CN103185755B - Sample pretreatment device for analyzing anions in alcohol amine solution - Google Patents
Sample pretreatment device for analyzing anions in alcohol amine solution Download PDFInfo
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- CN103185755B CN103185755B CN201110446638.4A CN201110446638A CN103185755B CN 103185755 B CN103185755 B CN 103185755B CN 201110446638 A CN201110446638 A CN 201110446638A CN 103185755 B CN103185755 B CN 103185755B
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- -1 alcohol amine Chemical class 0.000 title abstract 2
- 150000001450 anions Chemical class 0.000 title abstract 2
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 41
- 239000000945 filler Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000010790 dilution Methods 0.000 claims abstract description 8
- 239000012895 dilution Substances 0.000 claims abstract description 8
- 238000002203 pretreatment Methods 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 239000000741 silica gel Substances 0.000 claims description 2
- 229910002027 silica gel Inorganic materials 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 13
- 238000005374 membrane filtration Methods 0.000 abstract description 3
- 238000007865 diluting Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 41
- 239000012488 sample solution Substances 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 6
- 239000012491 analyte Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000012898 sample dilution Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000003113 dilution method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical class OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229940006280 thiosulfate ion Drugs 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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Abstract
The invention relates to a sample pretreatment device for analyzing anions in an alcohol amine solution; the device consists of a dilution constant volume module, a solid phase extraction module and a membrane filtration module; the diluting constant volume module is composed of a sample inlet pipe and a piston, the sample inlet pipe is a cylinder with constant volume scale lines, the outer diameter of the piston is matched with the inner diameter of the sample inlet pipe and is positioned in the sample inlet pipe, and a sample inlet hole is formed in the center of the upper end of the piston; the solid phase extraction module is composed of a solid phase extraction filler and a plurality of porous sieve plates, or is composed of an integral filler without sieve plates, and is embedded in the piston; the membrane filtration module has the same area size as the solid phase extraction module and is clamped between the solid phase extraction module and the piston; the device can achieve the purpose of removing various interferents in a sample at one time, and meet the requirement of direct sample introduction of the ion chromatograph.
Description
Technical field
The present invention relates to a kind of for analyzing the sample pre-treatments device of alkanolamine solution negative ion.
Background technology
Alkanolamine solution is the desulfuration solution of a class widespread use, comprises monoethanolamine, diethanolamine, and methyldiethanolamines etc., are mainly used in the desulfurization of rock gas and refinery gas.In device operation process, can there are the rotten a series of negative ion such as formate ion, acetate ion, oxalate denominationby, cyanide ion, sulfite ion, sulfate ion, thiosulfate ion and thiocyanate ion that generate of degraded in alkanolamine solution, cause purification efficiency to decline, device pressure transient and corrosion aggravation wait harm.Therefore, purification plant need to adopt chromatography of ions to detect the negative ion in alkanolamine solution and monitor its content.But the alkanolamine solution sample gathering in commercial plant wherein often contains more chaff interference can not Direct Analysis.For example, suspended solids thing, long chain alkanes etc., can work the mischief to the serviceable life of ion chromatographic column, the precision of impact analysis result and reappearance.In addition the ionization that, high concentration hydramine also can inhibition analysis thing causes negative effect to ion chromatography.Therefore, developing efficient, easy, reliable sample-pretreating method and device is the key that improves the negative ion detection level in alkanolamine solution.At present, the pre-treatment of this type of sample mainly utilizes filter membrane, and the general sample pre-treatments device such as Solid-Phase Extraction completes processing by manual operation.If according to real needs, design a kind of integrated Special sample pretreating device and can reduce the consuming time of hydramine sample pre-treatments, improve the repeatability of sample pre-treatments and reduce manual operation and bring error.
Summary of the invention
The object of this invention is to provide a kind of integrated for analyzing the sample pre-treatments device of alkanolamine solution negative ion, the hydraulic pressure that utilizes piston apparatus to produce makes sample solution successively by three sample preparation modules, reaches the multiple chaff interference in disposable removal sample.
Of the present invention for analyzing the sample pre-treatments device of alkanolamine solution negative ion, integrally integrated dilution constant volume module, Solid-Phase Extraction module and film filter module, by one, the sample feeding pipe with constant volume scale mark and a supporting piston form described dilution constant volume module, described Solid-Phase Extraction module is embedded on described piston, and described film filter module is clipped between Solid-Phase Extraction module and piston.
By one, the sample feeding pipe with constant volume scale mark and a supporting piston form the dilution constant volume module of described sample pre-treatments device; Described sample feeding pipe and piston material can be plastics or glass; In described sample feeding pipe by Sample Dilution to assigned scale line, then by piston cap at the sample introduction mouth of pipe, downwards compression piston makes sample solution successively by Solid-Phase Extraction module and film filter module, completes pre-treatment and the sample introduction of sample solution.
The Solid-Phase Extraction module of described sample pre-treatments device is embedded on the piston of dilution constant volume module, and this Solid-Phase Extraction module is made up of polylith (as two) porous sieve plate and a certain amount of solid phase extraction filler, or is made up of the overall filler without sieve plate; Adopt solid phase extraction filler or the filler combination that can adsorb nonpolar chaff interference.
The filler of described Solid-Phase Extraction module adopts solid phase extraction filler or the filler combination that can adsorb nonpolar chaff interference, as surface bond the silica gel particle of C18 or phenyl, and/or graphitized carbon, and/or activated charcoal etc.;
The film filter module of described sample pre-treatments device is to be made up of nylon or cellulose microporosity filter membrane, and its size, with identical with Solid-Phase Extraction module, is clipped between Solid-Phase Extraction module and piston; Its aperture can regulate according to detected sample; The general 0.22-0.45 μ m that selects;
This sample pre-treatments device is the disposable articles for use that make, to avoid Solid-Phase Extraction module contaminated samples.
In the time that sample solution is detected, the first step is to reduce the interference of enriched sample to analyte by dilute sample solution.Meanwhile, dilute sample also has the effect that reduces the sticky density of solution, is convenient to the follow-up treatment step such as Solid-Phase Extraction and membrane filtration.For ensureing analysis result accurately and reliably, Sample Dilution process is accurate quantification.In addition, because the chromatography of ions is the analytical approach based on concentration-response, the rinse step of also utilizing this device reduces analyte concentration in sample solution the probability of concentration change occurs in sample pretreatment process, thereby further improves the precision of sample pretreatment and the accuracy of stratographic analysis.
Second step: utilize the nonpolar chaff interference such as long chain alkane and benzene class in solid phase extraction filler adsorption sample, to avoid this type of chaff interference to be adsorbed onto the fixing upper ion chromatographic column that damages mutually.This step and conventional Solid-Phase Extraction make a big difference, and conventional method is with the analyte in solid phase extraction filler adsorption sample solution, then with leacheate, analysis is eluted, and reaches the object that analyte separates with chaff interference.The Solid-Phase Extraction that this sample processing device adopts is that direct adsorptive hindrance thing purifies sample solution, easier with conventional method, and there is no elution step without constant volume again, can be directly used in quantitative test.In addition, Solid-Phase Extraction process generally also will apply a power drive sample solution to sample solution and accelerate by solid phase extraction filler layer, and this device is exactly pressure downward while utilizing automatic sampler sample introduction, drive sample solution to complete sample pre-treatments and sample feeding simultaneously.
The 3rd step: utilize the solid particulate matter suspending in nylon or cellulose microporosity filter membrane filtering sample solution.After the filtration of the filter membrane of 0.22 μ m, sample solution has just met the requirement of ion chromatograph direct injected substantially.
brief description of the drawings
Fig. 1 sample pre-treatments device of the present invention fundamental diagram
Wherein: 1 sample feeding pipe, 2 film filter modules, 3 pistons, 4 sample holes, 5 sieve plates, 6 solid phase extraction fillers.
embodiment
Sample pre-treatments device of the present invention forms by diluting constant volume module, Solid-Phase Extraction module and film filter module; Dilution constant volume module is made up of sample feeding pipe 1 and piston 3, and sample feeding pipe 1 is a cylindrical shell with constant volume scale mark, and piston 3 external diameters and sample feeding pipe internal diameter match, and are positioned at sample feeding pipe, and center, piston upper end is provided with sample holes 4; Solid-Phase Extraction module is made up of solid phase extraction filler 6 and polylith porous sieve plate, or is made up of the overall filler without sieve plate, is embedded in piston 3; Film filter module 2 is made up of nylon or the cellulose microporosity filter membrane of aperture 0.22-0.45 μ m, and its size, with identical with Solid-Phase Extraction module, is clipped between Solid-Phase Extraction module and piston.
Claims (4)
1. for analyzing a sample pre-treatments device for alkanolamine solution negative ion, formed by dilution constant volume module, Solid-Phase Extraction module and film filter module; It is characterized in that: dilution constant volume module is made up of sample feeding pipe and piston, and sample feeding pipe is a cylindrical shell with constant volume scale mark, and piston external diameter and sample feeding pipe internal diameter match, and are positioned at sample feeding pipe, and center, piston upper end is provided with sample holes; Solid-Phase Extraction module is made up of solid phase extraction filler and polylith porous sieve plate, or is made up of the overall filler without sieve plate, is embedded in piston; Its size of film filter module, with identical with Solid-Phase Extraction module, is clipped between Solid-Phase Extraction module and piston; Described film filter module is positioned on Solid-Phase Extraction module.
2. according to claim 1 for analyzing the sample pre-treatments device of alkanolamine solution negative ion, it is characterized in that: described film filter module is made up of nylon or the cellulose microporosity filter membrane of aperture 0.22-0.45 μ m.
3. according to claim 1 for analyzing the sample pre-treatments device of alkanolamine solution negative ion, it is characterized in that: described solid phase extraction filler adopts solid phase extraction filler or the filler combination that can adsorb nonpolar chaff interference.
4. according to claim 1 for analyzing the sample pre-treatments device of alkanolamine solution negative ion, it is characterized in that: the silica gel particle of described solid phase extraction filler has been surface bond C18 or phenyl, and/or graphitized carbon, and/or activated charcoal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110446638.4A CN103185755B (en) | 2011-12-28 | 2011-12-28 | Sample pretreatment device for analyzing anions in alcohol amine solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110446638.4A CN103185755B (en) | 2011-12-28 | 2011-12-28 | Sample pretreatment device for analyzing anions in alcohol amine solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103185755A CN103185755A (en) | 2013-07-03 |
| CN103185755B true CN103185755B (en) | 2014-06-04 |
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|---|---|---|---|
| CN201110446638.4A Active CN103185755B (en) | 2011-12-28 | 2011-12-28 | Sample pretreatment device for analyzing anions in alcohol amine solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109142600A (en) * | 2018-10-18 | 2019-01-04 | 云南中烟工业有限责任公司 | A kind of method of 4 kinds of mercapturic acids in measurement smoker urine |
| CN111474249A (en) * | 2020-03-11 | 2020-07-31 | 台州学院 | Method for detecting organic alcohol amine compounds in environmental water sample |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0894597A (en) * | 1994-09-15 | 1996-04-12 | Hewlett Packard Co <Hp> | Solid-phase extraction method and solid-phase extractor |
| CN201229325Y (en) * | 2008-06-23 | 2009-04-29 | 玉溪师范学院 | Mini extraction separation device for trace material |
| CN201397320Y (en) * | 2009-03-04 | 2010-02-03 | 中国石油天然气股份有限公司 | Desorbing H in alcohol amine solution2S and CO2Experimental device of (2) |
| CN101995353A (en) * | 2010-10-25 | 2011-03-30 | 深圳出入境检验检疫局食品检验检疫技术中心 | Ultrafiltration membrane-solid phase extraction combined device for sample pretreatment and application thereof |
-
2011
- 2011-12-28 CN CN201110446638.4A patent/CN103185755B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0894597A (en) * | 1994-09-15 | 1996-04-12 | Hewlett Packard Co <Hp> | Solid-phase extraction method and solid-phase extractor |
| CN201229325Y (en) * | 2008-06-23 | 2009-04-29 | 玉溪师范学院 | Mini extraction separation device for trace material |
| CN201397320Y (en) * | 2009-03-04 | 2010-02-03 | 中国石油天然气股份有限公司 | Desorbing H in alcohol amine solution2S and CO2Experimental device of (2) |
| CN101995353A (en) * | 2010-10-25 | 2011-03-30 | 深圳出入境检验检疫局食品检验检疫技术中心 | Ultrafiltration membrane-solid phase extraction combined device for sample pretreatment and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| Determination of anions in amine solutions for sour gas treatment;Rainer Kadnar et al.;《Journal of Chromatography A》;19950707;第706卷(第1-2期);第339-343页 * |
| Rainer Kadnar et al..Determination of anions in amine solutions for sour gas treatment.《Journal of Chromatography A》.1995,第706卷(第1-2期), |
| 固相萃取-离子色谱法分析胺液中的热稳态盐离子组成;罗芳;《分析测试学报》;20040731;第23卷(第4期);第84-87页 * |
| 罗芳.固相萃取-离子色谱法分析胺液中的热稳态盐离子组成.《分析测试学报》.2004,第23卷(第4期), |
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