CN106442663A - Analysis method for hydrofluoric acid content in pickling solution - Google Patents
Analysis method for hydrofluoric acid content in pickling solution Download PDFInfo
- Publication number
- CN106442663A CN106442663A CN201611080781.5A CN201611080781A CN106442663A CN 106442663 A CN106442663 A CN 106442663A CN 201611080781 A CN201611080781 A CN 201611080781A CN 106442663 A CN106442663 A CN 106442663A
- Authority
- CN
- China
- Prior art keywords
- solution
- standard
- prepare
- electrode
- acid content
- 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
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
Landscapes
- 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)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to an analysis method for a hydrofluoric acid content in a pickling solution and belongs to the technical field of hydrofluoric acid analysis methods. A fluorinion selective electrode and a reference electrode are put in a solution to constitute a battery, and a potential value of the solution to be measured has a linear relationship with a logarithm value of fluorinion activity. A method of quantitatively adding a sample is used to calculate a change in a fluorinion concentration via a measured E value, and the fluorinion concentration is converted to the concentration of hydrofluoric acid via calculation at last. An accuracy and recovery rate experiment by detecting the influence of a nitric acid content in a pickling tank and detection temperature on fluorinion detection shows the method can meet requirements of routine pickling tank solution maintenance in a workshop.
Description
Technical field
The present invention relates in a kind of pickle fluohydric acid content analysis method, belong to analysis Fluohydric acid. method and technology neck
Domain.
Background technology
The chemical analysis detection of descaling bath in process of surface treatment requires to carry out the detection of Fluohydric acid., but traditional analysis hydrogen
The method of fluoric acid need to be using to chloroacetic acid and medicine thorium nitrate, and chloroacetic acid belongs to toxic articles, by country to toxic articles management
Require, need to carry out strict management and control, increased the difficulty of management, be also required to careful, otherwise gently simultaneously in use
Then lead to the symptoms such as dizziness, headache, Nausea and vomiting, heavy then cause consciousness forfeiture, reflexive respiratory arrest etc. suddenly, and nitric acid
Thorium is radioactive substance, not only environment is had an impact, will also result in infringement to the body of operator simultaneously, and due to country
Closely strengthen the management and control to this kind of material a bit, lead to current procuring and provisioning extremely difficult, and may therefore class reason lead to give birth to
The delay of product progress.Therefore it is badly in need of a kind of quick, accurate, nontoxic analysis method, the environmental protection meeting Fluohydric acid. detection will
Ask.
Content of the invention
It is an object of the invention to provide Fluoride Analysis in a kind of acid pickling groove liquid, it is mainly used in ion selective electrode method
The experiment of fluohydric acid content in measurement acid pickling groove liquid.
The present invention to achieve these goals, adopts the following technical scheme that：
The analysis method of fluohydric acid content in a kind of pickle, this analysis method comprises the steps of：
The alloy being dissolved is TC4, and meltage is 2g/L, and time of repose is more than 24h；Carry out the fluorion inspection of three kinds of systems
Survey, recovery of standard addition, between 95.38%-102.88%, meets measurement requirement, and concrete mode is as follows：
1st, prepare total ionic strength and adjust buffer solution：Prepared with sodium nitrate and sodium acetate solution, test solution pH is adjusted with glacial acetic acid
Value, meets pH value between 6.00 ~ 7.00；
2nd, prepare fluorination sodium standard solution：Weigh the working standard reagent fluorination in 105 DEG C ~ 110 DEG C dryings to constant weight exactly
Sodium 4.19g, the 50ml that adds water dissolve, and are diluted with water to 200ml, shake up；Then stepwise dilution, obtain 0.5,0.1,0.02,
0.004th, the fluorine standard solution of 0.0008mol/L；
3rd, prepare pickle：Nitric acid content：450g/L, the alloy being dissolved is 2g/L for TC4 meltage, and time of repose is more than
24h；
4th, standard test solution is prepared：
pF1：1*10-1 mol/LF：Take 5*10-1 mol/LF solution 20ml, add TISAB solution 20ml, be diluted to 100ml；
pF1.699：2*10-2 mol/LF：Take 1*10-1 mol/LF solution 20ml, add TISAB solution 20ml, be diluted to
100ml；
With the method for same gradient dilution, prepare solution pF2.396, pF3.097, pF3.796；
5th, pF Electrode Calibration：In ion meter pX measuring state, demarcate electrode, instrument enters demarcating module, uses standard testing curve
Solution is demarcated to electrode from low to high successively by concentration.
6th, measure：Instrument is switched to " sample interpolation pattern ", sets relevant parameter, add and be set to 0.2ml at the beginning of volume,
Start to measure；
After clean for electrode clean, put into standard solution；After stablizing Deng display, after confirmation, add prepare liquid 0.2ml, registration is steady
After fixed, if voltage change is in 16 ~ 40mv, press " confirmation " key, calculating concentration, parallel survey four times.
The present invention adopts ion meter, and fluoride ion selective electrode and reference electrode are put in solution, at this moment constitutes one group of electricity
Pond, the potential value of detected solution is linear with the logarithm value of fluorion activity.Just may be used using the method being quantitatively adding sample
By recording the change that E value calculates the concentration of fluorion, by calculating the concentration being finally converted into Fluohydric acid..By detection acid
In washing trough, nitric acid content and detection temperature carry out accuracy and response rate experiment to the impact that fluorion detects, show that this method can
Meet the demand that daily workshop acid pickling groove liquid is safeguarded.
Beneficial effects of the present invention：
Detect the content of Fluohydric acid. in acid pickling groove liquid using Fluoride ion selective electrode method, compensate for chemical analysis field in this regard
Blank avoid using to environment to operator's poisonous and harmful substance, realize environmental protection detection.
Brief description
Fig. 1 is the flow chart of the present invention.
Specific embodiment
Imitate the Main Ingredients and Appearance of descaling bath, the alloy being dissolved is TC4, meltage is about 2g/L, and time of repose is more than
24h.Carry out the fluorion detection of three kinds of systems, recovery of standard addition, between 95.38%-102.88%, meets measurement requirement.Tool
Body experiment method is as follows：
1st, prepare total ionic strength and adjust buffer solution（TISAB）：Prepared with certain proportion with sodium nitrate and sodium acetate solution, with
Test solution pH value is adjusted with glacial acetic acid, meets pH value between 6.00 ~ 7.00.
2nd, prepare fluorination sodium standard solution：Weigh the working standard reagent in 105 DEG C ~ 110 DEG C dryings to constant weight exactly
In small beaker, the 50ml that adds water dissolves sodium fluoride 4.19g, is diluted with water to 200ml, shakes up.Then stepwise dilution, obtains
0.5th, 0.1,0.02,0.004, the fluorine standard solution of 0.0008mol/L.
3rd, prepare pickle：Nitric acid content：450g/L, the alloy being dissolved is about 2g/L for TC4 meltage, during standing
Between be more than 24h.
4th, standard test solution is prepared：
pF1（1*10-1 mol/LF）：Take 5*10-1 mol/LF solution 20ml, add TISAB solution 20ml, be diluted to 100ml.
pF1.699（2*10-2 mol/LF）：Take 1*10-1 mol/LF solution 20ml, add TISAB solution 20ml, dilution
To 100ml.
With the method for same gradient dilution, prepare solution pF2.396, pF3.097, pF3.796.
5th, pF Electrode Calibration：In ion meter pX measuring state, then pressing " acknowledgement key " can demarcate electricity to press " demarcation " key
Pole.Instrument enters demarcating module.Successively electrode is demarcated from low to high by concentration with standard testing curve solution.
6 measurements：Instrument is switched to " sample interpolation pattern ", presses " measurement " key, set relevant parameter, add volume
Just it is set to 0.2ml, press " confirmation " key and start to measure.
After clean for electrode clean, put into standard solution.After stablizing Deng display, press " confirmation " key, add prepare liquid
0.2ml, after registration is stable, if voltage change is in 16 ~ 40mv, presses " confirmation " key, calculating concentration, parallel survey four times.
Claims (1)
1. in a kind of pickle the analysis method of fluohydric acid content it is characterised in that this analysis method comprises the steps of：
The alloy being dissolved is TC4, and meltage is 2g/L, and time of repose is more than 24h；Carry out the fluorion inspection of three kinds of systems
Survey, recovery of standard addition, between 95.38%-102.88%, meets measurement requirement, and concrete mode is as follows：
1st, prepare total ionic strength and adjust buffer solution：Prepared with sodium nitrate and sodium acetate solution, test solution pH is adjusted with glacial acetic acid
Value, meets pH value between 6.00 ~ 7.00；
2nd, prepare fluorination sodium standard solution：Weigh the working standard reagent fluorination in 105 DEG C ~ 110 DEG C dryings to constant weight exactly
Sodium 4.19g, the 50ml that adds water dissolve, and are diluted with water to 200ml, shake up；Then stepwise dilution, obtain 0.5,0.1,0.02,
0.004th, the fluorine standard solution of 0.0008mol/L；
3rd, prepare pickle：Nitric acid content：450g/L, the alloy being dissolved is 2g/L for TC4 meltage, and time of repose is more than
24h；
4th, standard test solution is prepared：
pF1：1*10-1 mol/LF：Take 5*10-1 mol/LF solution 20ml, add TISAB solution 20ml, be diluted to 100ml；
pF1.699：2*10-2 mol/LF：Take 1*10-1 mol/LF solution 20ml, add TISAB solution 20ml, be diluted to
100ml；
With the method for same gradient dilution, prepare solution pF2.396, pF3.097, pF3.796；
5th, pF Electrode Calibration：In ion meter pX measuring state, demarcate electrode, instrument enters demarcating module, uses standard testing curve
Solution is demarcated to electrode from low to high successively by concentration；
6th, measure：Instrument is switched to " sample interpolation pattern ", sets relevant parameter, add and be set to 0.2ml at the beginning of volume, open
Begin to measure；
After clean for electrode clean, put into standard solution；After stablizing Deng display, after confirmation, add prepare liquid 0.2ml, registration is steady
After fixed, if voltage change is in 16 ~ 40mv, press " confirmation " key, calculating concentration, parallel survey four times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611080781.5A CN106442663A (en) | 2016-11-30 | 2016-11-30 | Analysis method for hydrofluoric acid content in pickling solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611080781.5A CN106442663A (en) | 2016-11-30 | 2016-11-30 | Analysis method for hydrofluoric acid content in pickling solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106442663A true CN106442663A (en) | 2017-02-22 |
Family
ID=58224151
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611080781.5A Pending CN106442663A (en) | 2016-11-30 | 2016-11-30 | Analysis method for hydrofluoric acid content in pickling solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106442663A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375647A (en) * | 2018-03-02 | 2018-08-07 | 沈阳飞机工业（集团）有限公司 | A kind of titanium alloy etching tank liquid chemical analysis method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078709A (en) * | 2007-06-12 | 2007-11-28 | 巨石集团有限公司 | Glass fluorinion content measuring method |
| CN104267083A (en) * | 2014-10-21 | 2015-01-07 | 山东黄金矿业(莱州)有限公司精炼厂 | Method for measuring content of fluorine ions in hydrochloric acid by using ion meter |
| CN104730201A (en) * | 2015-03-04 | 2015-06-24 | 南昌航空大学 | Measurement method for content of hydrofluoric acid in titanium alloy pickling solution |
-
2016
- 2016-11-30 CN CN201611080781.5A patent/CN106442663A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101078709A (en) * | 2007-06-12 | 2007-11-28 | 巨石集团有限公司 | Glass fluorinion content measuring method |
| CN104267083A (en) * | 2014-10-21 | 2015-01-07 | 山东黄金矿业(莱州)有限公司精炼厂 | Method for measuring content of fluorine ions in hydrochloric acid by using ion meter |
| CN104730201A (en) * | 2015-03-04 | 2015-06-24 | 南昌航空大学 | Measurement method for content of hydrofluoric acid in titanium alloy pickling solution |
Non-Patent Citations (3)
| Title |
|---|
| 沈观根: "酸洗槽液中氢氟酸的测定", 《航天工艺》 * |
| 董惠英 等: "氟离子选择性电极法测定化工含氟废水", 《化工环保》 * |
| 许康 等: "氟离子选择性电极-标准加入法测定硫酸锌溶液中氟", 《冶金分析》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375647A (en) * | 2018-03-02 | 2018-08-07 | 沈阳飞机工业（集团）有限公司 | A kind of titanium alloy etching tank liquid chemical analysis method |
| CN108375647B (en) * | 2018-03-02 | 2020-11-06 | 沈阳飞机工业（集团）有限公司 | Chemical analysis method for titanium alloy corrosion tank liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108445057A (en) | A kind of preparation and analysis method for detecting the electrochemical sensor of heavy metal ion | |
| CN104267083A (en) | Method for measuring content of fluorine ions in hydrochloric acid by using ion meter | |
| Zhuo et al. | Activity coefficients of individual ions in aqueous solutions of sodium halides at 298.15 K | |
| CN106525906B (en) | A method of content of fluoride ion in detection per-fluoroalkyl sulfonyl inferior amine salt | |
| CN104614416A (en) | Detecting method of fluoride in soldering paste | |
| CN106770512A (en) | The assay method of fluohydric acid content in a kind of nitric hydrofluoric acid type Acidwash solution | |
| CN104198484A (en) | Method for testing fluorine content in solution | |
| CN103743804A (en) | Organic phosphorus electrochemical biosensor based on adsorption of nano particles | |
| Elzanfaly et al. | In-line potentiometric monitoring of dissolution behavior of verapamil hydrochloride versus traditional pharmacopeial method: A comparative study | |
| CN106442663A (en) | Analysis method for hydrofluoric acid content in pickling solution | |
| CN109212002A (en) | A method of with chloride ion in potentiometric titration detection niacin | |
| CN104569112A (en) | Continuous on-line water ion concentration detection method based on ion selective electrode | |
| Xu et al. | Development of electrochemical method for the determination of olaquindox using multi-walled carbon nanotubes modified glassy carbon electrode | |
| CN102937614A (en) | Method for analyzing content of free fluorin in lithium ion battery electrolyte salt LiBF4 | |
| CN104181158A (en) | Method for measuring concentration of tetravalent and pentavalent vanadium ions in vanadium battery electrolyte | |
| CN105466982A (en) | Method for detecting heavy metal in water | |
| Segura et al. | Miniaturization of cyclic voltammetry electronic systems for remote biosensing | |
| CN104237343A (en) | Preparation method and application of zirconium dioxide/porous polyaniline modified electrode | |
| CN105891289A (en) | Electrochemical method for measuring oxidation inducing time of grease | |
| CN107462567A (en) | A kind of method for determining lithium content in zirconium and zircaloy | |
| CN202383116U (en) | Distillation device for measuring fluorine ions | |
| CN102435663B (en) | Method for determining relative content of nickel hexacyanoferrate insoluble and soluble structures | |
| CN102323232B (en) | Method for testing content of potassium | |
| Ji et al. | Determination of the Activity Coefficients of NaCl in the System NaCl–NH4Cl–H2O | |
| CN108181372A (en) | The detection method of nitre sulphur ketone residual quantity in corn |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170222 |
|
| RJ01 | Rejection of invention patent application after publication |