CN109781634A - A kind of measuring method of chloride ion content - Google Patents
A kind of measuring method of chloride ion content Download PDFInfo
- Publication number
- CN109781634A CN109781634A CN201811564183.4A CN201811564183A CN109781634A CN 109781634 A CN109781634 A CN 109781634A CN 201811564183 A CN201811564183 A CN 201811564183A CN 109781634 A CN109781634 A CN 109781634A
- Authority
- CN
- China
- Prior art keywords
- chloride ion
- ion content
- measuring method
- electrolyte
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a kind of measuring methods of chloride ion content, specifically includes the following steps: specifically includes the following steps: S1: preparing silver chlorate standard solution: being separately added into ethylene glycol, silver nitrate solution, imitative electrolyte and chloride ion standard solution into the volumetric flask of five 25ml, it is shaken up after constant volume, stands reaction and generate silver chlorate turbid；S2: using spectrophotometer measurement absorbance, and absorbance-concentration values are carried out linear fit, obtain standard curve；S3: taking two volumetric flasks, and addition ethylene glycol, silver nitrate and a prepare liquid, constant volume shake up thereto, stands reaction；To another bottle of addition ethylene glycol, silver nitrate, imitative electrolyte, constant volume is shaken up, and does blank assay；S4: the content of chloride ion in prepare liquid is obtained with the standard curve in spectrophotometer combination step S2 again, further calculates practical chloride ion content.Beneficial effects of the present invention: this method accuracy is good, it is stable, easy, not by ion interferences other in electrolyte.
Description
Technical field
The present invention relates to a kind of chlorine ion content determination methods, it particularly relates to chlorine in a kind of electrolyte and diatomite
The measuring method of ion concentration.
Background technique
In electrolytic copper foil production, content is very low in the electrolytic solution for chloride ion, when copper ion is reduced to copper from cathode, chlorine
Ion plays an important role.In sulfate electroplate liquid, chloride ion can reduce anode polarization, eliminate high current density
The coating striped in area.The study found that cannot flatten performance height if chloride ion content is very little in electrolyte and analyse good brightness
Coating, chloride ion can promote the deposition of copper ion, increase the reduction current that chlorine ion concentration is conducive to increase copper ion.But chlorine from
Sub- concentration can not be excessively high, and when being more than a certain concentration, coarse phenomenon can occur for coating.
Though the common detection method of chloride ion is more, its accurate detection is always a problem.Original side in laboratory
Method is the chloride ion titration method in electrolyte, and this method requires testing staff to judge that white precipitate disappears in a manner of estimating, and
And can not rule out other factors interference, it is not very accurate.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of measuring method of chloride ion content, solves
Existing chloride test inaccuracy, the problem of vulnerable to interference.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
A kind of measuring method of chloride ion content, specifically includes the following steps:
S1: it prepares silver chlorate standard solution: being separately added into identical ethylene glycol, silver nitrate solution into the volumetric flask of five 25ml
And imitative electrolyte, the chloride ion standard solution of different volumes is added into the volumetric flask of above-mentioned five 25ml respectively again later, it is fixed
It is shaken up after appearance, stands reaction and generate silver chlorate turbid；
S2: the silver chlorate turbid generated in above-mentioned five volumetric flasks is poured into respectively in five cuvettes, with spectrophotometer list
Wavelength method measures the absorbance of solution in five cuvettes respectively under 420nm wavelength, absorbance-concentration values is carried out linear
Fitting obtains standard curve；
S3: taking the volumetric flask of two 25ml again, and ethylene glycol, silver nitrate and prepare liquid, constant volume is added in a volumetric flask thereto
It shakes up, stands reaction；Ethylene glycol, silver nitrate, imitative electrolyte are added into another volumetric flask, constant volume shakes up, and does blank assay；
S4: by two parts of solution in step S3, spectrophotometer is opened, blank assay described in step S3 is first done and is returned
Zero, the absorbance of prepare liquid is then measured again, and in conjunction with the standard curve of step S2, containing for chloride ion in prepare liquid can be obtained
Amount, further calculates out practical chloride ion content: C according to formulaIt is practical=CIt is to be measured* prepare liquid extension rate.
Further, the purity of ethylene glycol described in step S1 is to analyze pure, silver nitrate solution 1mol/L, imitates electrolyte
In contain copper sulphate and sulfuric acid.
Further, chloride ion standard solution described in step S1 is configured with potassium chloride and pure water, the purity of potassium chloride
For excellent pure grade, the concentration of chloride ion standard solution is 50-150ppm.
Further, each component volume fraction used in the silver chlorate standard solution is prepared in step S1 are as follows: second
Glycol adds 5.00ml, imitative electrolyte 5.00ml, silver nitrate solution 2.00ml.
Further, in step S1 in the silver chlorate standard solution of five volumetric flasks chlorine ion concentration be respectively as follows: 0ppm,
1ppm、2ppm、3ppm、4ppm。
Further, the time that reaction is stood described in step S1 and S3 is 0.5-1.5h.
Further, correction coefficient of determination >=0.99 of standard curve described in step S2.
Further, prepare liquid extension rate described in step S3 is 2-10 times.
Further, prepare liquid sample volume described in step S3 is 5.00ml.
Beneficial effects of the present invention: the detection method accuracy is not good, stable, easy, dry by ions other in electrolyte
It disturbs.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the according to embodiments of the present invention 1 standard solution standard curve obtained；
Fig. 2 is the according to embodiments of the present invention 2 standard solution standard curves obtained；
Fig. 3 is the according to embodiments of the present invention 3 standard solution standard curves obtained.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with specific embodiment, it is clear that described
Embodiment be only a part of the embodiment of the present invention, instead of all the embodiments.The embodiment is only used for explaining this hair
It is bright, it is not used in the limitation present invention.
Preparing experiment:
(1) 100pp chlorine standard solution is prepared: accurately weigh the dry potassium chloride of 0.21g, with pure water after completely dissolution constant volume in
In 1000ml volumetric flask, shake up spare；
(2) 0.1mol/L silver nitrate standard solution is prepared: dry silver nitrate solid 4.2467g is accurately weighed, it is abundant with pure water
Constant volume shakes up in 250ml volumetric flask after dissolution, and is stored in spare in brown bottle；
(3) 60ml pure water, 17g sulfuric acid (volume ratio 1:1), 35.15gCuSO are added in 250ml beaker4.5H2O is after completely dissolution
Be added 100ml volumetric flask in constant volume, shake up be put into it is spare in 50 DEG C of warm water.
Embodiment 1:
S1: taking the volumetric flask of 5 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, and imitative electrolyte 5.00ml shakes
It is even.
S2: the 100ppm chloride ion standard solution of different volumes, additional amount difference are separately added into above-mentioned 5 volumetric flasks
For 0ml, 0.25ml, 0.50ml, 0.75ml, 1.00ml, constant volume is shaken up, and stands reaction 1h, wherein 0ml is as blank sample, capacity
Chloride ion initial concentration is respectively 0ppm, 1ppm, 2ppm, 3ppm, 4ppm in bottle.
S3: above-mentioned five samples are poured into respectively in 10ml cuvette, with spectrophotometer unicast regular way in 420nm wavelength
Absorbance-concentration values are carried out linear fit, obtain standard curve, curvature correction by the lower absorbance for measuring each sample respectively
Coefficient of determination is 0.9999, and linear relationship is fine, description standard curve be it is qualified, the canonical plotting of acquisition is as shown in Figure 1；
S4: taking the volumetric flask of a 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, by prepare liquid pipette
It takes 5.00ml that constant volume in volumetric flask is added, shakes up, stand reaction 1h；A 25ml volumetric flask separately is taken, is separately added into ethylene glycol
It is shaken up after 5.00ml, silver nitrate 2.00ml, imitative electrolyte 5.00ml constant volume, does blank assay；
S5: spectrophotometer is opened, is first zeroed, then survey chloride ion content in prepare liquid, is read as C with blank sampleIt is to be measured=3.09mg/
L, chloride ion actual content C in electrolyteIt is practicalIt can be according to chloride ion content C in prepare liquidIt is to be measuredIt is calculated with following formula: CIt is practical=
CIt is to be measured*5=15.45mg/L。
Embodiment 2:
S1: taking the volumetric flask of 5 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, and imitative electrolyte 5.00ml shakes
It is even.
S2: the 100ppm chloride ion standard solution of different volumes, additional amount difference are separately added into above-mentioned 5 volumetric flasks
For 0ml, 0.25ml, 0.50ml, 0.75ml, 1.00ml, constant volume is shaken up, and stands reaction 1h, wherein 0ml is as blank sample, capacity
Chloride ion initial concentration is respectively 0ppm, 1ppm, 2ppm, 3ppm, 4ppm in bottle.
S3: above-mentioned five samples are poured into respectively in 10ml cuvette, with spectrophotometer unicast regular way in 420nm wavelength
Absorbance-concentration values are carried out linear fit, obtain standard curve, curvature correction by the lower absorbance for measuring each sample respectively
Coefficient of determination is 0.9997, and linear relationship is fine, description standard curve be it is qualified, the canonical plotting of acquisition is as shown in Figure 2；
S4: taking the volumetric flask of a 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, by prepare liquid pipette
It takes 5.00ml that constant volume in volumetric flask is added, shakes up, stand reaction 1h；A 25ml volumetric flask separately is taken, is separately added into ethylene glycol
It is shaken up after 5.00ml, silver nitrate 2.00ml, imitative electrolyte 5.00ml constant volume, does blank assay；
S5: spectrophotometer is opened, is first zeroed, then survey chloride ion content in prepare liquid, is read as C with blank sampleIt is to be measured=2.12mg/
L, chloride ion actual content C in electrolyteIt is practicalIt can be according to chloride ion content C in prepare liquidIt is to be measuredIt is calculated with following formula: CIt is practical=
CIt is to be measured*5=10.6mg/L。
Embodiment 3:
S1: taking the volumetric flask of 5 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, and imitative electrolyte 5.00ml shakes
It is even.
S2: the 100ppm chloride ion standard solution of different volumes, additional amount difference are separately added into above-mentioned 5 volumetric flasks
For 0ml, 0.25ml, 0.50ml, 0.75ml, 1.00ml, constant volume is shaken up, and stands reaction 1h, wherein 0ml is as blank sample, capacity
Chloride ion initial concentration is respectively 0ppm, 1ppm, 2ppm, 3ppm, 4ppm in bottle.
S3: above-mentioned five samples are poured into respectively in 10ml cuvette, with spectrophotometer unicast regular way in 420nm wavelength
Absorbance-concentration values are carried out linear fit, obtain standard curve, curvature correction by the lower absorbance for measuring each sample respectively
Coefficient of determination is 0.9997, and linear relationship is fine, description standard curve be it is qualified, the canonical plotting of acquisition is as shown in Figure 3；
S4: taking the volumetric flask of a 25ml, is separately added into ethylene glycol 5.00ml, silver nitrate 2.00ml, by prepare liquid pipette
It takes 5.00ml that constant volume in volumetric flask is added, shakes up, stand reaction 1h；A 25ml volumetric flask separately is taken, is separately added into ethylene glycol
It is shaken up after 5.00ml, silver nitrate 2.00ml, imitative electrolyte 5.00ml constant volume, does blank assay；
S5: spectrophotometer is opened, is first zeroed, then survey chloride ion content in prepare liquid, is read as C with blank sampleIt is to be measured=2.53mg/
L, chloride ion actual content C in electrolyteIt is practicalIt can be according to chloride ion content C in prepare liquidIt is to be measuredIt is calculated with following formula: CIt is practical=
CIt is to be measured*5=12.65mg/L。
It in summary it can be seen, the interference of artificial uncertain factor is eliminated using the application spectrophotometry, detect
Accuracy is good, stable, easy, realizes the unification of reliability and high efficiency.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of measuring method of chloride ion content, which is characterized in that specifically includes the following steps:
S1: it prepares silver chlorate standard solution: being separately added into identical ethylene glycol, silver nitrate solution into the volumetric flask of five 25ml
And imitative electrolyte, the chloride ion standard solution of different volumes is added into the volumetric flask of above-mentioned five 25ml respectively again later, it is fixed
It is shaken up after appearance, stands reaction and generate silver chlorate turbid；
S2: the silver chlorate turbid generated in above-mentioned five volumetric flasks is poured into respectively in five cuvettes, with spectrophotometer list
Wavelength method measures the absorbance of solution in five cuvettes respectively under 420nm wavelength, absorbance-concentration values is carried out linear
Fitting obtains standard curve；
S3: taking the volumetric flask of two 25ml again, and ethylene glycol, silver nitrate and prepare liquid, constant volume is added in a volumetric flask thereto
It shakes up, stands reaction；Ethylene glycol, silver nitrate, imitative electrolyte are added into another volumetric flask, constant volume shakes up, and does blank assay；
S4: by two parts of solution in step S3, spectrophotometer is opened, blank assay described in step S3 is first done and is returned
Zero, the absorbance of prepare liquid is then measured again, and in conjunction with the standard curve of step S2, containing for chloride ion in prepare liquid can be obtained
Amount, further calculates out practical chloride ion content: C according to formulaIt is practical=CIt is to be measured* prepare liquid extension rate.
2. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that second two described in step S1
The purity of alcohol is to analyze pure, silver nitrate solution 1mol/L, imitates and contains copper sulphate and sulfuric acid in electrolyte.
3. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that chlorine described in step S1 from
Substandard solution is configured with potassium chloride and pure water, and the purity of potassium chloride is excellent pure grade, and the concentration of chloride ion standard solution is 50-
150ppm。
4. a kind of measuring method of chloride ion content according to claim 1 to 3, which is characterized in that step S1
It is middle to prepare each component volume fraction used in the silver chlorate standard solution are as follows: ethylene glycol adds 5.00ml, imitative electrolyte
5.00ml, silver nitrate solution 2.00ml.
5. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that five capacity in step S1
Chlorine ion concentration is respectively as follows: 0ppm, 1ppm, 2ppm, 3ppm, 4ppm in the silver chlorate standard solution of bottle.
6. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that described in step S1 and S3
The time for standing reaction is 0.5-1.5h.
7. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that standard described in step S2
Correction coefficient of determination >=0.99 of curve.
8. a kind of measuring method of chloride ion content according to claim 1, which is characterized in that be measured described in step S3
Liquid extension rate is 2-10 times.
9. according to claim 1 or a kind of measuring method of chloride ion content described in 8 any one, which is characterized in that step
Prepare liquid sample volume described in S3 is 5.00ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811564183.4A CN109781634A (en) | 2018-12-20 | 2018-12-20 | A kind of measuring method of chloride ion content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811564183.4A CN109781634A (en) | 2018-12-20 | 2018-12-20 | A kind of measuring method of chloride ion content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109781634A true CN109781634A (en) | 2019-05-21 |
Family
ID=66497406
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811564183.4A Pending CN109781634A (en) | 2018-12-20 | 2018-12-20 | A kind of measuring method of chloride ion content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109781634A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110220964A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The measurement method of chloride ion in the copper electrolyte of electrolytic copper foil |
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110361339A (en) * | 2019-05-31 | 2019-10-22 | 衢州康鹏化学有限公司 | The detection method of chloride in imidodisulfuryl fluoride lithium salt |
| CN110726719A (en) * | 2019-10-17 | 2020-01-24 | 广西贺州市桂东电子科技有限责任公司 | Device and method for detecting content of chloride ions in anodic formed foil electrolyte |
| CN111007133A (en) * | 2019-12-25 | 2020-04-14 | 江苏国泰超威新材料有限公司 | Method for determining chloride ions in electrolyte for aluminum electrolytic capacitor |
| CN111751360A (en) * | 2020-05-28 | 2020-10-09 | 金川集团股份有限公司 | Method for rapidly determining chloride ions in lithium battery copper foil electrolyte |
| CN113959966A (en) * | 2021-10-20 | 2022-01-21 | 山东恒邦冶炼股份有限公司 | Method for measuring chlorine content in antimony-containing arsenic trioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102359944A (en) * | 2011-07-14 | 2012-02-22 | 内蒙古包钢钢联股份有限公司 | Determination method of chlorine content in iron-containing dust mud |
| CN102866121A (en) * | 2012-08-27 | 2013-01-09 | 长沙牧泰莱电路技术有限公司 | Method for analyzing concentration of chloride ions of electroplating liquid of printed circuit board (PCB) |
-
2018
- 2018-12-20 CN CN201811564183.4A patent/CN109781634A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102359944A (en) * | 2011-07-14 | 2012-02-22 | 内蒙古包钢钢联股份有限公司 | Determination method of chlorine content in iron-containing dust mud |
| CN102866121A (en) * | 2012-08-27 | 2013-01-09 | 长沙牧泰莱电路技术有限公司 | Method for analyzing concentration of chloride ions of electroplating liquid of printed circuit board (PCB) |
Non-Patent Citations (1)
| Title |
|---|
| 索春艳 等: "酸性镀铜溶液中氯离子分析方法研究", 《印制电路信息》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361339A (en) * | 2019-05-31 | 2019-10-22 | 衢州康鹏化学有限公司 | The detection method of chloride in imidodisulfuryl fluoride lithium salt |
| CN110220964A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The measurement method of chloride ion in the copper electrolyte of electrolytic copper foil |
| CN110220856A (en) * | 2019-06-05 | 2019-09-10 | 常州大学 | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil |
| CN110220964B (en) * | 2019-06-05 | 2020-04-28 | 常州大学 | Method for measuring chloride ions in copper electrolyte of electrolytic copper foil |
| CN110220856B (en) * | 2019-06-05 | 2021-07-27 | 常州大学 | Method for detecting content of chloride ions in electrodeposition liquid of electrolytic copper foil by flow injection method |
| CN110726719A (en) * | 2019-10-17 | 2020-01-24 | 广西贺州市桂东电子科技有限责任公司 | Device and method for detecting content of chloride ions in anodic formed foil electrolyte |
| CN111007133A (en) * | 2019-12-25 | 2020-04-14 | 江苏国泰超威新材料有限公司 | Method for determining chloride ions in electrolyte for aluminum electrolytic capacitor |
| CN111751360A (en) * | 2020-05-28 | 2020-10-09 | 金川集团股份有限公司 | Method for rapidly determining chloride ions in lithium battery copper foil electrolyte |
| CN113959966A (en) * | 2021-10-20 | 2022-01-21 | 山东恒邦冶炼股份有限公司 | Method for measuring chlorine content in antimony-containing arsenic trioxide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109781634A (en) | A kind of measuring method of chloride ion content | |
| CN105987900B (en) | The measuring method of sulfate ion in a kind of electrolyte for lithium ion battery | |
| CN103344641A (en) | Method for measuring zinc and nickel contents in zinc-nickel alloy electroplating solution | |
| CN104215738B (en) | A kind of method of Zr, Cu, Ni content in simultaneous determination Zr-Cu-Ni-Al non-crystaline amorphous metal | |
| Christian et al. | Coulometric Titration of Ammonia with Hypobromite Using Direct Amperometric End Point Detection. | |
| CN106525906B (en) | A method of content of fluoride ion in detection per-fluoroalkyl sulfonyl inferior amine salt | |
| CN110361339A (en) | The detection method of chloride in imidodisulfuryl fluoride lithium salt | |
| CN111157520B (en) | Quantitative detection reagent and detection method for sodium polydithio-dipropyl sulfonate in acid copper electroplating solution | |
| CN104076083A (en) | Heavy metal ion concentration test method adopting secondary sample injection | |
| CN1912611A (en) | Analysing method of excess alumina content in aluminium electrolyte | |
| CN103837381B (en) | The detection method of lithium ion content in anode oxidation groove liquid | |
| CN101576481B (en) | Method for measuring contents of anionic surface active substances by methylene blue spectrometry | |
| CN110346353A (en) | The test method of alumina content in a kind of aluminum electrolytic capacitor electrode foil | |
| Doménech-Carbó et al. | Electrochemical determination of boron in minerals and ceramic materials | |
| CN109030389A (en) | The measuring method of total sulfur in a kind of anode material for lithium-ion batteries | |
| CN104991035B (en) | Method for determining free methanesulfonic acid content in tin lead bismuth alloy electroplating solution | |
| CN101576529A (en) | Determination of sliver using precision electric potential titration | |
| CN101344504A (en) | Method for measuring fluorine content in system containing multiple cations | |
| CN106404870A (en) | Measuring method of trivalent and tetravalent vanadium ions in vanadium battery electrolyte | |
| Burmakina et al. | Determination of manganese (II) in wines by stripping voltammetry on solid electrodes | |
| CN108362822A (en) | A kind of scaling method of EDTA concentration of standard solution and its application | |
| CN112630213A (en) | Chemical analysis method for detecting ceramic metallization electroplating solution | |
| CN113311051A (en) | Method for rapidly determining content of free acid in lithium hexafluorophosphate electrolyte by coulometric titration digital end point method | |
| CN111007133A (en) | Method for determining chloride ions in electrolyte for aluminum electrolytic capacitor | |
| CN105628689A (en) | Method for measuring nickel content in Zn-Ni alloy coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190521 |
|
| RJ01 | Rejection of invention patent application after publication |