CN104730201B - Measurement method for content of hydrofluoric acid in titanium alloy pickling solution - Google Patents
Measurement method for content of hydrofluoric acid in titanium alloy pickling solution Download PDFInfo
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Abstract
The invention discloses a measurement method for content of hydrofluoric acid in a titanium alloy pickling solution. The titanium alloy pickling solution comprises the main components including nitric acid, the hydrofluoric acid and fluorotitanic acid. The measurement method adopts an acid-base titration method for measuring the content of the fluorotitanic acid, and adopts a calcium fluoride precipitation method for measuring the content of total fluorine in a bath solution; and the content of the fluorine in the fluorotitanic acid is subtracted by the content of the total fluorine to obtain the content of the hydrofluoric acid in the solution. The measurement method has the advantages that the interferences caused by the fluorotitanic acid can be effectively avoided; the adding standard recovery rate of the content of the hydrofluoric acid, measured by adopting the method, is more than 95%; and the determination requirements on the concentration of the hydrofluoric acid are met and the production can be smoothly carried out.
Description
Technical field
The present invention relates to a kind of analysis method of solution and in particular in a kind of titanium alloy pickle fluohydric acid content survey
Amount method.
Background technology
Titanium alloy because having excellent corrosion-resistant, high specific strength, high tenacity and the performance characteristics such as solderable, in aeroplane engine
There is important application in machine field, and the titanium alloy consumption of some advanced aero engines has accounted for the 25 ~ 40% of engine weight, this
Just the quality of titanium alloy parts is put forward higher requirement, and its quality testing means is mainly fluorescent penetrant detection.
Fluorescent penetrant detection is one of important method of the industrial component surface integrity of inspection.Titanium alloy parts glimmering
Light Liquid penetrant testing, is that the optical characteristics when ultraviolet irradiates detect that the opening of surface of the work lacks by some fluorescent materials
Fall into, this method is quick, accurately.Make a general survey of advanced engine component detection technique both at home and abroad, the parts of electromotor more than 90% need
Carry out penetrating inspection, this detection method has become the key technology ensureing end product quality.
The main technological steps that titanium alloy carries out fluorescent penetrant detection include: oil removing, washing, pickling, drying, infiltration, breast
Change, washing, be dried, imaging, be dried, observation, washing etc., wherein, pickling is most important step before fluorescent penetrant detection, and sour
In washing liquid, the content of Fluohydric acid. directly affects the surface quality of titanium alloy, and therefore, rapid and accurate determination fluohydric acid content, to raising
The quality of titanium alloy pickling processes and efficiency, have important practical significance at present.Meanwhile, efficiently Fluohydric acid. detection technique is
The key point of the further investigation of titanium alloy acid cleaning process and its mechanism.
At present, corporate boss will using thorium nitrate titration survey fluohydric acid content, this method with alizarin red s indicator, with a chloroethene
Acid buffering test solution ph.For newly joining tank liquor, this method is more accurate, and recovery of standard addition is 97 ~ 100%, and longer to use time
Tank liquor, due to the interference of impurity in tank liquor, the response rate of this method only has 85% ~ 90%.Additionally, the titration end-point of this method is difficult to judge
(gradual change and not mutated), therefore this method is difficult to instruct actual production.
Content of the invention
The present invention provides a kind of measuring method of fluohydric acid content in titanium alloy pickle, and the method disclosure satisfy that actual life
The needs producing, the high and practical feature of favorable reproducibility, accuracy.
The present invention is achieved like this, the measuring method of fluohydric acid content in a kind of titanium alloy pickle, first adopts acid
The method of alkalimetric titration measures the content of fluotitanic acid, then measures total Oil repellent using calcium chloride precipitation method, is then subtracted according to total fluoro quantity
Remove the Oil repellent in fluotitanic acid, just can calculate the content obtaining Fluohydric acid. in solution.
(1) determination of acid-basetitration fluotitanic acid content, accurately pipettes titanium alloy pickle 5 ml in 100 ml plastics capacity
In bottle, it is diluted with water to scale, shakes up, above-mentioned diluent pipettes 5 ml in 250 ml conical flasks, add in conical flask
Enter 10 ~ 20ml saturated potassium chloride solution, 15 ~ 30 ml dehydrated alcohol；Add 1 ~ 2 phenolphthalein indicator in above-mentioned test solution again, drip
Plus 0.1039 mol/l naoh standard solution to test solution become pink into terminal；Above-mentioned test solution is heated to just seething with excitement, continues Deca
0.1039 mol/l naoh standard solution to test solution become pink into terminal, record consumption v1.
(2) calcium chloride precipitation method measures total Oil repellent, again pipettes titanium alloy pickle 5 ml in 100 ml plastics capacity
In bottle, it is diluted with water to scale, shakes up, above-mentioned diluent pipettes 5 ml in 250ml beaker, and add 10 ~ 20 ml to go
Ionized water；To in beaker, Deca 2 mol/l naoh solution 3 ~ 5 ml, is heated to just seething with excitement, and flow water-cooled；By the examination after cooling
Liquid is fully transferred in suction funnel, and microporous filter membrane sucking filtration obtains filtrate.
Gained filtrate is fully transferred in 500 ml conical flasks, adds 1 ~ 2 methyl red indicator, first Deca 6 mol/
L hydrochloric acid is micro- red to solution, then Deca 0.1039 mol/l naoh standard solution just turns yellow as terminal to test solution.
Accurately add 20 ml chlorination calcium standard solutions, heated and boiled 5 min in above-mentioned test solution, be air cooled to micro- after room temperature
Hole filter membrane sucking filtration obtains filtrate.Filtrate is fully transferred in 250 ml conical flasks, adds 2mol/l naoh molten in above-mentioned test solution
Liquid, adds the 2 mol/l naoh solution of 1.25 ml, and adds solid calcon-carboxylic acid 0.05 g, use edta in every 10 ml test solutions
It is terminal that titrand drop to solution to be changed into pure blue from claret, and records its consumption v3.Parallel laboratory test three times, simultaneously
Do blank experiment.
(3) deduct the Oil repellent in the fluotitanic acid content of measurement with total Oil repellent of measurement, obtain in titanium alloy pickle
Fluohydric acid content, its concrete formula is as follows: fluohydric acid content is calculated as follows:
(1)
In formula: chfThe concentration of Fluohydric acid., g/l in titanium alloy pickle；
c1The concentration of sodium hydroxide titrand, mol/l；
v1The volume of the standard solution of sodium hydroxide being consumed, ml；
c2The concentration of calcium chloride titrand, mol/l；
v2The volume of the calcium chloride titrand being quantitatively adding, ml；
c3The concentration of edta titrand, mol/l；
v3The volume of the edta standard solution being consumed, ml；
v0The volume of taken tank liquor, ml；
The relative molar mass of 20.01 hf, g/mol.
The invention has the advantage that (1) this analysis method is using hydrogen fluorine in " calcium fluoride precipitate+acid base titration " test pickle
The content of acid, recovery of standard addition reaches height, can reach 95% ~ 105%；(2) this analysis method is accurate and effective, low cost, and enterprise produces
Easily grasp；(3) this analysis method can be analyzed to the fluohydric acid content in titanium alloy pickle in commercial production and safeguard.
Specific embodiment
For the accuracy of check analyses method, recovery of standard addition test, mark-on thing are carried out to certain 4 unknown dynamic pickles
For Fluohydric acid., 3 concentration levels of mark-on.Specific implementation method is as follows:
As former state: take dynamic pickle 50 ml in 100ml plastics volumetric flask, be diluted with water to graduation mark, shake up.
Mark-on sample 1: take dynamic pickle 50 ml in 100ml plastics volumetric flask, add the hydrogen that concentration is 8.650mol/l
Fluoric acid 20ml, is diluted with water to graduation mark, shakes up.
Mark-on sample 2: take dynamic pickle 50 ml in 100ml plastics volumetric flask, add the hydrogen that concentration is 8.650mol/l
Fluoric acid 25ml, is diluted with water to graduation mark, shakes up.
Mark-on sample 3: take dynamic pickle 50 ml in 100ml plastics volumetric flask, add the hydrogen that concentration is 8.650mol/l
Fluoric acid 30ml, is diluted with water to graduation mark, shakes up.
Then according to aforesaid analysis method is analyzed according to identical operating procedure to above-mentioned sample, acquired results are shown in
Table 1, table 2, table 3, table 4.
The recovery of standard addition experimental result of the dynamic tank liquor 1 of table 1
The recovery of standard addition experimental result of the dynamic tank liquor 2 of table 2
The recovery of standard addition experimental result of the dynamic tank liquor 3 of table 3
The recovery of standard addition experimental result of the dynamic tank liquor 4 of table 4
From above-mentioned analysis result, the recovery of standard addition of the analysis method of the present invention reaches the requirement (95% that enterprise specifies
~ 105%), meet production requirement.
Claims (1)
1. in a kind of titanium alloy pickle fluohydric acid content measuring method it is characterised in that: first adopt acid base titration method
Measure the content of fluotitanic acid, more total Oil repellent is measured using calcium chloride precipitation method, then deducted in fluotitanic acid according to total fluoro quantity
Oil repellent, just can calculate the content obtaining Fluohydric acid. in solution；
Described use determination of acid-basetitration fluotitanic acid content, its method is:
(1) accurately pipette titanium alloy pickle 5 ml in 100 ml plastics volumetric flasks, be diluted with water to scale, shake up,
(2) pipette 5 ml in above-mentioned diluent in 250 ml conical flasks, add 10 ~ 20ml saturation potassium chloride in conical flask
Solution, 15 ~ 30 ml dehydrated alcohol；
(3) add 1 ~ 2 phenolphthalein indicator in above-mentioned test solution again, Deca 0.1039 mol/l naoh standard solution is to test solution
Become pink into terminal, the concentration of described standard solution of sodium hydroxide is c1；
(4) above-mentioned test solution is heated to just seething with excitement, continue Deca 0.1039 mol/l naoh standard solution to test solution become pink into
Terminal, records consumption v1；
Described use calcium chloride precipitation method measures total Oil repellent, and its method is:
(1) pipette dynamic titanium alloy pickle 5 ml in 100 ml plastics volumetric flasks, be diluted with water to scale, shake up,
Pipette 5 ml in above-mentioned diluent in 250ml beaker, and add 10 ~ 20 ml deionized waters；
(2) to the 2 mol/l naoh solution of Deca in beaker 3 ~ 5 ml, it is heated to just seething with excitement, flow water-cooled, by the examination after cooling
Liquid is fully transferred in suction funnel, and microporous filter membrane sucking filtration obtains filtrate；
(3) gained filtrate is fully transferred in 500 ml conical flasks, adds 1 ~ 2 methyl red indicator, first Deca 6 mol/l
Hydrochloric acid is micro- red to solution, then Deca 0.1039 mol/l naoh standard solution just turns yellow as terminal to test solution；
(4) 20 ml chlorination calcium standard solutions are accurately added in above-mentioned test solution, the concentration of described chlorination calcium standard solution is c2, institute
The volume stating chlorination calcium standard solution is v2, heated and boiled 5 min, after being air cooled to room temperature, microporous filter membrane sucking filtration obtains filtrate, will filter
Liquid is fully transferred in 250 ml conical flasks, adds 2mol/l naoh solution in above-mentioned test solution, adds in every 10 ml test solutions
2 mol/l naoh solution of 1.25 ml, and add solid calcon-carboxylic acid 0.05 g, with edta titrand drop to solution by
It is terminal that claret is changed into pure blue, and the concentration of described edta titrand is c3, and record its consumption v3；
Described total Oil repellent with measurement deducts the Oil repellent in the fluotitanic acid content of measurement, obtains the hydrogen in titanium alloy pickle
Fluoric acid content, its concrete formula is as follows: fluohydric acid content is calculated as follows:
Wherein in (1) formula, chfThe concentration of Fluohydric acid., g/l in titanium alloy pickle；c1Sodium hydroxide standardized titration
The concentration of liquid, mol/l；v1The volume of the standard solution of sodium hydroxide being consumed, ml；c2Calcium chloride titrand
Concentration, mol/l；v2The volume of the calcium chloride titrand being quantitatively adding, ml；c3Edta titrand
Concentration, mol/l；v3The volume of the edta standard solution being consumed, ml；v0The volume of taken tank liquor, ml；
The relative molar mass of 20.01 hf, g/mol.
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| CN105136975B (en) * | 2015-09-01 | 2017-07-07 | 武汉钢铁(集团)公司 | A kind of method of Calcium Fluoride Content in measure fluorite |
| CN106442663A (en) * | 2016-11-30 | 2017-02-22 | 江西洪都航空工业集团有限责任公司 | Analysis method for hydrofluoric acid content in pickling solution |
| 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 |
| CN109580602A (en) * | 2018-11-29 | 2019-04-05 | 中国航发沈阳黎明航空发动机有限责任公司 | The method of inspection of fluorine ion in a kind of trade effluent |
| CN117001267B (en) * | 2023-05-31 | 2024-03-12 | 东莞市海发科技发展有限公司 | Workpiece renovating and repairing process |
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| SU819062A1 (en) * | 1979-04-16 | 1981-04-07 | Днепропетровский Институт Инженеровжелезнодорожного Транспорта Им.M.И.Калинина | Method of producing potassium hexafluorotitanate |
| JPH0666783A (en) * | 1992-08-24 | 1994-03-11 | Anatsuku:Kk | Method and instrument for measuring concentration of nitric acid and hydrofluoric acid in stainless steel pickling liquid |
| JP2001021548A (en) * | 1999-07-06 | 2001-01-26 | Kawasaki Steel Corp | Analytical method and device for free fluorine in solution containing hydrofluoric acid |
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