CN103344736A - Method for detecting content of sodium ions in water vapor of thermodynamic system by using ion chromatography - Google Patents
Method for detecting content of sodium ions in water vapor of thermodynamic system by using ion chromatography Download PDFInfo
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- CN103344736A CN103344736A CN2013102917294A CN201310291729A CN103344736A CN 103344736 A CN103344736 A CN 103344736A CN 2013102917294 A CN2013102917294 A CN 2013102917294A CN 201310291729 A CN201310291729 A CN 201310291729A CN 103344736 A CN103344736 A CN 103344736A
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Abstract
The invention provides a method for detecting content of sodium ions in water vapor of a thermodynamic system by using an ion chromatography. The method comprises the following steps of: placing a mobile phase in a leacheate storage tank, adding a collected water vapor sample through a sample adding hole between the leacheate storage tank and a separation column, bringing the detected sample to the separation column filled with ion exchange resin by the mobile phase, enabling a mobile phase of ions to be detected to flow out from the separation column and enter an inhibition column, filling ion exchange resin with charges opposite to charges of the separation column in the inhibition column; enabling the mobile phase flowing out from the inhibition column to enter an electrical conductivity detector; and preparing an Na<+> standard solution and a blank solution, drawing a standard working curve, and detecting the content of Na<+> in the sample. According to the method, contents of multiple groups of negative ions and positive ions from mu g/L level to mg/L level can be conveniently simultaneously detected by ion chromatography, and can also be detected accurately and rapidly by directly adopting a large-volume injection method without needing concentration and enrichment even if being subjected to mu g/L level analysis, with the analysis time of only several minutes to tens of minutes.
Description
Technical field
The present invention relates to a kind of detection method of sodion, be specifically related to the detection method of sodium ions content in a kind of therrmodynamic system steam.
Background technology
Sodium ions content is one of important indicator of generating plant steam quality.When carrying the impurity that some contain sodium in the steam, can cause spot corrosion, stress corrosion or the corrosion fatigue of steam turbine metal material, these corrosion regular meetings cause very big economic loss.The U.S. was once investigated the genset more than more than 200 the single-machine capacity 100MW; found that owing to the impurity in the steam causes the stopping accident that the steam turbine corrosion causes and compete up to 4.6%; the metal material that damages comprises alloy steel, stainless steel, even the superalloy steel.Therefore, for preventing fouling, salt crust, the corrosion of metal parts in the relieving system guarantees the safety and economic operation of system, must carry out strictness control and monitors sodium ions content in the Power Plant Water Vapor system.In addition, along with developing rapidly of power industry, improving constantly of unit parameter, requirement to the steam quality also improves constantly, the measuring technology of water-steam system sodium is generally dynamic method or on-line determination, the measurable value of stability requirement (0.03pNa) according to instrument reaches 0.69 μ g/L, but the sodium ions content in the actual value steam may be lower, that is to say, supervision index and measurable method is closely related, and dynamic method and the accuracy of online dynamic method also are subjected to a certain extent influences such as environment temperature, detected solution become to be grouped into, flow velocity.Extremely important in the next accurate test method of this background, can provide reference frame to unit operation technology mode and process modification.
Chromatography of ions (IC) is a kind of of high performance liquid chromatography, is mainly used in the mensuration of zwitterion in the testing sample.The advantage of chromatography of ions is that selectivity is good, highly sensitive, fast and convenient, in the industry especially high purity water field, its outstanding advantage is arranged.Chromatography of ions development since 1975 come out is very fast, is widely used in fields such as environmental monitoring, electric power, semi-conductor industry, food, petrochemical complex, health care and biochemistry.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to provide a kind of method that is applied to can accurately measure in the therrmodynamic system water vapour Trace Sodium ion, and this method accuracy height is not subjected to factor affecting such as temperature, other ion concentrations substantially.
Technical scheme of the present invention is, a kind ofly detects the method for sodium ions content in the therrmodynamic system steam with chromatography of ions, comprises separating column, and this method comprises:
A, will flow is stored in the leacheate hold-up vessel mutually, the steam sample of collecting is added entrance by the sample between described leacheate hold-up vessel and the separating column to add, flow and take institute's test sample product to be filled with ion exchange resin separating column, flowed out the mobile phase for the treatment of measured ion by separating column, enter suppressed column, in suppressed column, filled the ion exchange resin of electric charge and separating column opposite charge;
B, enter electric conductivity detector mutually from flowing of coming out of suppressed column;
C, configuration Na
+Standard solution and blank solution, drawing standard working curve, the Na in the working sample
+Content.
According to the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam of the present invention, preferably, be used for the deionized water of preparation leacheate and standard solution, its resistivity should be more than the 18.2M Ω .cm.
According to the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam of the present invention, preferably, it is characterized in that the filler in the described separating column is the organic ion exchange resin.
Further, the ion exchange resin in the described separating column has the physical arrangement of macropore or thin-shell type or porous surface stratotype.
Further, ion exchange resin in the described separating column is skeleton with the SDEB styrene diethylenebenzene interpolymer, introduce sulfonic group at phenyl ring, form strongly acidic cation-exchange, perhaps introduce tertiary amine groups at phenyl ring and form quaternary amine type strong-base anion-exchange resin.
According to the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam of the present invention, preferably, the adding of described sample adopts big volume sample quantitatively to encircle input mode.
Further, described sample volume is the 0.5-3 milliliter.
Further, described sample volume is the 0.8-2 milliliter.
The separating mechanism of chromatography of ions of the present invention mainly is ion-exchange method.Ion exchange principle is to adopt the ion exchange resin of low ion exchange capacity to come isolating ions, this is most widely used general in chromatography of ions, its main stuffing type is the organic ion exchange resin, be skeleton with the SDEB styrene diethylenebenzene interpolymer, introduce sulfonic group at phenyl ring, form strongly acidic cation-exchange, introduce tertiary amine groups and form quaternary amine type strong-base anion-exchange resin, this exchange resin has the physical arrangement of macropore or thin-shell type or porous surface stratotype, so that reach exchange equilibrium fast, the ion exchange resin acid and alkali-resistance can use in any pH scope, has easy regeneration and handles, the characteristics of long service life.
The whole instrument system partly is made up of fluid reservoir, ram pump, sampling valve, separating column, suppressed column, detecting device and data recording and processing system etc.When taking institute's test sample product to separating column when flowing, because the relative affinity of various ion pair separating column intermediate ion exchange resins varies in size, sample is separated into discontinuous bands of a spectrum at separating column, and successively by mobile phase wash-out, different kinds of ions uses electric conductivity detector to detect in the mensuration solution, this detecting device is sensitive and general, and the conductivity that detects is the general character of effects of ion. and be the simple function of ion concentration when low concentration, and linear with it.Yet because the mobile phase that ion-exchange separates nearly all is strong electrolyte, conductivity is general often " has flooded " signal for the treatment of measured ion fully than treating high two orders of magnitude of measured ion, introduces suppressed column in analysis process, has just solved this problem well.Method is exactly to flow out the mobile phase for the treatment of measured ion by separating column. before detection, be introduced into suppressed column, in suppressed column, filled the electric charge ion exchange resin opposite with separating column, thereby at suppressed column two simple and important chemical reactions take place, a reaction is to be transformed into low electricity mutually to lead component with flowing, to reduce the background conductance from the phase that flows: the 2nd, sample ions is transformed into its corresponding acid or alkali, lead to increase its electricity.The workflow of suppressed column plays the effect that the non-selectivity electric conductivity detector is transformed into the selectivity electric conductivity detector, and has increased the detection sensitivity for the treatment of measured ion.
In the sulfate by ion chromatography engineering, in testing process, there is not H
+Influence, remove the step of adding reagent from.Because the chromatographic column degree of separation is better, can measure different kinds of ions simultaneously, generally speaking, does not have interionic interference.In the sulfate by ion chromatography process, adopt the current constant mode sample introduction, do not have unit water sample flow velocity problem of unstable in the site test.
The chromatography of ions of the present invention is compared with online detection method with the detection of dynamic method, more accurately, fast and not influenced by the sample pH value value, the influence that is subjected to temperature and other foreign ions can be ignored substantially, measures more suitable for the sodium ions content in the steam sample in the therrmodynamic system.
Description of drawings
Fig. 1 is ion chromatography system pie graph of the present invention.
Fig. 2 is the Na+ standard working curve.
Fig. 3 is sample analysis detection figure.
Among the figure, 1-leacheate hold-up vessel, the 2-pump, the 3-sample adds entrance, 4-separating column, 5-guard column, 6-analytical column, 7-suppressed column, 8-electric conductivity detector, 9-chromatographic work station.Guard column and analytical column are formed the separating column part.
Embodiment
A kind of method with sodium ions content in the chromatography of ions detection therrmodynamic system steam of the present invention comprises separating column, and this method comprises:
A, will flow is stored in the leacheate hold-up vessel 1 mutually, the steam sample of collecting is added entrance 3 by the sample between described leacheate hold-up vessel and the separating column to add, flow and take institute's test sample product to be filled with ion exchange resin separating column, flowed out the mobile phase for the treatment of measured ion by separating column, enter suppressed column, in suppressed column, filled the ion exchange resin of electric charge and separating column opposite charge;
B, enter electric conductivity detector 8 mutually from flowing of coming out of suppressed column 7;
C, configuration Na
+Standard solution and blank solution, drawing standard working curve, the Na in the working sample
+Content.
As shown in Figure 1, the whole instrument system partly is made up of fluid reservoir, ram pump, sampling valve, separating column, suppressed column, detecting device and data recording and processing system etc.Be provided with sample between separating column and suppressed column and add entrance, sample can join sample with injection system or other modes and add in the entrance 3.The mobile sample of flowing through mutually in the leacheate in the hold-up vessel adds entrance, take institute's test sample product to separating column, because the relative affinity of various ion pair separating column intermediate ion exchange resins varies in size, sample is separated into discontinuous bands of a spectrum at separating column, and successively by mobile phase wash-out, different kinds of ions uses electric conductivity detector to detect in the mensuration solution, this detecting device is sensitive and general, the conductivity that detects is the general character of effects of ion. be the simple function of ion concentration when low concentration, and linear with it.Flowed out the mobile phase for the treatment of measured ion by separating column. before detection, be introduced into suppressed column, in suppressed column, filled the electric charge ion exchange resin opposite with separating column, thereby at suppressed column two simple and important chemical reactions take place, a reaction is to be transformed into low electricity mutually to lead component with flowing, to reduce the background conductance from the phase that flows: the 2nd, sample ions is transformed into its corresponding acid or alkali, lead to increase its electricity.The workflow of suppressed column plays the effect that the non-selectivity electric conductivity detector is transformed into the selectivity electric conductivity detector, and has increased the detection sensitivity for the treatment of measured ion.
This chromatography of ions experimental study is employed to be the ICS-5000 ion chromatograph of being produced by U.S. Dai An company (DIONEX), and this instrument is mainly by the double plunger gradient pump GS50 that back and forth connects; Electrochemical detector ED50; Constant temperature chromatogram case LC25; CSRS automatic regeneration rejector; IonPac CS16A separating column (3mm); IonPac CG12A guard column (2mm) is formed.
According to the debugging of instrument operation instructions, preparation instrument; Select suitable analytical column, rejector and corresponding condition of work and chromatographic condition, balanced system is steady to baseline.
According to factors such as cations in the performance of analytical column, the water sample to be measured, select to use big volume sample quantitatively to encircle input mode, this test sampling volume is about 1 milliliter.
The hybrid standard working solution
The preparation of middle mixed standard solution: according to cation type to be measured and various cationic detection sensitivity, accurately pipette an amount of required cationic standard stock solution, the dilute with water constant volume, be prepared into low mg/litre level (as: 1.0mg/L Na+, NH4, Mg2+, 2.0mg/L K+, Ca2+) mixed standard solution, store in polypropylene or the high-density polyethylene bottle, 4 ℃ of refrigerations are deposited, and mixed standard solution can be deposited a week in the middle of this.
The preparation of hybrid standard working solution: the hybrid standard working solution should be prepared in the sky, and the concentration range of hybrid standard working solution should comprise cationic concentration in the sample.Accurately pipette an amount of middle mixed standard solution, dilute with water constant volume, preparation hybrid standard working solution.Prepare the hybrid standard working solution of 2 blank solutions, at least five concentration levels.Be blank solution with the reagent water, each cationic concentration level is respectively 2.5 μ g/L, 5 μ g/L, 10 μ g/L, 15 μ g/L and 20 μ g/L or higher usually in the hybrid standard working solution.
The drafting of standard working curve
Analysis margin solution, serial hybrid standard working solution, the appearance time on the record spectrogram is determined each cationic retention time; Being ordinate with peak height or peak area, is horizontal ordinate with the cation concn, draws standard working curve by chromatographic work station, and ammonium ion adopts non-linear regression, and other ion adopts linear regression mode, and related coefficient should be greater than 0.995.The Na+ standard working curve is seen Fig. 2, and wherein ordinate is integrated value, and horizontal ordinate is concentration.
The sampling volume of standard working solution and water sample must be consistent during test.
Sample analysis
Water is reagent maximum in the trace analysis.The purity of water is related to the success or failure of trace analysis work.Therefore, when using chromatography of ions to carry out trace analysis, be used for the deionized water of preparation leacheate and standard, its resistivity should be more than the 18.2M Ω .cm.
The standard storage liquid of sodium: 1.000mg/mL is diluted to 10 μ g/mL and is sodium standard operation solution when using.By the working solution of gradient configuration sodium, can optionally prepare the working solution of variable concentrations according to demand, for example: C0=0 μ g/L, C1=0.2 μ g/L, C2=0.5 μ g/L, C3=1.0 μ g/L, C4=1.5 μ g/L, C5=2.0 μ g/L, directly enter ion chromatograph, with the peak area integration, the drawing standard curve, related coefficient reaches more than 0.995, can carry out the mensuration of Na+ in the sample.
Sample analysis is seen Fig. 3, is shown as the sample detection analysis of spectra, wherein Na
+Retention time be 9.783min.
The comparative example of the chromatography of ions of the present invention and other several methods:
During power plant's conventional operation, Na
+Monitoring was lost efficacy to monitor for thermal chemical test, condenser leak diagnostics and condensate water precision processing and was had important effect.This experimental study mainly compares experimental study by thermal chemical test, condensate water precision processing inefficacy monitoring and unit conventional operation to several sodion detection methods.
Thermal chemical test
This experimental study has been carried out test relatively by during the Waigaoqiao Power Plant thermal chemical test to several method of testings.Thermal chemical test is to specialize in steam-purity value and influence factor thereof, seeks to obtain the test of the boiler operatiopn condition of clean steam.Can determine boiler operatiopn operating modes such as the peak load of boiler and peak load pace of change, the highest permission water level of drum by thermal chemical test.
Keep normal and stably steam water-level be one of important measures of safe operation of the boiler, and in day-to-day operation, unit fluctuates steam water-level often because of the peak regulation varying loading.Steam water-level changes the purpose of test, namely is being held in the interior lifting of setting range or reducing steam water-level to the influence that steam quality causes, determining rational steam water-level traffic coverage.
The test water level be set to-50mm, 0mm and+the 50mm third gear, test omnidistance boiler capacity and maintain about 1000t/h, unit load 300MW.Test detects its Na to steam sampling after set steady runs on each steam water-level
+Content.Test findings sees Table 1.
Table 1 water level test saturated vapour test result (mean value, unit: μ g/L)
| Steam water-level (mm) | Dynamic method | On-line method | The chromatography of ions |
| -50 | 0.76 | 0.74 | 0.47 |
| 0 | 0.80 | 0.78 | 0.52 |
| +50 | 0.85 | 0.80 | 0.85 |
Test result from the test of table 1 water level, do not take place in the boiler water salt content under the condition of obviously fluctuation, testing longitudinal result steam Na+ content significantly fluctuation of generation the process that steam water-level changes as can be seen from dynamic method and on-line method, because the level of steam Na+ content own is lower, and the minimum detectability value near instrument, so it is not obvious that the test result of Na+ changes, so test can only draw and thinks steam Na for water level
+The relation that the micro fluctuation of content and steam water-level change is not remarkable, the conclusion that SEA LEVEL VARIATION can not impact steam quality.But from three kinds of test method lateral comparisons just as can be seen the minimum detectability of the test of the chromatography of ions be starkly lower than preceding two kinds of method of testings, and the sensitivity of test is also higher, as adopt the test findings of the chromatography of ions, just can draw steam water-level changes slightly influential to steam Na+ content, along with the rising of steam water-level, steam Na
+Content is on the rise, but-50mm～+ when changing in the 50mm scope, the conclusion that can impact steam quality not.
The chromatography of ions has certain advantage for traditional dynamic test method and on-line testing method as can be seen from the actual motion of three kinds of sodion method of testings thermal chemical test, its high precision, high measurement sensitivity can provide more accurate, more reliable test figure for test, provide foundation for proposing conclusion (of pressure testing) accurately.
The chromatography of ions measuring technology since coming out the seventies in last century development rapidly, because of its have simple to operate fast, selectivity is good, sensitivity is higher, can measure multi-component advantage simultaneously, be used widely.In thermal power plant's water analysis, classic method is not only time-consuming, and to measuring trace components or existing the water quality of more interfering material helpless especially.With the twin columns ion chromatography system of " separating column+suppressed column+electric conductivity detector ", can solve the mensuration problem of Na+ easily.Chromatography of ions can be measured the polycomponent yin, yang ion concentration of μ g/L to mg/L level easily simultaneously, and accurately, fast.Particularly " only the add the water technology " appearance of (only add water) makes background conductance lower, and gradient elution is easier, more convenient, even μ g/L level is analyzed, also need not enrichment method, can directly adopt large volume sample injection method, only need a few minutes to arrive dozens of minutes analysis time.
Claims (8)
1. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam comprises separating column, and it is characterized in that: this method comprises:
A, will flow is stored in the leacheate hold-up vessel mutually, the steam sample of collecting is added entrance by the sample between described leacheate hold-up vessel and the separating column to add, flow and take institute's test sample product to be filled with ion exchange resin separating column, flowed out the mobile phase for the treatment of measured ion by separating column, enter suppressed column, in suppressed column, filled the ion exchange resin of electric charge and separating column opposite charge;
B, enter electric conductivity detector mutually from flowing of coming out of suppressed column;
C, configuration Na
+Standard solution and blank solution, drawing standard working curve, the Na in the working sample
+Content.
2. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 1 is characterized in that be used for the deionized water of preparation leacheate and standard solution, its resistivity should be more than the 18.2M Ω .cm.
3. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 1 is characterized in that the filler in the described separating column is the organic ion exchange resin.
4. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 3 is characterized in that the ion exchange resin in the described separating column has the physical arrangement of macropore or thin-shell type or porous surface stratotype.
5. the method that detects sodium ions content in the therrmodynamic system steam with chromatography of ions according to claim 4, it is characterized in that, ion exchange resin in the described separating column is skeleton with the SDEB styrene diethylenebenzene interpolymer, introduce sulfonic group at phenyl ring, form strongly acidic cation-exchange, perhaps introduce tertiary amine groups at phenyl ring and form quaternary amine type strong-base anion-exchange resin.
6. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 1 is characterized in that the adding of described sample adopts big volume sample quantitatively to encircle input mode.
7. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 6 is characterized in that described sample volume is the 0.5-3 milliliter.
8. the method with sodium ions content in the chromatography of ions detection therrmodynamic system steam according to claim 7 is characterized in that described sample volume is the 0.8-2 milliliter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109342638A (en) * | 2018-11-29 | 2019-02-15 | 浙江树人学院 | A method of detecting nitrile, quaternary ammonium salt and its impurity ammonium, potassium, calcium ion content in blocking using cation exchange inhibition conductance method |
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| US3926559A (en) * | 1973-08-06 | 1975-12-16 | Dow Chemical Co | Method and apparatus for quantitative chromatographic analysis of cationic species |
| US4101460A (en) * | 1973-10-02 | 1978-07-18 | The Dow Chemical Company | High performance ion exchange composition |
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| CN109342638A (en) * | 2018-11-29 | 2019-02-15 | 浙江树人学院 | A method of detecting nitrile, quaternary ammonium salt and its impurity ammonium, potassium, calcium ion content in blocking using cation exchange inhibition conductance method |
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Application publication date: 20131009 |