CN108152442A - The method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder - Google Patents
The method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder Download PDFInfo
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- CN108152442A CN108152442A CN201711297792.3A CN201711297792A CN108152442A CN 108152442 A CN108152442 A CN 108152442A CN 201711297792 A CN201711297792 A CN 201711297792A CN 108152442 A CN108152442 A CN 108152442A
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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
A kind of method that sodium hydroxide separation EDTA back titrations measure aluminium element in ferro-aluminum powder, including：Step 1: prepare ethyl ammonium buffer solution and copper standard titration solution；Step 2: ferro-aluminum powder sample is taken to prepare test solution；Step 3: add in PAN indicator after test solution heating is boiled, test solution is titrated to copper standard titration solution and stable aubergine occurs, then sodium fluoride solid is added in, PAN indicator is added after boiling, test solution is titrated to copper standard titration solution again and stable aubergine occurs, writes down the quantity of consumed copper standard titration solution；Step 4: calculate the mass percent of aluminium in ferro-aluminum powder sample.This invention removes the interference of matrix in measure and coexistence elements, sample analysis precision and accuracy are improved, it is fast and convenient, be easily achieved.
Description
Technical field
The present invention relates to metallochemistry composition measurement fields, and in particular to a kind of sodium hydroxide separation-EDTA back titrations
The method for measuring aluminium element in ferro-aluminum powder.
Background technology
Ferro-aluminum powder is mainly used in the alumetizing process of turbo blade, is obtained by alumetizing process as bianry alloy powder
Aluminized coating can significantly improve the high temperature oxidation resistance of material, resistance to air (seawater etc.) corrosivity, while can effectively improve steel
The resistance to corrosion of the alloys such as iron and Ni-based, cobalt-based.The aluminium element added in alumetizing process is due to belonging to soft metal, in alloy
In can not add in excessive, accurate detection and stringent control should be carried out to its content, to ensure its quality in alumetizing process
Stability.
Invention content
It is an object of the invention to the problems in for the above-mentioned prior art, provide a kind of sodium hydroxide separation-EDTA and return
The method of aluminium element in titration measuring ferro-aluminum powder, this method is fast and convenient, is easily achieved.
To achieve these goals, the technical solution adopted by the present invention includes the following steps：
Step 1: prepare acetic acid-ammonium acetate buffer solution and copper standard titration solution；
Step 2: adding in sulfuric acid into ferro-aluminum powder sample and being heated to being completely dissolved, it is molten to be then slowly added to sodium hydroxide
Liquid is added water and is boiled to precipitating, and with water constant volume after cooling, is shaken up, and is stood, and filter is done after making precipitation agglomerate layered；
The clear liquid that layering obtains is pipetted, hydrochloric acid is added in, excess EDTA solution and paranitrophenol indicator is added in after boiling, adjust
After saving solution pH value, the acetic acid-ammonium acetate buffer solution that step 1 is prepared is added in, shakes up to obtain test solution；
Step 3: adding in PAN indicator after test solution heating is boiled, being titrated to test solution with copper standard titration solution occurs surely
Then fixed aubergine is added in sodium fluoride solid, PAN indicator is added after boiling, then be titrated to copper standard titration solution
There is stable aubergine in test solution, writes down the quantity of consumed copper standard titration solution；
Step 4: calculate the mass percent of aluminium in ferro-aluminum powder sample：
In above formula,
The substance withdrawl syndrome of C- copper standard titration solutions, unit mol/L；
V- consumes the volume of copper standard titration solution, unit mL when titrating；
M- sample weighting amounts, unit g；
MM quality of 0.02698- aluminium, unit g/mmol.
Prepare acetic acid-ammonium acetate buffer solution method be：200g ammonium acetates are weighed, are dissolved in 500mL water, add in 25mL
Glacial acetic acid is diluted with water to 1000mL, shakes up；The pH value of acetic acid-ammonium acetate buffer solution is 5.5~6.
Prepare copper standard titration solution method be：
It weighs 0.6354g simple metal copper to be placed in 250mL beakers, adds in 10mL nitric acid, dissolve by heating, the matter of simple metal copper
It measures score and is not less than 99.9%；10mL sulfuric acid is added, is evaporated to and emits sulfuric acid cigarette, is cooled down, 50mL water is added in, boils dissolving salt
Class；Room temperature is cooled to, is moved into 1000mL volumetric flasks, is diluted with water to required scale, shakes up.
Step 2 weighs 0.10g ferro-aluminum powder samples and is placed in 150mL beakers, and it is completely molten that addition 10mL sulfuric acid is heated to sample
Solution；Cooling is slowly added to sodium hydroxide solution to appearance is precipitated, after amount 10mL, adds water to test solution volume as 70mL, boil
2min, hole is but；It moves into 250mL volumetric flasks with water constant volume, shakes up, stand, filter is done after making precipitation agglomerate layered.
The clear liquid 25.00mL that layering obtains is pipetted, is placed in 300mL conical flasks；8mL hydrochloric acid is added in, boils and keeps 5min
~10min；Add in excess EDTA solution, add in 0.2ml paranitrophenol indicator, with ammonium hydroxide adjust test solution be in it is yellowish, at this time
The pH value of solution is 5, adds in 20mL acetic acid-ammonium acetate buffer solutions, shakes up to obtain test solution.
The paranitrophenol indicator uses solution of the mass concentration for 2.0g/L.
Test solution heating is boiled in step 3 and keeps 2min~3min, adds in the PAN indicator of 0.8ml, is dripped with copper standard
Determine solution to be titrated, until it is terminal that stable aubergine, which occurs, in test solution；Then the sodium fluoride solid of 1.5g is added in, boils holding
2min~3min adds the PAN indicator of 0.4ml, then is titrated with copper standard titration solution, until stabilization occurs in test solution
Aubergine is terminal, writes down the milliliter number of consumed copper standard titration solution.
The PAN indicator uses ethanol solution of the mass concentration for 1g/L.
Compared with prior art, the present invention has following advantageous effect：By sulfuric acid dissolution ferro-aluminum powder sample, instead of passing
Sal prunella mixed acid used by system method can have the function that effectively to control sample solution acidity, be beneficial to follow-up hydroxide
Sodium precipitation separation ferro-aluminum.Conventional method uses cupferron or sodium fluoride matrix separation elemental iron, and iron is avoided to measure aluminium and is generated
Interference, but cupferron belongs to poisonous and hazardous organic reagent, precipitation separation needs the condition below 10 DEG C to carry out, and molten
Liquid acidity needs to be strict controlled in more than 2mol/L, and the neutral chelate precipitation that otherwise cupferron is generated with iron easily treat by absorption
Element aluminum is surveyed, causes analysis result relatively low, so conventional method is very high to the technical merit requirement of operating environment and operating personnel,
Otherwise the loss of aluminium measure is easily caused, the sodium fluoride partition method that conventional method uses, which need to pass through, to be complexed, precipitates, dissolving, smoldering, turning
Move and etc., reagents citric acid ammonium, ammonium oxalate, sodium fluoride, hydrochloric acid, boric acid, nitric acid, perchloric acid etc. are consumed, test procedure is numerous and diverse,
It is excessive to introduce reagent, transfer test solution is unfavorable to high-content Al-single crystal repeatedly, easily causes the loss of element aluminum to be measured, shadow in the process
Ring experimental accuracy.For the present invention using sodium hydroxide solution matrix separation elemental iron, sodium hydroxide and iron can quickly agglomerate life
Into precipitation, separating effect is preferable, and operating process is easy, less using reagent, reduces the wind that pollution may be introduced in operating process
Danger.The method that conventional method uses EDTA direct titration aluminium, and element aluminum to be measured is complexed by EDTA solution first in the present invention, uses
After copper standard solution overtitration EDTA, the aluminium that sodium fluoride complexing is combined with EDTA is added in, then titrated and discharged with copper standard solution
The EDTA gone out, calculating acquire aluminum amount, using the method for copper standard solution back titration EDTA, can effectively improve titration accuracy.
In addition, conventional method uses Zinc standard solution as titrant, and the present invention is using copper standard solution, conventional method titration process
Change colour unobvious, is progressive, without jumping phenomenon, it is higher to be easy to cause testing result.Titration end-point discoloration of the present invention is apparent,
Accuracy of detection is high.Summary, the present invention in weak acid medium, are complexed using sodium hydroxide matrix separation elemental iron with excessive EDTA
Aluminium measures aluminium content with back titration, is tested by sample solubility test, Matrix effects, separation method is tested, titration method tries
It tests, determines the conditions such as best dissolving acid, separation method, titration method, eliminate the dry of matrix and coexistence elements in measuring
It disturbs, improves sample analysis precision and accuracy.It is fast and convenient, be easily achieved compared to other methods.The recycling then carried out
Rate and precision test, it was demonstrated that assay method of the present invention is easy, quick, accurate, reliable.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
The present invention uses analytically pure reagent and distilled water or the water of suitable purity in analysis.
The method that sodium hydroxide separation-EDTA back titrations of the present invention measure aluminium element in ferro-aluminum powder, includes the following steps：
(1) preparation of reagents；
Acetic acid-ammonium acetate buffer solution (pH value is about 5.5~6).
200g ammonium acetates are weighed, are dissolved in 500mL water, 25mL glacial acetic acids is added in, is diluted with water to 1000mL, shakes up.
Copper standard titration solution：0.01mol/L.
The simple metal copper (mass fraction is not less than 99.9%) for weighing 0.6354g is placed in 250mL beakers, adds in 10mL's
Nitric acid dissolves by heating；10mL sulfuric acid is added, is evaporated to and emits sulfuric acid cigarette, it is slightly cold, 50mL water is added in, boils dissolved salts；Cooling
To room temperature, move into 1000mL volumetric flasks, be diluted with water to scale and shake up.
(2) preparation of test solution；
2.1) 0.10g samples (being accurate to 0.0001g) are weighed, are placed in 150mL beakers, add in 10mL sulfuric acid (sulfuric acid：Water
=1:1), sample is heated to be completely dissolved；It is slightly cold, it is slowly added to sodium hydroxide solution (300g/L) to precipitation and occurs, Zai Guoliang
10mL adds water to test solution volume about 70mL, boils 2min, cooling；It moves into 250mL volumetric flasks with water constant volume, shakes up.It stands,
Filter is done after making precipitation agglomerate layered.2.2) the clear liquid 25.00mL that dry filter obtains is pipetted, is placed in 300mL conical flasks.Add in 8mL
Hydrochloric acid (ρ is about 1.19g/mL) carefully boils 5min~10min, adds in excess EDTA solution (0.02mol/L) (depending on containing for Al
Depending on amount), 0.2ml paranitrophenols indicator (2.0g/L) is added in, adjusting test solution with ammonium hydroxide, (solution ph is about at this time in yellowish
5), to add in 20mL acetic acid-ammonium acetate buffer solutions, shaking up to obtain test solution.
(3) it titrates；
2min~3min is boiled into test solution heating, the PAN indicator (1g/L ethanol solutions) of 0.8ml is added in, immediately with copper
It is that terminal (does not remember reading that standard titration solution (0.01mol/L), which is titrated to test solution stable aubergine occur,.Test solution during titration
Temperature should be controlled at 70 DEG C or more, otherwise terminal unobvious).Then 1.5g sodium fluoride solids are added in, boil 2min~3min, then
The PAN indicator (1g/L ethanol solutions) of 0.4ml is added in, being titrated to test solution with copper standard titration solution (0.01mol/L) is presented
Stable aubergine is terminal (test solution temperature and terminal colour should be grasped consistent with first time at this time, in order to avoid titration error), note
The milliliter number of lower consumed copper standard titration solution (0.01mol/L).
(4) calculating of analysis result
The mass fraction ω of aluminium, numerical value are represented with %：
In formula：
The substance withdrawl syndrome of C- copper standard titration solutions, unit are mole every liter (mol/L)；
V- consumes the volume of copper standard titration solution when titrating, unit is milliliter (mL)；
M- sample weighting amounts, unit are gram (g)；
MM quality of 0.02698- aluminium, unit are gram every mM (g/mmol).
The calculating of the rate of recovery；
Two parts of aluminium standard sample A (containing aluminium 50.85%), aluminium standard sample B (containing aluminium 49.50%) are prepared respectively, according to examination
Proved recipe method is tested, and calculates the rate of recovery
The calculating of precision
The standard sample containing aluminium 49.50% is prepared, is tested according to test method, parallel determination 6 times, calculates RSD.
Under attached relevant experimental result data：
Precision Experiment result
Rate of recovery experimental result
Pass through the rate of recovery and precision test, it is seen that measurement result of the present invention is accurate, reliable.
Claims (8)
1. a kind of method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder, which is characterized in that including：
Step 1: prepare acetic acid-ammonium acetate buffer solution and copper standard titration solution；
Step 2: adding in sulfuric acid into ferro-aluminum powder sample and being heated to being completely dissolved, it is then slowly added to sodium hydroxide solution extremely
It precipitates, adds water and boil, with water constant volume after cooling, shake up, stand, filter is done after making precipitation agglomerate layered；
The clear liquid that layering obtains is pipetted, hydrochloric acid is added in, excess EDTA solution and paranitrophenol indicator is added in after boiling, adjust molten
After liquid pH value, the acetic acid-ammonium acetate buffer solution that step 1 is prepared is added in, shakes up to obtain test solution；
Step 3: adding in PAN indicator after test solution heating is boiled, being titrated to test solution with copper standard titration solution there is stabilization
Then aubergine adds in sodium fluoride solid, PAN indicator is added after boiling, then be titrated to test solution with copper standard titration solution
There is stable aubergine, write down the quantity of consumed copper standard titration solution；
Step 4: calculate the mass percent of aluminium in ferro-aluminum powder sample：
In above formula,
The substance withdrawl syndrome of C- copper standard titration solutions, unit mol/L；
V- consumes the volume of copper standard titration solution, unit mL when titrating；
M- sample weighting amounts, unit g；
MM quality of 0.02698- aluminium, unit g/mmol.
2. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 1, special
Sign is that the method for preparing acetic acid-ammonium acetate buffer solution is：200g ammonium acetates are weighed, are dissolved in 500mL water, add in 25mL
Glacial acetic acid is diluted with water to 1000mL, shakes up；The pH value of acetic acid-ammonium acetate buffer solution is 5.5~6.
3. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 1, special
Sign is that the method for preparing copper standard titration solution is：
It weighs 0.6354g simple metal copper to be placed in 250mL beakers, adds in 10mL nitric acid, dissolve by heating, the quality point of simple metal copper
Number is not less than 99.9%；10mL sulfuric acid is added, is evaporated to and emits sulfuric acid cigarette, is cooled down, 50mL water is added in, boils dissolved salts；Again
It is cooled to room temperature, moves into 1000mL volumetric flasks, be diluted with water to required scale, shake up.
4. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 1, special
Sign is that step 2 weighs 0.10g ferro-aluminum powder samples and is placed in 150mL beakers, and it is completely molten that addition 10mL sulfuric acid is heated to sample
Solution；Cooling is slowly added to sodium hydroxide solution to appearance is precipitated, after amount 10mL, adds water to test solution volume as 70mL, boil
2min, hole is but；It moves into 250mL volumetric flasks with water constant volume, shakes up, stand, filter is done after making precipitation agglomerate layered.
5. according to the method that the sodium hydroxide separation-EDTA back titrations of claim 1 or 4 measure aluminium element in ferro-aluminum powder,
It is characterized in that, pipetting the clear liquid 25.00mL that layering obtains, it is placed in 300mL conical flasks；8mL hydrochloric acid is added in, boils holding
5min~10min；Add in excess EDTA solution, add in 0.2ml paranitrophenol indicator, with ammonium hydroxide adjust test solution be in it is yellowish,
The pH value of solution is 5 at this time, adds in 20mL acetic acid-ammonium acetate buffer solutions, shakes up to obtain test solution.
6. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 5, special
Sign is that the paranitrophenol indicator uses solution of the mass concentration for 2.0g/L.
7. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 1, special
Sign is, boils test solution heating in step 3 and keeps 2min~3min, the PAN indicator of 0.8ml is added in, with copper standardized titration
Solution is titrated, until it is terminal that stable aubergine, which occurs, in test solution；Then the sodium fluoride solid of 1.5g is added in, boils holding
2min~3min adds the PAN indicator of 0.4ml, then is titrated with copper standard titration solution, until stabilization occurs in test solution
Aubergine is terminal, writes down the milliliter number of consumed copper standard titration solution.
8. the method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder according to claim 7, special
Sign is：The PAN indicator uses ethanol solution of the mass concentration for 1g/L.
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Cited By (2)
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| CN112326872A (en) * | 2020-11-04 | 2021-02-05 | 中国航发哈尔滨轴承有限公司 | Method for detecting concentration of magnesium sulfate and nickel sulfate in multi-component mixed nickel electroplating solution |
| CN113866344A (en) * | 2021-08-31 | 2021-12-31 | 浙江方圆检测集团股份有限公司 | Method for measuring mass fraction of aluminum oxide in aluminum water treatment agent by potentiometric titration |
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| CN112326872A (en) * | 2020-11-04 | 2021-02-05 | 中国航发哈尔滨轴承有限公司 | Method for detecting concentration of magnesium sulfate and nickel sulfate in multi-component mixed nickel electroplating solution |
| CN113866344A (en) * | 2021-08-31 | 2021-12-31 | 浙江方圆检测集团股份有限公司 | Method for measuring mass fraction of aluminum oxide in aluminum water treatment agent by potentiometric titration |
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