CN102680555A - Method for measuring free acid concentration in acid liquid - Google Patents
Method for measuring free acid concentration in acid liquid Download PDFInfo
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- CN102680555A CN102680555A CN201210092681XA CN201210092681A CN102680555A CN 102680555 A CN102680555 A CN 102680555A CN 201210092681X A CN201210092681X A CN 201210092681XA CN 201210092681 A CN201210092681 A CN 201210092681A CN 102680555 A CN102680555 A CN 102680555A
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Abstract
The invention provides a fast and accurate method for measuring free acid concentration in acid liquid. An automatic potentiometric titrator is used to measure total acidity of the acid liquid. EDTA (ethylene diamine tetraacetic acid) which prevents iron ions, aluminum ions and the like from hydrolyzing is used as a screening agent to eliminate influence of hydrolysis of the iron ions, the aluminum ions and the like to free acid measurement. The defect that pH jump of the free acid is fully or partially covered during automatic potentionmetric titration is avoided. Jump of equivalent point is increased, and accuracy of the measurement is increased. An analysis result is automatically calculated according to an input formula. Operation time from analysis to result obtaining is shortened to less than 10 minutes. In addition, the method is low in sampling amount, fine in reproducibility, and accurate in analysis results. By the method, labor intensity of analysts is reduced, and labor productivity is emancipated.
Description
Technical field
The present invention relates to the method for free acid concentration in the acid solution.
Background technology
In the flat cold-rolled sheet production run, carry out pickling to the continuous casting billet surface, to remove the iron scale on surface with acid solution.The free acid concentration of acid solution can produce certain influence to the surface treatment quality, so measure in the acid solution total Cf quickly and accurately the research and the improvement of pickling effect and acid cleaning process is had very big directive function.
Measure the manual titrimetry of many employings soda acid or the potentiometric titration of free concentration in the acid solution at present.Manual titration operation is loaded down with trivial details, length consuming time.During titration; Along with pH in the titration process raises; Ferric ion in the acid solution is prone to generate deposition with alkali and indicator; Disturb the judgement of terminal point, it is higher that the deposition consumption part sodium hydroxide that synkaingenesis becomes can cause measuring the result, even adopt variable color methyl orange early also can produce serious systematic error as indicator.If directly in potentiometric titration, carried out titration with standard solution of sodium hydroxide, titration results has shown a plurality of equivalent points, and each equivalent point hop is little, needs the equivalent point of artificial analysis and judgement free acid, is easy to generate ambiguity and mistake.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method of fast, accurately measuring in the acid solution free acid concentration, to eliminate the influence that iron, the hydrolysis of aluminium plasma are measured free acid.
For solving the problems of the technologies described above, the present invention provides a kind of method of fast, accurately measuring free acid concentration in the acid solution, and this method utilizes automatical potentiometric titrimeter that total acidity in the acid solution is measured; For the influence that elimination iron, the hydrolysis of aluminium plasma are measured free acid, be that screening agent prevents iron, aluminium plasma generation hydrolysis, the defective that the pH hop of free acid is covered wholly or in part when avoiding automatic potentiometric titration with EDTA; Thereby the equivalent point hop is increased, increased the accuracy of measuring, and calculate analysis result automatically through the formula of input; Make the running time calculate the result and foreshorten in the 10min from analyzing; And the method sampling amount in this project is little, favorable reproducibility, and analysis result is accurate; Reduce analyst's labour intensity effectively, liberated labour productive forces.It is characterized in that, may further comprise the steps:
Step 1, pipette an amount of acid solution to be measured, on automatical potentiometric titrimeter with free acid concentration scope in the preparatory titration of the standard solution of sodium hydroxide acid solution to be measured;
Step 2, pipette a acid solution to be measured in addition, add distilled water diluting and maybe need not dilute, make in the acid solution to be measured the concentration of free acid concentration and NaOH standard titration solution suitable, obtain treating the titration acid solution;
Step 3, in treating the titration acid solution, add the EDTA sodium salt solution, make and treat that the facile hydrolysis metallic ion is by complexing fully in the titration acid solution;
Step 4, on automatical potentiometric titrimeter with the automatic titration of NaOH standard titration solution, and pass through
Calculate and treat the concentration C of titration acid solution middle reaches from acid
(free acid)In the formula (1), V
AcidFor treating the acid solution volume of titration, C
(NaOH)Concentration, V for the NaOH standard titration solution
(NaOH)Titration volume for the NaOH standard titration solution;
Step 5, repeating step 2～4, the more than one free acid concentration of treating the titration acid solution that obtains is got the mean value of free acid concentration, is multiplied by the dilution ratio coefficient again, promptly draws the free acid concentration of acid solution to be measured.
Preferably, in the said adding EDTA sodium salt solution molal weight of EDTA with treat that the facile hydrolysis metallic ion molal weight in the titration acid solution is suitable.
Optimize, in said step 4,, treat the concentration C of titration acid solution free acid by automatic calculating of automatical potentiometric titrimeter and demonstration formula (1) input automatical potentiometric titrimeter
(free acid)
More optimal, will average and take advantage of dilution ratio coefficient computing input automatical potentiometric titrimeter, calculate and show the free acid concentration of acid solution to be measured automatically by automatical potentiometric titrimeter.
Beneficial effect of the present invention is:
The existence of EDTA sodium salt reagent; Effectively complexing the hydrolysis metallic ion in the acid solution, the pH hop of free acid is covered wholly or in part when avoiding automatic potentiometric titration, and does not have the hydrionic defective in the ferric hydroxide precipitate absorption acid solution; The equivalent point hop is increased, increased the accuracy of measuring.
Free acid pH hop is obvious, makes on automatical potentiometric titrimeter, to import computing formula, calculates analysis result automatically, accurately, fast.
Below in conjunction with embodiment technical scheme of the present invention is further specified.
Embodiment
(1) pipettes the acid solution of 1～10mL, add an amount of distilled water, on automatical potentiometric titrimeter,, confirm the probable ranges of free acid concentration in the acid solution to be measured with the preparatory titration of certain density standard solution of sodium hydroxide.
(2) pipette a acid solution to be measured in addition, add distilled water diluting and maybe need not dilute, make the concentration of dissociate in the acid solution to be measured acid concentration and NaOH standard titration solution suitable, obtain treating the titration acid solution.
(3) in treating the titration acid solution, add the EDTA sodium salt solution, make and treat that the facile hydrolysis metallic ion is by complexing fully in the titration acid solution; The addition of EDTA sodium salt solution should be slightly excessive, makes to shelter fully and can not interference measurement, is 1.05～1.5 times of facile hydrolysis metal.
(4) on automatical potentiometric titrimeter, import
Formula (1) and mean value, dilution factor computing formula; Calculate the free acid concentration C that treats the titration acid solution with NaOH standard titration solution automatic titrimeter
(free acid)
(5) repeating step (2)～(4); The two or more free acid concentrations of treating the titration acid solution that obtain; Automatical potentiometric titrimeter calculates the mean value of treating titration acid solution free acid concentration automatically, is multiplied by the dilution ratio coefficient of acid solution again, promptly draws the free acid concentration of acid solution to be measured.
Embodiment 1
The hydrochloric approximately 12mol/L of concentration of free acid in the preparatory calibrated and calculated electroplate liquid.
Preparation 0.1mol/L NaOH standard solution uses the Potassium Hydrogen Phthalate standard reagent to demarcate, and the concentration that obtains this NaOH standard titration solution is C
(NaOH)=0.1042mol/L.
Take by weighing about 3.72gEDTA-Na in the beaker of 500mL, add about 300mL water, low-temperature heat all is cooled to room temperature after the dissolving, is diluted to 1000mL, and obtaining concentration is the EDTA solution of 0.01mol/L.
Obtain the 10.00mL electroplate liquid in the 100mL volumetric flask, be diluted with water to scale.Get electroplate liquid 10.00mL after the dilution again in the 100mL volumetric flask, water is diluted to scale again.Get again two parts of solution 10.00mL after the dilution, put into the 100mL beaker respectively.Divide other, in two 100mL beakers, adding 5mL concentration is EDTA solution, the distilled water 40mL of 0.01mol/L, puts into the stirring magneton, and electrode is immersed in the solution.NaOH standard titration solution with 0.1042mol/L carries out potentiometric titration automatically; The NaOH standard titration solution volume that visible twice titration consumes from the titration figure is respectively 11.860mL and 11.740mL; Mean value is 11.800mL; Computing formula through editor's input is calculated, and shows that the concentration that draws the acid solution free acid is 12.2956mol/L.
Embodiment 2
The concentration of free sulfuric acid is about 2mol/L in the calibrated and calculated copper electrolyte in advance.
Preparation 0.1mol/L NaOH standard solution uses the Potassium Hydrogen Phthalate standard reagent to demarcate, and the concentration that obtains this NaOH standard titration solution is C
(NaOH)=0.1242mol/L.
Take by weighing about 18.61gEDTA-Na in the beaker of 100mL, add about 40mL water, low-temperature heat all is cooled to room temperature after the dissolving, is diluted to 100mL, and obtaining concentration is the EDTA solution of 0.5mol/L.
Obtain the 5.00mL electroplate liquid in the 100mL volumetric flask, be diluted with water to scale.Get two parts of solution 10.00mL after the dilution, put into the 100mL beaker respectively.Divide other, in two 100mL beakers, adding 15mL concentration is EDTA solution, the distilled water 30mL of 0.5mol/L, puts into the stirring magneton, and electrode is immersed in the solution.NaOH standard titration solution with 0.1242mol/L carries out potentiometric titration automatically; The NaOH standard titration solution volume that visible twice titration consumes from the titration figure is respectively 17.745mL and 17.735mL; Mean value is 17.740mL; Computing formula through editor is calculated automatically, shows that the concentration that draws the acid solution free acid is 2.2033mol/L.
Embodiment 3
The concentration of free acid is about 0.1mol/L in the calibrated and calculated Automobile Plate pickle in advance.
Preparation 0.1mol/L NaOH standard solution uses the Potassium Hydrogen Phthalate standard reagent to demarcate, and the concentration that obtains this NaOH standard titration solution is C
(NaOH)=0.1149mol/L.
Take by weighing about 3.72gEDTA-Na in the beaker of 500mL, add about 300mL water, low-temperature heat all is cooled to room temperature after the dissolving, is diluted to 1000mL, obtains the EDTA solution that concentration is about 0.01mol/L.
Obtain two parts of 2.00mL electroplate liquids respectively in the 100mL beaker, divide other, in two 100mL beakers, add 1mL0.01mol/LEDTA solution, distilled water 60mL, put into the stirring magneton, electrode is immersed in the solution.NaOH standard titration solution with 0.1149mol/L carries out potentiometric titration automatically; It is thus clear that the NaOH standard titration solution volume that twice titration consumes is respectively 1.727mL and 1.735mL, the concentration that calculates the acid solution free acid through the computing formula of editing automatically is 0.0994mol/L from titration figure.
It should be noted last that; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement technical scheme of the present invention; And not breaking away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (4)
1. method of measuring in the acid solution free acid concentration is characterized in that may further comprise the steps:
Step 1, pipette an amount of acid solution to be measured, on automatical potentiometric titrimeter with free acid concentration scope in the preparatory titration of the standard solution of sodium hydroxide acid solution to be measured;
Step 2, pipette a acid solution to be measured in addition, add distilled water diluting and maybe need not dilute, make in the acid solution to be measured the concentration of free acid concentration and NaOH standard titration solution suitable, obtain treating the titration acid solution;
Step 3, in treating the titration acid solution, add the EDTA sodium salt solution, make and treat that the facile hydrolysis metallic ion is by complexing fully in the titration acid solution;
Step 4, on automatical potentiometric titrimeter with the automatic titration of NaOH standard titration solution, and pass through
Calculate and treat the concentration C of titration acid solution middle reaches from acid
(free acid)In the formula (1), V
AcidFor treating the acid solution volume of titration, C
(NaOH)Concentration, V for the NaOH standard titration solution
(NaOH)Titration volume for the NaOH standard titration solution;
Step 5, repeating step 2～4, the more than one free acid concentration of treating the titration acid solution that obtains is got the mean value of free acid concentration, is multiplied by the dilution ratio coefficient again, promptly draws the free acid concentration of acid solution to be measured.
2. the method for free acid concentration is characterized in that in the mensuration acid solution according to claim 1, in the said adding EDTA sodium salt solution molal weight of EDTA with treat that the facile hydrolysis metallic ion molal weight in the titration acid solution is suitable.
3. the method for free acid concentration is characterized in that in the mensuration acid solution according to claim 1 and 2, in said step 4, with formula (1) input automatical potentiometric titrimeter, is treated the concentration C of titration acid solution free acid by automatic calculating of automatical potentiometric titrimeter and demonstration
(free acid)
4. the method for free acid concentration in the mensuration acid solution according to claim 3; It is characterized in that; In said step 5, will average and take advantage of dilution ratio coefficient computing input automatical potentiometric titrimeter, calculate and show the free acid concentration of acid solution to be measured automatically by automatical potentiometric titrimeter.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102879356A (en) * | 2012-09-28 | 2013-01-16 | 邢台钢铁线材精制有限责任公司 | Method for measuring concentration of passivation tank liquid for galvanization |
| CN103196979A (en) * | 2013-02-27 | 2013-07-10 | 哈尔滨飞机工业集团有限责任公司 | Determination method for sodium hydroxide in alkaline chemical milling solution for aluminum alloy |
| CN103412027A (en) * | 2013-08-01 | 2013-11-27 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for testing cobalt in high-chrome and high-temperature alloy |
| CN103412028A (en) * | 2013-08-01 | 2013-11-27 | 中国航空工业集团公司北京航空材料研究院 | Method for testing content of sodium oxide in silica sol |
| CN106872550A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
| CN107271603A (en) * | 2017-07-08 | 2017-10-20 | 湖南有色金属研究院 | A kind of copper electrolyte sulfuric acid, copper, the method for continuously measuring of nickel content |
| CN109164094A (en) * | 2018-08-23 | 2019-01-08 | 中航力源液压股份有限公司 | A kind of detection method of high temperature manganese phosphating liquor |
| CN111781081A (en) * | 2020-06-18 | 2020-10-16 | 邯郸钢铁集团有限责任公司 | Pickling line waste hydrochloric acid concentration detection device and method |
| CN113219025A (en) * | 2021-05-07 | 2021-08-06 | 安徽大学 | Method for quantitatively detecting potassium bromate |
| CN113533629A (en) * | 2021-07-20 | 2021-10-22 | 广东先导稀材股份有限公司 | Method for determining content of free hydrochloric acid in tellurium tetrachloride sample |
| CN113759073A (en) * | 2021-09-26 | 2021-12-07 | 山西沁新能源集团股份有限公司 | Analysis and detection method for multiple components in waste liquid or recovery liquid of mixed acid |
| CN115575561A (en) * | 2022-09-16 | 2023-01-06 | 核工业北京化工冶金研究院 | Method for measuring concentration of nitric acid in dissolving tank |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102879356A (en) * | 2012-09-28 | 2013-01-16 | 邢台钢铁线材精制有限责任公司 | Method for measuring concentration of passivation tank liquid for galvanization |
| CN103196979A (en) * | 2013-02-27 | 2013-07-10 | 哈尔滨飞机工业集团有限责任公司 | Determination method for sodium hydroxide in alkaline chemical milling solution for aluminum alloy |
| CN103196979B (en) * | 2013-02-27 | 2015-04-29 | 哈尔滨飞机工业集团有限责任公司 | Determination method for sodium hydroxide in alkaline chemical milling solution for aluminum alloy |
| CN103412027A (en) * | 2013-08-01 | 2013-11-27 | 中国航空工业集团公司北京航空材料研究院 | Analysis method for testing cobalt in high-chrome and high-temperature alloy |
| CN103412028A (en) * | 2013-08-01 | 2013-11-27 | 中国航空工业集团公司北京航空材料研究院 | Method for testing content of sodium oxide in silica sol |
| CN103412028B (en) * | 2013-08-01 | 2015-04-15 | 中国航空工业集团公司北京航空材料研究院 | Method for testing content of sodium oxide in silica sol |
| CN106872550B (en) * | 2015-12-11 | 2019-06-18 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
| CN106872550A (en) * | 2015-12-11 | 2017-06-20 | 上海梅山钢铁股份有限公司 | The detection method of free acid content in a kind of tin methane sulfonate system electroplate liquid |
| CN107271603A (en) * | 2017-07-08 | 2017-10-20 | 湖南有色金属研究院 | A kind of copper electrolyte sulfuric acid, copper, the method for continuously measuring of nickel content |
| CN109164094A (en) * | 2018-08-23 | 2019-01-08 | 中航力源液压股份有限公司 | A kind of detection method of high temperature manganese phosphating liquor |
| CN111781081A (en) * | 2020-06-18 | 2020-10-16 | 邯郸钢铁集团有限责任公司 | Pickling line waste hydrochloric acid concentration detection device and method |
| CN113219025A (en) * | 2021-05-07 | 2021-08-06 | 安徽大学 | Method for quantitatively detecting potassium bromate |
| CN113219025B (en) * | 2021-05-07 | 2023-07-25 | 安徽大学 | Method for quantitatively detecting potassium bromate |
| CN113533629A (en) * | 2021-07-20 | 2021-10-22 | 广东先导稀材股份有限公司 | Method for determining content of free hydrochloric acid in tellurium tetrachloride sample |
| CN113533629B (en) * | 2021-07-20 | 2024-03-26 | 广东先导稀材股份有限公司 | Method for measuring content of free hydrochloric acid in tellurium tetrachloride sample |
| CN113759073A (en) * | 2021-09-26 | 2021-12-07 | 山西沁新能源集团股份有限公司 | Analysis and detection method for multiple components in waste liquid or recovery liquid of mixed acid |
| CN115575561A (en) * | 2022-09-16 | 2023-01-06 | 核工业北京化工冶金研究院 | Method for measuring concentration of nitric acid in dissolving tank |
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Application publication date: 20120919 |