CN103185755A - 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 the sample pre-treatments device of analyzing the alkanolamine solution negative ion

Technical field

The present invention relates to a kind of for the sample pre-treatments device of analyzing the 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.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 can take place in alkanolamine solution in the device operation process, cause purification efficiency to descend, device pressure transient and corrosion aggravation wait harm.Therefore, purification plant need adopt chromatography of ions to detect the negative ion in the alkanolamine solution and monitor its content.Yet the alkanolamine solution sample of gathering in the commercial plant wherein often contains more chaff interference can not directly be analyzed.For example, the suspended solids thing, long chain alkanes etc. can work the mischief impact analysis result's precision and reappearance to the serviceable life of ion chromatographic column.In addition, the ionization that the high concentration hydramine also can the inhibition analysis thing causes negative effect to ion chromatography.Therefore, efficient, easy, the reliable sample-pretreating method of exploitation and device are the keys that improves the negative ion detection level in the alkanolamine solution.At present, the pre-treatment of this type of sample mainly utilizes filter membrane, and general sample pre-treatments device such as Solid-Phase Extraction is finished processing by manually-operated.If according to real needs, design a kind of integrated special-purpose sample pre-treatments device and can reduce the consuming time of hydramine sample pre-treatments, the repeatability of raising sample pre-treatments also reduces manual operation and brings error.

Summary of the invention

The purpose of this invention is to provide a kind of integrated for the sample pre-treatments device of analyzing the 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 the disposable removal sample.

Of the present invention for the sample pre-treatments device of analyzing the alkanolamine solution negative ion, integrated integratedly dilution constant volume module, Solid-Phase Extraction module and film filter module, described dilution constant volume module is made of sample introduction pipe and a supporting piston of a band constant volume scale mark, described Solid-Phase Extraction module is embedded on the described piston, and described film filter module is clipped between Solid-Phase Extraction module and the piston.

The dilution constant volume module of described sample pre-treatments device is made of sample introduction pipe and a supporting piston of a band constant volume scale mark; Described sample introduction pipe and piston material can be plastics or glass; In described sample introduction pipe, sample is diluted to the assigned scale line, then with 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, finishes 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 of polylith (as two) porous sieve plate and a certain amount of solid phase extraction filler, and perhaps the whole filler by no sieve plate constitutes; Adopt solid phase extraction filler or the filler combination that to 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 of nylon or cellulose microporosity filter membrane, and its area size is clipped between Solid-Phase Extraction module and the piston with identical with the Solid-Phase Extraction module; Its aperture can be regulated according to the sample that detects; 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.

When sample solution was detected, the first step was to reduce enriched sample to the interference of analyte by dilute sample solution.Meanwhile, dilute sample also has the effect that reduces the sticking density of solution, is convenient to treatment steps such as follow-up Solid-Phase Extraction and membrane filtration.For guaranteeing analysis result accurately and reliably, the sample dilution is accurate quantification.In addition, because the chromatography of ions is based on the analytical approach of concentration-response, the rinse step of also utilizing this device reduces that the probability of concentration change takes place analyte concentration in the sample solution in sample pretreatment process, thereby further improves the precision of sample pretreatment and the accuracy of stratographic analysis.

Second step: utilize nonpolar chaff interferences such as long chain alkane in the solid phase extraction filler adsorption sample and benzene class, damage ion chromatographic column to avoid this type of chaff interference to be adsorbed onto fixing going up mutually.This step and conventional Solid-Phase Extraction have very big difference, and conventional method is with the analyte in the solid phase extraction filler adsorption sample solution, with leacheate analysis is eluted then, reaches the purpose 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, and is easier with conventional method, and do not have elution step to need not constant volume again, can be directly used in quantitative test.In addition, the Solid-Phase Extraction process generally also will apply a power drive sample solution to sample solution and accelerate by the solid phase extraction filler layer, and this device is exactly pressure downward when utilizing the automatic sampler sample introduction, drives sample solution simultaneously and finishes sample pre-treatments and sample feeding.

The 3rd step: utilize the solid particulate matter that suspends in nylon or the cellulose microporosity filter membrane filtering sample solution.After the filtration through the filter membrane of 0.22 μ m, sample solution has just satisfied the requirement of ion chromatograph direct injected substantially.

Description of drawings

Fig. 1 sample pre-treatments device of the present invention fundamental diagram

Wherein: 1 sample introduction 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 is made of dilution constant volume module, Solid-Phase Extraction module and film filter module; Dilution constant volume module is made ofsample introduction pipe 1 andpiston 3, andsample introduction pipe 1 is the cylindrical shell of a band constant volume scale mark, andpiston 3 external diameters and sample introduction bore are complementary, and are positioned at the sample introduction pipe, and center, piston upper end is provided withsample holes 4; The Solid-Phase Extraction module is made of solidphase extraction filler 6 and polylith porous sieve plate, or is made of the whole filler of no sieve plate, is embedded in thepiston 3; Film filter module 2 is made of nylon or the cellulose microporosity filter membrane of aperture 0.22-0.45 μ m, and its area size is clipped between Solid-Phase Extraction module and the piston with identical with the Solid-Phase Extraction module.

Claims (4)

1. a sample pre-treatments device that is used for analyzing the alkanolamine solution negative ion is made of dilution constant volume module, Solid-Phase Extraction module and film filter module; It is characterized in that: dilution constant volume module is made of sample introduction pipe and piston, the cylindrical shell of sample introduction Guan Weiyi band constant volume scale mark, and piston external diameter and sample introduction bore are complementary, and are positioned at the sample introduction pipe, and center, piston upper end is provided with sample holes; The Solid-Phase Extraction module is made of solid phase extraction filler and polylith porous sieve plate, or is made of the whole filler of no sieve plate, is embedded in the piston; Its area size of film filter module is clipped between Solid-Phase Extraction module and the piston with identical with the Solid-Phase Extraction module.

2. according to claim 1 for the sample pre-treatments device of analyzing the alkanolamine solution negative ion, it is characterized in that: described film filter module is made of nylon or the cellulose microporosity filter membrane of aperture 0.22-0.45 μ m.

3. according to claim 1 for the sample pre-treatments device of analyzing the 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 the sample pre-treatments device of analyzing the 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.

Images