CN101509904B - Low-voltage ion chromatography for simultaneously analyzing silicates and phosphate in water sample - Google Patents
Low-voltage ion chromatography for simultaneously analyzing silicates and phosphate in water sample Download PDFInfo
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- CN101509904B CN101509904B CN2009100586604A CN200910058660A CN101509904B CN 101509904 B CN101509904 B CN 101509904B CN 2009100586604 A CN2009100586604 A CN 2009100586604A CN 200910058660 A CN200910058660 A CN 200910058660A CN 101509904 B CN101509904 B CN 101509904B
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Abstract
The invention relates to a low-pressure ion chromatography for simultaneously analyzing silicate and phosphate in a water sample. The working pressure of an analytical instrument is 2 to 3 multiplied by 10<5> Pa, and an analysis-detection fluid passage consists of an anion exchange column, a mixer, a reactor and an optical flow cell which are sequentially connected in series. The low-pressure ionchromatography comprises the following steps of: (1) mixing eluent E and colored solution R in the analysis and detection fluid passage, and generating a base line which is surveyed and drawn when the formed mixture enters the optical flow cell; and (2) in the analysis and detection fluid passage, adsorbing the silicate and phosphate contained in the sample by the anion exchange column, eluting and carrying the silicate and phosphate adsorbed by the anion exchange column to enter the mixer by the eluent E to be mixed with the colored solution R entering the analysis and detection fluid passage through a colored solution fluid passage. The formed mixture enters the reactor for continuous mixing and reacts to generate colored complex compound, and by the optical flow cell, and the solution containing the colored complex compound generates a spectrogram to be surveyed and drawn.
Description
Technical field
The invention belongs to water sample mesosilicic acid salt, phosphatic analytical approach, particularly a kind of silicate and phosphatic method analyzed simultaneously.
Background technology
Water sample mesosilicic acid salt, phosphatic analysis, prior art adopt the flow injection method to detect respectively usually, and promptly silicate, phosphate adopt different reagent systems respectively, and single job can only obtain water sample mesosilicic acid salt or phosphatic testing result.
Nobutake Nakatani etc. discloses and has a kind ofly analyzed river mesosilicic acid salt simultaneously and phosphatic method (is seen ANALYTICA CHIMICA ACTA 2008 by ion exclusion chromatography and post-column derivation, 619,110～114), though this method can obtain the testing result of silicate by single job, can obtain phosphatic testing result again, but owing to adopt ion exclusion chromatography (cation seperation column) also under high pressure to analyze, thereby the analysis cost height, instrument and equipment is complicated.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of while analysis water-like mesosilicic acid salt and phosphatic low-voltage ion chromatography are provided, adopt this kind method, not only just can obtain silicate and phosphatic testing result by single job, and the analysis cost reduction, simple to operation.
While analysis water-like mesosilicic acid salt of the present invention and phosphatic low-voltage ion chromatography are under low pressure operated, by in the analyzing and testing stream, anion-exchange column being set, the differential migration (affinity of phosphate and anion-exchange column is greater than the affinity of silicate and anion-exchange column) that utilizes silicate and phosphate to form with the different affinity of anion-exchange column realizes analyzing simultaneously (the spectrum peak of silicate is preceding, and phosphatic spectrum peak is in the back).
While analysis water-like mesosilicic acid salt of the present invention and phosphatic low-voltage ion chromatography use the analytical instrument that comprises sample flow path, eluent stream, colour developing liquid stream, sampling valve and analyzing and testing stream, and the working pressure of analytical instrument is 2～3 * 10
5Pa, described analyzing and testing stream is made up of the anion-exchange column that is connected in series successively, mixer, reactor and optical flow cell, may further comprise the steps:
(1) make eluent E enter the analyzing and testing stream through eluent stream, sampling valve, make colour developing liquid R enter the analyzing and testing stream through colour developing liquid stream, in the analyzing and testing stream, eluent E mixes with colour developing liquid R, and formed mixed liquor enters optical flow cell generation baseline and surveyed and drawn;
(2) under the promotion of eluent E, sample S enters the analyzing and testing stream through sample flow path, sampling valve, in the analyzing and testing stream, contained silicate of sample and phosphate are adsorbed by anion-exchange column, silicate that anion-exchange column is adsorbed and phosphate are by eluent E wash-out and carry and enter mixer and mix with the colour developing liquid R that enters the analyzing and testing stream through colour developing liquid stream, formed mixed liquor enters reactor and continues the living reaction generation of hybrid concurrency colored complex, and the solution that contains coloured complex compound produces spectrogram by optical flow cell and surveyed and drawn;
(3) use the known standard specimen of a series of silicate, phosphate concn to replace sample S successively, repeat above-mentioned steps (1) and (2), obtain a series of standard specimen spectrograms;
(4) spectrogram and the described a series of standard specimen spectrogram with described sample S compares, and calculates silicate, phosphate content among the described sample S.
In the said method, described eluent E is the NaCl aqueous solution, and described colour developing liquid R is sodium dodecylsulphonate-nitric acid-sodium molybdate aqueous solution.Among the described eluent E, the concentration of NaCl is 3g/L～7g/L.Among the described colour developing liquid R, the concentration of sodium dodecylsulphonate is 5 * 10
-4Mol/L～7 * 10
-4Mol/L, the concentration of nitric acid is 0.1mol/L～0.3mol/L, the concentration of sodium molybdate is 0.04mol/L～0.06mol/L.
In the said method, the light path of optical flow cell is 20mm～30mm, and the detection wavelength is 360nm～390nm.
The present invention has following beneficial effect:
1, adopts the method for the invention, use once cover instrument, a kind of reagent system, can obtain silicate and phosphatic testing result simultaneously, both can save analysis time, can reduce the configuration of analytical instrument and the use of analytical reagent again by single job.
2,, provide a kind of technical scheme of different designs, because operation under low pressure with respect to disclosed methods such as Nobutake Nakatani, institute uses instrument to be low-voltage instrument, compare with disclosed methods such as Nobutake Nakatani, apparatus structure is simpler, and analysis cost is lower.
3, the method for the invention is highly sensitive, SiO
3The detection limit of-Si can reach 0.02mg/L, PO
4The detection limit of-P can reach 0.03mg/L.
Description of drawings
Fig. 1 is the process chart of while analysis water-like mesosilicic acid salt of the present invention and phosphatic low-voltage ion chromatography, also is the structure diagram of supporting analytical instrument.
Fig. 2 is the spectrogram that adopts the method for the invention that standard specimen is analyzed;
Fig. 3 adopts the method for the invention that standard specimen is analyzed the working curve of drafting, wherein, and Fig. 3-the 1st, silicate working curve, Fig. 3-the 2nd, phosphate working curve.
Among the figure, 1-low-lift pump, 2-auto injection valve, 3-anion-exchange column, 4-mixer, 5-reactor, 6-optical flow cell, 7-fluorescence detector, 8-computer processing system, S-tested sample or standard specimen, E-eluent, R-colour developing liquid, W-waste liquid.
Embodiment
Below by embodiment while analysis water-like mesosilicic acid salt of the present invention and phosphatic low-voltage ion chromatography are described further.
Present embodiment carries out precision by the analysis of standard specimen to be measured, and step is as follows:
1, the preparation of silicate-phosphate standard specimen
(1) SiO
3The preparation of-Si standard specimen mother liquor
With Na
2SiF
6105 ℃ of oven dry 1 hour, place exsiccator to be cooled to room temperature then.Take by weighing oven dry and cooled Na
2SiF
61.0045g in the 500ml volumetric flask, add deionized water dissolving, constant volume, be mixed with SiO
3-Si concentration is that the mother liquor of 300mg/L keeps in Dark Place;
(2) PO
4The preparation of-P standard specimen mother liquor
110～115 ℃ of oven dry 1～2 hour, place exsiccator to be cooled to room temperature then potassium dihydrogen phosphate.Take by weighing oven dry and cooled potassium dihydrogen phosphate 1.318g and in the 1000ml volumetric flask, add deionized water dissolving, constant volume, preparation PO
4-P concentration is that the mother liquor of 300mg/L is standby;
(3) SiO that takes a morsel
3-Si standard specimen mother liquor and PO
4-P standard specimen mother liquor is diluted to deionized water and contains PO
4-P concentration 3.4mg/L, contain SiO
3The mixed standard solution of-Si 1.4mg/L.
2, the preparation of eluent E
Taking by weighing NaCl 3g adds deionized water and is mixed with the eluent E that NaCl concentration is 3g/L.
3, the preparation of colour developing liquid R
Take by weighing sodium molybdate 12.1g and put into the 1000ml volumetric flask, add deionized water 400ml, add sodium dodecylsulphonate 0.16g, dense HNO again
3(14mol/L) 14.3ml after the sodium molybdate dissolving, adds water to graticule, and the concentration that promptly is mixed with sodium dodecylsulphonate is 6 * 10
-4The concentration of mol/L, nitric acid is that the concentration of 0.2mol/L, sodium molybdate is the colour developing liquid of 0.05mol/L.
4, the testing and drawing of standard specimen spectrogram
Employing is tested by the low-voltage ion chromatograph of technical flow design shown in Figure 1, and the low-lift pump 1 in the instrument is a triple channel low pressure peristaltic pump, pump discharge 0.2～1.0ml/min, working pressure 2～3 * 10
5Pa.Optical flow cell 6 is the 28mm light path, and the detection wavelength is 390nm.Reactor 4 is the coiled structure, is that the polyfluortetraethylene pipe coiling of 0.5mm forms by internal diameter, and length is 4.5m; Mixer 4 is a three-port structure.Anion-exchange column 3 diameter of section φ 5mm, column length 30mm, column packing is the anion exchange resins that contains quaternary amine functional group.Described anion exchange resins can be bought commercial goods (model Dowexl, produced in USA), also can make by oneself, and its preparation method is seen " ion-exchange and polymeric adsorbent " (HeBing Lin, Huang Wenqiang chief editor, Science and Technology of Shanghai education publishing house, February nineteen ninety-five).
At first carry out the baseline mapping, open the power switch of instrument, under the driving of low-lift pump 1, eluent E enters the analyzing and testing stream through eluent stream, sampling valve 2, and detect anion-exchange column 3 in the stream by analysis and enter mixer 4 and mix with the colour developing liquid R that enters the mixer 4 in the analyzing and testing stream through colour developing liquid stream, formed mixed liquor enters optical flow cell 6, and fluorescence detector 7 is transferred to computer processing system 8 with signal and promptly draws a baseline on computer display.After the baseline mapping is finished, by low-lift pump 1 with standard specimen S through sample flow path, sampling valve 2 is sent into the analyzing and testing stream, standard specimen S enters the anion-exchange column 3 in the analyzing and testing stream under the promotion of eluent E, contained silicate and phosphate are adsorbed by anion-exchange column, silicate that anion-exchange column 3 is adsorbed and phosphate are by eluent E wash-out and carry and enter mixer 4 and mix with the colour developing liquid R that enters the analyzing and testing stream through colour developing liquid stream, formed mixed liquor enters reactor 5 and continues the living reaction generation of hybrid concurrency colored complex, the solution that contains coloured complex compound enters optical flow cell 6, fluorescence detector 7 is transferred to computer processing system 8 is promptly drawn tested standard specimen on computer display spectrogram with signal, as shown in Figure 2.As can be drawn from Figure 2: SiO
3The relative standard deviation of-Si is 3.11%, PO
4The relative standard deviation of-P is 1.33%, all satisfies and analyzes requirement.
Present embodiment is measured the working curve of standard specimen, and step is as follows:
1, the preparation of silicate-phosphate standard specimen
(1) SiO
3The preparation of-Si standard specimen mother liquor
SiO
3The preparation of-Si standard specimen mother liquor is identical with embodiment 1.
(2) PO
4The preparation of-P standard specimen mother liquor
PO
4The preparation of-P standard specimen mother liquor is identical with embodiment 1.
(3) SiO
3-Si and PO
4The preparation of-P standard specimen
Draw the SiO of few steps (1) preparation respectively
3The PO of-Si standard specimen mother liquor and step (2) preparation
4-P standard specimen mother liquor with the deionized water dilution, is mixed with following SiO
3-Si and PO
4-P series standard specimen:
PO
4-P0.120mg/L；SiO
3-Si?1.40mg/L、PO
4-P?0.250mg/L；SiO
3-Si?2.80mg/L、PO
4-P0.50mg/L；SiO
3-Si?4.20mg/L、PO
4-P?1.00mg/L；SiO
3-Si?5.50mg/L、PO
4-P?1.50mg/L；SiO
3-Si?5.60mg/L、PO
4-P?2.00mg/L；SiO
3-Si?8.40mg/L、PO
4-P?3.00mg/L；SiO
3-Si?11.20mg/L、PO
4-P?4.00mg/L。
2, the preparation of eluent E
Taking by weighing NaCl 7g adds deionized water and is mixed with the eluent E that NaCl concentration is 7g/L.
3, the preparation of colour developing liquid R
Take by weighing sodium molybdate 14.52g and put into the 1000ml volumetric flask, add deionized water 400ml, add sodium dodecylsulphonate 0.187g, dense HNO again
3(14mol/L) 21.5ml after the sodium molybdate dissolving, adds water to graticule, and the concentration that promptly is mixed with sodium dodecylsulphonate is 7 * 10
-4The concentration of mol/L, nitric acid is that the concentration of 0.3mol/L, sodium molybdate is the colour developing liquid of 0.06mol/L.
4, the testing and drawing of standard specimen spectrogram
With a series of silicate of step 1 preparation and phosphate standard specimen S with embodiment 1 described instrument, press embodiment 1 described method and operate, obtain a series of standard specimen spectrograms, see Fig. 3 according to the working curve that the standard specimen spectrogram is drawn, as can be seen from Figure 3: the linear relationship of the working curve that obtains is good.
Present embodiment is analyzed contained silicate and phosphate in the rivers water, and step is as follows:
1, the preparation of eluent E
Identical with embodiment 2.
2, the preparation of colour developing liquid R
Identical with embodiment 2.
3, the testing and drawing of sample spectrogram
With sample S with embodiment 1 described instrument, press embodiment 1 described method operation, acquisition sample spectrogram.
4, the sample testing result calculates
Spectrogram and the embodiment 2 a series of standard specimen spectrograms of described sample S are compared,, calculate silicate, phosphate content among the described sample S according to the working curve of embodiment 2.
Claims (2)
1. simultaneously analysis water-like mesosilicic acid salt and phosphatic low-voltage ion chromatography, it is characterized in that using the analytical instrument that comprises sample flow path, eluent stream, colour developing liquid stream, sampling valve and analyzing and testing stream, the working pressure of analytical instrument is 2～3 * 10
5Pa, described analyzing and testing stream is made up of the anion-exchange column that is connected in series successively, mixer, reactor and optical flow cell, said method comprising the steps of:
(1) make eluent E enter the analyzing and testing stream through eluent stream, sampling valve, make colour developing liquid R enter the analyzing and testing stream through colour developing liquid stream, eluent E mixes in the mixer of analyzing and testing stream with colour developing liquid R, and formed mixed liquor enters optical flow cell generation baseline and surveyed and drawn;
(2) under the promotion of eluent E, sample S enters the analyzing and testing stream through sample flow path, sampling valve, in the analyzing and testing stream, contained silicate of sample S and phosphate are adsorbed by anion-exchange column, silicate that anion-exchange column is adsorbed and phosphate are by eluent E wash-out and carry and enter mixer and mix with the colour developing liquid R that enters the analyzing and testing stream through colour developing liquid stream, formed mixed liquor enters reactor and continues the living reaction generation of hybrid concurrency colored complex, and the solution that contains coloured complex compound produces spectrogram by optical flow cell and surveyed and drawn;
(3) use the known standard specimen of a series of silicate, phosphate concn to replace sample S successively, repeat above-mentioned steps (1) and (2), obtain a series of standard specimen spectrograms;
(4) spectrogram and the described a series of standard specimen spectrogram with described sample S compares, and calculates silicate, phosphate content among the described sample S;
Described eluent E is the NaCl aqueous solution, and the concentration of NaCl is 3g/L～7g/L; Described colour developing liquid R is sodium dodecylsulphonate-nitric acid-sodium molybdate aqueous solution, and the concentration of sodium dodecylsulphonate is 5 * 10
-4Mol/L～7 * 10
-4Mol/L, the concentration of nitric acid is 0.1mol/L～0.3mol/L, the concentration of sodium molybdate is 0.04mol/L～0.06mol/L; The column packing of described anion-exchange column is the anion exchange resins that contains quaternary amine functional group.
2. while analysis water-like mesosilicic acid salt according to claim 1 and phosphatic low-voltage ion chromatography, the light path that it is characterized in that optical flow cell is 20mm～30mm, the detection wavelength is 360nm～390nm.
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| CN101813704A (en) * | 2010-04-08 | 2010-08-25 | 四川大学 | Automatic and quick measurement method and device of high-concentration silicate |
| CN102707005B (en) * | 2012-06-18 | 2014-11-26 | 四川大学 | Method for synchronously analyzing ferric iron and ferrous iron in water sample online |
| CN103983710A (en) * | 2014-05-19 | 2014-08-13 | 浙江大学 | Method for determining silicate and phosphate ions with ion chromatography post-column derivatization method |
| CN105911202B (en) * | 2016-04-22 | 2018-04-24 | 四川大学 | Low-voltage ion chromatograph based on three-way magnetic valve |
| CN106018637B (en) * | 2016-06-03 | 2018-06-05 | 四川大学 | Have both low pressure ion chromatography and the instrument and application method of low pressure Flow Injection Analysis |
| US11480526B2 (en) | 2020-01-21 | 2022-10-25 | Mettler-Toledo Thornton, Inc. | Instrument for sequential analysis for silica and phosphate in aqueous solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1945291A (en) * | 2006-10-25 | 2007-04-11 | 四川大学 | Method for analyzing phosphate in sea water and estuary water |
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| CN1945291A (en) * | 2006-10-25 | 2007-04-11 | 四川大学 | Method for analyzing phosphate in sea water and estuary water |
Non-Patent Citations (3)
| Title |
|---|
| JP昭60－61656A 1985.04.09 |
| Nobutake Nakatani,et al.Simultaneous spectrophotometric determination of phosphate and silicate ions in river water by using ion-exclusion chromatographic separation and post-column derivatization.《analytica chimica acta》.2008,第110－114页. * |
| Shengjie Hou,et al.Simultaneous determination of silicon and phosphorus in soil and plants by reversed-phase ion-pair chromatography.《Talanta》.2007,第178-182页. * |
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