CN102830117A - Device and method for carrying out continuous flow detection on bicarbonates in water - Google Patents
Device and method for carrying out continuous flow detection on bicarbonates in water Download PDFInfo
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- CN102830117A CN102830117A CN2012103499718A CN201210349971A CN102830117A CN 102830117 A CN102830117 A CN 102830117A CN 2012103499718 A CN2012103499718 A CN 2012103499718A CN 201210349971 A CN201210349971 A CN 201210349971A CN 102830117 A CN102830117 A CN 102830117A
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Abstract
The invention discloses a device and a method for carrying out continuous flow detection on bicarbonates in water. The method comprises the following steps of: firstly, introducing a standard sample or a water sample to be detected at a lower flow velocity, and mixing and reacting the standard sample or the water sample to be detected with a sulfuric acid solution at a constant flow velocity; secondly, mixing and reacting the reacted solution with a developing agent at a certain temperature at a non-constant flow velocity; and finally, under the pushing of a peristaltic pump, carrying out continuous flow type sampling on the solution obtained after reaction, and injecting into a spectrophotometer to detect. With the adoption of the device and the method provided by the invention, the flow velocities and the sampling times of the standard sample or the water sample to be detected and the developing agent can be respectively adjusted, so that the standard sample or the water sample to be detected and the developing agent are sufficiently mixed, and therefore, bicarbonates in the standard sample or the water sample to be detected entirely participate in the reaction within short time, so that the sample amount is reduced, the time of detecting bicarbonates in the water is shortened, and meanwhile, the sensitivity of detecting bicarbonates in the water is improved.
Description
Technical field
The present invention relates to by means of the chemistry of measuring material or physical property is tested or the device and method of amalyzing substances, specifically, relate to the pick-up unit and the detection method of hydrocarbonate in the chemical analysis field.
Background technology
For hydrocarbonate Determination on content in natural water and the untainted surface water help to judge water quality kind, understand its source, excessive hydrocarbonate can destroy rock, concrete structure.Hydrocarbonate in the irrigation water is an important evidence of confirming whether this water is suitable for irrigating.Being usually used in estimating the surge capability and the metal dissolubility and the toxicity therein of water body for the hydrocarbonate in waste water, the sewage, is the judgement property index to processing procedure control.The existence of hydrocarbonate can influence the desalination performance of electro-adhesion device in the desalination field, and its content is an important indicator of decision electro-adhesion device operation stability.Therefore, the hydrocarbonate in the water body is measured important Practical significance is arranged.
The method that hydrocarbonate detects comprises chemical titration, potentiometric titration, non-inhibition type anion-exchange chromatography, inhibition type anion-exchange chromatography, non-inhibition type ion-exclusion chromatography etc.Wherein, chemical titration and potentiometric titration, bigger to the demand of sample, once measure the minimum 50ml of needs, and titration end-point is difficult for judging that accurately other acid-base materials that exist in the water are understood influential to the result, so practical operation gets up to have difficulties.Non-inhibition type anion-exchange chromatography technical difficulty is big, and higher to operator's competency profiling, complex operation not too is beneficial to popularization.Inhibition type anion-exchange chromatography and non-inhibition type ion-exclusion chromatography Chang Yinwei and weak acid anion such as F-, formic acid, acetate etc. altogether drip washing causes qualitative, quantitative comparison is difficult.
Summary of the invention
What the present invention will solve is above-mentioned technical matters of the prior art; Hydrocarbonate continuous flow pick-up unit and detection method in a kind of water are provided; This device and method is sensitive, accurate, easy, quick, environmental friendliness, is suitable for the detection of hydrocarbonate such as surface water, underground water and waste water.
In order to solve the problems of the technologies described above, the present invention is achieved through following technical scheme:
Hydrocarbonate continuous flow pick-up unit in a kind of water; Comprise sample flow path; Sample flow path be connected in primary heater after the sulfuric acid stream is parallelly connected, connect with secondary heater after said primary heater and the parallel connection of developer stream, said secondary heater is connected in spectrophotometer.
Hydrocarbonate continuous flow detection method in a kind of water, this method is carried out according to following steps:
A. prepare standard specimen;
The preparation sulfuric acid solution: the dose volume mark is 1% ~ 5% sulfuric acid solution;
The preparation developer: in 1L distilled water, dissolve 0.4 ~ 0.9g sodium carbonate, the soda mint of 0.2 ~ 0.6g, and the adding massfraction is phenolphthalein ethanolic solution 0.5 ~ 4.0ml of 1%;
B. standard specimen or water sample to be measured mix with the online uniform flow of sulfuric acid solution, and under the promotion of peristaltic pump, pass through 30 ~ 60 ℃ primary heater; The flow velocity of standard specimen or water sample to be measured, sulfuric acid solution is 0.5 ~ 2.0ml min
-1
C. the developer that step (a) is prepared is introduced with the flow velocity that is higher than standard specimen or water sample to be measured, mix with the online not uniform flow of mixed liquor after step (b) is handled, and the secondary heater through 30 ~ 80 ℃ reacts under the promotion of peristaltic pump; The flow velocity of developer is 0.8 ~ 3.0ml min
-1
D. through peristaltic pump step (c) reaction back solution is carried out continuous streaming sample introduction, the injection spectrophotometer detects with the detection wavelength of 400 ~ 600nm.
The volume fraction of preparation sulfuric acid solution is 1.5% in the said step (a).
When preparing developer in the said step (a), the adding quality of sodium carbonate is 0.6g, and the adding quality of soda mint is 0.5g, and the addition of phenolphthalein ethanolic solution is 2.5ml;
The sample injection time of standard specimen or water sample to be measured is 50 ~ 150s in the said step (b), and the sample injection time of sulfuric acid solution is 70 ~ 200s, and the temperature of primary heater is 35 ℃.
The sample injection time of the developer in the said step (c) is 70 ~ 200s, and the temperature of secondary heater is 45 ℃.
It is 550nm that spectrophotometer in the said step (d) detects wavelength.
The invention has the beneficial effects as follows:
(1) the present invention is through regulating the flow velocity and the sample injection time of standard specimen or water sample to be measured, developer respectively; Promptly reduce the flow velocity of standard specimen or water sample to be measured and shorten sample injection time; Improve the flow velocity of developer and prolong sample injection time, standard specimen or water sample to be measured are fully mixed with developer, thereby the hydrocarbonate in interior standard specimen of assurance short time or the water sample to be measured is participated in reaction fully; Reduced amount of samples; Shorten the time that hydrocarbonate detects in the water, simultaneously, improved the sensitivity that hydrocarbonate detects in the water.
(2) the whole apparatus structure that adopts of the present invention is simple, and the stream failure rate is very low, and the consumption of sample and reagent significantly reduces, and can be widely used in the analysis and the on-line monitoring of hydrocarbonate such as surface water, underground water and waste water.
Description of drawings
Accompanying drawing is the structural representation of pick-up unit provided by the present invention.
Among the figure: 1, sample flow path; 2, the sulfuric acid stream; 3, primary heater; 4, the developer stream; 5, secondary heater; 6, spectrophotometer.
Embodiment
Shown in accompanying drawing, pick-up unit of the present invention specifically is formed by connecting in sample flow path 1, sulfuric acid stream 2, primary heater 3, developer stream 4, secondary heater 5 and spectrophotometer 6.Wherein, sample flow path 1 and sulfuric acid stream 2 parallelly connected backs are through primary heaters 3, after primary heater 3 and developer stream 4 are parallelly connected, connect with secondary heater 5, and said secondary heater 5 is connected in series in spectrophotometer 6.
Embodiment 1
1, the preparation of hydrocarbonate mark liquid: dissolving 10.00g soda mint is settled to 1L with distilled water, mixing in 800ml distilled water.Solution is mixed with mass concentration successively and is respectively 100mg L thus
-1, 80mg L
-1, 60mg L
-1, 40mg L
-1, 20mg L
-1, 10mg L
-1, 5mg L
-1The hydrocarbonate standard solution, be settled to 100ml.
The preparation sulfuric acid solution: the dose volume mark is 1% sulfuric acid solution;
The preparation developer: dissolving 0.4g sodium carbonate in 1L distilled water, the soda mint of 0.2g, and the adding massfraction is 1% phenolphthalein ethanolic solution 0.5ml;
2, with standard specimen or water sample to be measured with 0.5ml min
-1Flow velocity introduce through sample flow path 1, sample introduction 50s is that 1% sulfuric acid solution sample introduction 70s uniform flow mixes with volume fraction, then under the promotion of peristaltic pump through 30 ℃ primary heater 3, react the generation carbon dioxide.
3, the flow velocity of control developer stream is 0.8ml min
-1, sample introduction 100s makes standard specimen or water sample to be measured after the processing mix with the online variable speed of developer, under the promotion of peristaltic pump, gets in the secondary heater 5, under 30 ℃ of conditions, reacts.
4, under the promotion of peristaltic pump, reacted solution is carried out continuous streaming sample introduction, the flow cell of injection spectrophotometer 6 detects with the detection wavelength of 400nm, and waste liquid is discharged.
After detect accomplishing, be that horizontal ordinate, peak area are ordinate drawing standard curve, obtain the typical curve regression equation with the mass concentration of hydrocarbonate series standard solution; According to the peak area of hydrocarbonate in the water sample to be measured, utilize gained typical curve regression equation, calculate the mass concentration of hydrocarbonate in the water sample to be analyzed.
The analytical characteristic amount of hydrocarbonate is following: the range of linearity 0.18 ~ 100mg L of hydrocarbonate
-1, detect and be limited to 0.037mg L
-1, relative standard deviation is 1.3 ~ 3.9%.
1, the preparation of hydrocarbonate mark liquid: dissolving 10.00g soda mint is settled to 1L with distilled water, mixing in 800ml distilled water.Solution is mixed with mass concentration successively and is respectively 100mg L thus
-1, 80mg L
-1, 60mg L
-1, 40mg L
-1, 20mg L
-1, 10mg L
-1, 5mg L
-1The hydrocarbonate standard solution, be settled to 100ml.
The preparation sulfuric acid solution: the dose volume mark is 1.5% sulfuric acid solution;
The preparation developer: dissolving 0.6g sodium carbonate in 1L distilled water, the soda mint of 0.5g, and the adding massfraction is 1% phenolphthalein ethanolic solution 2.5ml;
2, with standard specimen or water sample to be measured with 1.2ml min
-1Flow velocity introduce through sample flow path 1, sample introduction 100s is that 1.5% sulfuric acid solution sample introduction 150s uniform flow mixes with volume fraction, then under the promotion of peristaltic pump through 35 ℃ primary heater 3, react the generation carbon dioxide.
3, the flow velocity of control developer stream is 2.0ml min
-1, sample introduction 150s makes standard specimen or water sample to be measured after the processing mix with the online variable speed of developer, under the promotion of peristaltic pump, gets in the secondary heater 5, under 45 ℃ of conditions, reacts.
4, under the promotion of peristaltic pump, reacted solution is carried out continuous streaming sample introduction, the flow cell of injection spectrophotometer 6 detects with the detection wavelength of 550nm, and waste liquid is discharged.
After detect accomplishing, be that horizontal ordinate, peak area are ordinate drawing standard curve, obtain the typical curve regression equation with the mass concentration of hydrocarbonate series standard solution; According to the peak area of hydrocarbonate in the water sample to be measured, utilize gained typical curve regression equation, calculate the mass concentration of hydrocarbonate in the water sample to be analyzed.
The analytical characteristic amount of hydrocarbonate is following: the range of linearity 0.15 ~ 100mg L of hydrocarbonate
-1, detect and be limited to 0.023mg L
-1, relative standard deviation is 0.8 ~ 2.2%.
1, the preparation of hydrocarbonate mark liquid: dissolving 10.00g soda mint is settled to 1L with distilled water, mixing in 800ml distilled water.Solution is mixed with mass concentration successively and is respectively 100mg L thus
-1, 80mg L
-1, 60mg L
-1, 40mg L
-1, 20mg L
-1, 10mg L
-1, 5mg L
-1The hydrocarbonate standard solution, be settled to 100ml.
The preparation sulfuric acid solution: the dose volume mark is 5% sulfuric acid solution;
The preparation developer: dissolving 0.9g sodium carbonate in 1L distilled water, the soda mint of 0.6g, and the adding massfraction is 1% phenolphthalein ethanolic solution 4.0ml;
2, with standard specimen or water sample to be measured with 2.0ml min
-1Flow velocity introduce through sample flow path 1, sample introduction 150s is that 5% sulfuric acid solution sample introduction 200s uniform flow mixes with volume fraction, then under the promotion of peristaltic pump through 60 ℃ primary heater 3, react the generation carbon dioxide.
3, the flow velocity of control developer stream is 3.0ml min
-1, sample introduction 200s makes standard specimen or water sample to be measured after the processing mix with the online variable speed of developer, under the promotion of peristaltic pump, gets in the secondary heater 5, under 80 ℃ of conditions, reacts.
4, under the promotion of peristaltic pump, reacted solution is carried out continuous streaming sample introduction, the flow cell of injection spectrophotometer 6 detects with the detection wavelength of 600nm, and waste liquid is discharged.
After detect accomplishing, be that horizontal ordinate, peak area are ordinate drawing standard curve, obtain the typical curve regression equation with the mass concentration of hydrocarbonate series standard solution; According to the peak area of hydrocarbonate in the water sample to be measured, utilize gained typical curve regression equation, calculate the mass concentration of hydrocarbonate in the water sample to be analyzed.
The analytical characteristic amount of hydrocarbonate is following: the range of linearity 0.2 ~ 100mg L of hydrocarbonate
-1, detect and be limited to 0.045mg L
-1, relative standard deviation is 1.6 ~ 3.4%.
Experiment showed, that the present invention has reagent easy and simple to handle, quick, required, sample size is little, accuracy is high, eco-friendly characteristics, can be applied to the detection or the on-line monitoring of hydrocarbonate such as surface water, underground water and waste water.
Although above the preferred embodiments of the present invention are described; But the present invention is not limited to above-mentioned embodiment, and above-mentioned embodiment only is schematically, is not restrictive; Those of ordinary skill in the art is under enlightenment of the present invention; Not breaking away under the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, these all belong within protection scope of the present invention.
Claims (7)
1. hydrocarbonate continuous flow pick-up unit in the water; It is characterized in that; Comprise sample flow path; Sample flow path be connected in primary heater after the sulfuric acid stream is parallelly connected, connect with secondary heater after said primary heater and the parallel connection of developer stream, said secondary heater is connected in spectrophotometer.
2. hydrocarbonate continuous flow detection method in the water is characterized in that this method is carried out according to following steps:
A. prepare standard specimen;
The preparation sulfuric acid solution: the dose volume mark is 1% ~ 5% sulfuric acid solution;
The preparation developer: in 1L distilled water, dissolve 0.4 ~ 0.9g sodium carbonate, the soda mint of 0.2 ~ 0.6g, and the adding massfraction is phenolphthalein ethanolic solution 0.5 ~ 4.0ml of 1%;
B. standard specimen or water sample to be measured mix with the online uniform flow of sulfuric acid solution, and under the promotion of peristaltic pump, pass through 30 ~ 60 ℃ primary heater; The flow velocity of standard specimen or water sample to be measured, sulfuric acid solution is 0.5 ~ 2.0ml min
-1
C. the developer that step (a) is prepared is introduced with the flow velocity that is higher than standard specimen or water sample to be measured, mix with the online not uniform flow of mixed liquor after step (b) is handled, and the secondary heater through 30 ~ 80 ℃ reacts under the promotion of peristaltic pump; The flow velocity of developer is 0.8 ~ 3.0ml min
-1
D. through peristaltic pump step (c) reaction back solution is carried out continuous streaming sample introduction, the injection spectrophotometer detects with the detection wavelength of 400 ~ 600nm.
3. hydrocarbonate continuous flow detection method is characterized in that in a kind of water according to claim 2, and the volume fraction of preparation sulfuric acid solution is 1.5% in the said step (a).
4. hydrocarbonate continuous flow detection method in a kind of water according to claim 2; It is characterized in that when preparing developer in the said step (a), the adding quality of sodium carbonate is 0.6g; The adding quality of soda mint is 0.5g, and the addition of phenolphthalein ethanolic solution is 2.5ml.
5. hydrocarbonate continuous flow detection method in a kind of water according to claim 2; It is characterized in that; The sample injection time of standard specimen or water sample to be measured is 50 ~ 150s in the said step (b), and the sample injection time of sulfuric acid solution is 70 ~ 200s, and the temperature of primary heater is 35 ℃.
6. hydrocarbonate continuous flow detection method is characterized in that in a kind of water according to claim 2, and the sample injection time of the developer in the said step (c) is 70 ~ 200s, and the temperature of secondary heater is 45 ℃.
7. hydrocarbonate continuous flow detection method is characterized in that in a kind of water according to claim 2, and it is 550nm that the spectrophotometer in the said step (d) detects wavelength.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107621449A (en) * | 2017-02-13 | 2018-01-23 | 中国石油天然气股份有限公司 | CO in gas purification amine liquid2Continuous flow analysis method of content |
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Application publication date: 20121219 |