire solid-phase micro-extraction fibre
Stainless steel wire one end 5 cm that are 0.15 mm by diameter are placed in the hydrochloric acid solution that concentration is the palladium bichloride of 0.5 g/L, concentration of hydrochloric acid is 0.1 mol/L, 25 ℃ of reaction 60 min, after taking out, water rinses the palladium coating generating, and obtains palladium coating stainless steel wire solid-phase micro-extraction fibre.
embodiment 2: the preparation of palladium coating stainless steel wire solid-phase micro-extraction fibre
Stainless steel wire one end 5 cm that are 0.25 mm by diameter are placed in the hydrochloric acid solution that concentration is the palladium bichloride of 1.0 g/L, concentration of hydrochloric acid is 0.5 mol/L, 20 ℃ of reaction 80 min, after taking out, water rinses the palladium coating generating, and obtains palladium coating stainless steel wire solid-phase micro-extraction fibre.
embodiment 3: the preparation of palladium coating stainless steel wire solid-phase micro-extraction fibre
Stainless steel wire one end 5 cm that are 0.18 mm by diameter are placed in the hydrochloric acid solution that concentration is the palladium bichloride of 1.5 g/L, concentration of hydrochloric acid is 0.2 mol/L, 25 ℃ of reaction 40 min, after taking out, water rinses the palladium coating generating, and obtains palladium coating stainless steel wire solid-phase micro-extraction fibre (scanning electron microscope (SEM) photograph as shown in Figure 1).
embodiment 4: the preparation of palladium coating iron wire solid-phase micro-extraction fibre
Iron wire one end 5 cm that are 0.2 mm by diameter are placed in the hydrochloric acid solution that concentration is the palladium bichloride of 1.0 g/L, and concentration of hydrochloric acid is 0.5 mol/L, 35 ℃ of reaction 30 min, and after taking out, water rinses the palladium coating generating, and obtains palladium coating iron wire solid-phase micro-extraction fibre.
embodiment 5: the preparation of palladium coating iron wire solid-phase micro-extraction fibre
Iron wire one end 5 cm that are 0.25 mm by diameter are placed in the hydrochloric acid solution that concentration is the palladium bichloride of 2.0 g/L, concentration of hydrochloric acid is 0.2 mol/L, 20 ℃ of reaction 30 min, after taking out, water rinses the palladium coating generating, and obtains palladium coating iron wire solid-phase micro-extraction fibre.
Claims (4)
1. a preparation method for palladium coating solid phase micro-extraction fiber, is characterized in that wire one end is placed in to palladium solution reacts certain hour, forms palladium coating in wire surface.
2. the method for claim 1, is characterized in that wire is stainless steel wire, the iron wire of diameter 0.1-0.3 mm.
3. the method for claim 1, is characterized in that palladium solution is the hydrochloric acid solution of palladium bichloride, and palladium bichloride concentration is 0.5-3.0 g/L, and concentration of hydrochloric acid is 0.05-3.0 mol/L.
4. the method for claim 1, is characterized in that it is 20-150 min that wire one end is placed in to the palladium solution reaction time, and reaction temperature is 0-50 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410083682.7A CN103801275A (en) | 2014-03-10 | 2014-03-10 | Preparation method of palladium coating solid-phase micro-extraction fiber |
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| CN201410083682.7A CN103801275A (en) | 2014-03-10 | 2014-03-10 | Preparation method of palladium coating solid-phase micro-extraction fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109289816A (en) * | 2018-10-29 | 2019-02-01 | 湖北文理学院 | A kind of sulfhydryl modified spiral mixing rod and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10286561A (en) * | 1997-04-17 | 1998-10-27 | Kawasaki Steel Corp | Method for separation and analysis of silicon and phosphorus |
| CN101385972A (en) * | 2008-10-31 | 2009-03-18 | 华东师范大学 | Metal micro-fiber loaded silver catalyst and use thereof |
| CN101648137A (en) * | 2009-09-18 | 2010-02-17 | 华东师范大学 | Metal carrier load gold catalyst and application thereof in preparing aldehyde or ketone by selectively oxidizing catalytic alcohol |
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2014
- 2014-03-10 CN CN201410083682.7A patent/CN103801275A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10286561A (en) * | 1997-04-17 | 1998-10-27 | Kawasaki Steel Corp | Method for separation and analysis of silicon and phosphorus |
| CN101385972A (en) * | 2008-10-31 | 2009-03-18 | 华东师范大学 | Metal micro-fiber loaded silver catalyst and use thereof |
| CN101648137A (en) * | 2009-09-18 | 2010-02-17 | 华东师范大学 | Metal carrier load gold catalyst and application thereof in preparing aldehyde or ketone by selectively oxidizing catalytic alcohol |
Non-Patent Citations (4)
| Title |
|---|
| JIAHENG HE ET AL: ""Adsorption of 125I on palladium coated silver wire"", 《 JOURNAL OF RADIOANALYTICAL AND NUCLEAR CHEMISTRY》 * |
| JUANJUAN FENG ET AL: ""Au nanoparticles as a novel coating for solid-phase microextraction"", 《 JOURNAL OF CHROMATOGRAPHY A》 * |
| VANESA ROMERO ET AL: ""Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry"", 《SPECTROCHIMICA ACTA PART B》 * |
| 刘海霞等: "一种新型固相微萃取金属涂层的制备及其分析应用研究", 《甘肃省化学会第二十八届年会暨第十届中学化学教学经验交流会论文集》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109289816A (en) * | 2018-10-29 | 2019-02-01 | 湖北文理学院 | A kind of sulfhydryl modified spiral mixing rod and its preparation method and application |
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Application publication date: 20140521 |