CN102937590A - Active aluminum detection method - Google Patents
Active aluminum detection method Download PDFInfo
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- CN102937590A CN102937590A CN2012104800115A CN201210480011A CN102937590A CN 102937590 A CN102937590 A CN 102937590A CN 2012104800115 A CN2012104800115 A CN 2012104800115A CN 201210480011 A CN201210480011 A CN 201210480011A CN 102937590 A CN102937590 A CN 102937590A
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- solution
- container
- activated aluminum
- assay method
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Abstract
The invention discloses an active aluminum detection method. The method comprises the following steps of: preparing a Fe2(SO4)3 solution; weighing and dissolving the sample in the following specific processes of accurately weighing an aluminum powder sample in a container, and slowly adding the Fe2(SO4)3 solution prepared in the first step and 10% of a sulfuric acid solution into the container; instantly sealing an opening of the container and only leaving an outlet which is communicated with a NaHCO3 solution; quickly adding the NaHCO3 solution into the container, slightly swinging the container, and subsequently putting the container on a heat source to heat and boil till the reaction is complete; titrating the solution and calculating in the following specific processes of taking the container (namely a triangular flask) down, cooling the container to a room temperature, then dropwise adding a sodium diphenylamine sulfonate indicator into the container, and instantly titrating the solution by a K2Cr2O7 solution till the solution changes from green to purple or hyacinthine as a result; and then calculating the content of active aluminum by a formula. The active aluminum detection method has the beneficial effects of no need for purchasing special equipment, simple operation and high detection precision.
Description
Technical field
The present invention relates to the mensuration of activated aluminum, be specifically related to utilize oxide-reduction method to measure the method for active aluminium content.
Background technology
Aluminium powder is a kind of crucial starting material of heat release welding compound, participate in the chemical reaction of heat release welding directly, the quality of the fierce degree of impact reaction and generation joint, so the quality control to aluminium powder is quite important, but in the storage process of aluminium powder, inevitably to contact with air, thus at the aluminium powder Surface Creation one deck AL
2O
3The oxide layer film.In the occasion of the performance of utilizing metallic aluminium, this part is nonactive aluminium.In existing aluminium powder, the analytical approach of activated aluminum is GB--gas volumetric method is measured activated aluminum, the principle that gas volumetric method is measured activated aluminum is that sample reacts with NaOH, wherein activated aluminum displaces the hydrogen of equivalent, calculates the content of activated aluminum according to the volumescope of hydrogen.The method is applicable to the mensuration that in aluminium powder, the activated aluminum amount is greater than 80%.Although the method is GB, principle own is reliably classical,, because the method need to have special gasmetry instrument, cost is higher, and operation requirements is strict, and condition is harsher, does not slightly note easily causing larger error.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, provides a kind of and utilizes redox method to carry out method for measuring to activated aluminum, and the method need not be purchased specialized equipment, operates also very simply, has solved the technical matters existed in the prior art.
For solving above-mentioned technical matters, the present invention by the following technical solutions:
A kind of activated aluminum assay method, comprise the steps:
Step 1, preparation Fe
2(SO
4)
3Reagent;
Step 2, the weighing of sample, dissolving: detailed process is as follows:
Step 2-1, accurately take the aluminium powder sample in container, slowly adds the Fe of preparation in step 1
2(SO
4)
3Solution and 10% sulfuric acid solution;
Step 2-2, seal a bottle immediately, and only stay an outlet and saturated NaHCO
3Solution communicates, and (carbon dioxide is insoluble to NaHCO
3In solution, avoid carbon dioxide to lose);
Step 2-3 adds rapidly saturated NaHCO in container
3Solution, the jog container, then be placed on container (ground triangular flask) on thermal source heating and boil until react completely that (meaning of step 2-3 is: 1, NaHCO
3Add thermal decomposition and produce carbon dioxide, make in triangular flask to be full of carbon dioxide, avoid oxygen to enter, make the ferrous ion that is reduced again oxidized; 2, heating impels Fe
2(SO
4)
3The quickening of reacting with AL);
Step 3, the solution titration, result is calculated, and detailed process is as follows:
Step 3-1 takes off container and is cooled to room temperature, and container is removed to closed state;
Step 3-2, then add 2-4 and drip the diphenylamine sulfonic acid sodium salt indicator, K used immediately
2Cr
2O
7Standard solution is titrated to by green changing to and occurs that purple or hyacinthine are terminal;
Then get final product the content of calculated activity aluminium, calculate and utilize following formula to carry out:
The percentage composition of activated aluminum=
* 100
In formula:
V: be the K consumed
2Cr
2O
7The volume of standard solution (ml);
M: be K
2Cr
2O
7The volumetric molar concentration of standard solution;
G: be sample heavy (g);
26.98 be the molal weight of aluminium.
Further technical scheme is:
Above-mentioned step 1 detailed process is as follows: take 330 gram Fe
2(SO
4)
3In 750 m l water, add 98% the concentrated sulphuric acid of 75 ml, be heated to dissolve, be diluted in the 1000ml volumetric flask after cooling.
Between above-mentioned step 3-1 and step 3-2, increase following steps, add mixture of sulfuric phosphoric acid and water (to add the effect of mixture of sulfuric phosphoric acid to have two: one, control the needed acidity of titration; The 2nd, indicator discoloration is sharper);
In above-mentioned step 2-1, the aluminium powder sample taken is 0.15～0.20 gram, the Fe added
2(SO
4)
3Solution is 25～35m1.
In above-mentioned step 2-3, the saturated NaHCO added
3Solution is 65～75ml.
Above-mentioned step 2-2 concrete operations the contents are as follows: immediately with the rubber plug jam-pack container finish of separating funnel and discharge hose is housed, and an insertion of outlet is filled to saturated NaHCO
3In the beaker of solution, (carbon dioxide is insoluble to NaHCO
3In solution, avoid carbon dioxide to escape).
In the step added between above-mentioned step 3-1 and step 3-2, the mixture of sulfuric phosphoric acid added is 12～18ml, and the water added is 25～35ml.
In above-mentioned step 2-3, concrete operations the contents are as follows: add rapidly saturated NaHCO from separating funnel
3Solution, the jog container, then container is placed on thermal source heating boil more than 30 minutes (1, NaHCO
3Add thermal decomposition and produce carbon dioxide, make in triangular flask to be full of carbon dioxide, avoid oxygen to enter, make the ferrous ion that is reduced again oxidized; 2, heating impels Fe
2(SO
4)
3The quickening of reacting with AL.) until react completely.
The mass volume ratio of above-mentioned diphenylamine sulfonic acid sodium salt indicator is 1%, above-mentioned NaHCO
3The NaHCO that solution is 15%
3Solution, above-mentioned K
2Cr
2O
7The volumetric molar concentration of solution is 0.05mol/L.
Above-mentioned mixture of sulfuric phosphoric acid is that 98% sulfuric acid be take volume ratio and mixed as 1:4 with 85% phosphoric acid.
Compared with prior art, the invention has the beneficial effects as follows:
1, need not purchase specialized equipment, simple to operate;
2, measuring accuracy is higher.
Embodiment
Below the present invention is further elaborated.
Principle of the present invention is as follows:
Sample is at inert gas (CO
2) protection under, be dissolved in excessive and use H
2SO
4The Fe of acidifying
2(SO
4)
3In solution, heat, the activated aluminum in sample is a reductive agent, and itself is oxidized and generate Al
2(SO
4)
3, Fe
3+Be reduced to Fe
2+, according to the K consumed
2Cr
2O
7Amount carry out the content of calculated activity aluminium.
Reaction equation is:
2AL+3Fe
2(SO
4)
3=?AL(SO
4)
3+6FeSO
4
AL
2O
3+3H
2SO
4=?AL
2(SO
4)
3+3H
2O
K
2Cr
2O
7+6FeSO4+7H
2SO
4=Cr
2(SO
4)3+3Fe
2(SO
4)
3+K
2SO
4+7H
2O
Specific embodiments of the invention are as follows:
Introduce first that the required instrument of using is as follows in the present embodiment:
Separating funnel: 250 ml, 2
Buret: 50 ml, 1
Ground triangular flask: 500 ml, 2
Foregoing description is not really wanted the instrument that will use required for the present invention is defined as to foregoing and can not replaces, and in fact, in the present invention, as long as can reach the instrument of the function of above-mentioned instrument, all can be used as instrument of the present invention and uses.
The reagent used in invention is as follows:
The 1%(mass volume ratio: 1 gram diphenylamine sulfonic acid sodium salt is dissolved in 100 ml water) the diphenylamine sulfonic acid sodium salt indicator.
Mixture of sulfuric phosphoric acid: 98% sulfuric acid mixes with the 1:4 volume ratio with 85% phosphoric acid.
15% NaHCO3 saturated solution: 15 gram NaHCO3 are dissolved in 100ml water.
10% aqueous sulfuric acid: measure 98% concentrated sulphuric acid 10ml in 90ml water.
(0.05mol/L) K
2Cr
2O
7Solution: take 2.4516 grams in 105 ℃ dry to constant weight reference level K
2Cr
2O
7, be dissolved in water in the volumetric flask of 1000 ml, be settled to scale.
Below describe again the working of an invention process of wanting in detail:
Example 1:
In below implementing, the sample of take is as the criterion as 0.15 gram, introduces the specific implementation process of this method, and a kind of activated aluminum assay method, comprise the steps:
Step 1, preparation Fe
2(SO
4)
3Reagent; Detailed process is as follows: take 330 gram Fe
2(SO
4)
3In 750 m l water, add 98% the concentrated sulphuric acid of 75 ml, be heated to dissolve, be diluted in the 1000ml volumetric flask after cooling.
Step 2, the weighing of sample, dissolving: detailed process is as follows: accurately take a certain amount of (such as but not limited to 0.15 gram) aluminium powder sample in 500 ml ground triangular flasks, 25～35 m1(that slowly add in step 1 preparation are 30 m1 preferably) Fe
2(SO
4)
3Solution; Use the rubber plug jam-pack bottleneck of separating funnel and discharge hose is housed immediately, and an insertion of outlet is filled to saturated NaHCO
3In the beaker of solution, (carbon dioxide is insoluble to NaHCO
3In solution, avoid carbon dioxide to lose), reverse the piston of separating funnel, add rapidly preferably 70ml of 65-75ml(from separating funnel) 15% NaHCO
3Solution, jog ground triangular flask, then be placed on the ground triangular flask on thermal source heating and boil that more than 30 minutes, (effect is: 1, NaHCO
3Add thermal decomposition and produce carbon dioxide, make in triangular flask to be full of carbon dioxide, avoid oxygen to enter, make the ferrous ion that is reduced again oxidized; 2, heating impels Fe
2(SO
4)
3The quickening of reacting with AL.) until react completely;
Step 3, (be cooled to room temperature, the careful taking-up is inserted in 15%Na H CO to take off the ground triangular flask
3The hose of saturated solution and the plug on triangular flask; Add again 2～4 (best 3) diphenylamine sulfonic acid sodium salt indicator, use immediately K
2Cr
2O
7Solution (0.05mol/L) is titrated to by green changing to and occurs that purple or hyacinthine are terminal;
Then get final product the content of calculated activity aluminium, calculate and utilize following formula to carry out:
Activated aluminum (%)=
* 100
In formula:
V: be the K consumed
2Cr
2O
7The volume of standard solution (ml);
M: be K
2Cr
2O
7The volumetric molar concentration of standard solution;
G: be sample heavy (g);
26.98 be the molal weight of aluminium.
Embodiment 2:
Embodiment 2 is with the unique difference of embodiment 1, among step 3, before adding the diphenylamine sulfonic acid sodium salt indicator, adds 15ml mixture of sulfuric phosphoric acid and about 30 ml water.Add the effect of mixture of sulfuric phosphoric acid to have two: one, control the needed acidity of titration; The 2nd, indicator discoloration is sharper; It is more accurate to make to measure.
Table 1 is one group of data of the related method of patent of the present invention and GB activated aluminum detection method (GB3169.1-1982) parallel testing, result shows method measurement result of the present invention (parallel≤0.8%) in tolerance, can meet the demands fully, and convenient and easy.
Table 1
Claims (10)
1. an activated aluminum assay method, is characterized in that: comprise the steps:
Step 1, preparation Fe
2(SO
4)
3Reagent;
Step 2, the weighing of sample, dissolving: detailed process is as follows:
Step 2-1, accurately take the aluminium powder sample in container, slowly adds the Fe of preparation in step 1
2(SO
4)
3Solution and 10% sulfuric acid solution;
Step 2-2, seal a bottle immediately, and only stay an outlet and NaHCO
3Solution communicates;
Step 2-3, add rapidly NaHCO
3Solution, the jog container, then be placed on container heating on thermal source and boil
DirectlyTo reacting completely;
Step 3, the solution titration, result is calculated, and detailed process is as follows:
Step 3-1 takes off container (triangular flask) and is cooled to room temperature, and container is opened;
Step 3-2, then add 2-4 and drip the diphenylamine sulfonic acid sodium salt indicator, K used immediately
2Cr
2O
7Solution is titrated to by green changing to and occurs that purple or hyacinthine are terminal;
Then get final product the content of calculated activity aluminium, calculate and utilize following formula to carry out:
The percentage composition of activated aluminum=
* 100
In formula:
V: be the K consumed
2Cr
2O
7The volume of solution (ml);
M: be K
2Cr
2O
7The volumetric molar concentration of solution;
G: be sample heavy (g);
26.98 be the molal weight of aluminium.
2. activated aluminum assay method according to claim 1, it is characterized in that: described step 1 detailed process is as follows: take 330 gram Fe
2(SO
4)
3In 750 m l water, add the concentrated sulphuric acid that 75 ml concentration are 98%, be heated to dissolve, be diluted in the 1000ml volumetric flask after cooling.
3. activated aluminum assay method according to claim 1, is characterized in that: between described step 3-1 and step 3-2, increase following steps: add mixture of sulfuric phosphoric acid and water.
4. activated aluminum assay method according to claim 1, it is characterized in that: in described step 2-1, the aluminium powder sample taken is 0.15～0.20 gram, the Fe added
2(SO
4)
3Solution is 25～35m1, and 10% sulfuric acid solution is 50 m1.
5. activated aluminum assay method according to claim 1 is characterized in that: in described step 2-3, and the saturated NaHCO added
3Solution is 65～75ml.
6. activated aluminum assay method according to claim 1, it is characterized in that: described step 2-2 concrete operations the contents are as follows: immediately with the rubber plug jam-pack container finish of separating funnel and discharge hose is housed, and an insertion of outlet is filled to saturated NaHCO
3In the container of solution.
7. activated aluminum assay method according to claim 3, it is characterized in that: in described step, the mixture of sulfuric phosphoric acid added is 18ml, the water added is 35ml.
8. activated aluminum assay method according to claim 6, it is characterized in that: in described step 2-3, concrete operations the contents are as follows: reverse the separating funnel piston, add rapidly saturated NaHCO from separating funnel
3Solution, the jog container, then be placed on container heating on thermal source and boil
DirectlyTo reacting completely.
9. activated aluminum assay method according to claim 1, it is characterized in that: the mass volume ratio of described diphenylamine sulfonic acid sodium salt indicator is 1%, described NaHCO
3The NaHCO that solution is 15%
3Solution, described K
2Cr
2O
7The molar volume of solution is than being 0.05mol/L.
10. activated aluminum assay method according to claim 3 is characterized in that: described mixture of sulfuric phosphoric acid is that 98% sulfuric acid be take volume ratio and mixed as 1:4 with 85% phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104800115A CN102937590A (en) | 2012-11-23 | 2012-11-23 | Active aluminum detection method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012104800115A CN102937590A (en) | 2012-11-23 | 2012-11-23 | Active aluminum detection method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104568937A (en) * | 2015-01-12 | 2015-04-29 | 中华人民共和国山东出入境检验检疫局 | Determination method for content of metal aluminum in aluminum smelting slag |
| CN106769300A (en) * | 2016-12-13 | 2017-05-31 | 班俊生 | The assay method of effective aluminium and activated silica in a kind of gibbsitic bauxite |
| CN108061778A (en) * | 2017-11-06 | 2018-05-22 | 山西太钢不锈钢股份有限公司 | The detection method of metallic aluminium in aluminum deoxidier |
| CN109406715A (en) * | 2018-12-21 | 2019-03-01 | 鞍钢实业微细铝粉有限公司 | A kind of organic matter passivation aluminium powder active aluminium content detection method |
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| CN101718689A (en) * | 2009-12-21 | 2010-06-02 | 中国航空工业集团公司北京航空材料研究院 | Method for measuring contents of aluminum, titanium, manganese, nickel, tungsten and iron in cobalt-base alloy |
| CN102109468A (en) * | 2010-12-17 | 2011-06-29 | 南昌航空大学 | Method for analyzing aluminum alloy oxidization solution |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104568937A (en) * | 2015-01-12 | 2015-04-29 | 中华人民共和国山东出入境检验检疫局 | Determination method for content of metal aluminum in aluminum smelting slag |
| CN106769300A (en) * | 2016-12-13 | 2017-05-31 | 班俊生 | The assay method of effective aluminium and activated silica in a kind of gibbsitic bauxite |
| CN106769300B (en) * | 2016-12-13 | 2019-07-30 | 班俊生 | The effective measuring method of aluminium and activated silica in a kind of gibbsitic bauxite |
| CN108061778A (en) * | 2017-11-06 | 2018-05-22 | 山西太钢不锈钢股份有限公司 | The detection method of metallic aluminium in aluminum deoxidier |
| CN109406715A (en) * | 2018-12-21 | 2019-03-01 | 鞍钢实业微细铝粉有限公司 | A kind of organic matter passivation aluminium powder active aluminium content detection method |
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Application publication date: 20130220 |