CN109187701A - Fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid - Google Patents
Fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid Download PDFInfo
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- CN109187701A CN109187701A CN201811069774.4A CN201811069774A CN109187701A CN 109187701 A CN109187701 A CN 109187701A CN 201811069774 A CN201811069774 A CN 201811069774A CN 109187701 A CN109187701 A CN 109187701A
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- zinc sulfate
- electroplate liquid
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- fluid samples
- fluorinion concentration
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- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 title claims abstract description 37
- 229960001763 zinc sulfate Drugs 0.000 title claims abstract description 37
- 229910000368 zinc sulfate Inorganic materials 0.000 title claims abstract description 37
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 title claims abstract description 28
- 239000012530 fluid Substances 0.000 claims abstract description 21
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011737 fluorine Substances 0.000 claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 18
- 238000007747 plating Methods 0.000 claims abstract description 17
- 239000012086 standard solution Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- -1 iron ion Chemical class 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000012556 adjustment buffer Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 5
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910001431 copper ion Inorganic materials 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000007853 buffer solution Substances 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 2
- 229940038773 trisodium citrate Drugs 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000005097 cold rolling Methods 0.000 abstract description 7
- 238000009713 electroplating Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005259 measurement Methods 0.000 abstract description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 5
- 238000000691 measurement method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229910001448 ferrous ion Inorganic materials 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004204 optical analysis method Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006664 bond formation reaction Methods 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses fluorinion concentrations in a kind of fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid, belong to technical field of analytical chemistry.It includes the potential value E for measuring zinc sulfate plating fluid samples to be measured respectively using electrode0And the potential value E of sample after fluorine standard solution is addeds, then fluorinion concentration C in fluid samples is electroplated in zinc sulfate to be measured0Meet following relationship:
Description
Technical field
The present invention relates to the measurements of electroplate liquid intermediate ion concentration used in cold rolling electroplating zine plate, belong to technique of analytical chemistry neck
Domain, more particularly to fluorinion concentration in a kind of fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid.
Background technique
The presence of fluorine ion can corrode the electrode in electrolytic cell in the electroplate liquid that cold rolling electroplating zine plate production process uses, and make
The increase of forming apparatus loss.Therefore, the content control of fluorine ion is an important project in electroplate liquid.Preferably to refer to
Conduction cooling rolls the concentration of the fluorine ion in Electrolytic Galvanizing Line control electroplate liquid, it is necessary to grasp the detection of content of fluoride ion in electroplate liquid
Method.However the measuring method not in relation to content of fluoride ion in electroplate liquid in the prior art.
There are many current measuring methods in relation to content of fluoride ion: volumetric analysis, Optical Analysis Method, the chromatography of ions and
Fluoride ion selective electrode method etc., the wherein detection of Optical Analysis Method soluble fluoride suitable for domestic water, and use from
Sub- chromatography rule needs in advance to handle sample distillation, cumbersome, is not suitable for production scene and uses；Fluoride ion selective electrode method
It is common fluorine ion analysis method, belongs to one of ion selective electrode, by is carried out to certain specific ion
Ion concentration specific in solution is converted into the current potential of response, to realize chemical quantity → electrical quantities by the response of selectivity
Conversion, and it is finally reached the measurement to effects of ion concentration.The measuring speed of Fluoride ion selective electrode method is fast, but it is to measurement
The requirement of solution is also higher.The pH value of solution will be suitable for that other solions of influence fluorinion concentration control simultaneously in solution
Easily remove.
However contain a large amount of zinc ion, a small amount of iron ion, Asia in the electroplate liquid that uses of cold rolling electroplating zine plate production process
Iron ion and copper ion, even if after zinc ion is removed, remaining iron ion, ferrous ion and copper ion etc. also can be right in solution
Measurement result has an impact.Therefore, there is an urgent need for fluorine in a kind of electroplate liquid that energy rapid survey cold rolling electroplating zine plate production process uses
The measuring method of ion concentration.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of convenient and efficient measurement cold rolling electroplating zine plate production processes to make
The measuring method of fluorinion concentration in electroplate liquid.
To achieve the above object, the invention discloses a kind of fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electricity
Fluorinion concentration in plating solution, it includes the potential value E for measuring zinc sulfate plating fluid samples to be measured respectively using electrode0And fluorine is added
The potential value E of sample after standard solutions, then fluorinion concentration C in fluid samples is electroplated in zinc sulfate to be measured0Meet following mathematical relationship
Formula:
Δ E=E in formula0-ES；
C0: fluorinion concentration in zinc sulfate plating fluid samples to be measured, unit mg/L；
V0: the volume of zinc sulfate plating fluid samples to be measured, unit mL；
Cs: the concentration of fluorine standard solution, unit mg/L；
Vs: the volume of fluorine standard solution, unit mL；
S: electrode used therein slope.
Further, the Δ E meets following relationship:
Wherein, E0And EsAbide by Nernst equation, it may be assumed that
E0=K-SlgCO；Es=K-SlgCs；
K is the constant including the current potential of inside and outside reference electrode, liquid junction potential etc.；
Preferably, the fluoride ion selective electrode and reference electrode of activation are inserted through into zinc sulfate plating fluid samples, and
Stable potential value is read under stirring；
Preferably, fluorine standard solution is added from trend zinc sulfate plating fluid samples using potentiometric titrimeter.
Further, the fluorine standard solution volume is the 1%~4% of zinc sulfate electroplate liquid volume of sample to be measured, described
The concentration of fluorine standard solution is 100mg/L.
Preferably, zinc sulfate electroplate liquid volume of sample to be measured is 10mL, and the fluorine standard solution of addition is 0.1~0.4mL.
Preferably, fluorine standard solution is that the pure sodium fluoride of the analysis dried is configured to solution using deionized water.
Further, the acidity of the zinc sulfate plating fluid samples to be measured is adjusted to 5.0~8.0.
Further, to zinc sulfate to be measured plating fluid samples in be added for be complexed zinc ion, iron ion, ferrous ion and
The ionic strength adjustment-buffer of copper ion, the ionic strength adjustment-buffer are the configuration process of TISAB buffer solution are as follows: weigh 100g
Trisodium citrate pours into 2L beaker, weighs 114g sodium chloride and is appended to beaker, is completely dissolved two kinds of reagents simultaneously with the water of 1L
After mixing be added 100mL acetic acid, stir evenly, with mass percent be 20% sodium hydroxide solution adjust pH to 5.0~
6.0, the solution in beaker is finally diluted to 2L with water.
The measurement method that the present invention designs needs to adjust the acid of zinc sulfate plating fluid samples to be measured before measuring electromotive force
Degree, this is because acidity has serious influence to the testing result of fluorine ion, acidity is higher in solution, F-Can with hydrogen bond formation with
H in solution+The reticular structure for forming (HF) n, reduces F-Activity.PH value is excessively high, and solution acidity is relatively low, fluorine ion selection
Electrode, the La on electrode film3+It is likely to form La (OH)3, cause the parameter of electrode to change, i.e., either acidity is higher
Or it is lower, it can all influence the accuracy of testing result.Therefore, the suitable acidity of the application solution to be measured is pH value 5.0
Between~8.0.
The measurement method that the present invention designs uses the mode of addition ionic strength adjustment-buffer to reduce zinc sulfate plating to be measured
The interference of zinc ion, iron ion, ferrous ion and copper ion in fluid samples.
The measurement method that the present invention designs has obtained relationship:
Wherein, due to the fluorine standard solution volume added of the present invention is zinc sulfate electroplate liquid volume of sample to be measured 1%~
4%, i.e. influence of the fluorine standard solution volume to zinc sulfate electroplate liquid volume of sample is bigger, therefore it is molten to ignore fluorine ion standard
Influence of the liquid maximum adding quantity to testing result, therefore be following relationship by above-mentioned relationship abbreviation:
The beneficial effects are mainly reflected as follows following aspects:
The method that the present invention designs can be convenient efficiently measurement production scene and is electroplated in fluid samples with zinc sulfate to be measured
The content of fluorine ion reduces equipment loss and has realistic meaning to fluorinion concentration in cold rolling electroplating zinc unit allocation electroplate liquid.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
The invention discloses fluorine ion in a kind of fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid is dense
Degree, specifically includes following process:
1) pipetting 10mL zinc sulfate plating fluid samples to be measured respectively and being placed in 4 volumes marked as A, B, C, D is 250mL's
In polytetrafluoroethylene beaker, using solution acidity in each beaker of sodium hydroxide solution adjustment of 0.1mol/L to PH 5.0~8.0
Between, it is identical to control the sodium hydroxide solution volume being added in each beaker；
2) ionic strength adjustment-buffer (TISAB) of 20mL is added into above-mentioned each beaker respectively by experiment demand；
3) fluoride ion selective electrode and reference electrode (calomel electrode) of activation are inserted through into above-mentioned each sample solution,
Stable potential value E is read under stirrings；
4) then potentiometric titrimeter is used to sequentially add volume into above-mentioned each sample solution automatically as 0.1mL, 0.2mL,
The fluorine standard solution (100mg/L) of 0.3mL, 0.4mL measure stable potential value E after mixing evenly0；
According to relationship:
Calculate separately out fluorinion concentration in each sample solution, and use weighted average method calculate fluorinion concentration for
0.72mg/L；
In order to further verify the accuracy of above-mentioned measurement method, last time experiment 4 times, obtained result such as following table are repeated
Shown in 1:
1 fluorinion concentration list of table
It is 0.71mg/L with the content of fluoride ion in measuring method detection sample, the standard deviation of testing result is
0.022mg/L；
In order to prove the feasibility of said determination method, the 40mL sample is accurately pipetted into 50mL volumetric flask, is added
1.0mL fluorine ion standard solution (100mg/L), is diluted to 50mL.At this point, in sample fluorine ion content be [(40 × 0.71)+
100] ÷ 50=2.57mg/L uses the measured value of said determination method for 2.62mg/L, recovery rate 102%, completely can be with
Meet needs.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment
Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention
It is required that protection scope.
Claims (5)
1. fluorinion concentration in a kind of fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid, it is characterised in that: it
Potential value E including measuring zinc sulfate plating fluid samples to be measured respectively using electrode0And the electricity of sample after fluorine standard solution is added
Place value Es, then fluorinion concentration C in fluid samples is electroplated in zinc sulfate to be measured0Meet following relationship:
Δ E=E in formula0-ES；
C0: fluorinion concentration in zinc sulfate plating fluid samples to be measured, unit mg/L；
V0: the volume of zinc sulfate plating fluid samples to be measured, unit mL；
Cs: the concentration of fluorine standard solution, unit mg/L；
Vs: the volume of fluorine standard solution, unit mL；
S: electrode used therein slope.
2. fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid according to claim 1,
It is characterized by: the Δ E meets following relationship:
3. fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid according to claim 1,
It is characterized by: the fluorine standard solution volume is the 1%~4% of zinc sulfate electroplate liquid volume of sample to be measured, the fluorine standard
The concentration of solution is 100mg/L.
4. fluoride ion selective electrode described according to claim 1~any one of 3-Standard Addition Method for Determination zinc sulfate electroplate liquid
Middle fluorinion concentration, it is characterised in that: the acidity pH value of the zinc sulfate plating fluid samples to be measured is adjusted to 5.0~8.0.
5. fluoride ion selective electrode described according to claim 1~any one of 3-Standard Addition Method for Determination zinc sulfate electroplate liquid
Middle fluorinion concentration, it is characterised in that: be added into zinc sulfate to be measured plating fluid samples for zinc ion, iron ion, Asia to be complexed
The ionic strength adjustment-buffer of iron ion and copper ion, the ionic strength adjustment-buffer are the configuration process of TISAB buffer solution are as follows:
It weighs 100g trisodium citrate to pour into 2L beaker, weighs 114g sodium chloride and be appended to beaker, it is with the water of 1L that two kinds of reagents are complete
Fully dissolved and mix after be added 100mL acetic acid, stir evenly, with mass percent be 20% sodium hydroxide solution adjust pH to
5.0~6.0, the solution in beaker is finally diluted to 2L with water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811069774.4A CN109187701A (en) | 2018-09-13 | 2018-09-13 | Fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811069774.4A CN109187701A (en) | 2018-09-13 | 2018-09-13 | Fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid |
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| CN109187701A true CN109187701A (en) | 2019-01-11 |
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|---|---|---|---|
| CN201811069774.4A Pending CN109187701A (en) | 2018-09-13 | 2018-09-13 | Fluorinion concentration in fluoride ion selective electrode-Standard Addition Method for Determination zinc sulfate electroplate liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110057881A (en) * | 2019-05-16 | 2019-07-26 | 瓮福（集团）有限责任公司 | The rapid assay methods of fluorine in a kind of fluorine-containing slag |
| CN110231375A (en) * | 2019-07-10 | 2019-09-13 | 广西川金诺化工有限公司 | A kind of detection method of standard addition method to fluorine content in phosphoric acid and its phosphate |
| CN110763749A (en) * | 2019-10-22 | 2020-02-07 | 湖北兴福电子材料有限公司 | A kind of detection method of fluoride ion in acid-containing etching solution |
| CN111650331A (en) * | 2020-07-02 | 2020-09-11 | 广东佳纳能源科技有限公司 | Method for measuring fluorine content in nickel-cobalt-manganese ternary material |
| CN113776904A (en) * | 2021-08-27 | 2021-12-10 | 柳州钢铁股份有限公司 | Method for measuring calcium fluoride in fluorite |
| CN114935598A (en) * | 2022-04-06 | 2022-08-23 | 武汉大学 | Detection method for gas-liquid phase product after SF6 degradation |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110057881A (en) * | 2019-05-16 | 2019-07-26 | 瓮福（集团）有限责任公司 | The rapid assay methods of fluorine in a kind of fluorine-containing slag |
| CN110231375A (en) * | 2019-07-10 | 2019-09-13 | 广西川金诺化工有限公司 | A kind of detection method of standard addition method to fluorine content in phosphoric acid and its phosphate |
| CN110231375B (en) * | 2019-07-10 | 2021-03-30 | 广西川金诺化工有限公司 | Method for detecting fluorine content in phosphoric acid and phosphoric acid salt thereof by standard addition method |
| CN110763749A (en) * | 2019-10-22 | 2020-02-07 | 湖北兴福电子材料有限公司 | A kind of detection method of fluoride ion in acid-containing etching solution |
| CN110763749B (en) * | 2019-10-22 | 2022-05-06 | 湖北兴福电子材料有限公司 | Method for detecting fluorine ions in acid-containing etching solution |
| CN111650331A (en) * | 2020-07-02 | 2020-09-11 | 广东佳纳能源科技有限公司 | Method for measuring fluorine content in nickel-cobalt-manganese ternary material |
| CN113776904A (en) * | 2021-08-27 | 2021-12-10 | 柳州钢铁股份有限公司 | Method for measuring calcium fluoride in fluorite |
| CN113776904B (en) * | 2021-08-27 | 2024-03-01 | 柳州钢铁股份有限公司 | Method for determining calcium fluoride in fluorite |
| CN114935598A (en) * | 2022-04-06 | 2022-08-23 | 武汉大学 | Detection method for gas-liquid phase product after SF6 degradation |
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