CN1762527A - Novel solid phase micro extraction head and its preparation method - Google Patents
Novel solid phase micro extraction head and its preparation method Download PDFInfo
- Publication number
- CN1762527A CN1762527A CN200510094423.5A CN200510094423A CN1762527A CN 1762527 A CN1762527 A CN 1762527A CN 200510094423 A CN200510094423 A CN 200510094423A CN 1762527 A CN1762527 A CN 1762527A
- Authority
- CN
- China
- Prior art keywords
- solid phase
- phase micro
- extraction head
- novel solid
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002470 solid-phase micro-extraction Methods 0.000 title claims description 29
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920000767 polyaniline Polymers 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002347 injection Methods 0.000 claims abstract description 10
- 239000007924 injection Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 7
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 3
- 239000002184 metal Substances 0.000 abstract 3
- 238000004853 microextraction Methods 0.000 abstract 3
- 239000007787 solid Substances 0.000 abstract 2
- 239000012153 distilled water Substances 0.000 abstract 1
- 238000002848 electrochemical method Methods 0.000 abstract 1
- 238000007689 inspection Methods 0.000 abstract 1
- 238000012806 monitoring device Methods 0.000 abstract 1
- 238000012544 monitoring process Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000004817 gas chromatography Methods 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 239000006200 vaporizer Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VQXSOUPNOZTNAI-UHFFFAOYSA-N Pyrethrin I Natural products CC(=CC1CC1C(=O)OC2CC(=O)C(=C2C)CC=C/C=C)C VQXSOUPNOZTNAI-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000005181 nitrobenzenes Chemical class 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000003993 organochlorine pesticide Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- HYJYGLGUBUDSLJ-UHFFFAOYSA-N pyrethrin Natural products CCC(=O)OC1CC(=C)C2CC3OC3(C)C2C2OC(=O)C(=C)C12 HYJYGLGUBUDSLJ-UHFFFAOYSA-N 0.000 description 2
- VJFUPGQZSXIULQ-XIGJTORUSA-N pyrethrin II Chemical compound CC1(C)[C@H](/C=C(\C)C(=O)OC)[C@H]1C(=O)O[C@@H]1C(C)=C(C\C=C/C=C)C(=O)C1 VJFUPGQZSXIULQ-XIGJTORUSA-N 0.000 description 2
- IZUKQUVSCNEFMJ-UHFFFAOYSA-N 1,2-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1[N+]([O-])=O IZUKQUVSCNEFMJ-UHFFFAOYSA-N 0.000 description 1
- WDCYWAQPCXBPJA-UHFFFAOYSA-N 1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1 WDCYWAQPCXBPJA-UHFFFAOYSA-N 0.000 description 1
- FYFDQJRXFWGIBS-UHFFFAOYSA-N 1,4-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=C([N+]([O-])=O)C=C1 FYFDQJRXFWGIBS-UHFFFAOYSA-N 0.000 description 1
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000001448 anilines Chemical class 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 238000005844 autocatalytic reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
A new solid micro-extraction bulk and its preparing method, belonging to the technique field of environmental monitoring device. Inserting the metal wire into the injection device to make it become simple solid micro-extraction bulk; employing the front end of the metal wire as working electrode, combining with the platinum sheet electrode and saturated calomel reference electrode to form a three electrode system; putting it to the acid solution containing amino-benzene; forming the polyaniline coating stick to the surface of the front end of the metal wire by using electrochemical method; washing with second distilled water and methanol solution, and getting the new micro-extraction bulk. The product possesses good extracting selectivity for the trace organic pollutant of polar, non-polar, volatile and involatile. The product possesses good physical and chemical stability and long durability comparing with the commercial coating. The extraction bulk is suit for the analysis of various organic substance in the complex example, and good application potential in the field of environmental monitoring, food safety, checking and quarantine inspection, and etc.
Description
One, technical field
The present invention relates to a kind of solid phase micro-extracting head that is applied to multiple environmental pollutant analysis and preparation method thereof.
Two, background technology
SPME (SPME) is the sample pretreatment technology that grows up early 1990s.It combines with various analysis to the analysis of organic matter especially volatility and semi-volatile organic matter, has obtained deep research and application widely.But the commercial SPME solid phase coating kind that is used for actual analysis at present is limited, and be to rely on physisorption to make fixingly to be coated with stain mutually mostly on frangible quartz fibre surface, thereby heat endurance relatively poor (200～280 ℃ of serviceability temperatures), lack (generally being about 40～100 times) service life, and cost an arm and a leg, directly limited the range of application of SPME method.Therefore developing high selectivity, high power capacity, solid phase coating material efficient, Heat stability is good is the important directions of SPME method research.
Polyaniline is as a kind of the most common conducting polymer, and is ripe day by day in the research of electrochemical field, but that the application in environmental protection only limits to is antifouling, aspects such as anticorrosion and sensor, and other application are actually rare.This seminar finds that then the special construction of polyaniline determines it will become a kind of adsorbent of function admirable.In conjunction with its electrochemical properties, used as SPME (SPME) adsorbent, and SPME (SPME) device carried out simple reformation, successful analysis phthalate, nitrobenzene, n-alkane, organo-chlorine pesticide, pyrethrin pesticide and some other volatility phenyl amines and phenolic comp ' ds pollution.
Mentioned the preparation of novel solid phase micro extraction head polyaniline coating in State Intellectual Property Office of the People's Republic of China's invention disclosed patent " preparation of SPME novel extraction head polyaniline coating " (publication number is CN 1417580A).Preparation technology is simple for this method, and gained coating effect of extracting is better.But the material (as alkohol and amine) that this patent is only mentioned polarity has effect of extracting, so since its range of application be subjected to bigger restriction.
Three, summary of the invention
1. goal of the invention: the purpose of this invention is to provide a kind of novel solid phase micro extraction head that can be widely used in various organic pollutant analysis in the environment and preparation method thereof.
2. technical scheme:
Technical scheme of the present invention is:
A kind of preparation method of novel solid phase micro extraction head, it may further comprise the steps:
(1) wire is inserted in the injection device, make it form simple and easy solid-phase micro-extracting device;
(2) make the work electrode with front end of wire, to electrode, saturated calomel reference electrode is formed three-electrode system, puts into the acid solution that contains aniline in conjunction with platinized platinum;
(3) adopt potential sweep method, potentiostatic method, galvanostatic method or impulse polarization method to form the polyaniline coating that adheres to the front end of wire surface;
(4) with redistilled water and methanol solution washing, promptly make novel solid phase micro extraction head.
Wire in the step of the present invention (1) is convenient to later sampling and is got final product as long as hardness can satisfy in the insertion injection device, uses diameter: 0.1～0.5mm usually, length: the wire of 0.5～1.5cm, commonly used is stainless steel wire, low price and be easy to obtain.Acid solution in the step (2) does not have specific (special) requirements, no matter weak acid strong acid all can, only otherwise the work that influences electrode system gets final product, preferably adopt sulfuric acid solution, hydrochloric acid solution or phosphoric acid solution, the pH value is less than 4.All effect preferably can be arranged when the concentration of aniline is 0.1～0.5 mol, according to test, the concentration of suggestion aniline is 0.2 mol.
Can adopt in the step (3) potential sweep method, potentiostatic method, galvanostatic method or impulse polarization method all can, commonly used is potential sweep method and galvanostatic method.When adopting potential sweep method in the step (3), condition of work is :-0.2～1.0V, 25～35mVs
-1When adopting galvanostatic method in the step (3), condition of work is: current density is 0.2～10.0mA/cm
2
Of the present inventionly also provide a kind of novel solid phase micro extraction head, comprise injection device and wire, there is polyaniline coating on the front end of wire surface.
This novel solid phase micro extraction head is prepared from according to above-described method.
This solid phase micro-extracting head is first use before in the gas-chromatography vaporizer 200～280 ℃, the aging 2～3h that heats up occurs up to the free from admixture peak.
Principle of the present invention: according to aniline " autocatalysis ", adopt electrochemical process, with the polyaniline electropolymerization on wire, to form polyaniline coating.
3. beneficial effect: characteristics of the present invention are that polyaniline is that direct electropolymerization is on wire, in the process of electropolymerization, between the organic and inorganic phase (being solid phase coating and wire surface) is to pass through chemical bonding, so than commercial quartz fibre post higher physical stability is arranged, and has very strong heat endurance, anti-organic solvent, big adsorption capacity and extraction equilibrium ability fast.As long as suitable operation, hundreds of times repeated use and long the placement can not change its effect of extracting.Aspect pollutant analysis, no matter be polarity, nonpolar, volatility and all available polyaniline of difficult volatile organic pollution are analyzed, and this has broken the restriction of the conventional similar principle that mixes.The present invention is simple in structure, be easy to make, and has a extensive future.
Four, Figure of description
Structural representation when Fig. 1 uses for a kind of novel solid phase micro extraction head of the present invention;
Fig. 2 is solid phase micro-extracting head polyaniline coating sem photograph of the present invention (A:150 a times, B:10000 doubly);
Fig. 3 is for using solid phase micro-extracting head SPME nitrobenzene compounds gas chromatogram of the present invention.
Five, embodiment
Embodiment 1
With diameter is 0.35 millimeter wire 11, inserts in the injection device 12, makes it form easy solid-phase micro-extracting device, makes the work electrode with wire one end, and to electrode, saturated calomel reference electrode is formed three-electrode system in conjunction with platinized platinum.This three-electrode system is put into 0.2M aniline+0.5M sulfuric acid solution liquid, in-0.2～1.0V scope, 25～35mV s
-1Under the condition, circulation 10～20 circles, what obtain black adheres to electrode surface polyaniline coating 13.Use redistilled water and methanol solution Washing 1～2 minute at last, promptly make the polyaniline coating extracting head.This solid phase micro-extracting head is first use before in the gas-chromatography vaporizer 200～280 ℃, the aging 2～3h that heats up occurs up to the free from admixture peak.
With diameter is 0.25 millimeter wire 11, inserts in the injection device 12, makes it form easy solid-phase micro-extracting device, makes the work electrode with wire one end, and to electrode, saturated calomel reference electrode is formed three-electrode system in conjunction with platinized platinum.This three-electrode system is put into 0.2M aniline+0.5M hydrochloric acid solution, under the 0.6V condition, oxidation 10 minutes, what obtain black adheres to electrode surface polyaniline coating 13.Use redistilled water and methanol solution Washing 1～2 minute at last, promptly make the polyaniline coating extracting head.This solid phase micro-extracting head is first use before in the gas-chromatography vaporizer 200～280 ℃, the aging 2～3h that heats up occurs up to the free from admixture peak.
Embodiment 3
With diameter is 0.45 millimeter wire, inserts in the injection device, makes it form easy solid-phase micro-extracting device, makes the work electrode with wire one end, and to electrode, saturated calomel reference electrode is formed three-electrode system in conjunction with platinized platinum.This three-electrode system is put into 0.3M aniline+0.5M sulfuric acid solution liquid, and specimen current density is 0.2～10.0mA/cm when galvanostatic method
2Current density under polymerization, what obtain black adheres to the electrode surface polyaniline coating.Use redistilled water and methanol solution Washing 1～2 minute at last, promptly make the polyaniline coating extracting head.This solid phase micro-extracting head is first use before in the gas-chromatography vaporizer 200～280 ℃, the aging 2～3h that heats up occurs up to the free from admixture peak.
Embodiment 4:
With diameter is 0.1 millimeter wire 11, inserts in the injection device 12, makes it form easy solid-phase micro-extracting device, makes the work electrode with wire one end, and to electrode, saturated calomel reference electrode is formed three-electrode system in conjunction with platinized platinum.This three-electrode system is put into 0.1M aniline+1M hydrochloric acid solution, under the 0.6V condition, oxidation 20 minutes, what obtain black adheres to electrode surface polyaniline coating 13.Use redistilled water and methanol solution Washing 1～2 minute at last, promptly make the polyaniline coating extracting head.This solid phase micro-extracting head is first use before in the gas-chromatography vaporizer 200～280 ℃, the aging 2～3h that heats up occurs up to the free from admixture peak.
Embodiment 5:
Basic operation is with embodiment 1, be diameter wiry be 0.5 millimeter, three-electrode system is put into 0.5M aniline+0.3M phosphoric acid solution, all the other are all identical.
Embodiment 6:
Basic operation is with embodiment 4, be diameter wiry be 0.2 millimeter, three-electrode system is put into 1.0M aniline+0.5M acetic acid solution, all the other are all identical.
Embodiment 7:
With 5 kinds of phthalate compounds of polyaniline coating extraction (repefral, diethylester, two propylene esters, di-n-butyl, di-isooctyl solution, concentration are respectively 1,1,1,0.04,0.04ppm).The laggard gas-chromatography of extraction certain hour is resolved.The result shows that this extracting head has good effect of extracting.The PA extracting head of producing with Supelco company under similarity condition compares, and finds that both effect of extracting are close.
The GC/FID operating condition: HP-5 capillary quartz column (30m * 320 μ m * 0.25 μ m), heating schedule: 60 ℃ keep 2min, rise to 120 ℃ with 20 ℃/min, and 8 ℃/min rises to 180 ℃ and keep 4min, and 15 ℃/min rises to 250 ℃, keeps 12min.Injector temperature: 280 ℃, detector temperature: 300 ℃.Nitrogen: 10.26psi; Hydrogen: 40mL/min; Air: 300mL/min.
Embodiment 8:
Polyaniline coating is to the extraction of 15 kinds of organo-chlorine pesticides (concentration is 200ppt).The result shows that this head has good effect of extracting, and detectability reaches the ppt level, and reappearance is fine.
GC/ECD operating condition: DB-17 capillary quartz column (30m * 250 μ m * 0.25 μ m), heating schedule: 60 ℃ keep 0min, rise to 170 ℃ with 25 ℃/min, 4 ℃/min rises to 190 ℃, 8 ℃/min rises to 230 ℃, keeps 4min, and 1 ℃/min rises to 240 ℃, 25 ℃/min rises to 260 ℃, keeps 7min.Injector temperature: 260 ℃, detector temperature: 320 ℃.Nitrogen: 11.79psi.
Embodiment 9:
8 kinds of nitrobenzene compounds (1:20ppb nitrobenzene of polyaniline coating extraction; 2:2ppb 1,2, the 4-trichloro-benzenes; 3:1ppb 4-chloronitrobenzene; 4:0.5ppb 1,2,3, the 5-tetrachlorobenzene; 5:0.5ppb 1,2,3, the 4-tetrachlorobenzene; 6:1.5ppb p-dinitro benzene; 7:7ppb m-dinitro benzene; 8:4.5ppb the o-dinitro benzene), the gas chromatogram after the parsing (Fig. 3) shows: this coating has good selectivity, and detectability reaches the ppt level, and reappearance is fine.
The GC/ECD operating condition: DB-17 capillary quartz column (30m * 250 μ m * 0.25 μ m), heating schedule: 60 ℃ keep 0min, rise to 100 ℃ with 10 ℃/min, keep 6min, 8 ℃/min rises to 160 ℃, and 3 ℃/min rises to 200 ℃, 10 ℃/min rises to 250 ℃, keeps 2min.Injector temperature: 250 ℃, detector temperature: 300 ℃.Nitrogen: 14.33psi.
Embodiment 10:
Polyaniline coating is to the extraction of 6 kinds of pyrethrin pesticides (concentration is 5ppb).The result shows that this head has good effect of extracting, and detectability reaches the ppt level, and reappearance is fine.
The GC/ECD operating condition: DB-17 capillary quartz column (30m * 250 μ m * 0.25 μ m), heating schedule: 80 ℃ keep 0min, rise to 200 ℃ with 30 ℃/min, and 4 ℃/min rises to 260 ℃, and 0.5 ℃/min rises to 280 ℃, keep 5min.Injector temperature: 260 ℃, detector temperature: 320 ℃.Nitrogen: 12.7psi.
Claims (8)
1, a kind of preparation method of novel solid phase micro extraction head is characterized in that may further comprise the steps:
(1) wire is inserted in the injection device, make it form simple and easy solid-phase micro-extracting device;
(2) make the work electrode with front end of wire, to electrode, saturated calomel reference electrode is formed three-electrode system, puts into the acid solution that contains aniline in conjunction with platinized platinum;
(3) adopt potential sweep method, potentiostatic method, galvanostatic method or impulse polarization method to form the polyaniline coating that adheres to the front end of wire surface;
(4) with redistilled water and methanol solution washing, promptly make novel solid phase micro extraction head.
2, the preparation method of a kind of novel solid phase micro extraction head according to claim 1 is characterized in that step
(1) wire described in is a stainless steel wire.
3, the preparation method of a kind of novel solid phase micro extraction head according to claim 1 and 2 is characterized in that the acid solution in the step (2) is sulfuric acid solution, hydrochloric acid solution or phosphoric acid solution, and the pH value is less than 4.
4, the preparation method of a kind of novel solid phase micro extraction head according to claim 1 and 2 is characterized in that the concentration of aniline in the step (2) is 0.2 mol.
5, the preparation method of a kind of novel solid phase micro extraction head according to claim 1 and 2, when it is characterized in that adopting potential sweep method in the step (3), condition of work is :-0.2～1.0V, 25～35mVs
-1
6, the preparation method of a kind of novel solid phase micro extraction head according to claim 1 and 2, when it is characterized in that adopting galvanostatic method in the step (3), condition of work is: current density is 0.2～10.0mA/cm
2
7, a kind of novel solid phase micro extraction head comprises injection device and wire, it is characterized in that there is polyaniline coating on the front end of wire surface.
8, a kind of novel solid phase micro extraction head according to claim 7 is characterized in that making according to claim 1 or 2 described preparation methods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510094423.5A CN1762527A (en) | 2005-09-19 | 2005-09-19 | Novel solid phase micro extraction head and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200510094423.5A CN1762527A (en) | 2005-09-19 | 2005-09-19 | Novel solid phase micro extraction head and its preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1762527A true CN1762527A (en) | 2006-04-26 |
Family
ID=36746979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200510094423.5A Pending CN1762527A (en) | 2005-09-19 | 2005-09-19 | Novel solid phase micro extraction head and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1762527A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480540B (en) * | 2008-01-12 | 2010-12-08 | 山东蓬莱小鸭洗涤设备有限公司 | Methanol extracting machine |
| CN102728323A (en) * | 2012-07-11 | 2012-10-17 | 济南大学 | Preparation method of sliver-carbon nano-material composite coating metal wire solid-phase micro-extraction fiber |
| CN104771934A (en) * | 2014-12-31 | 2015-07-15 | 中国广州分析测试中心 | Solid phase micro-extraction apparatus |
| CN110118839A (en) * | 2019-06-03 | 2019-08-13 | 红河学院 | The GC/MS fingerprint map construction method and its application of oldenlandia diffusa |
| CN110694600A (en) * | 2019-11-12 | 2020-01-17 | 红河学院 | Solid phase micro-extraction head and preparation method and application thereof |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
| CN112316489A (en) * | 2019-08-05 | 2021-02-05 | 中国科学院微生物研究所 | Solid phase microextraction dual temperature control device and method |
-
2005
- 2005-09-19 CN CN200510094423.5A patent/CN1762527A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101480540B (en) * | 2008-01-12 | 2010-12-08 | 山东蓬莱小鸭洗涤设备有限公司 | Methanol extracting machine |
| CN102728323A (en) * | 2012-07-11 | 2012-10-17 | 济南大学 | Preparation method of sliver-carbon nano-material composite coating metal wire solid-phase micro-extraction fiber |
| CN102728323B (en) * | 2012-07-11 | 2014-03-26 | 济南大学 | Preparation method of sliver-carbon nano-material composite coating metal wire solid-phase micro-extraction fiber |
| CN104771934A (en) * | 2014-12-31 | 2015-07-15 | 中国广州分析测试中心 | Solid phase micro-extraction apparatus |
| CN110118839A (en) * | 2019-06-03 | 2019-08-13 | 红河学院 | The GC/MS fingerprint map construction method and its application of oldenlandia diffusa |
| CN110118839B (en) * | 2019-06-03 | 2022-02-18 | 红河学院 | Construction method and application of GC/MS (gas chromatography/mass spectrometry) fingerprint spectrum of oldenlandia diffusa |
| CN112316489A (en) * | 2019-08-05 | 2021-02-05 | 中国科学院微生物研究所 | Solid phase microextraction dual temperature control device and method |
| CN110694600A (en) * | 2019-11-12 | 2020-01-17 | 红河学院 | Solid phase micro-extraction head and preparation method and application thereof |
| CN110694600B (en) * | 2019-11-12 | 2022-04-15 | 红河学院 | Solid phase micro-extraction head and preparation method and application thereof |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1762527A (en) | Novel solid phase micro extraction head and its preparation method | |
| Liu et al. | A novel TiO2 nanotube array/Ti wire incorporated solid-phase microextraction fiber with high strength, efficiency and selectivity | |
| Asadollahzadeh et al. | Solid-phase microextraction of phthalate esters from aqueous media by electrochemically deposited carbon nanotube/polypyrrole composite on a stainless steel fiber | |
| El Mhammedi et al. | Electrochemical determination of para-nitrophenol at apatite-modified carbon paste electrode: Application in river water samples | |
| Govindhan et al. | Electrochemical sensor based on carbon nanotubes for the simultaneous detection of phenolic pollutants | |
| Alizadeh et al. | A novel high selective and sensitive para-nitrophenol voltammetric sensor, based on a molecularly imprinted polymer–carbon paste electrode | |
| Wang et al. | A novel fluorinated polyaniline-based solid-phase microextraction coupled with gas chromatography for quantitative determination of polychlorinated biphenyls in water samples | |
| Yang et al. | Simultaneous determination of hydroquinone and catechol using poly (p‐aminobenzoic acid) modified glassy carbon electrode | |
| Wang et al. | Determination of Hydrogen Peroxide in Rainwater by Using a Polyaniline Film and Platinum Particles Co‐Modified Carbon Fiber Microelectrode | |
| CN103543233B (en) | The assay method of short chain or medium chain chlorinated paraffin content in a kind of coating | |
| WO2013033383A2 (en) | Molecularly imprinted polymers for detection of contaminants | |
| Babaei et al. | A sensor for simultaneous determination of dopamine and morphine in biological samples using a multi-walled carbon nanotube/chitosan composite modified glassy carbon electrode | |
| Arfin et al. | Review on detection of phenol in water | |
| Cirrincione et al. | Development of an electrochemical sensor based on carbon black for the detection of cannabidiol in vegetable extracts | |
| Wang et al. | Direct electrochemical tyrosinase biosensor based on mesoporous carbon and Co3O4 nanorods for the rapid detection of phenolic pollutants | |
| Falciola et al. | Platinum‐Based and Carbon‐Based Screen Printed Electrodes for the Determination of Benzidine by Differential Pulse Voltammetry | |
| Field et al. | Robust fabrication of selective and reversible polymer coated carbon nanotube-based gas sensors | |
| Banitaba et al. | Preparation and evaluation of a novel solid-phase microextraction fiber based on poly (3, 4-ethylenedioxythiophene) for the analysis of OCPs in water | |
| Mehdinia et al. | Preparation and evaluation of thermally stable nano‐structured self‐doped polythiophene coating for analysis of phthalate ester trace levels | |
| Wang et al. | Polyaniline-based fiber for headspace solid-phase microextraction of substituted benzenes determination in aqueous samples | |
| Mehdinia et al. | Preparation and evaluation of solid-phase microextraction fiber based on nano-structured copolymer of aniline and m-amino benzoic acid coating for the analysis of fatty acids in zooplanktons | |
| Mugo et al. | Thin film composite conductive polymers chemiresistive sensor and sample holder for methanol detection in adulterated beverages | |
| Feng et al. | Facile fabrication of ionic liquid doped polycarbazole coating for the headspace solid-phase microextraction of some environmental pollutants | |
| CN101468306A (en) | Titanium-containing solid phase micro-extraction head and preparation method thereof | |
| Deussi Ngaha et al. | Aminoalcohol‐functionalization of Alkali Palm Oil Fiber and Application as Electrochemical Sensor for 2‐Nitrophenol Determination |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |