CN103823017A - Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy - Google Patents
Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy Download PDFInfo
- Publication number
- CN103823017A CN103823017A CN201310538554.2A CN201310538554A CN103823017A CN 103823017 A CN103823017 A CN 103823017A CN 201310538554 A CN201310538554 A CN 201310538554A CN 103823017 A CN103823017 A CN 103823017A
- Authority
- CN
- China
- Prior art keywords
- solution
- titanium alloy
- dilution
- milliliter
- etchant 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
Landscapes
- ing And Chemical Polishing (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for accurate measurement on nitric acid content of a chemical corrosion solution for titanium alloy. With the presence of high concentration sulfuric acid, NO<3-> is reduced into NO through ferrous sulfate, and the excessive ferrous sulfate is titrated through potassium permanganate standard solution; a Gaikeli funnel is used during the experiment, carbon dioxide produced by sodium bicarbonate ensures complete exhausting of air from an erlenmeyer flask, and carbon dioxide constantly produced during the reaction protects the solution and prevents the entry of external air, so as to ensure sufficient reduction of the solution while preventing the interference from oxygen in the air. The above points show that the experiment method saves time, and can eliminate the influence of metal impurities and other weak-acid or weak-base salt solutions; the end point mutation is obvious during solution titration, so as to measure more accurate nitric acid content.
Description
Technical field
The invention belongs to chemical analysis technology field, be specially the method for nitric acid content in a kind of Accurate Determining titanium alloy chemistry etchant solution.
Background technology
Titanium alloy chemistry etchant solution Main Ingredients and Appearance is nitric acid and hydrofluorite, is applied to the milling of titanium alloy, except dust, painted and surperficial pre-etching etc.
At present, the mensuration of nitric acid content in GB and navigation mark, mainly contains acid base titration and Oxidation-Reduction Volumetric Analysis Method.In the method that can inquire, relate to the steps such as sample separates, point gets, redox, titration, and there is following restriction in conventional method: acid base titration can only be applied to the solution of metal impurities not and other weak acid and weak base salts; To the mensuration of nitric acid content in acid mixture, can only be calculated by indirect method; In the time of application oxidation-reduction method, because of the interference of oxygen in air, the accuracy of measurement of nitric acid content is lower; In relevant criterion, redox titration also needs instrumentation-potentiometric titrimeter.
Summary of the invention
The technical matters solving
The problem existing for solving prior art, provide a kind of quick, direct, process is simple, titration end-point sudden change obviously, and the assay method of nitric acid content in the chemical corrosion solution that accuracy is high, precision is good, and can be used in the mensuration of nitric acid in polyacid mixed solution, even if contain a large amount of TiO in solution
2+, Fe
3+also can not impact measuring Deng metallic impurity, the present invention proposes the method for nitric acid content in a kind of Accurate Determining titanium alloy chemistry etchant solution.
Technical scheme
Technical scheme of the present invention is:
The method of nitric acid content in described a kind of Accurate Determining titanium alloy chemistry etchant solution, is characterized in that: adopt following steps:
Step 1: get V milliliter titanium alloy chemistry etchant solution, the dilution of preparation M milliliter titanium alloy chemistry etchant solution;
Step 2: the dilution of the titanium alloy chemistry etchant solution of preparing from step 1, divide and get N milliliter dilution to conical flask;
Step 3: add excessive ferrous sulfate standard solution, excess bicarbonate solid, sulfuric acid to dividing in the conical flask of getting N milliliter dilution successively, obtain the dilution of the titanium alloy chemistry etchant solution being reduced;
Step 4: funnel in described conical flask bottle mouth position closes the lid gram, in funnel, add saturated sodium bicarbonate solution, obtain sealing by the dilution of the titanium alloy chemistry etchant solution being reduced;
Step 5: the conical flask that is stamped sealing funnel is heated to boiling, make solution in conical flask be become faint yellow from brown, take off conical flask, place and be no more than 5 minutes at room temperature, again conical flask is positioned over and in cold water, is cooled to room temperature, the dilution of the titanium alloy that obtains being reduced chemistry etchant solution;
Step 6: take off funnel in lid gram, toward adding distil water in conical flask, being titrated to solution with Standard Potassium Permanganate Solution, to be light red be terminal, obtains the titration dilution of the chemical etchant solution of titanium alloy completely; Wherein the actual concentrations of Standard Potassium Permanganate Solution is Cmol/L, and the Standard Potassium Permanganate Solution of consumption is V2 milliliter;
Step 7: adopt the N milliliter dilution in N ml distilled water alternative steps 2, then repeating step 3, to step 6, carries out blank test, and the Standard Potassium Permanganate Solution that obtains consuming in blank test is V1 milliliter;
Step 8: according to formula
Obtain nitric acid content HNO in titanium alloy chemistry etchant solution
3(g/L), wherein V0 is the titanium alloy chemistry etchant solution volume containing in the N milliliter dilution got of step 2 point, V0=V*N/M.
The method of nitric acid content in described a kind of Accurate Determining titanium alloy chemistry etchant solution, it is characterized in that: the process of preparing the dilution of titanium alloy chemistry etchant solution in step 1 is: with teflon pipette, extract V milliliter titanium alloy chemistry etchant solution, be placed in the M milliliter teflon volumetric flask that is added with in advance distilled water, add distilled water diluting to scale, this solution is shaken up to the dilution of the titanium alloy chemistry etchant solution that obtains mixing.
Beneficial effect
The advantage of this method:
(1) this method is not subject to the impact of metallic impurity, can measure the solution of metal impurities and other weak acid and weak base salts.
(2) this method can directly be measured the content of nitric acid in acid mixture.
(3) fast, step is easy in this method reaction, and titration end-point changes obviously.
(4) this method is used funnel in lid gram, under the protection of carbon dioxide, reacts, and has well completely cut off air, has removed the impact that in air, oxygen is measured nitric acid, and method accuracy is high.
(5) do not need special equipment or instrument, method is simple.
The present invention, under high-concentration sulfuric acid exists, uses ferrous sulphate reductive NO
3-become NO, excessive ferrous sulphate carries out titration with Standard Potassium Permanganate Solution.In process of the test use lid gram in funnel; the carbon dioxide that sodium bicarbonate produces is discharged the air in conical flask completely; the carbon dioxide constantly producing in reaction plays a protective role to solution, has completely cut off extraneous air, avoids the interference of oxygen in air when solution is fully reduced.Can find out from above these aspects, the method for this experiment is saved time, and has got rid of the impact of the solution of metallic impurity and other weak acid and weak base salts.When solution titration, end point mutation is obvious, can obtain nitric acid content more accurately.
Embodiment
Below in conjunction with specific embodiment, the present invention is described:
Embodiment 1:
The present embodiment is take titanizing groove milling liquid as example, and the wherein method of nitric acid content of measuring adopts following steps:
Step 1, accurately draws 5.00mL titanium alloy chemistry etchant solution with teflon transfer pipet, is placed in the 500mL teflon volumetric flask that is added with in advance 400 ml distilled waters, adds distilled water diluting to scale, and this solution is shaken up.The dilution of the titanium alloy chemistry etchant solution that obtains mixing.
Step 2, accurately draws the above-mentioned dilution of 5.00mL with teflon transfer pipet, is placed in 500mL conical flask.Obtain a point dilution of getting the titanium alloy chemistry etchant solution in 500mL conical flask.
Step 3, accurately adds 25.00mL0.1mol/L ferrous sulphate standard solution to point getting in the 500mL conical flask of dilution of titanium alloy chemistry etchant solution, then adds successively 10g sodium bicarbonate solid, adds rapidly 25mL sulfuric acid.Obtain the dilution of the titanium alloy chemistry etchant solution being reduced.
Step 4, funnel in above-mentioned 500mL conical flask bottle mouth position closes the lid gram adds saturated sodium bicarbonate solution in funnel.Obtain sealing by the dilution of the titanium alloy chemistry etchant solution being reduced.
Step 5, the 500mL conical flask that is stamped sealing funnel is placed on electric furnace and is heated to boil, solution is become faint yellow from brown, take off immediately the 500mL conical flask on electric furnace, in room temperature, place 2 minutes, more above-mentioned 500mL conical flask is positioned over and in cold water, is cooled to room temperature.The dilution of the titanium alloy chemistry etchant solution that obtains being reduced.
Step 6, takes off funnel in lid gram, and toward adding distil water 200-250mL in above-mentioned 500mL conical flask, being titrated to solution with Standard Potassium Permanganate Solution, to be light red be terminal.Obtain the titration dilution of titanium alloy chemistry etchant solution completely.Wherein the actual concentrations of Standard Potassium Permanganate Solution is Cmol/L, and the Standard Potassium Permanganate Solution of consumption is V2 milliliter.
Step 7: use in addition 5 milliliters of dilutions in 5 ml distilled water alternative steps 2, then repeating step 3, to step 6, carries out blank test, and the Standard Potassium Permanganate Solution that obtains consuming in blank test is V1 milliliter;
Step 8: according to formula
Obtain nitric acid content HNO in titanium alloy chemistry etchant solution
3(g/L), wherein V0 is the titanium alloy chemistry etchant solution volume containing in 5 milliliters of dilutions getting of step 2 point, V0=5*5/500 milliliter.In formula, 0.021 is the quality that 1.00 milliliters of Standard Potassium Permanganate Solutions are equivalent to nitric acid, and unit is gram, wherein Standard Potassium Permanganate Solution c (1/5KMnO
4)=1.0000mol/L.The present embodiment calculates nitric acid content HNO in titanizing groove milling liquid
3=320g/L.
Claims (2)
1. a method for nitric acid content in Accurate Determining titanium alloy chemistry etchant solution, is characterized in that: adopt following steps:
Step 1: get V milliliter titanium alloy chemistry etchant solution, the dilution of preparation M milliliter titanium alloy chemistry etchant solution;
Step 2: the dilution of the titanium alloy chemistry etchant solution of preparing from step 1, divide and get N milliliter dilution to conical flask;
Step 3: add excessive ferrous sulfate standard solution, excess bicarbonate solid, sulfuric acid to dividing in the conical flask of getting N milliliter dilution successively, obtain the dilution of the titanium alloy chemistry etchant solution being reduced;
Step 4: funnel in described conical flask bottle mouth position closes the lid gram, in funnel, add saturated sodium bicarbonate solution, obtain sealing by the dilution of the titanium alloy chemistry etchant solution being reduced;
Step 5: the conical flask that is stamped sealing funnel is heated to boiling, make solution in conical flask be become faint yellow from brown, take off conical flask, place and be no more than 5 minutes at room temperature, again conical flask is positioned over and in cold water, is cooled to room temperature, the dilution of the titanium alloy that obtains being reduced chemistry etchant solution;
Step 6: take off funnel in lid gram, toward adding distil water in conical flask, being titrated to solution with Standard Potassium Permanganate Solution, to be light red be terminal, obtains the titration dilution of the chemical etchant solution of titanium alloy completely; Wherein the actual concentrations of Standard Potassium Permanganate Solution is Cmol/L, and the Standard Potassium Permanganate Solution of consumption is V2 milliliter;
Step 7: adopt the N milliliter dilution in N ml distilled water alternative steps 2, then repeating step 3, to step 6, carries out blank test, and the Standard Potassium Permanganate Solution that obtains consuming in blank test is V1 milliliter;
Step 8: according to formula
Obtain nitric acid content HNO in titanium alloy chemistry etchant solution
3(g/L), wherein V0 is the titanium alloy chemistry etchant solution volume containing in the N milliliter dilution got of step 2 point, V0=V*N/M.
2. the method for nitric acid content in a kind of Accurate Determining titanium alloy chemistry etchant solution according to claim 1, it is characterized in that: the process of preparing the dilution of titanium alloy chemistry etchant solution in step 1 is: with teflon pipette, extract V milliliter titanium alloy chemistry etchant solution, be placed in the M milliliter teflon volumetric flask that is added with in advance distilled water, add distilled water diluting to scale, this solution is shaken up to the dilution of the titanium alloy chemistry etchant solution that obtains mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310538554.2A CN103823017A (en) | 2013-11-01 | 2013-11-01 | Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310538554.2A CN103823017A (en) | 2013-11-01 | 2013-11-01 | Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103823017A true CN103823017A (en) | 2014-05-28 |
Family
ID=50758180
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310538554.2A Pending CN103823017A (en) | 2013-11-01 | 2013-11-01 | Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103823017A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104360010A (en) * | 2014-11-15 | 2015-02-18 | 江西师范大学 | Analytic method for measuring content of each component in sulfuric acid and nitric acid mixture |
| CN106018669A (en) * | 2016-05-26 | 2016-10-12 | 沈阳富创精密设备有限公司 | Method for detecting concentration of nitric acid in chemical polishing solution containing nitric acid and phosphoric acid |
| CN109813836A (en) * | 2019-01-17 | 2019-05-28 | 瓮福（集团）有限责任公司 | The rapid assay methods of nitric acid in chemical polishing tank liquor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949859A (en) * | 2010-09-10 | 2011-01-19 | 江南机器（集团）有限公司 | Continuous determination method of sodium nitrite-potassium nitrate mixed salt in salt bath |
| CN102419325A (en) * | 2011-07-27 | 2012-04-18 | 中国科学院青海盐湖研究所 | Method for determining strontium calcium barium in strontium carbonate |
| CN102621273A (en) * | 2012-04-17 | 2012-08-01 | 昊诚光电（太仓）有限公司 | Method for detecting mixed acid solution in manufacturing process of polycrystalline silicon solar cell |
-
2013
- 2013-11-01 CN CN201310538554.2A patent/CN103823017A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949859A (en) * | 2010-09-10 | 2011-01-19 | 江南机器（集团）有限公司 | Continuous determination method of sodium nitrite-potassium nitrate mixed salt in salt bath |
| CN102419325A (en) * | 2011-07-27 | 2012-04-18 | 中国科学院青海盐湖研究所 | Method for determining strontium calcium barium in strontium carbonate |
| CN102621273A (en) * | 2012-04-17 | 2012-08-01 | 昊诚光电（太仓）有限公司 | Method for detecting mixed acid solution in manufacturing process of polycrystalline silicon solar cell |
Non-Patent Citations (2)
| Title |
|---|
| 彭玉玲 等: "硫酸亚铁按氧化还原滴定法测定钠硝石中硝酸根的含量", 《盐矿测试》, vol. 26, no. 2, 30 April 2007 (2007-04-30), pages 165 - 166 * |
| 无: "磷化液中硝酸浓度的测定", 《金属制品》, 25 October 1982 (1982-10-25), pages 35 - 37 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104360010A (en) * | 2014-11-15 | 2015-02-18 | 江西师范大学 | Analytic method for measuring content of each component in sulfuric acid and nitric acid mixture |
| CN106018669A (en) * | 2016-05-26 | 2016-10-12 | 沈阳富创精密设备有限公司 | Method for detecting concentration of nitric acid in chemical polishing solution containing nitric acid and phosphoric acid |
| CN109813836A (en) * | 2019-01-17 | 2019-05-28 | 瓮福（集团）有限责任公司 | The rapid assay methods of nitric acid in chemical polishing tank liquor |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101334365B (en) | Determination method for chloride ion content of temper rolling liquor for steel plate rolling | |
| CN106290334B (en) | The chemistry in detecting of cobalt and manganese content in cobalt manganese raw material | |
| CN104297246B (en) | Method for measuring magnesium content in aluminum magnesium alloy powder | |
| CN103439454B (en) | Method for measuring vanadium pentoxide content by potentiometric titration | |
| CN103512879A (en) | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy | |
| CN103823017A (en) | Method for accurate measurement on nitric acid content of chemical corrosion solution for titanium alloy | |
| CN103439328B (en) | The assay method of magnesium metal in inactivating magnesium desulfurizing agent | |
| CN101334379A (en) | Water fluorine content determination method | |
| CN103776953A (en) | Determination method of content of cobalt in lithium battery ternary positive electrode material | |
| Jaselskis et al. | Determination of micro and semimicroamounts of aluminum using fluoride activity electrode | |
| CN103454264A (en) | Determination method of contents of vanadium, titanium and chromium in natural microalloy iron powder | |
| CN109633079A (en) | A method of vanadium and ammonium content in detection metavanadate solution | |
| CN105467070A (en) | Method for quick measurement of ferric ion content in sulfate process titanium dioxide decomposing titanium liquor | |
| CN104215634A (en) | Method for determining content of tin in tungsten concentrate | |
| CN104101576A (en) | Method for determining nickel content in steel or iron alloy | |
| CN104062396A (en) | Method for measuring content of nitrogen in metal lithium and lithium alloy | |
| Lanza et al. | Differential-pulse polarographic determination of molybdenum in steel | |
| CN103954574A (en) | Method for testing content of tungsten in ferroniobium | |
| CN104515828A (en) | Calcium content determination method for low-calcium aluminum ferromanganese | |
| CN103592411B (en) | A kind of method of testing of capsule core release amount of concrete chemical self-repair microcapsule | |
| CN101344504A (en) | Method for measuring fluorine content in system containing multiple cations | |
| CN105021684B (en) | The measuring method of hydrogenation efficiency, oxidation efficiency and raffinate concentration during hydrogen dioxide solution production by anthraquinone process | |
| CN103175829A (en) | Rapid analysis method of copper in leachate | |
| Kriege et al. | The spectrophotometric determination of sulphur in iron alloys: Methylene blue method | |
| CN105842175A (en) | Method for determination of content of titanium in ferrosilicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140528 |