CN108169227A - The improved method that Zn content is surveyed in a kind of complexometry - Google Patents
The improved method that Zn content is surveyed in a kind of complexometry Download PDFInfo
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- CN108169227A CN108169227A CN201711345748.5A CN201711345748A CN108169227A CN 108169227 A CN108169227 A CN 108169227A CN 201711345748 A CN201711345748 A CN 201711345748A CN 108169227 A CN108169227 A CN 108169227A
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
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Abstract
The present invention proposes the improved method that Zn content is surveyed in a kind of complexometry, zinc ion solution is titrated to indicator discoloration with EDTA, solution after discoloration is detected with uv-spectrophotometric agent, color signal is converted into light absorbing strength signal, it as titrimetric standard, and then eliminates different people and has the problem of different color differentiation abilities, traditional titration method is improved, artificial experimental error is substantially reduced, more people's test results are almost consistent.
Description
Technical field
The present invention relates to analytical chemistry field, more particularly to a kind of improved method of complexometry survey Zn content.
Background technology
Zinc (Zinc) is the metal of the 4th " common ", is only second to iron, aluminium and copper, silvery white is presented in appearance, in modern industry
In for there is indelible status on battery manufacture, be a considerable metal.In addition, zinc is needed by human micro
One of element plays extremely important work in the important physiology courses such as growth in humans's development, reproduction heredity, immune, endocrine
With.It is given instruction agent with methyl orange when EDTA complexometries detect Zn content, claret is made to become glassy yellow in titration process,
Since everyone is different to the sensitivity of color, the result that may be titrated is multifarious, will for this problem in this method
Traditional titration method is optimized.
Zinc ion is usually contained in the industrial wastewater that metal smelt excludes, need to pass through processing could discharge.It is complexed with EDTA
Method detects Zn content, and the discharge for waste water provides a standard.Because usually contained in waste water copper, nickel, cobalt, cadmium etc. interfere from
Son generally uses NaS2O3Masking is detected again.But it since individual is different to the discrimination of color, causes merely with color
Distinguishing titration end-point can cause the repeatability of test to be deteriorated.This law sets the standard of titration end-point, and to facilitate solution, this is asked
Topic.
Invention content
The present invention proposes the improved method that Zn content is surveyed in a kind of complexometry, reduces prior art individual to color area
Divide experimental error caused by difference.
The technical proposal of the invention is realized in this way：
The improved method that Zn content is surveyed in a kind of complexometry, includes the following steps：
(1) the zinc ion solution of 2~4g/L is prepared；
(2) the EDTA titers of 0.2~1g/L are prepared；
(3) 20.00mL zinc ions solution is pipetted in 250ml triangular flasks, 1 drop methyl orange is added to make indicator, in ammonium hydroxide
Become yellow with to solution from red, rinse bottle wall with little water, add 20mL NaAc-HAc buffer solutions, add 1 drop xylenol orange
Make indicator；
(4) content of the EDTA needed for calculating, and then calculate the volume of the EDTA, according to calculating volume by EDTA
Titer is titrated in zinc ion solution, and solution becomes glassy yellow by claret at this time.
(5) solution of glassy yellow will be become with UV-3600Plus type UV spectrophotometer measurings, the spy that will be scanned
The absorption intensity for levying the most strong characteristic peak in peak is standard absorption intensity.
(6) more people is allowed to titrate the zinc ion solution of unknown concentration with EDTA titrations respectively, the solution after titration is used
After UV-3600Plus type UV spectrophotometer measurings, after adjusting titration results three times with standard absorption intensity contrast, according to
EDTA content calculation calcium ion concentrations used, carry out the comparison of result.
Further, detection wave band is 300~800nm in the step (5).
Further, more artificial at least 10 people in the step (6).
Further, the step (1) is specially and weighs 0.5~1g of metallic zinc to be placed in 250mL beakers, adds in 20mL
0.1M hydrochloric acid dissolves by heating, and constant volume is in 500mL volumetric flasks.
Further, the step (2) is specially to weigh 0.1~0.5g EDTA constant volumes in 500mL volumetric flasks.
Further, the purity of the zinc is 99.99%.
The beneficial effects of the invention are as follows：
(1) solution of reference colour is detected by the present invention with uv-spectrophotometric agent, and color signal is converted into absorption
The strength signal of light as titrimetric standard, and then eliminates different people and has the problem of different color differentiation abilities, to passing
The titration method of system is improved, and artificial experimental error is substantially reduced；
(2) more people's test results are almost consistent.
Specific embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that institute
Embodiment 1
(1) preparation of zinc ion solution：Metallic zinc (99.99%) 0.5g is weighed in 250mL beakers, adding in 20mL
0.1M hydrochloric acid dissolves by heating, and constant volume is in 500mL volumetric flasks.
(2) preparation of EDTA titers：It is for use in 500mL volumetric flasks to weigh EDTA 0.1g constant volumes.
(3) 20.00mL Zinc standard solutions are pipetted in 250ml triangular flasks, 1 drop methyl orange are added to make indicator, in ammonium hydroxide
Become yellow with to solution from red, rinse bottle wall with little water, add 20mL NaAc-HAc buffer solutions, add 1 drop xylenol orange
Make indicator, it is terminal to be titrated to solution to fade to glassy yellow by claret with EDTA.
(4) content of the EDTA needed for calculating, and then calculate the volume of the EDTA, according to calculating volume by EDTA
Titer is titrated in zinc ion solution, and solution becomes glassy yellow by claret at this time.
(5) by the UV-3600Plus type UV spectrophotometer measurings of solution at this time, detection wave band for 300~
The absorption intensity of the most strong characteristic peak of the characteristic peak scanned is standard absorption intensity by 800nm.
(6) 10 people is allowed to titrate the zinc ion solution of unknown concentration with EDTA titrations respectively, the solution after titration is used
After UV-3600Plus type UV spectrophotometer measurings, after adjusting titration results three times with standard absorption intensity contrast, according to
EDTA content calculations calcium ion concentration used, carries out the comparison of result, and test data is as follows：
| Sample | This law test result | National standard measurement result |
| 1 | 0.35mmol/L | 0.53mmol/L |
| 2 | 0.34mmol/L | 0.37mmol/L |
| 3 | 0.35mmol/L | 0.40mmol/L |
| 4 | 0.36mmol/L | 0.35mmol/L |
| 5 | 0.35mmol/L | 0.32mmol/L |
| 6 | 0.35mmol/L | 0.42mmol/L |
| 7 | 0.36mmol/L | 0.36mmol/L |
| 8 | 0.35mmol/L | 0.35mmol/L |
| 9 | 0.35mmol/L | 0.50mmol/L |
| 10 | 0.34mmol/L | 0.48mmol/L |
It can be seen that after the standard for setting final titration results by data in table, the test of 10 different people
As a result it is almost the same, up-down error 0.2mmol/L, but it is significantly bigger than normal without the method titration results error of established standards.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (6)
1. the improved method that Zn content is surveyed in a kind of complexometry, which is characterized in that include the following steps：
(1) the zinc ion solution of 2~4g/L is prepared；
(2) the EDTA titers of 0.2~1g/L are prepared；
(3) 20.00mL zinc ions solution is pipetted in 250ml triangular flasks, and 1 drop methyl orange is added to make indicator, is neutralized to ammonium hydroxide
Solution becomes yellow from red, rinses bottle wall with little water, adds 20mL NaAc-HAc buffer solutions, 1 drop xylenol orange is added to indicate
Agent；
(4) content of the EDTA needed for calculating, and then calculate the volume of the EDTA, according to calculating volume by EDTA titers
It is titrated in zinc ion solution, solution becomes glassy yellow by claret at this time.
(5) the solution UV-3600Plus type UV spectrophotometer measurings that glassy yellow will be become, by the characteristic peak scanned most
The absorption intensity of strong characteristic peak is standard absorption intensity.
(6) more people is allowed to titrate the zinc ion solution of unknown concentration with EDTA titrations respectively, by the solution UV- after titration
After 3600Plus type UV spectrophotometer measurings, after adjusting titration results three times with standard absorption intensity contrast, according to used
EDTA content calculation calcium ion concentrations, carry out the comparison of result.
2. the improved method that Zn content is surveyed in complexometry as described in claim 1, which is characterized in that examined in the step (5)
Survey wave band is 300~800nm.
3. the improved method that Zn content is surveyed in complexometry as described in claim 1, which is characterized in that more in the step (6)
Artificial at least 10 people.
4. the improved method that Zn content is surveyed in complexometry as described in claim 1, which is characterized in that the step (1) is specific
It is placed in 250mL beakers to weigh 0.5~1g of metallic zinc, adds in 20mL 0.1M hydrochloric acid and dissolve by heating, constant volume is in 500mL capacity
In bottle.
5. the improved method that Zn content is surveyed in complexometry as described in claim 1, which is characterized in that the step (2) is specific
To weigh 0.1~0.5g EDTA constant volumes in 500mL volumetric flasks.
6. the improved method that Zn content is surveyed in complexometry as claimed in claim 4, which is characterized in that the purity of the zinc is
99.99%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711345748.5A CN108169227A (en) | 2017-12-15 | 2017-12-15 | The improved method that Zn content is surveyed in a kind of complexometry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109658794A (en) * | 2019-01-27 | 2019-04-19 | 重庆大学 | For automatically determining the experiment device for teaching in double reaction reagent system reaction time |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021555A (en) * | 2015-07-15 | 2015-11-04 | 沈阳大学 | Method for detecting zinc content in oyster product by dual-wavelength spectrophotometric method |
| CN106198854A (en) * | 2016-07-08 | 2016-12-07 | 长春黄金研究院 | A kind of Direct spectrophotometry method in billon |
-
2017
- 2017-12-15 CN CN201711345748.5A patent/CN108169227A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105021555A (en) * | 2015-07-15 | 2015-11-04 | 沈阳大学 | Method for detecting zinc content in oyster product by dual-wavelength spectrophotometric method |
| CN106198854A (en) * | 2016-07-08 | 2016-12-07 | 长春黄金研究院 | A kind of Direct spectrophotometry method in billon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109658794A (en) * | 2019-01-27 | 2019-04-19 | 重庆大学 | For automatically determining the experiment device for teaching in double reaction reagent system reaction time |
| CN109658794B (en) * | 2019-01-27 | 2021-03-02 | 重庆大学 | Teaching experiment device for automatically measuring reaction time of double-reaction reagent system |
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Application publication date: 20180615 |
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