CN208780664U - A kind of ion chromatography sample pretreatment apparatus - Google Patents
A kind of ion chromatography sample pretreatment apparatus Download PDFInfo
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- CN208780664U CN208780664U CN201821222324.XU CN201821222324U CN208780664U CN 208780664 U CN208780664 U CN 208780664U CN 201821222324 U CN201821222324 U CN 201821222324U CN 208780664 U CN208780664 U CN 208780664U
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Abstract
The utility model provides a kind of sample pretreatment apparatus of ion chromatography, belongs to instrument analysis technology field.Described device includes the amberplex for separating water sample intermediate ion, for separating the dialyser of ion and organic matter, for providing the electrode plate of ion-drive power, for distinguishing the partition and clamping device of each compartment；The amberplex, dialyser, partition cooperate, and form compartment by gripping means grips；The amberplex, wherein cation-exchange membrane is placed in the anode side close to electrode, and anion-exchange membrane is placed in the side of the cathode close to electrode, so that water sample intermediate ion is retained in sample room without entering in electrode chamber, avoids being lost.The utility model can extract ion from water sample to be measured, can directly be analyzed using ion chromatography；The process makes the chromatographic column of ion chromatography from the interference of large amount of organic, stablizes separating effect and increases the service life of chromatographic column.
Description
Technical field
The utility model belongs to instrument analysis technology field, and especially a kind of sample pretreatment suitable for ion chromatography fills
It sets, including the amberplex for separating ion and the dialyser for obstructing organic matter.
Background technique
Anion such as chloride ion, bromide ion, iodide ion in water sample are the common counters in water analysis, with ion color
What spectrum can be convenient detects it.The chromatography of ions has many advantages, such as quick separating, high sensitivity, but to sample introduction solution
The requirement of degree of purity is relatively high.Because the organic matter and particulate matter in water sample easily reduce ion chromatographic column blocking, column effect, contracting
The service life of shorter chromatogram column, in general, the sample especially actual water sample detected with ion chromatograph needs advanced
Row pretreatment, removes the wherein substances such as organic matter, particulate matter.
A kind of chromatography of anion in liquid is disclosed in Chinese utility model patent specification CN201720663253.6
Purification device before detecting, purification device is successively by syringe 1, cation exchange column 2,3 and of reversed phase extraction column before which detects
0.22 μm of 4 four part of injecting type filter membrane connects and composes, wherein cation exchange column 2 is greater than to remove radius in fluid sample
The cation of sodium, such as Ca2+、Mg2+、Zn2+、Mn2+、Fe3+Equal metal ions, make sample obtain preliminary purification.C18 reversed phase extraction
Column can generate reservation to most of organic matter in aqueous phase substrate, and salts substances can pass through without reservation pillar, therefore
The organic matter in liquid can be removed well.It is removed finally by 0.22 μm of injecting type filter membrane and is greater than 0.22 μm in fluid sample
Grain, prevents the ion chromatographic column of high pressure liquid chromatograph from blocking.
Although can effectively be eliminated organic in water sample using the combination of cation exchange column, reversed phase extraction column C18
Object, particulate matter.But step is more, cumbersome, and cation exchange column and reversed phase extraction column are all consumptive materials, are only capable of using one
It is secondary, so using above method higher cost；Therefore be badly in need of the pretreated device of ion chromatography sample a kind of, can it is convenient,
The impurity such as organic matter and particulate matter in economic removal water sample.
Summary of the invention
In view of the deficiency of the prior art, the utility model provides one kind and can be more convenient, rapidly by water sample
It is pre-processed, removes the impurity such as organic matter and particulate matter therein, met ion chromatography sample introduction demand, preferably protect chromatography
The device of column.
The utility model includes handing over for separating the ion of water sample intermediate ion for the device of ion chromatography sample pretreatment
Film is changed, for separating the dialyser of organic matter, for providing the electrode plate of electric field, for distinguishing the partition of each compartment；It should be from
Proton exchange, dialyser, partition, which cooperate, forms different compartments；The amberplex, wherein cation-exchange membrane is put
It is disposed adjacent to the anode side of electrode, anion-exchange membrane is placed in the side of the cathode close to electrode, protects water sample intermediate ion
Sample room is stayed in without entering in electrode chamber, avoids being lost；It is dilute acid soln that anode chamber, which is passed through liquid, and cathode chamber is passed through liquid
For dilute alkaline soln, the continuous activating ion exchange membrane of the hydrogen ion and hydroxide ion provided by both liquid, to guarantee
Amberplex is in optimum Working.
In the above-mentioned technical solutions, one layer of dialyser is placed among amberplex, can generate following technical effect；
Water sample to be measured is passed through sample room 20, ultrapure water is passed through sample room 19, and under electric field action, anion in water sample to be measured can be to
The anode 5 of the electrode is mobile, dialyser 7 is passed through, into sample room 19；Anion can not continue across the sun of amberplex
Film 6, therefore be retained in sample room 19；Organic matter contained in water sample to be measured is largely electroneutral and due to size
Limitation can not penetrate dialyser 7, be retained in sample room 20；Cation in water sample to be measured is under electric field action to electrode yin
9 direction of pole is mobile, but can not be by the cavity block 8 of amberplex, therefore is retained in sample room 20；Liquid in sample room 19
The anion in water sample to be measured is contained, can directly be analyzed using ion chromatography；The process makes the chromatographic column of ion chromatography
From the interference of most of organic matter and particulate matter, can reduce influence and increase chromatographic column of the organic matter to detection uses the longevity
Life.
As a preferred embodiment of the utility model, wherein the aperture of dialyser is the cellulose membrane less than 200Da；
As a preferred embodiment of the utility model, which need to be for the slightly elastic material for being also easy to produce deformation
Material, makes the compartment closeness, no leakage；
As a preferred embodiment of the utility model, the sulfuric acid that the dilute acid soln in the electrode chamber is 10mmol/L,
The dilute alkaline soln is the sodium hydroxide of 20mmol/L；
To enable the sample pretreatment apparatus of the utility model adequately to come out the ion extraction in water sample, as this reality
With a novel preferred embodiment, wherein amberplex is less than 1mm with distance between dialyser；
To enable the sample pretreatment apparatus of the utility model to be enriched with components in water sample, ion color is improved
The detection of spectrum limits, ultrapure by the water sample and sample room 19 that enter sample room 20 as a preferred embodiment of the utility model
The flow velocity of water is adjusted, and the function of ion enrichment, stream of the 20 water sample flow velocity of sample room relative to 19 ultrapure water of sample room may be implemented
The multiple of speed is the multiple of ion enrichment；
Detailed description of the invention
The schematic diagram of Fig. 1 the utility model sample pretreatment apparatus
The structural schematic diagram of Fig. 2 the utility model sample pretreatment apparatus
Specific embodiment
The most preferred embodiment of the utility model is described below referring to attached drawing.
Embodiment 1: determinand is the ion chromatography sample pretreatment apparatus of anion in water sample
Fig. 1 shows the utility model ion chromatography sample pretreatment apparatus, including shell 11, positioned at the anode of enclosure interior
Electrode 5, cation-exchange membrane 6, dialyser 7, anion-exchange membrane 8, cathode electrode 9；It is connected with liquid line on shell 11, point
Not Wei anode chamber's liquid flow into pipe 1, sample flow into pipe 2, sample flow into pipe 3, cathode chamber liquid flow into pipe 4, liquid flow into pipe point
Power is not provided by water pump 11,12,13,14；Cation-exchange membrane 6, dialyser 7 belonging to form in shell sample room 1 and
The sample room 2 that dialyser 7, anion-exchange membrane 8 form；Liquid effuser road, respectively sample room are also connected on shell 11
19 effusers 15,20 effuser 17 of sample room and sewer pipe 16,18.
Fig. 2 shows the structures of ion chromatography sample pretreatment apparatus of the present invention, including shell 31,32；Partition 33,34,35；
Cation-exchange membrane 36, anion-exchange membrane 37, dialyser 38.
For anion in water sample under electric field action, the anode 5 of Xiang Suoshu electrode is mobile, passes through and seeps under the action of electric field
Film 7 is analysed, into sample room 19；But most of organic matter can not pass through dialyser 7 because not charged and size limits in water sample, still
It is retained in sample room 20；Collect liquid (the i.e. liquid of 19 effuser 15 of sample room outflow for being passed through the sample room 19 of ultrapure water
Body), this liquid contains the anion in water sample to be measured, and eliminates most organic matter, can directly with ion chromatography into
Row analysis；
The process that ion is extracted from detected water sample is completed through the above steps.
This example chooses tap water as tested water sample, verifies pretreating effect.In experiment, voltage is straight between two electrode plates
20V is flowed, tap water is passed through to sample room 20, is passed through ultrapure water in sample room 19；Tap water sample introduction flow velocity and ultrapure water flow velocity are all
For 0.5ml/min, the dilute sulfuric acid for being pumped into 10mmol/L by sample feeding pipe 1 with the flow velocity of 1ml/min, sample feeding pipe 4 are with 1ml/min's
Flow velocity is pumped into the sodium hydroxide solution of 20mmol/L；
Initial water quality indicator and index after pretreatment are as follows:
From the results, it was seen that original chloride ion-containing 8.31mg/L, sulfate ion 8.18mg/ in water sample tap water to be measured
L, the ultrapure water being passed through when initial in sample room 19, chloride ion-containing, sulfate ion are all 0, after pretreatment in middle sample room 19
Water sample chloride ion-containing 8.21mg/L, sulfate ion 8.05mg/L, i.e., after pretreatment, the ion in water sample tap water to be measured
Almost whole is extracted in ultrapure water, and extraction efficiency is chloride ion 98.8%, sulfate ion 98.4%；Tap water water sample
In organic matter (in terms of TOC) only seldom (about 6.3%) is brought into ultrapure water, and by preprocessor structure it is found that this portion
Point organic matter be all small organic molecule because dialyser can be penetrated, into chromatographic column after be easy by ion chromatography
Leacheate elution, the influence to chromatographic column are smaller.
Embodiment 2: determinand is ion chromatography pretreatment unit cationic in water sample
Fig. 1 shows the utility model ion chromatography sample pretreatment apparatus, including shell 11, positioned at the anode of enclosure interior
Electrode 5, cation-exchange membrane 6, dialyser 7, anion-exchange membrane 8, cathode electrode 9；Liquid line is connected on shell, respectively
Pipe 1 is flowed into for anode chamber's liquid, sample flows into pipe 2, sample flows into pipe 3, cathode chamber liquid flows into pipe 4, liquid inflow pipe difference
Power is provided by water pump 11,12,13,14；The sample room 1 and dialysis that the amberplex 6 belonging to, dialyser 7 form in shell
The sample room 2 that film 7, amberplex 8 form；Be also connected with liquid effuser road on shell, respectively sample effuser 17 with
And sewer pipe 16,15,18.
With being distinguished as in embodiment 1, extracting target is the cation in water sample, therefore water sample to be measured surpasses into sample room 19
Pure water is into sample room 20；Cation in water sample is under electric field action, and the cathode 9 of Xiang Suoshu electrode is mobile, in the effect of electric field
Under across dialyser 7, into sample room 20；But most of organic matter is seeped because the limitation of not charged and size can not pass through in water sample
Film is analysed, is remained in sample room 19；Collect efflux (the i.e. liquid of the outflow of discharge pipe 17 for being passed through the sample room 20 of ultrapure water
Body), this liquid contains the anion in water sample to be measured, and eliminates most organic matter, can directly with ion chromatography into
Row analysis.
Embodiment 3: determinand is anion in water sample, the ion chromatography pretreatment unit with concentrating function
The pretreatment unit structure of this example is identical with embodiment 1, as shown in Figure 1.
This example chooses tap water as tested water sample, and adds 0.03mg/L bromide ion wherein to verify pretreatment effect
Fruit.In experiment, voltage is direct current 20V between two electrode plates, is passed through water sample to be measured to sample room 20, is passed through in sample room 19 ultrapure
Water；Tap water water sample sample introduction flow velocity is 0.9ml/min, ultrapure water flow velocity is 0.3ml/min, by sample feeding pipe 1 with 1ml/min's
Flow velocity is pumped into the dilute sulfuric acid of 10mmol/L, sample feeding pipe 4 is pumped into the sodium hydroxide solution of 20mmol/L with the flow velocity of 1ml/min；
Initial water quality indicator and index after pretreatment are as follows:
From the results, it was seen that original chloride ion-containing 8.31mg/L, bromide ion 0.03mg/L, sample room 19 in water sample to be measured
In it is initial when the ultrapure water that is passed through, chloride ion-containing, sulfate ion are all 0；Water sample after pretreatment in middle sample room 19 contains chlorine
Ion 24.2mg/L, sulfate ion 0.087mg/L, i.e., after pretreatment, ion in water sample to be measured is almost whole to be mentioned
It gets in ultrapure water, bioaccumulation efficiency is 2.91 times of chloride ion, 2.97 times of bromide ion.Equally, the organic matter in water sample (in terms of TOC)
Only seldom bring into ultrapure water, and by preprocessor structure it is found that this partial organic substances because can penetrate dialyser,
Be all small organic molecule, into chromatographic column after be easy to be eluted by the leacheate of ion chromatography, the influence to chromatographic column is smaller.
Claims (4)
1. a kind of ion chromatography sample pretreatment apparatus, including the amberplex for separating water sample intermediate ion, for providing
The electrode plate of ion-drive power, for distinguishing the partition of each compartment；The amberplex, dialyser, partition mutual cooperation group
At different compartments；It is dilute acid soln that anode chamber, which is passed through liquid, and it is dilute alkaline soln that cathode chamber, which is passed through liquid,；
It is characterized in that placing one layer of dialyser between the amberplex；The amberplex, cation-exchange membrane are put
It is disposed adjacent to the anode side of electrode, anion-exchange membrane is placed in the side of the cathode close to electrode.
2. sample pretreatment apparatus according to claim 1, which is characterized in that the aperture of dialyser is less than 200Da's
Cellulose membrane.
3. sample pretreatment apparatus according to claim 1, which is characterized in that the amberplex is the same as dialyser spacing
From less than 1mm.
4. sample pretreatment apparatus according to claim 1, which is characterized in that flow rate of liquid is sample in the sample room 19
The multiple of flow rate of liquid in product room 20.
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| CN201821222324.XU CN208780664U (en) | 2018-07-31 | 2018-07-31 | A kind of ion chromatography sample pretreatment apparatus |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693300A (en) * | 2018-07-31 | 2018-10-23 | 深圳合核环境科技有限公司 | A kind of ion chromatography sample pretreatment apparatus and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693300A (en) * | 2018-07-31 | 2018-10-23 | 深圳合核环境科技有限公司 | A kind of ion chromatography sample pretreatment apparatus and method |
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