CN103185755B - Sample pretreatment device for analyzing anions in alcohol amine solution - Google Patents

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

A kind of for analyzing the sample pre-treatments device of alkanolamine solution negative ion

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 ofsample feeding pipe 1 andpiston 3, andsample feeding pipe 1 is a cylindrical shell with constant volume scale mark, andpiston 3 external diameters and sample feeding pipe internal diameter match, and are positioned at sample feeding pipe, and center, piston upper end is provided withsample holes 4; Solid-Phase Extraction module is made up of solidphase extraction filler 6 and polylith porous sieve plate, or is made up of the overall filler without sieve plate, is embedded inpiston 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.

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