CN110261335A - A method of measurement poly-epoxy succinic acid content - Google Patents
A method of measurement poly-epoxy succinic acid content Download PDFInfo
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- CN110261335A CN110261335A CN201910550067.5A CN201910550067A CN110261335A CN 110261335 A CN110261335 A CN 110261335A CN 201910550067 A CN201910550067 A CN 201910550067A CN 110261335 A CN110261335 A CN 110261335A
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- succinic acid
- epoxy succinic
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention discloses a kind of methods for measuring poly-epoxy succinic acid content, the absorbance of poly-epoxy succinic acid and dodecyl benzyl dimethyl ammonium chloride associated matter solution in circulation water sample to be measured is measured at 420nm wavelength, and the concentration of poly-epoxy succinic acid in recirculated water is determined by predetermined calibration curve.The method of the present invention is quick, easy, and used medicament is more stable and cheap, can satisfy the measurement of poly-epoxy succinic acid content in recirculated water.
Description
Technical field
The invention belongs to analysis technical fields, and what is involved is the measurements of poly-epoxy succinic acid in industrial cycle aqueous systems.Tool
It is to be determined polymer in industrial circulating water according to the interaction of cationic surfactant and poly-epoxy succinic acid for body
In concentration.
Background technique
In recent years, by be discharged into using the phosphorus containg substances in water treatment agent medicament and cause the rich battalion of water plant in water
It is increasingly serious to support pollution, it is stringent to phosphorus content emission request based on this country, so that without phosphorus water treatment agent becomes development
Trend.Poly-epoxy succinic acid is without phosphorus, biodegradable and has stronger anticorrosion-antiscaling property, therefore is usually used in without phosphorus water
In treatment agent.
Guarantee the scale inhibitor function of industrial circulating cooling water, the anti-incrustation corrosion inhibitor in water body must be maintained at certain
In concentration range.For the content of medicament without phosphorus in recirculated water, common measuring method has fluorescent traccer technique.United States Patent (USP)
This method is described in 5958778, but the fluorescent material stable structure that this method uses, it is not degradable, it is brought to environment
Secondary pollution.Furthermore the polymer in medicament can be degraded with the growth of time, and content reduces；But fluorescent material contains
Amount is basically unchanged, so that measurement result is bigger than normal.Patent CN201110154759 describes a kind of pinacyanol chloride light splitting
The method that photometry measures poly-epoxy succinic acid content in recirculated water, pinacyanol chloride used are expensive and unstable.
Patent CN201610892294 measures the concentration of polymer using gravimetric method, and water sample needs filtering, separation, dialysis, this
Method and step is cumbersome.Patent CN105987902A measures anionic polymer content in industrial water using the dye of positive ion,
Many dyes of positive ion are unstable in solution state.
Summary of the invention
It is an object of the present invention to provide a kind of methods of poly-epoxy succinic acid content in Accurate Determining industrial circulating water.
For above-mentioned purpose, the technical solution adopted in the present invention is made of following step:
1, poly-epoxy succinic acid is added into ultrapure water, prepares the standard water sample of the poly-epoxy succinic acid containing various concentration, to
Dodecyl benzyl dimethyl ammonium chloride is added in the standard water sample, dodecyl dimethyl Benzylmagnesium chloride in every liter of standard water sample
The additional amount of ammonium is 100~400mg, then with the pH value of NaOH adjustment criteria water sample is 7~10, room temperature standing 20~40 minutes,
Then the absorbance that system is corresponded to ultraviolet specrophotometer measurement difference poly-epoxy succinic acid concentration at 420nm wavelength, draws
The standard curve that absorbance value processed changes with poly-epoxy succinic acid concentration in standard water sample.
2, according to be measured circulation water sample of method identical with step 1 test containing poly-epoxy succinic acid at 420nm wavelength
Absorbance calculate the content of poly-epoxy succinic acid in circulation water sample to be measured in conjunction with the linear equation of step 1 standard curve.
In said determination method, the additional amount of dodecyl benzyl dimethyl ammonium chloride is in preferably every liter of standard water sample
200~300mg.
It is further preferably 8~9 with the pH value of NaOH adjustment criteria water sample in said determination method.
Beneficial effects of the present invention are as follows:
The present invention is in certain wave strong point measurement poly-epoxy succinic acid and cationic surfactant dodecyl dimethyl benzyl
The absorbance of ammonium chloride associated matter solution, and poly-epoxy succinic acid in recirculated water is determined by predetermined calibration curve
Concentration.This method is quick, easy, and used medicament is more stable and cheap, can quickly measure polycyclic oxygen in recirculated water
Succinic acid content.
Detailed description of the invention
Fig. 1 is that the additional amount of dodecyl benzyl dimethyl ammonium chloride is 300mgL-1When absorbance value with standard water sample
The standard curve of middle poly-epoxy succinic acid concentration variation.
Fig. 2 is the absorption light that dodecyl benzyl dimethyl ammonium chloride and various concentration poly-epoxy succinic acid form polymer
Spectrum, wherein 1 is 300mgL-1The absorption curve of dodecyl benzyl dimethyl ammonium chloride, 2 be 20mgL-1Poly- epoxy succinic
The absorption curve of acid, 3~6 be successively 300mgL-1Dodecyl benzyl dimethyl ammonium chloride and 8,15,20,40mgL-1It is poly-
The absorption curve of Epoxysuccinic acid.
Fig. 3 is influence of the pH value to dodecyl benzyl dimethyl ammonium chloride and poly-epoxy succinic acid system absorbance value.
Fig. 4 is to stablize the time to the shadow of dodecyl benzyl dimethyl ammonium chloride and poly-epoxy succinic acid system absorbance value
It rings.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
1, poly-epoxy succinic acid is added into ultrapure water, prepares contain 4,12,20,40mgL respectively-1Poly-epoxy succinic acid
Dodecyl benzyl dimethyl ammonium chloride is added into the standard water sample for standard water sample, dodecyl two in every liter of standard water sample
The additional amount of methylbenzyl ammonium chloride is 300mg, then with the pH value of NaOH adjustment criteria water sample is 8, room temperature standing 30 minutes, so
The absorbance for corresponding to system with ultraviolet specrophotometer measurement difference poly-epoxy succinic acid concentration at 420nm wavelength afterwards, draws
The standard curve that absorbance value changes with poly-epoxy succinic acid concentration in standard water sample.
What absorbance used in the present invention was determined according to langbobier law: A=ε lc, wherein A is absorbance, and ε is to form
The absorptivity of object is closed, l is optical path length, and c is the concentration of poly-epoxy succinic acid.For poly-epoxy succinic acid in measurement recirculated water system
Concentration, first measure its calibration curve.At wavelength 420nm, school is made with the absorbance that poly-epoxy succinic acid concentration is corresponding
Directrix curve is shown in Fig. 1.Equation of linear regression are as follows: A=0.0193+0.0132c (mgL-1), R2=0.9937.
2, according to be measured circulation water sample of method identical with step 1 test containing poly-epoxy succinic acid at 420nm wavelength
Absorbance calculate the content of poly-epoxy succinic acid in circulation water sample to be measured in conjunction with the linear equation of step 1 standard curve.
In order to determine the method for the present invention, inventor has carried out a large amount of laboratory research test, and specific test is as follows:
1, measuring method
For any polymer, the factor that need to be evaluated is the interaction of polymer and surfactant first.For
It determines that poly-epoxy succinic acid and dodecyl benzyl dimethyl ammonium chloride are formed by the interaction of associated matter, measures associated matter
Absorption spectrum, see Fig. 2.Fig. 2 is shown, contains 300mgL-1The aqueous solution of dodecyl benzyl dimethyl ammonium chloride and contain
20mg·L-1The equal very little of the absorbance of the aqueous solution of poly-epoxy succinic acid, when in dodecyl benzyl dimethyl ammonium chloride aqueous solution
When middle addition poly-epoxy succinic acid, absorbance value is significantly increased, and both shows that interaction forms associated matter, and absorbance value with
The increase of poly-epoxy succinic acid concentration and increase.Therefore this method can be used to measure the content of poly-epoxy succinic acid.In addition, by
Associated matter known to Fig. 2 is maximum in 400nm absorbance value.But due to 400nm be visual field and ultraviolet region boundary, interference compared with
Greatly.According to the principle of " absorbing maximum, interference minimum ", the present invention is selected at 420nm wavelength and measures.Although under sensitivity
Drop, but interfering can be much smaller.
2, the influence of pH
Poly-epoxy succinic acid is added into ultrapure water, prepares and contains 20mgL-1The standard water sample of poly-epoxy succinic acid, to this
Dodecyl benzyl dimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride in every liter of standard water sample are added in standard water sample
Additional amount be 300mg, then with NaOH difference adjustment criteria water sample pH value be 3,4,5,6,7,8,9,10,11, room temperature stand
30 minutes, corresponding body under different pH value then was measured with ultraviolet specrophotometer and lies in absorbance at 420nm, as a result sees Fig. 3.
Fig. 3 shows that absorbance value is larger in pH=7~10, and absorbance value is maximum when pH=8, therefore the present invention is preferably in pH=8
Carry out measuring.
3, the influence of different dodecyl benzyl dimethyl ammonium chloride additive amounts
Poly-epoxy succinic acid is added into ultrapure water, prepares contain 4,12,20,40mgL respectively-1The mark of poly-epoxy succinic acid
Quasi- water sample.100,200,300,400mg dodecyl benzyl dimethyl ammonium chloride are added by every liter of standard water sample respectively, then use
The pH value of NaOH adjustment criteria water sample is 8, and room temperature stands 30 minutes, is then measured with ultraviolet specrophotometer in identical dodecane
When base dimethyl benzyl ammonium chloride additive amount, various concentration poly-epoxy succinic acid corresponding body lies in the absorbance at 420nm wavelength,
Draw the standard curve that absorbance value changes with poly-epoxy succinic acid concentration in standard water sample.It the results are shown in Table 1.
The system equation of the different dodecyl benzyl dimethyl ammonium chloride concentration of table 1
The slope of calibration curve is bigger, and the sensitivity of illustration method increases；R2Closer to 1, the accuracy of illustration method
It is higher.Based on this, the additive amount of the preferred dodecyl benzyl dimethyl ammonium chloride of the present invention is 200~300mgL-1。
3, stablize the influence of time
Since both poly-epoxy succinic acid and dodecyl benzyl dimethyl ammonium chloride have charge, the two forms association
Object.Poly-epoxy succinic acid is added into ultrapure water, prepares and contains 20mgL-1The standard water sample of poly-epoxy succinic acid, to the standard water
Dodecyl benzyl dimethyl ammonium chloride is added in sample, the addition of dodecyl benzyl dimethyl ammonium chloride in every liter of standard water sample
Amount is 300mg, then with the pH value of NaOH adjustment criteria water sample is 8, then room temperature standing different time uses ultraviolet specrophotometer
It measures corresponding body under different time of repose and lies in absorbance at 420nm, as a result see Fig. 3.As seen from the figure, with the increasing of time
Long, the increase of associated matter is settled in the solution, measures absorbance value reduction.Therefore, after the present invention preferably stands 30min
Measure absorbance value.
4, mark-on reclaims are tested
It according to the method for embodiment 1, is 20.0mgL to poly-epoxy succinic acid additional amount-1Simulated water sample carry out mark-on
Recovery test the results are shown in Table 2.
2 recovery testu result of table
As can be seen from Table 2, as a result the recovery of standard addition of the method for the present invention compares and accurately may be used between 92.0%~105.5%
It leans on.
5, actual water sample is measured
Circulation water sample is taken from scene, water sample is measured according to the method for embodiment 1, measurement result is shown in Table 3.
The analysis result of 3 water sample of table
Claims (3)
1. a kind of method for measuring poly-epoxy succinic acid content, it is characterised in that:
(1) poly-epoxy succinic acid is added into ultrapure water, the standard water sample of the poly-epoxy succinic acid containing various concentration is prepared, to the mark
Dodecyl benzyl dimethyl ammonium chloride is added in quasi- water sample, dodecyl benzyl dimethyl ammonium chloride in every liter of standard water sample
Additional amount is 100~400mg, then with the pH value of NaOH adjustment criteria water sample is 7~10, room temperature standing 20~40 minutes, then
The absorbance that system is corresponded to ultraviolet specrophotometer measurement difference poly-epoxy succinic acid concentration at 420nm wavelength, draws and inhales
The standard curve that shading value changes with poly-epoxy succinic acid concentration in standard water sample；
(2) according to be measured circulation water sample of method identical with step (1) test containing poly-epoxy succinic acid at 420nm wavelength
Absorbance calculates the content of poly-epoxy succinic acid in circulation water sample to be measured in conjunction with the linear equation of step (1) standard curve.
2. the method for measurement poly-epoxy succinic acid content according to claim 1, it is characterised in that: in every liter of standard water sample
The additional amount of dodecyl benzyl dimethyl ammonium chloride is 200~300mg.
3. the method for measurement poly-epoxy succinic acid content according to claim 1, it is characterised in that: use NaOH adjustment criteria
The pH value of water sample is 8~9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112683825A (en) * | 2020-12-24 | 2021-04-20 | 洛阳强龙实业有限公司 | Method for measuring concentration of phosphorus-free medicament polymer scale inhibition dispersant in circulating water |
| CN114538478A (en) * | 2022-03-15 | 2022-05-27 | 南京安淮创新药物研究院有限公司 | Preparation method of sodium bicarbonate particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105717054A (en) * | 2016-02-22 | 2016-06-29 | 石家庄给源环保科技有限公司 | Detection method and detection device for online detection of scale and corrosion inhibitor concentration in circulating cooling water and circulating cooling water treatment control system |
-
2019
- 2019-06-24 CN CN201910550067.5A patent/CN110261335A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105717054A (en) * | 2016-02-22 | 2016-06-29 | 石家庄给源环保科技有限公司 | Detection method and detection device for online detection of scale and corrosion inhibitor concentration in circulating cooling water and circulating cooling water treatment control system |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112683825A (en) * | 2020-12-24 | 2021-04-20 | 洛阳强龙实业有限公司 | Method for measuring concentration of phosphorus-free medicament polymer scale inhibition dispersant in circulating water |
| CN114538478A (en) * | 2022-03-15 | 2022-05-27 | 南京安淮创新药物研究院有限公司 | Preparation method of sodium bicarbonate particles |
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