CN109358056A - A method of 7050 zinc in aluminium alloy contents of measurement - Google Patents
A method of 7050 zinc in aluminium alloy contents of measurement Download PDFInfo
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- CN109358056A CN109358056A CN201811597854.7A CN201811597854A CN109358056A CN 109358056 A CN109358056 A CN 109358056A CN 201811597854 A CN201811597854 A CN 201811597854A CN 109358056 A CN109358056 A CN 109358056A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Abstract
The present invention provides a kind of methods for measuring 7050 zinc in aluminium alloy contents, comprising the following steps: after a) 7050 aluminum alloy specimens are dissolved in acid, sodium fluoride saturated solution is added, obtains mixed liquor；B) after the pH of the mixed liquor being adjusted to 4~6, ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and sodium hexametaphosphate solution is added, obtains intermediate fluid；C) it after buffer being added into the intermediate fluid, adds acid-base indicator and is titrated with EDTA standard solution；D) Zn content in 7050 aluminum alloy specimen is calculated according to formula (1).In measuring method provided by the invention, first 7050 aluminium alloys are dissolved in acid, add sodium fluoride screening agent, after then adjusting pH to 4~6, ammonium fluoride, thiocarbamide, hydroxylamine hydrochloride and calgon screening agent are added, buffer, acid-base indicator are eventually adding and is titrated.Test method of the invention can it is quick and convenient, accurately measure Zn content.
Description
Technical field
The present invention relates to technical field of alloy material, in particular to a kind of method for measuring 7050 zinc in aluminium alloy contents.
Background technique
7050 aluminium alloys belong to Al-Zn-Mg-Cu aluminum alloy, are a kind of heat treatable aluminium alloys of high intensity, have pole
High intensity and anti-strip corrosion and stress corrosion resistant fracture property are widely used to aerospace industry, mold processing, machine
The fields such as tool equipment.Main alloy element in 7050 aluminium alloys includes zinc, and Zn content is to the intensity of 7050 aluminium alloys, anticorrosive
Etc. performances have larger impact.
Currently, the measurement of 7050 zinc in aluminium alloy contents is divided into chemical analysis and two kinds of instrumental method, it is specific: instrument
Device analytic approach is using photo-electric direct reading spectrometer or inductive coupling Atomic Emission Spectrometer AES detection Zn content.Chemical analysis is main
For what is used in national standard GB/T 20975.8-2008 " the 8th part of aluminium and aluminum alloy chemically analysis method: the measurement of Zn content "
EDTA titration, detailed process are that " by 7050 aluminum alloy specimen dissolving with hydrochloric acid, evaporation removes excess acid, with 2mol/L hydrochloric acid
Dissolved salts are filtered to remove insoluble matter.By filtrate by strong-base anion-exchange resin, eluted with the hydrochloric acid of 0.005mol/L
Zinc on resin；Using dithizone as indicator, zinc is titrated with EDTA standard solution ".
However, in above-mentioned instrumental method, it is necessary to expensive instrument is relied on, and in chemical analysis, it needs using specific
Exchanger resin is not easy to purchase, and cumbersome, is unfavorable for actually using.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of method for measuring 7050 zinc in aluminium alloy contents, the present invention
The test method of offer without being difficult to the exchanger resin obtained and not depending on expensive instrument, can be fast and convenient determine
Zn content in 7050 alloys.
The present invention provides a kind of methods for measuring 7050 zinc in aluminium alloy contents, comprising the following steps:
A) after 7050 aluminum alloy specimens being dissolved in acid, sodium fluoride saturated solution is added, obtains mixed liquor；
B) after the pH of the mixed liquor being adjusted to 4~6, be added ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and
Sodium hexametaphosphate solution obtains intermediate fluid；
C) it after buffer being added into the intermediate fluid, adds acid-base indicator and is titrated with EDTA standard solution；
D) Zn content in 7050 aluminum alloy specimen is calculated according to formula (1):
In formula (1), C is the concentration of EDTA standard solution, unit mol/L；
V1The volume of consumed EDTA standard solution, unit mL when to titrate；
V2For the volume of EDTA standard solution consumed by titration blank test solution, unit mL；
M is the molal weight of zinc, unit g/mol；
m0For the quality of 7050 aluminum alloy specimens, unit g.
Preferably, the amount ratio of the sodium fluoride saturated solution and 7050 aluminum alloy specimens is (48~52) mL:
0.2000g。
Preferably, the mass ratio of the ammonium fluoride in the ammonium fluoride solution and 7050 aluminum alloy specimens is (4~5):
0.2000；
The mass ratio of thiocarbamide and 7050 aluminum alloy specimens in the thiourea solution is (1~2): 0.2000；
The mass ratio of hydroxylamine hydrochloride and 7050 aluminum alloy specimens in the hydroxylamine hydrochloride solution is (0.3~0.7):
0.2000；
The mass ratio of calgon and 7050 aluminum alloy specimens in the sodium hexametaphosphate solution is (1.0~1.5):
0.2000。
Preferably, the buffer is hexamethylenetetramine.
Preferably, in the step c), the pH that buffer is added to solution is 4~6.
Preferably, in the step b), the pH of the mixed liquor is adjusted to 4~6 specifically:
P-nitrophenol indicator is added into the mixed liquor, is neutralized to solution displaing yellow with ammonium hydroxide, then in hydrochloric acid
With take off to yellow, and make pH 4~6.
Preferably, the acid-base indicator is xylenol orange-methylene blue indicator.
Preferably, in the step c), acid-base indicator is added specifically:
Xylenol orange indicator is first added dropwise, then methylene blue indicator is added dropwise to solution purpling red.
Preferably, in the step a), the acid is the mixed acid of hydrochloric acid solution and nitric acid liquid.
Preferably, the concentration of the hydrochloric acid solution is 5.8~6.2mol/L；
The concentration of the nitric acid liquid is 7.2~7.6mol/L；
The volume ratio of the hydrochloric acid solution and nitric acid liquid is (280~320): 50.
The present invention provides a kind of methods for measuring 7050 zinc in aluminium alloy contents, comprising the following steps: a) by 7050 aluminium
After alloy sample is dissolved in acid, sodium fluoride saturated solution is added, obtains mixed liquor；B) pH of the mixed liquor is adjusted to 4
After~6, ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and sodium hexametaphosphate solution is added, obtains intermediate fluid；C) to institute
It states after buffer is added in intermediate fluid, add acid-base indicator and is titrated with EDTA standard solution；D) institute is calculated according to formula (1)
State the Zn content in 7050 aluminum alloy specimens.In measuring method provided by the invention, first 7050 aluminium alloys are dissolved in acid, then
Sodium fluoride screening agent is added, after then adjusting pH to 4~6, adds ammonium fluoride, thiocarbamide, hydroxylamine hydrochloride and calgon and covers
Agent is covered, buffer, acid-base indicator are eventually adding and is titrated.The present invention is sheltered by the way that specific screening agent is added by several times
Interfering ions such as aluminium, iron, copper, manganese, and control specific titratable acidity, can be in the solution in 7050 aluminium alloy of direct titration
Zinc gets rid of the dependence to detecting instrument, avoids using valuableness and is difficult to the exchanger resin obtained, can be quickly and easily real
The measurement of existing Zn content, while guaranteeing its measurement accuracy.
Specific embodiment
The present invention provides a kind of methods for measuring 7050 zinc in aluminium alloy contents, comprising the following steps:
A) after 7050 aluminum alloy specimens being dissolved in acid, sodium fluoride saturated solution is added, obtains mixed liquor；
B) after the pH of the mixed liquor being adjusted to 4~6, be added ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and
Sodium hexametaphosphate solution obtains intermediate fluid；
C) it after buffer being added into the intermediate fluid, adds acid-base indicator and is titrated with EDTA standard solution；
D) Zn content in 7050 aluminum alloy specimen is calculated according to formula (1):
In formula (1), C is the concentration of EDTA standard solution, unit mol/L；
V1The volume of consumed EDTA standard solution, unit mL when to titrate；
V2For the volume of EDTA standard solution consumed by titration blank test solution, unit mL；
M is the molal weight of zinc, unit g/mol；
m0For the quality of 7050 aluminum alloy specimens, unit g.
In measuring method provided by the invention, first 7050 aluminium alloys are dissolved in acid, add sodium fluoride screening agent, so
Afterwards adjust pH to 4~6 after, add ammonium fluoride, thiocarbamide, hydroxylamine hydrochloride and calgon screening agent, be eventually adding buffer,
Soda acid is indicated and is titrated.The present invention shelters the interfering ions such as aluminium, iron, copper, manganese by the way that specific screening agent is added by several times, and
Control specific titratable acidity, zinc that can in the solution in 7050 aluminium alloy of direct titration, get rid of to detecting instrument according to
Rely, avoids using valuableness and be difficult to the exchanger resin obtained, can quickly and easily realize the measurement of Zn content, guarantee simultaneously
Its measurement accuracy.
According to the present invention, after first 7050 aluminum alloy specimens are dissolved in acid, sodium fluoride saturated solution is added, is mixed
Liquid
The present invention is not particularly limited the type of 7050 aluminium alloys, is 7050 aluminium alloy well known to those skilled in the art
?.The present invention is not particularly limited the source of 7050 aluminium alloy, for general commercially available product or according to those skilled in the art
Customary preparation methods known to member obtain.
In the present invention, the acid is preferably the mixed acid of hydrochloric acid solution and nitric acid liquid, can be sufficiently molten faster using the acid
Solution, and do not influence test accuracy.In the present invention, the concentration of the hydrochloric acid solution is preferably 5.8~6.2mol/L；The nitric acid liquid
Concentration be preferably 7.2~7.6mol/L；The volume ratio of the hydrochloric acid solution and nitric acid liquid is preferably (280~320): 50, it is more excellent
It is selected as 300:50.
In the present invention, the amount ratio of 7050 aluminum alloy specimen and acid is not particularly limited, can be by 7050 aluminium alloys
Sufficiently dissolution, preferably 0.2000g:(20~30) mL, more preferably 0.2000g:25mL；Under above-mentioned amount ratio, both
It can sufficiently dissolve and sour dosage can be reduced to the greatest extent, to reduce subsequent neutralization, adjust the amount of reagent in the programs such as pH, reduce behaviour
Make time, and save the cost.
In the present invention, the temperature of the dissolution is preferably 50~80 DEG C.After being heated to dissolution completely, preferably also boiled
Boiling；The time boiled is preferably 1~3min, more preferably 2min.After above-mentioned boil, preferably also cooled down；It is described
It is cooling to be preferably cooled to room temperature.
After above-mentioned cooling, sodium fluoride saturated solution is added into lysate.In the present invention, the sodium fluoride saturated solution
It is preferably (48~52) mL: 0.2000g with the amount ratios of 7050 aluminum alloy specimens, more preferably 50mL: 0.2000g.It will fluorination
Sodium saturated solution and the lysate after mixing, obtain mixed liquor.
According to the present invention, after obtaining mixed liquor, the pH of the mixed liquor is adjusted to 4~6, be added ammonium fluoride solution,
Thiourea solution, hydroxylamine hydrochloride solution and sodium hexametaphosphate solution, obtain intermediate fluid.
The pH that the present invention adjusts mixed liquor is 4~6, is conducive to subsequent screening agent to the masking of interfering ion and subsequent
The stability of titration, so as to guarantee that titration goes on smoothly and improves accuracy.In the present invention, it is furthermore preferred that by described mixed
The pH for closing liquid is adjusted to 5.
In the present invention, the concrete operations that the pH of mixed liquor is adjusted to 4~6 are preferred are as follows: add into the mixed liquor
Enter p-nitrophenol indicator, be neutralized to solution displaing yellow with ammonium hydroxide, then be neutralized with hydrochloric acid to yellow and take off, and make pH 4~
6.The present invention adjusts the acidity of solution using ammonium hydroxide and hydrochloric acid cooperation, and the pH of control solution, energy are indicated using p-nitrophenol
Enough adjustings for effectively realizing pH, and will not influence the accuracy of measurement.Wherein, the concentration of the p-nitrophenol indicator is preferred
For 1~3g/L, more preferably 2g/L；The additive amount of the p-nitrophenol indicator is not particularly limited, according to this field skill
The conventional additive amount of indicator in titration operation known to art personnel.The density of the ammonium hydroxide is preferably 0.9g/mL.Institute
The concentration for stating hydrochloric acid is preferably 5.8~6.2mol/L.
After above-mentioned adjusting pH, ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and sodium hexametaphosphate solution is added.
Present invention introduces specific ammonium fluoride, thiocarbamide, hydroxylamine hydrochloride and calgon, solution of these substances after the present invention adjusts pH
Collective effect in system can effectively shelter the interfering ions such as aluminium, iron, copper, manganese, provide effective titration for direct titration test
Environment can if any one of above-mentioned specific screening agent is replaced with other screening agents or lacks any one of them screening agent
Test is interfered, test result mistake is caused.
Wherein, the mass ratio of the ammonium fluoride in the ammonium fluoride solution and 7050 aluminum alloy specimens is preferably (4~5):
0.2000, more preferably 4.5: 0.2000.The concentration of ammonium fluoride solution of the present invention is preferably 280~320g/L, more preferably
For 300g/L.
The mass ratio of thiocarbamide and 7050 aluminum alloy specimens in the thiourea solution is preferably (1~2): 0.2000, it is more excellent
It is selected as 1.5: 0.2000.The concentration of thiourea solution of the present invention is preferably 80~120g/L, more preferably 100g/L.
The mass ratio of hydroxylamine hydrochloride and 7050 aluminum alloy specimens in the hydroxylamine hydrochloride solution is preferably (0.3~0.7):
0.2000, more preferably 0.5: 0.2000.The concentration of hydroxylamine hydrochloride solution of the present invention is preferably 80~120g/L, more preferably
For 100g/L.
The mass ratio of calgon and 7050 aluminum alloy specimens in the sodium hexametaphosphate solution be preferably (1.0~
1.5): 0.2000, more preferably 1.2: 0.2000.The concentration of sodium hexametaphosphate solution of the present invention is preferably 60~100g/
L, more preferably 80g/L.The present invention is using specific screening agent and controls it in above-mentioned amount ranges, can more effectively adequately
Sheltering the interference ions, and the accuracy for influencing titration will not be interfered on titration.Above-mentioned screening agent and solution system is abundant
After mixing, intermediate fluid is obtained.
According to the present invention, after obtaining intermediate fluid, buffer is added into the intermediate fluid, adds acid-base indicator simultaneously
It is titrated with EDTA standard solution.
Present invention introduces the acidity that buffer carrys out maintenance system, preferably make system controlling pH 4~6.It is sheltered being added
It after agent, introduces buffer and carrys out maintenance system acidity within the above range, stable titration environment can be provided for subsequent titration, had
Conducive to raising accuracy of measurement.In the present invention, the buffer is preferably hexamethylenetetramine.The present invention is to the buffer
Dosage is not particularly limited, and can be maintained system under above-mentioned pH, it is preferred that the mass ratio of buffer and 7050 samples
For (8~10): 0.2000, more preferably 9: 0.2000.In the present invention, the buffer is preferably added in the form of a solution, buffering
The concentration of agent solution is preferably 280~320g/L, more preferably 300g/L.
In the present invention, the acid-base indicator is preferably xylenol orange-methylene blue indicator, is matched using above-mentioned indicator
It closes, can be improved the accuracy of titration.In the system environment that the pH that previous step is formed is 4~6, if individually selecting xylenol
Orange indicator (color change interval 5.3~6.3), when pH value of solution > 6.3, take on a red color, and when pH value of solution < 6.3 is in yellow, and titration end-point is molten
Liquid color should be by red flavescence color, but through testing, and end point mutation is unobvious, is not easy to observe, and be easy to cause titration inaccuracy；Through grinding
Study carefully, select xylenol orange and methylene blue mixed indicator, obviously can accurately determine titration end-point, so that it is quasi- to improve measurement
Exactness.In the present invention, xylenol orange indicator is preferably first added dropwise, then methylene blue indicator to solution is added dropwise is adjusted to aubergine and be
Only.Wherein, the concentration of xylenol orange indicator is preferably 3~5g/L, more preferably 4g/L.The concentration of methylene blue indicator is excellent
It is selected as 1~3g/L, more preferably 2g/L.The present invention is not particularly limited the additive amount of the indicator, according to this field skill
The conventional addition operation of compound indicator known to art personnel.
It in the present invention, after acid-base indicator is added, is titrated with EDTA standard solution, until solution is mutated by aubergine
Until brilliant blue green.In some embodiments of the invention, the concentration of the EDTA standard solution is 0.009177mol/L.This
Invention is not particularly limited the preparation method of EDTA standard solution, according to conventional formulation method well known to those skilled in the art
?.
In the present invention, after reaching titration end-point, the Zn content in 7050 aluminum alloy specimen is calculated according to formula (1):
In formula (1), C is the concentration of EDTA standard solution, unit mol/L；
V1The volume of consumed EDTA standard solution, unit mL when to titrate；
V2For the volume of EDTA standard solution consumed by titration blank test solution, unit mL；The blank test
Refer to that blank sample is tested, i.e., the testing experiment carried out when not adding 7050 aluminum alloy specimen；
M is the molal weight of zinc, unit g/mol；
m0For the quality of 7050 aluminum alloy specimens, unit g.Institute value ω (Zn) is indicated with %.
In the present invention, the measurement range of above-mentioned test method is preferably 5.7%~6.7%, can accurately test out Zn
The Zn content of the aluminium alloy of content within the above range.
The present invention provides a kind of methods for measuring 7050 zinc in aluminium alloy contents, and 7050 aluminium alloys are first dissolved in acid
In, sodium fluoride screening agent is added, after then adjusting pH to 4~6, adds ammonium fluoride, thiocarbamide, hydroxylamine hydrochloride and hexa metaphosphoric acid
Sodium screening agent is eventually adding buffer, soda acid indicates and is titrated.Sheltered by the way that specific screening agent is added by several times aluminium, iron,
Interfering ions such as copper, manganese, and control specific titratable acidity, zinc that can in the solution in 7050 aluminium alloy of direct titration, pendulum
The dependence to detecting instrument has been taken off, avoided using valuableness and has been difficult to the exchanger resin obtained, can quickly and easily realize zinc
The measurement of content, while guaranteeing its measurement accuracy.
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.In following embodiment, mixed acid be 6mol/L by 300mL concentration hydrochloric acid solution+50mL concentration be 7mol/L nitric acid
Liquid mixed preparing obtains.In test process, the dropwise operation of each raw material is carried out using rubber head dropper.
Embodiment 1
1.1 the test of sample
Weigh 7050 aluminium alloy sample of 0.2000g (trade mark 7050-E6312, by southwestern Aluminum (group) Limited Liability public affairs
Department provides) it is placed in 500mL conical flask, it is added in 25mL mixture of hydrochloric acid and nitric acid, being slowly heated to dissolution, (temperature is completely
60 DEG C), 2min is boiled, is cooled to room temperature, 50mL sodium fluoride saturated solution is added, is mixed.Then 1 drop p-nitrophenol is added
Solution (2g/L) is neutralized to the rigid displaing yellow of solution with ammonium hydroxide (0.90g/mL), then is neutralized to yellow just with hydrochloric acid (6mol/L)
It takes off, it is about 5 that excessive dropwise addition 2, which drops to pH, and 15mL ammonium fluoride solution (300g/L), 15mL thiourea solution (100g/ is then added
L), 5mL hydroxylamine hydrochloride solution (100g/L), 15mL sodium hexametaphosphate solution (80g/L), mix well.Later, 30mL six is added
Four amine aqueous solution of methine (300g/L) is added dropwise 4 drops xylenol orange indicator (4g/L), then methylene blue indicator (2g/L) is added dropwise
Until being adjusted to aubergine, solution is titrated to EDTA standard solution (0.009177mol/L), brilliant blue green is mutated by aubergine.
The analysis of 1.2 results
(1) accuracy
Operation repetitive twice, and according to formula (1) calculating Zn content, takes the average value of test result twice as procedure described above
It is compared as final result, and with Zn content standard value in 7050 aluminum alloy specimens, as a result referring to table 1.
The test result of 1 embodiment 1 of table
(2) precision
According to above-mentioned test process to sample METHOD FOR CONTINUOUS DETERMINATION 7 times, the standard deviation of test result is calculated according to formula (2):
Wherein, σ is standard deviation；For the average value of n times measurement result；XiFor the value of i-th measurement；N is measurement time
Number.
It is computed, σ 0.064.
Embodiment 2
The test of 1.1 samples
Weigh 7050 aluminium alloy sample (trade mark 7050-1#, by Southwest Aluminum (Group) Co., Ltd. of 0.2000g
There is provided) it is placed in 500mL conical flask, it is added in 25mL mixture of hydrochloric acid and nitric acid, is slowly heated to dissolve (temperature 70 completely
DEG C), 2min is boiled, is cooled to room temperature, 50mL sodium fluoride saturated solution is added, is mixed.Then it is molten that 1 drop p-nitrophenol is added
Liquid (2g/L) is neutralized to the rigid displaing yellow of solution with ammonium hydroxide (0.90g/mL), then is neutralized to yellow with hydrochloric acid (6mol/L) and just takes off
Go, it is excessive that be added dropwise 2 to drop to pH is about 5, be then added 15mL ammonium fluoride solution (300g/L), 15mL thiourea solution (100g/L),
5mL hydroxylamine hydrochloride solution (100g/L), 15mL sodium hexametaphosphate solution (80g/L), mix well.Later, it is added 30mL six times
4 drops xylenol orange indicator (4g/L) are added dropwise in tetramine solution (300g/L), then methylene blue indicator (2g/L) tune is added dropwise
Until aubergine, solution is titrated to EDTA standard solution (0.009177mol/L), brilliant blue green is mutated by aubergine.
The analysis of 1.2 results
(1) accuracy
Operation repetitive twice, and according to formula (1) calculating Zn content, takes the average value of test result twice as procedure described above
It (is tested by ICP Atomic Emission Spectrometer AES) as final result, and with Zn content standard value in 7050 aluminum alloy specimens
It compares, as a result referring to table 2.
The test result of 2 embodiment 2 of table
(2) precision
According to the test method test precision of embodiment 1, the results show that σ is 0.060.
Embodiment 3
The test of 1.1 samples
Weigh 7050 aluminium alloy sample (trade mark 7050-2#, by Southwest Aluminum (Group) Co., Ltd. of 0.2000g
There is provided) it is placed in 500mL conical flask, it is added in 25mL mixture of hydrochloric acid and nitric acid, is slowly heated to dissolve (temperature 65 completely
DEG C), 2min is boiled, is cooled to room temperature, 50mL sodium fluoride saturated solution is added, is mixed.Then it is molten that 1 drop p-nitrophenol is added
Liquid (2g/L) is neutralized to the rigid displaing yellow of solution with ammonium hydroxide (0.90g/mL), then is neutralized to yellow with hydrochloric acid (6mol/L) and just takes off
Go, it is excessive that be added dropwise 2 to drop to pH is about 5, be then added 15mL ammonium fluoride solution (300g/L), 15mL thiourea solution (100g/L),
5mL hydroxylamine hydrochloride solution (100g/L), 15mL sodium hexametaphosphate solution (80g/L), mix well.Later, it is added 30mL six times
4 drops xylenol orange indicator (4g/L) are added dropwise in tetramine solution (300g/L), then methylene blue indicator (2g/L) tune is added dropwise
Until aubergine, solution is titrated to EDTA standard solution (0.009177mol/L), brilliant blue green is mutated by aubergine.
The analysis of 1.2 results
(1) accuracy
Operation repetitive twice, and according to formula (1) calculating Zn content, takes the average value of test result twice as procedure described above
It (is tested by ICP Atomic Emission Spectrometer AES) as final result, and with Zn content standard value in 7050 aluminum alloy specimens
It compares, as a result referring to table 3.
The test result of 3 embodiment 3 of table
(2) precision
According to the test method test precision of embodiment 1, the results show that σ is 0.065.
Test method of the invention and existing chemical analysis are compared it is found that the present invention is without being difficult to the friendship purchased
Resin is changed, operating process is enormously simplified, the Zn content in 7050 aluminium alloy of measurement that can be fast and convenient；Meanwhile by above-mentioned
Test result is it is found that test method of the invention has high accuracy and precision.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.To these embodiments
A variety of modifications will be readily apparent to those skilled in the art, the general principles defined herein can be with
Without departing from the spirit or scope of the present invention, it realizes in other embodiments.Therefore, the present invention will not be limited
In the embodiments shown herein, and it is to fit to widest model consistent with the principles and novel features disclosed in this article
It encloses.
Claims (10)
1. a kind of method for measuring 7050 zinc in aluminium alloy contents, which comprises the following steps:
A) after 7050 aluminum alloy specimens being dissolved in acid, sodium fluoride saturated solution is added, obtains mixed liquor；
B) after the pH of the mixed liquor being adjusted to 4~6, ammonium fluoride solution, thiourea solution, hydroxylamine hydrochloride solution and six is added partially
Sodium radio-phosphate,P-32 solution obtains intermediate fluid；
C) it after buffer being added into the intermediate fluid, adds acid-base indicator and is titrated with EDTA standard solution；
D) Zn content in 7050 aluminum alloy specimen is calculated according to formula (1):
In formula (1), C is the concentration of EDTA standard solution, unit mol/L；
V1The volume of consumed EDTA standard solution, unit mL when to titrate；
V2For the volume of EDTA standard solution consumed by titration blank test solution, unit mL；
M is the molal weight of zinc, unit g/mol；
m0For the quality of 7050 aluminum alloy specimens, unit g.
2. the method according to claim 1, wherein the sodium fluoride saturated solution and 7050 aluminum alloy specimens
Amount ratio is (48~52) mL: 0.2000g.
3. the method according to claim 1, wherein ammonium fluoride and 7050 aluminium alloys in the ammonium fluoride solution
The mass ratio of sample is (4~5): 0.2000；
The mass ratio of thiocarbamide and 7050 aluminum alloy specimens in the thiourea solution is (1~2): 0.2000；
The mass ratio of hydroxylamine hydrochloride and 7050 aluminum alloy specimens in the hydroxylamine hydrochloride solution is (0.3~0.7): 0.2000；
The mass ratio of calgon and 7050 aluminum alloy specimens in the sodium hexametaphosphate solution is (1.0~1.5):
0.2000。
4. the method according to claim 1, wherein the buffer is hexamethylenetetramine.
5. method according to claim 1 or 4, which is characterized in that in the step c), the pH of buffer to solution is added
It is 4~6.
6. the method according to claim 1, wherein the pH of the mixed liquor is adjusted to 4 in the step b)
~6 specifically:
Into the mixed liquor be added p-nitrophenol indicator, be neutralized to solution displaing yellow with ammonium hydroxide, then be neutralized with hydrochloric acid to
Yellow is taken off, and makes pH 4~6.
7. the method according to claim 1, wherein the acid-base indicator is that xylenol orange-methylene blue refers to
Show agent.
8. method according to claim 1 or claim 7, which is characterized in that in the step c), it is specific that acid-base indicator is added
Are as follows:
Xylenol orange indicator is first added dropwise, then methylene blue indicator is added dropwise to solution purpling red.
9. the method according to claim 1, wherein the acid is hydrochloric acid solution and nitric acid liquid in the step a)
Mixed acid.
10. according to the method described in claim 9, it is characterized in that, the concentration of the hydrochloric acid solution is 5.8~6.2mol/L；
The concentration of the nitric acid liquid is 7.2~7.6mol/L；
The volume ratio of the hydrochloric acid solution and nitric acid liquid is (280~320): 50.
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| CN201811597854.7A CN109358056A (en) | 2018-12-26 | 2018-12-26 | A method of 7050 zinc in aluminium alloy contents of measurement |
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