CN104535669B - A kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam - Google Patents
A kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam Download PDFInfo
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- CN104535669B CN104535669B CN201410705239.9A CN201410705239A CN104535669B CN 104535669 B CN104535669 B CN 104535669B CN 201410705239 A CN201410705239 A CN 201410705239A CN 104535669 B CN104535669 B CN 104535669B
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- 150000001450 anions Chemical class 0.000 title claims abstract description 31
- 238000012360 testing method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- 150000002500 ions Chemical class 0.000 claims abstract description 37
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000010828 elution Methods 0.000 claims abstract description 11
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 9
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 230000001629 suppression Effects 0.000 claims abstract description 4
- 238000003556 assay Methods 0.000 abstract description 3
- 150000007524 organic acids Chemical class 0.000 abstract description 3
- 238000005374 membrane filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 238000001514 detection method Methods 0.000 description 12
- 238000000926 separation method Methods 0.000 description 11
- 238000011084 recovery Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000012086 standard solution Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 4
- 238000013459 approach Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 150000001449 anionic compounds Chemical class 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001412 inorganic anion Inorganic materials 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 1
- 238000005571 anion exchange chromatography Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 carboxylate anion Chemical class 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910001411 inorganic cation Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam, adopt capillary ion chromatography to measure the multiple trace anion in fired power generating unit steam, described trace anion is F
-, Cl
-, SO
4 2-, Br
-, NO
3 -, NO
2 -, PO
4 3-, CH
3cOO
-, HCOO
-and C
2o
4 2-, concrete steps are as follows: by water sample to be detected after 0.45 μm of membrane filtration, inject the sample introduction quantitative loop of ion chromatograph; Does is chromatography of ions testing conditions: anion analysis post IonPac? AS18? Capillary, guard column IonPac? AG18? Capillary, the column temperature of anion analysis post and guard column is 30 DEG C; Leacheate is KOH solution, gradient elution; The suppression electric current of rejector is 11mA, flow velocity: 0.010mL/min; Sampling volume: 10 μ L.Methods analyst speed of the present invention is fast, and testing result accurately and reliably, is suitable for trace inorganic negative ion and small molecular organic acid assay in fired power generating unit steam.
Description
Technical field
The present invention relates to a kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam, belong to ion chromatography technical field.
Background technology
Along with developing rapidly of power industry, generating plant high parameter, large sized unit are increasing, more and more higher to the requirement of Steam-water Quality in Water vapour images, analytical approach and means of testing are had higher requirement, adopts more high sensitivity, more high accuracy and analytical approach and monitoring technology become inevitable requirement faster.In power plant thermal system, inorganic anion and organic molecule carboxylate anion are main corrosivity negative ion, very large corrosive attack is had to heat power equipments such as steam turbines, its content of Accurate Determining will provide sufficient data reference for water quality purifying and equipment anticorrosion, and tool is of great significance.
Since chromatography of ions came out from 1975, as the important branch of high performance liquid chromatography, be one of technology of analytical chemistry field fast development, be the first-selected analytical approach of zwitterion compound always.Chromatography of ions plays an important role in generating plant water and steam quality control, becoming one of prefered method that in the high-purity steam of thermal power plant, inorganic anion and inorganic cation measure, become etching problem in research power plant thermal system and the powerful tool of process thereof and means, and be proposed as the analytical approach of trace anion in generating plant steam in 2005---" DL/T954-2005 fuel-burning power plant water-steam test method ".But conventional analysis type ion chromatogram eluate flow velocity is comparatively large, is difficult to accomplish operation of starting shooting continuously, and needs the sample size of larger volume, large batch of steam is detected limited.
In addition, fluorine ion, formate and acetate are three kinds of common trace anions in fired power generating unit steam, and the retention of these three kinds of negative ion is close, and existing detection method is difficult to realize being separated preferably it, easily causes the error of detection.
Summary of the invention
For above-mentioned prior art, the object of this invention is to provide a kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam.Adopt the chromatography of ions, exchange separating column IonPacAS18 with high-efficiency anion, under KOH gradient conditions, direct injected, quickly and accurately to the F in boiler of power plant steam sample
-, Cl
-, SO
4 2-, Br
-, NO
3 -, NO
2 -, PO
4 3-, CH
3cOO
-, HCOO
-, C
2o
4 2-measure Deng ten kinds of trace anions.What be continuously long-running and detect is reproducible, and realizes the good separation of fluorine ion, formate and acetate preferably.
For achieving the above object, the present invention adopts following technical proposals:
Can the method for multiple trace anion in Simultaneously test fired power generating unit steam, adopt capillary ion chromatography to measure the multiple trace anion in fired power generating unit steam, described trace anion is F
-, Cl
-, SO
4 2-, Br
-, NO
3 -, NO
2 -, PO
4 3-, CH
3cOO
-, HCOO
-and C
2o
4 2-, concrete steps are as follows:
Water sample to be detected is directly injected the sample introduction quantitative loop of ion chromatograph; Chromatography of ions testing conditions is: anion analysis post IonPacAS18Capillary (250 × 0.4mm), guard column IonPacAG18Capillary (50 × 0.4mm), and the column temperature of anion analysis post and guard column is 30 DEG C; Leacheate is KOH solution, gradient elution; The suppression electric current of rejector is 11mA, flow velocity: 0.010mL/min; Sampling volume: 10 μ L;
The program of described gradient elution is :-5 ~ 2min, and the concentration of leacheate KOH solution is 2mmol/L; 2 ~ 40min, the concentration of leacheate KOH solution is 2 ~ 30mmol/L; 40 ~ 42min, the concentration of leacheate KOH solution is 30 ~ 50mmol/L; 42 ~ 52min, the concentration of leacheate KOH solution is 50mmol/L.
Preferably, described leacheate adopts DionexEG leacheate generator to produce online, in conjunction with online negative ion acquisition equipment (CR-ATC), eliminates CO in air
2impact.
Beneficial effect of the present invention:
(1) the chromatographic column internal diameter that the present invention is used is only 0.4mm, and under identical sample size condition, sensitivity is 100 times of conventional ion chromatogram, and Monitoring lower-cut can be low to moderate ng/L, is highly suitable for the detection of components in unit steam.And capillary ion chromatography flow velocity is at about 0.010mL/min, greatly save the consumption of mobile phase, also the moment is in standby, equilibrium state to make instrument can keep operation continuously, there is high sample throughput, without the need to repeating production standard curve, easy to use, be very suitable for unit Water Vapor Quality in enormous quantities monitoring.
(2) the present invention adopts gradient elution, and the component single injected sampling surveyed just can ensure peak shape and degree of separation, component can be made again to go out peak at Best Times, and realize the good separation of fluorine ion, formate and acetate preferably.
(3) methods analyst speed of the present invention is fast, and testing result accurately and reliably, is suitable for trace inorganic negative ion and small molecular organic acid assay in fired power generating unit steam.
Accompanying drawing explanation
Fig. 1 is the chromatography of ions figure of mixed standard solution, wherein, and 1.F
-; 2.CH
3cOO
-; 3.HCOO
-; 4.Cl
-; 5.NO
2 -; 6.Br
-; 7.NO
3 -; 8.SO
4 2-; 9.C
2o
4 2-; 10.PO
4 3-; Ion concentration is 10 μ g/L;
Fig. 2 is the chromatography of ions figure of steam sample detection, wherein, and 1.F
-; 2.CH
3cOO
-; 3.HCOO
-; 4.Cl
-; 5.NO
2 -; 6.NO
3 -; 7.SO
4 2-; 8.C
2o
4 2-.
Embodiment
The present invention is further illustrated in conjunction with the embodiments, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1:
1. instrument and reagent
DionexICS-5000 type ion chromatograph is (containing degree pumps such as DP-5 capillary level; EG-KOH kapillary leacheate generator, kapillary electric conductivity detector, AS-AP automatic sampler); Chromeleon6.8 chromatographic work station (Dai An company of the U.S.); ACES-300 capillary suppressor, CRD200 kapillary carbon dioxide remover, IonPacAG18Capillary guard column (50 × 0.4mm; Dionex), IonPacAS18Capillary analytical column (250 × 0.4mm, Dionex).
Negative ion mixed standard solution (100mg/L) and each ion standard solution (1000mg/L) all purchased from American O2si companies, then be diluted to standard working solution with deionized water step by step.Certain power plant taken from by steam sample, and experimental water is the ultrapure water of resistivity 18.2M Ω cm.
2. chromatographic test strip piece optimization:
The selection of 2.1 chromatographic systems
The internal diameter of its chromatographic column of capillary type chromatography of ions is 0.4mm; leacheate flow velocity 0.010mL/min; year consumes leacheate only 5.26L; can continue not shut down work; remain balanced steady state; realize sample with to survey, save start equilibration time required in the past, and improve analysis result stability and repeatability.Detect very convenient for batch samples, be highly suitable for steam sample intermediate ion separation determination in enormous quantities.
Capillary chromatography column internal diameter (0.4mm) is 1/100 of conventional type ion chromatographic column (4mm), and under same sample size, tested ion signal response can improve 100 times.When system baseline noise is constant, capillary type ion chromatography system sample requirements is less, and detection limit is lower, and sensitivity is higher.Therefore, in fired power generating unit steam trace anion detection in adopt capillary type ion chromatography system.
The selection of 2.2 chromatographic columns
The inorganic anion surveyed due to the present invention and organic molecule all exist with anionic form in the basic conditions, and high performance anion exchange chromatography method should be adopted to be separated.Selection has certain hydrophobic alkanol quaternary ammonium hydrophilic chromatographic column IonPacAS18, can realize the good separation of fluorine ion, formate and acetate preferably.Meanwhile, because institute's measured ion is trace, high column capacity chromatographic column is needed to carry out large volume sample injection analysis.To sum up, be the detection of multiple trace anion in realization simultaneously fired power generating unit steam, the present invention selects IonPacAS18 high-efficient high-capacity three amount anion exchange analytical column.
The optimization of 2.3 leacheate Gradient program
KOH eluent ion is less than Na to Stationary liquid affinity
2cO
3and NaHCO
3, select KOH various ion can be made to reach better separation as leacheate.But because KOH easily absorbs CO in air
2, easily change the composition of leacheate, baseline wander is larger, and the present invention selects DionexEG leacheate generator to produce KOH online as leacheate, in conjunction with online negative ion acquisition equipment (CR-ATC), eliminates CO in air
2impact, baseline stability, noise is little, and method has good reappearance.CRD200 kapillary carbon dioxide remover is installed after capillary suppressor, before kapillary electric conductivity detector, the CO in leacheate background and sample can be removed further
3 2-, reduce noise, and improve and CO
3 2-the SO that retention is close
4 2-degree of separation, Be very effective.
When adopting degree drip washing mode such as grade, high concentration leacheate can cause weak retained fraction degree of separation to be deteriorated, and low eluent concentration drip washing can cause again disengaging time oversize, cannot meet actual separation requirement.Therefore, the mode of gradient elution should be adopted to the separation of components.Due to F
-, CH
3cOO
-retention close, be ensure both separating effect, the present invention is found after being summed up by great many of experiments: adopt low concentration 2mmol/L drip washing; Afterwards for accelerating the drip washing speed of the stronger ion of retention, adopt the drip washing gradient progressively raised; PO
4 3-retention is the strongest, should adopt high concentration drip washing, therefore eluent concentration be brought up to 50mmol/L, accelerates PO
4 3-drip washing speed.The condition of gradient elution optimized is :-5 ~ 2min, and the concentration of leacheate KOH solution is 2mmol/L; 2 ~ 40min, the concentration of leacheate KOH solution is 2 ~ 30mmol/L; 40 ~ 42min, the concentration of leacheate KOH solution is 30 ~ 50mmol/L; 42 ~ 52min, the concentration of leacheate KOH solution is 50mmol/L.(in condition of gradient elution, "-5 " refer to the pre-wash-out of leacheate 5 minutes with 2mmol/L)
To sum up, the chromatographic test strip part optimized is: anion analysis post IonPacAS18Capillary (250 × 0.4mm), guard column IonPacAG18Capillary (50 × 0.4mm), the column temperature of anion analysis post and guard column is 30 DEG C; Leacheate is KOH solution, gradient elution; The suppression electric current of rejector is 11mA, flow velocity: 0.010mL/min; Sampling volume: 10 μ L;
The program of gradient elution is :-5 ~ 2min, and the concentration of leacheate KOH solution is 2mmol/L; 2 ~ 40min, the concentration of leacheate KOH solution is 2 ~ 30mmol/L; 40 ~ 42min, the concentration of leacheate KOH solution is 30 ~ 50mmol/L; 42 ~ 52min, the concentration of leacheate KOH solution is 50mmol/L.
Under this chromatographic test strip part, survey component single injected sampling and both can ensure peak shape and degree of separation, component can be made again to go out peak at Best Times.The results are shown in Figure 1.
Embodiment 2:
1. linear relationship, the range of linearity and detection limit are investigated
The linear relationship of 10 kinds of anion concentrations that investigation the present invention detects and peak area.The hybrid standard product solution of preparation series concentration, adopts the chromatographic test strip part that embodiment 1 is optimized, each concentration determination 3 times, getting the mean value of its peak area, take peak area as ordinate, and titer mass concentration is horizontal ordinate, Criterion working curve, linear equation and related coefficient are in table 1.The wherein mass concentration (μ g/L) of y to be peak area (μ Smin), x be component, related coefficient all between 0.9990 ~ 0.9995, linearly better.The detection limit (S/N=3) of 10 kinds of negative ion is between 0.05 ~ 0.8 μ g/L.
Table 1 linear equation, related coefficient and detection limit
2. repeatability is investigated
Draw the negative ion mixed standard solution to be measured of appropriate 1.0 μ g/L, repeat sample introduction 7 times, the chromatographic test strip part adopting embodiment 1 to optimize detects, and record chromatogram, relative standard deviation is in table 2.The relative standard deviation scope of retention time is 0.03 ~ 0.17%, and the relative standard deviation scope of peak area is 1.23 ~ 5.38%, and the relative standard deviation scope 0.95 ~ 4.57% of peak height, the relative standard deviation scope of sample size, repeatability is all fine.
Table 2 repeated experiment result
After DionexICS-5000 type ion chromatograph runs 96 hours continuously, again carry out replica test.Draw the negative ion mixed standard solution to be measured of appropriate 1.0 μ g/L, repeat sample introduction 7 times, the results are shown in Table 3.The relative standard deviation of the relative standard deviation of retention time, the relative standard deviation of peak area, peak height is all in 0.03 ~ 5.81% scope.Visible, long-time continuous start does not affect the repeatability of experimental result.
Repeated experiment after table 3 runs 96 hours continuously
Embodiment 3:
Sample determination and recovery of standard addition experiment
Get three fired power generating unit steam samples, be numbered sample-1, sample-2 and sample-3 respectively, under the chromatographic test strip part that embodiment 1 is optimized, adopt external standard method to carry out quantitative test, the detection chromatogram of sample is shown in Fig. 2 (sample-3), the results are shown in Table 4.For the accuracy of the method for inspection, choose the recovery testu that 3 variable concentrations levels made by sample-1, the recovery is in table 5.Result shows, this method meets the requirement of water analysis.
Table 4 sample size testing result
Note: n.d represents and does not detect.
Table 5 determination of recovery rates result (n=6)
Note: n.d represents and does not detect.
After ion chromatograph runs 96 hours continuously, again carry out sample detection.Get certain unit fresh collection steam sample, make the recovery testu of 3 variable concentrations levels, the recovery is in table 6.The result of contrast table 5 and table 6 is visible, and long-time continuous start does not affect the repeatability of experimental result.
Determination of recovery rates result (n=6) after table 6 runs 96 hours
Note: n.d represents and does not detect.
To sum up, can find out, select capillary ion chromatography that instrument can be kept often to open and be in equilibrium state, improve the analysis efficiency of sample; Capillary ion chromatography obtain more high sensitivity time, required sample volume is less, saved sample cost and time consumption; Methods analyst speed is fast, and testing result accurately and reliably, is suitable for trace inorganic negative ion and small molecular organic acid assay in fired power generating unit steam.
Claims (3)
1. can the method for multiple trace anion in Simultaneously test fired power generating unit steam, it is characterized in that, adopt capillary ion chromatography to measure the multiple trace anion in fired power generating unit steam, described trace anion is F
-, Cl
-, SO
4 2-, Br
-, NO
3 -, NO
2 -, PO
4 3-, CH
3cOO
-, HCOO
-and C
2o
4 2-, concrete steps are as follows:
Water sample to be detected is directly injected the sample introduction quantitative loop of ion chromatograph; Chromatography of ions testing conditions is: anion analysis post IonPacAS18Capillary, guard column IonPacAG18Capillary, and the column temperature of anion analysis post and guard column is 30 DEG C; Leacheate is KOH solution, gradient elution; The suppression electric current of rejector is 11mA, flow velocity: 0.010mL/min; Sampling volume: 10 μ L;
The program of described gradient elution is :-5 ~ 2min, and the concentration of leacheate KOH solution is 2mmol/L; 2 ~ 40min, the concentration of leacheate KOH solution is 2 ~ 30mmol/L; 40 ~ 42min, the concentration of leacheate KOH solution is 30 ~ 50mmol/L; 42 ~ 52min, the concentration of leacheate KOH solution is 50mmol/L.
2. a kind of as claimed in claim 1 can the method for multiple trace anion in Simultaneously test fired power generating unit steam, it is characterized in that, described leacheate adopts DionexEG leacheate generator to produce online.
3. according to claim 1 a kind of can the method for multiple trace anion in Simultaneously test fired power generating unit steam, it is characterized in that, the internal diameter of anion analysis post IonPacAS18Capillary and guard column IonPacAG18Capillary is 0.4mm.
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