CN105136695A - OPA-NH4 <+> -SO3<2-> reaction-based sulfite ion spectroscopic measurement method and application - Google Patents
OPA-NH4 <+> -SO3<2-> reaction-based sulfite ion spectroscopic measurement method and application Download PDFInfo
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Abstract
The present invention discloses an OPA-NH4 <+> -SO3<2-> reaction-based sulfite ion spectroscopic measurement method which is as follows: an o-phthalaldehyde solution, an EDTA-NaOH buffer fluid and an ammonia nitrogen solution are successively added into a sulfite ion standard solution or a water sample, evenly shaken, placed at a certain temperature for reaction to equilibrium, and taken out and cooled to room temperature, spectrophotometer measuring wavelength is set for measuring solution absorbance A, the solution absorbance A is used as vertical coordinates, sulfite ion concentrations are used as x-coordinates for making a working curve; in a sample solution, sample solution absorbance As is measured according to the above method; and according to the working curve and the sample solution absorbance As, sulfite ion content in the sample solution can be quantified. The OPA-NH4 <+> -SO3<2-> reaction-based sulfite ion spectroscopic measurement method has the advantages of no need of use of toxic reagents, lower detection limits, higher sensitivity and the like.
Description
Technical field
The present invention relates to the mensuration of sulfite ion, be specifically related to a kind of based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction and application thereof.
Background technology
The method of current detection water sample sulfite radical ion mainly contains pararosaniline hydrochloridc spectrophotometric method and phenanthroline-Fe
3+spectrophotometric method.Hydrochloric para-rosaniline method measures process and uses more mercury salt, has certain potential hazard, be unsuitable for widely using to human and environment; Phenanthroline-Fe
3+method concentration limit is 0.052mg/L, and detectability is relatively high, and the sample lower for sulfite ion content is helpless.
Summary of the invention
The object of this invention is to provide a kind of based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction.The method is without the need to using toxic reagent, and detectability is lower, and sensitivity is higher, fast.
Realize the technical scheme of the object of the invention:
The present invention according to, when pH is greater than 11, sulfite ion in water sample can react with o-phthalaldehyde(OPA) (OPA) and ammonia nitrogen and generate aubergine material, the absorbance of this aubergine material is directly proportional to the concentration of sulfite ion under certain condition, based on this, establish the spectral photometry method of sulfite ion.
A kind of based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction, comprises the steps:
(1) in the sulfite ion standard solution within the scope of 25mL0.00-8.00mg/L, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, arranging spectrophotometric determination wavelength is 550nm, measures the absorbance A of solution; Take ion concentration of inferior sulfate radical as horizontal ordinate, absorbance A is ordinate drawing curve;
(2) in 25mL sample solution, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, the absorbance A that spectrophotometric determination wavelength is 550nm, working sample solution is set
s;
(3) according to the absorbance A of above-mentioned working curve and sample solution
s, the sulfite ion content in quantitative sample solution.
Applicant is based on OPA-NH
4 +-SO
3 2-reaction has utilized spectral photometry method to do and has measured the specific experiment of ion concentration of inferior sulfate radical, and obtains the optimum reaction condition of the method for the invention from these experiments.
One, instrument and reagent
Key instrument is BT124D analytical balance (Beijing Sai Duolisi instrument system company limited), electrothermal thermostat water bath (Shanghai He De experimental facilities company limited), UV-2550 ultraviolet-visible spectrophotometer (Japanese Shimadzu Corporation).
This research agents useful for same is analytical reagent if no special instructions, and pure water used is reverse osmosis water.Main agents solution has:
(1) 10.6g/L o-phthalaldehyde(OPA) solution: take 2.12g o-phthalaldehyde(OPA) solid, be dissolved in 70mL methanol solution (chromatographically pure), after it dissolves, then add 125mL ultrapure water, shake up sealing outsourcing masking foil stored refrigerated, obtain the o-phthalaldehyde(OPA) solution of 10.6g/L.
(2) Na
2sO
3standard reserving solution: take 0.50g anhydrous Na
2sO
3solid, is dissolved in 500mL ultrapure water, shakes up stored refrigerated.Its actual concentrations is demarcated by iodo-sodium thiosulfate titrimetry.
(3) 0.050g/LNa
2sO
3standard solution: by Na
2sO
3standard reserving solution dilution obtains.Use preparation on the same day.
(4) 20mmol/L ammonia nitrogen storing solution: accurately take 0.33g through (NH
4)
2sO
4, a small amount of water-soluble solution is also settled to 150mL, 4 DEG C of stored refrigerated.
(5) 5.0mmol/L ammonia nitrogen solution liquid: diluted by ammonia nitrogen storing solution and obtain.
(6) EDTA-NaOH damping fluid: take 26.0gEDTA solid and 6.0gNaOH solid, then adds 500mL ultrapure water and makes it dissolve completely.
(7) 0.10mol/LNaOH solution: take 1.0gNaOH solid, is dissolved in 250mL ultrapure water.Two, experimental technique
Pipette sulfite ion standard solution within the scope of 25mL0.00-8.00mg/L respectively (by 0.050g/LNa
2sO
3standard solution dilution configuration form) or sample solution in 50mL color comparison tube, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, 5.0mLEDTA-NaOH damping fluid, 3.0mL5.0mmol/L ammonia nitrogen solution, namely OPA consumption (this studies the amount that described consumption refers to the reagent that unit water sample or standard solution add) is 0.42g/L (obtaining divided by 25mL calculates with the quality adding reagent OPA), ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50, shake up reaction under being placed on certain temperature and extremely balance (equilibration time is relevant with temperature of reaction), take out, after being cooled to room temperature, arranging spectrophotometric determination wavelength is 550nm, measure the absorbance A of solution.
Three, the optimum reaction condition obtained from experiment
1, extinction spectrum curve
Pipette the sulfite ion standard solution 25mL of 3.0mg/L, add reagent by above-mentioned experimental technique, after question response balance, measure the absorption spectrum of this reactant liquor in visible region with ultraviolet-visible spectrophotometer, result as shown in Figure 1.Fig. 1 shows, reaction solution has absorption maximum platform in 540-560nm scope, and therefore, following experimental selection 550nm is for measuring wavelength.
2, the determination of reagent dosage
Based on OPA-NH
4 +-SO
3 2-reaction assay sulfite ion main agents used is OPA and ammonia nitrogen solution, and wherein, the concentration of OPA and ammonia nitrogen solution can affect the completeness of this reaction, and then affects the absorbance of reactant liquor.For this reason, with the sulfite ion standard solution of 25mL6.0mg/L for investigating object, with single_factor method, investigate the consumption of OPA and ammonia nitrogen to the impact of reactant liquor absorbance.
The determination of OPA consumption
Fix other reagent dosages as described in experimental technique, in the scope of 0-0.42g/L, investigate the impact of OPA consumption on reactant liquor absorbance, result as shown in Figure 2.Fig. 2 shows, along with the increase of OPA concentration, reactant liquor absorbance presents first to be increased fast, the trend then tended towards stability gradually.Specifically, when OPA consumption is increased to 0.085g/L from 0, reactant liquor absorbance presents quick increase trend; When being increased to 0.21g/L from 0.085, absorbance increases trend and eases up; Within the scope of 0.21-0.42g/L, absorbance is tending towards constant.Illustrate, when OPA consumption is at 0.21-0.42g/L, the amount of OPA enough meets the demand of reaction, and does not affect the process of reaction.Visible, the better usable range of OPA is 0.21-0.42g/L.Following experiment control OPA consumption is 0.42g/L, namely adds 10.6g/LOPA solution 1mL in 25mL liquid to be measured.
The determination of ammonia nitrogen consumption
Fix other reagent dosages as described in experimental technique, adopt single_factor method within the scope of 0-0.80mmoL/L, investigate the impact of ammonia nitrogen consumption on reactant liquor absorbance, result as shown in Figure 3.Fig. 3 shows, along with the increase of ammonia nitrogen consumption, absorbance presents the trend first increasing and tend towards stability afterwards, when ammonia nitrogen consumption changes within the scope of 0.60-0.80mmoL/L, absorbance is tending towards constant, namely, within the scope of this, ammonia nitrogen consumption fully can meet the demand of reaction, and does not affect the process of reaction.Illustrate, the better usable range of ammonia nitrogen is 0.60-0.80mmoL/L, and following experiment control ammonia nitrogen consumption is 0.60mmoL/L, namely adds 5.0mmol/L ammonia nitrogen solution 3.0mL in 25mL liquid to be measured.
3, the impact of pH
Experiment finds, OPA-NH
4 +-SO
3 2-the reaction product color of system is relevant with reactant liquor pH, for this reason, with the inferior sulfate radical standard solution of 6.0mg/L for investigating object, empirically adding OPA consumption and ammonia nitrogen consumption described in method, regulating the pH of reactant liquor by changing 0.1mol/LNaOH solution usage.When reactant liquor pH is in 9.15-13.07 range, OPA-NH
4 +-SO
3 2-the color of the reaction product of system lists in table 1.Table 1 shows, when pH is within the scope of 9.15-10.85, reaction product is yellow; When pH changes within the scope of 11.20-12.85, reaction product is aubergine complex compound.This method generates aubergine complex compound based on reaction and sets up, and therefore, investigate pH further within the scope of 11.20-12.85, the relation of absorbance and pH, result as shown in Figure 4.As shown in Figure 4, within the scope of the pH investigated, increase with pH, absorbance presents slow increase trend, and visible pH is one of key factor affecting reactant liquor absorbance.Generally make pH value of solution be stabilized in certain limit by adding buffer solution, consider the control of absorbance and pH value of solution, the pH of following experiment control reactant liquor is 11.50.By repeatedly testing, when to add prepared EDTA-NaOH damping fluid in 25mL inferior sulfate radical standard solution or the actual water sample such as river, underground water be 5.0mL, the pH of Absorbable organic halogens reactant liquor is about 11.50.
The color of reaction product under table 1 condition of different pH
4, the determination of reacting balance time
Usually, temperature of reaction can affect reaction rate.In order to determine the equilibration time at differential responses temperature, with the sulfite ion standard solution of 6.0mg/L for object, empirically described in method, add reagent, under different temperature conditions, investigate the variation tendency of absorbance along with the reaction time, thus determine reacting balance time.Under having investigated 15 DEG C, 23 DEG C, 26 DEG C, 30 DEG C, 35 DEG C, 40 DEG C and 45 DEG C of 7 temperature respectively, absorbance is along with the variation tendency in reaction time, the results are shown in Figure 5-Figure 11.Result shows, regardless of at what temperature, reactant liquor absorbance, along with the prolongation in reaction time, presents the trend first increasing and be tending towards constant afterwards.Fig. 5 shows, when temperature of reaction is 15 DEG C, the reaction time, absorbance tended towards stability more than after 150min, and reaction reaches equilibrium state substantially; Fig. 6 shows, when temperature of reaction is 23 DEG C, when the reaction time is more than 80min, absorbance is tending towards constant, and reaction reaches equilibrium state, can at least stablize to 150min; Fig. 7 shows, at 26 DEG C, time when reacted more than 60min, reaction reach balance, but when reacted between more than after 100min, absorbance presents slow downtrending, illustrates react between 60min to 100min, keep steady state (SS), Absorbable organic halogens 40min; Fig. 8 shows, at 30 DEG C, reacting balance time is 50min, reacts and keep equilibrium state within the scope of 50min to 90min, i.e. the sustainable 40min of equilibrium state; Fig. 9 shows, at 35 DEG C, the equilibration time of reaction is 30min, Absorbable organic halogens to 60min, the sustainable 30min of equilibrium state; Figure 10 shows, at 40 DEG C, it is 25min that reaction reaches equilibration time, and may persist to 50min, equilibrium state can keep 25min; Figure 11 shows, at 45 DEG C, the equilibration time of reaction is 15min, and Absorbable organic halogens, to 30min, can keep 15min.Visible, along with the increase of temperature of reaction, reaction reaches balance required time and shortens gradually, and meanwhile, also there is shortening trend the balance retention time.Reach at each temperature balance required time and balance the duration list in table 2.
Start time and end time is reacted at table 2 differential responses temperature
Four, working curve and detectability
Under selected top condition, sulfite ion standard serial solution within the scope of preparation finite concentration, empirically adds reagent described in method, and reaction is to balance at a certain temperature, measure absorbance, investigate the relation (working curve) of absorbance and reaction density.Result shows, at 40 DEG C, when within the scope of ion concentration of inferior sulfate radical 0.00-8.00mg/L, working curve presents linear relationship, and as shown in figure 12, linear equation is A=0.103C+0.021 (n=7, R
2=0.9983), in equation, A is absorbance, and C is the concentration of sulfite ion, and unit is mg/L.Different time, the minor differences of environment residing for environmental baseline and instrument, can cause the measurement result of working curve variant, therefore, when measuring unknown sample, answers Simultaneously test working curve.
Detectability refers to that a certain analytical approach can detect Cmin or the minimum of test substance in the given degree of reliability from sample.Configure 7 parts of blank samples, empirically method adds reagent, and reaction is to balance, measure absorbance, result is 0.005 ± 0.00108 (n=7), calculates detectability with 3*SD/ working curve slope, the same day, working curve was A=0.124C+0.022 (n=7, R
2=0.9966), therefore, detectability result of calculation is 0.026mg/L.
Five, substrate recovery of standard addition
The substrate recovery of standard addition of water sample:
Respectively with river (taking from city flower river, Guilin), underground water (taking from Guilin Electronic Science and Technology Univ. Hua Jiang school district), mountain spring water (taking from Yao's mountain breeze scenic spot, Guilin City) for substrate, the spiked levels of sulfite ion is 0,0.250,0.500,1.00,2.00,4.00 and 6.00mg/L, measure substrate mark-on curve; The working curve on Simultaneously test same day.With substrate mark-on rate of curve divided by the same day working curve slope calculate average substrate recovery of standard addition, result is as shown in table 3.Table 3 shows, the substrate recovery of standard addition of river, underground water and mountain spring water is respectively 99.4%, 104.3% and 102.9%, illustrate that river, underground water and mountain spring water substrate are noiseless to mensuration, the method that this research is set up is suitable for measuring the fresh water water samples such as river, underground water and mountain spring water.
The substrate mark-on curve of table 3 different base and substrate recovery of standard addition
The substrate recovery of standard addition of white granulated sugar water sample:
The white granulated sugar water sample of configuration 4.0% (w/v).With this white granulated sugar water sample for substrate, measure substrate recovery of standard addition by concentration mark-on listed by table 4.Table 4 shows, white granulated sugar water sample two substrate recovery of standard addition mean values of 4.0% (w/v) are respectively 107.4% and 100.2%, illustrates that the white granulated sugar water sample of 4.0% (w/v) is noiseless to mensuration.Namely this studies the content that described method is applicable to measuring white granulated sugar water sample sulfite radical ion
Table 4 white granulated sugar water sample substrate recovery of standard addition
Above-mentioned experiment shows, OPA-NH
4 +-SO
3 2-reaction can generate mauve material, and this material has absorption maximum platform at 540-560nm.Based on this, establish the spectral photometry new method being applicable to measuring river, underground water, mountain spring water and white granulated sugar water sample sulfite radical ion.The range of linearity of the method is 0.00-8.00mg/L, and method detects and is limited to 0.026mg/L.The substrate recovery of standard addition of water sample is between 99.4% ~ 107.4%.With existing method phenanthroline-Fe
3+spectrophotometric method is compared, measurement result there was no significant difference.When temperature of reaction is more than 35 DEG C, reaction reaches balance required time and is less than 30min.The present invention is successfully applied to the mensuration of river sample sulfite radical ion, and result and phenanthroline-Fe
3+the measurement result there was no significant difference of spectrophotometric method.Relative to the spectral photometry method of existing sulfite ion, the method that this research is set up is without the need to using the reaction reagents such as mercury salt that toxicity is very strong, and the advantage such as it is lower to have detectability, and sensitivity is higher, quick.
Accompanying drawing explanation
The abosrption spectrogram of Fig. 1 sulfite ion and OPA, ammonia nitrogen reaction product;
Fig. 2 is the effect diagram of OPA consumption to reactant liquor absorbance;
Fig. 3 is the effect diagram of ammonia nitrogen consumption to reactant liquor absorbance;
Fig. 4 is the effect diagram of pH to reactant liquor absorbance;
Fig. 5 is temperature of reaction when being 15 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Fig. 6 is temperature of reaction when being 23 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Fig. 7 is temperature of reaction when being 26 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Fig. 8 is temperature of reaction when being 30 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Fig. 9 is temperature of reaction when being 35 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Figure 10 is temperature of reaction when being 40 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Figure 11 is temperature of reaction when being 45 DEG C, and reactant liquor absorbance is with the changing trend diagram in reaction time;
Figure 12 is the working curve diagram of absorbance and inferior sulfate radical reaction density.
Embodiment
A kind of based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction, comprises the steps:
(1) in the sulfite ion standard solution within the scope of 25mL0.00-8.00mg/L, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, arranging spectrophotometric determination wavelength is 550nm, measures the absorbance A of solution; Take ion concentration of inferior sulfate radical as horizontal ordinate, absorbance A is ordinate drawing curve;
(2) in 25mL sample solution, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, the absorbance A that spectrophotometric determination wavelength is 550nm, working sample solution is set
s;
(3) according to the absorbance A of above-mentioned working curve and sample solution
s, the sulfite ion content in quantitative sample solution.
Under selected top condition, the sulfite ion standard serial solution within the scope of preparation finite concentration, empirically adds reagent described in method, and reaction is to balance at a certain temperature, measures absorbance, investigates the working curve of absorbance and reaction density.Result shows, at 40 DEG C, when within the scope of ion concentration of inferior sulfate radical 0.00-8.00mg/L, working curve presents linear relationship, and as shown in figure 12, linear equation is A=0.103C+0.021 (n=7, R
2=0.9983), in equation, A is absorbance, and C is the concentration of sulfite ion, and unit is mg/L.Different time, the minor differences of environment residing for environmental baseline and instrument, can cause the measurement result of working curve variant, therefore, when measuring unknown sample, answers Simultaneously test working curve.Detectability refers to that a certain analytical approach can detect Cmin or the minimum of test substance in the given degree of reliability from sample.Configure 7 parts of blank samples, empirically method adds reagent, and reaction is to balance, measure absorbance, result is 0.005 ± 0.00108 (n=7), calculates detectability with 3*SD/ working curve slope, the same day, working curve was A=0.124C+0.022 (n=7, R
2=0.9966), therefore, detectability result of calculation is 0.026mg/L.Adopt this research method for building up to measure the content of the sulfite ion in two river samples, meanwhile, adopt phenanthroline-Fe
3+spectrophotometric method measures water sample, and carry out result comparison, data list in table 5.This is studied the result that described method records two river samples and is respectively 3.76 ± 0.046 (n=4) and 6.65 ± 0.17 (n=4) mg/L.Check the measurement result difference of two kinds of methods with t method of inspection, the statistic t calculated value of two sample determination results is all less than critical value when degree of confidence is 95%, therefore this law and existing phenanthroline-Fe
3+the result of water by Spectrophotometry sample sulfite radical ion is without work difference.Illustrate, the method that this research is set up successfully can measure actual water sample sulfite radical ion content, and measurement result is reliable.
Table 5 this law and phenanthroline-Fe
3+the comparison of spectrophotometric method
Claims (5)
1. one kind based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction, is characterized in that, comprise the steps:
(1) in the sulfite ion standard solution within the scope of 25mL0.00-8.00mg/L, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, spectrophotometric determination wavelength is set, measures the absorbance A of solution; Take ion concentration of inferior sulfate radical as horizontal ordinate, absorbance A is ordinate drawing curve;
(2) in sample solution, add 1.0mL10.6g/L o-phthalaldehyde(OPA) solution successively, the EDTA-NaOH damping fluid 5.0mL of EDTA concentration to be 52.0g/L and NaOH concentration be 12.0g/L, 3.0mL5.0mmol/L ammonia nitrogen solution, namely, OPA consumption is 0.42g/L, and ammonia nitrogen consumption is 0.60mmol/L, pH is 11.50; Shake up; Under being placed in certain temperature, reaction is to balance; After taking-up is cooled to room temperature, spectrophotometric determination wavelength is set, the absorbance A of working sample solution
s;
(3) according to the absorbance A of above-mentioned working curve and sample solution
s, the sulfite ion content in quantitative sample solution.
2. method according to claim 1, is characterized in that, the spectrophotometric determination wavelength of described setting is 550nm.
3. method according to claim 1, is characterized in that, the working curve of absorbance and reaction density is 40 DEG C time, and the range of linearity of working curve is 0.00-8.00mg/L.
4. method according to claim 1, is characterized in that, the detection of method of the present invention is limited to 0.026mg/L.
5. one kind based on OPA-NH
4 +-SO
3 2-the spectral photometry method of the sulfite ion of reaction is measuring the application in river, underground water, mountain spring water or white sugar water.
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| CN107091823A (en) * | 2016-02-18 | 2017-08-25 | 常州罗盘星检测科技有限公司 | A kind of low-concentration ammonia-nitrogen fluoroscopic examination solid reagent and its detection method |
| CN107356562A (en) * | 2017-08-16 | 2017-11-17 | 广西师范大学 | One kind tetraphenylboron sodium part regulation and control Nano Silver catalytically active surface plasmon absorption spectroscopic assay NH4+Method |
| CN107478734A (en) * | 2017-06-29 | 2017-12-15 | 河北工业大学 | The chromatography of ions detection method of sulfate radical and inferior sulfate radical is determined in a kind of desulfurization seawater simultaneously |
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