CN108663497A - A method of measuring Dissolved H in Liquid Al-Si Alloy content - Google Patents
A method of measuring Dissolved H in Liquid Al-Si Alloy content Download PDFInfo
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Abstract
A kind of method measuring Dissolved H in Liquid Al-Si Alloy content disclosed by the invention, includes the following steps：Step 1, first one section of clip is used as sample on pre-prepd aluminum alloy sample, then one section of clip is used as cosolvent on remaining aluminum alloy sample；Then after obtained sample and cosolvent being distinguished cleaned dose of cleaning, sample and cosolvent are put into for use in storage solvent；Step 2 will be put into the measurement that hydrogen content is carried out in hydrogen determinator through step 1 treated sample and cosolvent.The present invention can accurately measure the hydrogen content in aluminium alloy using optimal degassing power, degassing time, analysis minute, analysis power and the time of integration.
Description
Technical field
The invention belongs to analyzing detecting method technical fields, and in particular to a method of measuring Dissolved H in Liquid Al-Si Alloy content.
Background technology
Hydrogen mainly exists in the form of interstitial solid solution or hydride in a metal, and exceeded hydrogen content is to cause brittleness
The main reason for.Hydrogen is the harmful element in aluminium and aluminium alloy, and solubility of the hydrogen in solid aluminum is much lower compared with liquid aluminium, due to
Hydrogen atom radius (0.053nm) is small, is easy to spread in a metal, easily infiltrates into the inside of metal under certain condition, and condition becomes
Be easy to be precipitated from the inside of metal again when change, so with the development of aerospace cause, hydrogen content in aluminium more and more by
To stringent control.It is dialled since aluminium alloy is relatively more living, surface is easy to pollute and adsorbs hydrogen, and existing assay method can not be surveyed accurately
Try Dissolved H in Liquid Al-Si Alloy content.
Invention content
The object of the present invention is to provide a kind of methods measuring Dissolved H in Liquid Al-Si Alloy content, can accurately measure the hydrogen in aluminium alloy
Content.
The technical solution adopted in the present invention is, a method of measuring Dissolved H in Liquid Al-Si Alloy content, which is characterized in that including
Following steps：
Step 1, first one section of clip is used as sample on pre-prepd aluminum alloy sample, then on remaining aluminum alloy sample
One section of clip is used as cosolvent；Then after obtained sample and cosolvent being distinguished cleaned dose of cleaning, by sample and cosolvent
It is put into for use in storage solvent；
Step 2 will be put into the measurement that hydrogen content is carried out in hydrogen determinator through step 1 treated sample and cosolvent.
The features of the present invention also characterized in that
The aluminium alloy pole of aluminum alloy sample a diameter of 5.5mm~6mm made of lathe is refined；Sample mass is
2g, size areCosolvent quality is 0.5g.
Storage solvent in step 1 is petroleum ether or ether.
The cleaning process of step 1 is specially：First sample and cosolvent are cleaned through 10% sodium hydroxide solution of mass fraction
2min, then 2min is cleaned through 30% nitric acid of volume fraction, most it is cleaned by ultrasonic 3 times through absolute ethyl alcohol afterwards, each scavenging period is
2min。
Step 2 is specially：First sample and cosolvent are added separately in hydrogen determinator, then to the graphite crucible in hydrogen determinator
Degassing process twice is carried out, analysis measurement finally is carried out to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.25KW, degassing time 30s, second of the work(that deaerates for the first time
Rate is 1.30KW, degassing time 65s；Analysis minute is 100s~120s, and analysis power is 1.2KW~1.5KW；Integral
Time is 75s~85s.
The model EMGA-621W of hydrogen determinator.
The beneficial effects of the present invention are：
The method of the measurement Dissolved H in Liquid Al-Si Alloy content of the present invention, first shears aluminium alloy, cleaning treatment, can prevent outer
Boundary's factor causes hydrogen analysis result unstable, to ensure accuracy of detection；The method of the measurement Dissolved H in Liquid Al-Si Alloy content of the present invention, is adopted
With optimal degassing power, degassing time, analysis minute, analysis power and the time of integration, aluminium alloy can be accurately measured
In hydrogen content.
Specific implementation mode
The present invention is described in detail With reference to embodiment.
A kind of method measuring Dissolved H in Liquid Al-Si Alloy content of the present invention, is specifically implemented according to the following steps：
Step 1, first one section of clip is used as sample on pre-prepd aluminum alloy sample, then on remaining aluminum alloy sample
One section of clip is used as cosolvent；Then after obtained sample and cosolvent being distinguished cleaned dose of cleaning, by sample and cosolvent
It is put into for use in storage solvent；
Since aluminium alloy fusing point is low (660.37 DEG C), the fusing points such as common gas analysis cosolvent iron, copper, nickel, tin, tungsten are equal
Aluminum alloy sample is tested higher than aluminium alloy, therefore aluminium alloy test sample can only be selected itself as cosolvent.
The aluminium alloy pole of aluminum alloy sample a diameter of 5.5mm~6mm made of lathe is refined；Sample mass is
2g, size areCosolvent quality is 0.5g.
The sampling method of sample is affected to the analysis result of Dissolved H in Liquid Al-Si Alloy, high-temperature machining is avoided, using machine
It when tool processing prepares sample, can only be processed using the methods of vehicle, milling, saw, avoid using coolant liquid as possible in process.This
Invention aluminum alloy sample is formed using lathe is refined, and rotating speed, the depth of cut and the turning of lathe are strictly controlled during vehicle
Number.
Since the hydrogen content in aluminium alloy is very low, aluminum alloy sample quality is too small to cause accuracy of detection to reduce, and aluminium closes
Golden sample quality, which crosses conference, causes injection port to get stuck, and sample cannot be fallen into crucible.According to EMGA-621W type hydrogen determinator instruments into
The size of sample mouth is granular (about 2g or so) at the length of about 20mm by aluminum alloy sample hydraulic cutter, pays attention to preventing in shear history
Aluminum alloy sample overheat adversely affects analysis result, it is ensured that accuracy of detection.
Step 1 cleaning process is specially：First sample and cosolvent are cleaned through 10% sodium hydroxide solution of mass fraction
2min, then 2min is cleaned through 30% nitric acid of volume fraction, to remove assay sample surface oxide layer；It is most super through absolute ethyl alcohol afterwards
Sound cleans 3 times, and each scavenging period is 2min, to remove specimen surface pollutant to be analyzed.
Storage solvent in step 1 is petroleum ether or ether, and the preferred petroleum ether of the present invention ensures sample and air insulated,
Sample is avoided to cause hydrogen test result deviation occur because of suction-operated.
The present invention is to carrying out contrast test, test result such as table 1 before and after sample pretreating；
1 test result of table
Find out aluminum alloy sample measurement result stabilization after processing from the test result of table 1, aluminium is removed by chemical treatment
Alloy sample surface oxide layer and surface contaminant enable aluminum alloy to sample cleanup, not contaminated；The sample prepared must be use up
It is analyzed soon, since aluminum alloy surface adsorptivity is extremely strong, when the aluminum alloy sample handled well is not exposed to long in air
Between, sample is stored in petroleum ether when wouldn't analyze, standing time must not exceed 4 hours.
Step 2, by through step 1, treated that aluminum alloy sample is put into carries out the measurement of hydrogen content in hydrogen determinator.
Step 2 is specially：First sample and cosolvent are added separately in hydrogen determinator, then to the graphite crucible in hydrogen determinator
Degassing process twice is carried out, analysis measurement finally is carried out to the hydrogen content in sample.
The purpose of first time degassing process is the foreign gases such as the hydrogen in removing crucible；The purpose of second of degassing process is
Remove the foreign gases such as the hydrogen in fluxing agent.
The analysis parameter of hydrogen determinator is：Power is deaerated for the first time for 6.25KW~7.0KW, degassing time 30s, for the second time
Degassing power is 1.3KW~1.5KW, degassing time 65s；Analysis minute is 100s~120s, and analysis power is 1.2KW
~1.5KW；The time of integration is 75s~85s；The model EMGA-621W of hydrogen determinator.
The specific choice process of the analysis parameter of the assay method of the present invention is as follows：
1) selection of degassing power；
It is 1.30KW first to fix second step degassing power, selects different first step degassing power, sky is carried out with fluxing agent
White experiment, degassing power when blank value tends towards stability is best.Test result is shown in Table 2.
Influence of the different first step degassing power of table 2 to blank value
| Deaerate power KW | 4.0 | 5.0 | 6.0 | 6.25 | 6.5 | 7.0 |
| Blank value ug/g | 0.159 | 0.11 | 0.083 | 0.051 | 0.050 | 0.051 |
The first step deaerates power since 6.25KW as can be seen from Table 2, and blank value tends towards stability；Then first step degassing work(
Rate is 6.25KW~7.0KW.
First step degassing power is fixed again, selects different second step degassing power, it is empty with fluxing agent into line blank test
Degassing power when white value tends towards stability is best.Test result is shown in Table 3.
Influence of the different second step degassing power of table 3 to blank value
| Deaerate power KW | 0.80 | 1.00 | 1.20 | 1.30 | 1.40 | 1.50 |
| Blank value ug/g | 0.12 | 0.091 | 0.078 | 0.050 | 0.052 | 0.049 |
Second step deaerates power since 1.30KW as can be seen from Table 3, and blank value tends towards stability, then second step degassing work(
Rate is 1.3KW~1.5KW.
2) selection of power is analyzed：
Different analysis power are tested with identical aluminum alloy sample, test result is shown in Table in 4.
Influence of the different analysis power of table 4 to hydrogen measurement result
As can be seen from Table 4, when analysis power is 1.20KV~1.50KV, hydrogen content measured value tends towards stability；Analysis power exists
Detected value later 2.00KV starts to reduce, and unstable, causes heating speed too fast this is because power is excessively high, graphite crucible
Middle aluminum alloy sample splashes, and hydrogen release, which is put, in aluminum alloy sample not exclusively causes measurement result relatively low, and repeatability is bad.Therefore it is of the invention
Analysis power be 1.2KW~1.5KW.
3) selection of analysis time
Different analysis times are tested with identical aluminium alloy aluminum alloy sample, test result is shown in Table in 5.
Influence of the different analysis times of table 5 to hydrogen measurement result
| Analysis time s | 70 | 80 | 90 | 100 | 110 | 120 | 130 |
| Hydrogen content ug/g | 0.099 | 0.136 | 0.189 | 0.209 | 0.205 | 0.207 | 0.182 |
As can be seen from Table 5, when analysis time is 100s~120s, hydrogen content measured value tends towards stability；Analysis time is in 130s
Later detected value starts to reduce, and unstable, this is because analysis time long causes nitrogen in separator to enter detector shadow
Ring the testing result to hydrogen content；So the analysis time of the present invention is 100s~120s.
3) selection of the time of integration
The different times of integration are tested with identical aluminum alloy sample, test result is shown in Table in 6.
Influence of the different times of integration of table 6 to hydrogen measurement result
| Time of integration s | 60 | 65 | 70 | 75 | 80 | 85 | 90 |
| Hydrogen content ug/g | 0.101 | 0.149 | 0.177 | 0.210 | 0.205 | 0.203 | 0.075 |
As can be seen from Table 6, the time of integration, between 75s~85s, hydrogen content measured value tends towards stability；Analysis time is more than 90s
Detected value starts to reduce, and unstable, this is because the time of integration it is long cause hydrogen to discharge completely, release profiles decline suddenly
Influence the testing result of hydrogen content.So the time of integration of the present invention is 75s~85s.
The specific determination step of hydrogen content is：The F12 function keys for first pressing hydrogen determinator or the START on heating unit front panel
Key, opens the sample-adding lid of hydrogen determinator, and cosolvent is poured into cosolvent slot, and sample is put into sample slot, is closed the lid；It presses again and determines hydrogen
The F12 function keys of instrument or the START keys on heating unit front panel, electrode furnace body decline, and upper and lower electrode tip is cleaned with water with brush,
After carefully wiping upper and lower electrode tip and cavity with clean white silk, graphite crucible is placed on lower electrodes base；It is fixed to press again
The F12 function keys of hydrogen instrument or the START keys on heating unit front panel, electrode furnace body rises, in the graphite crucible of hydrogen determinator
Cosolvent carry out degassing process twice, liquid-bath (cosolvent of fusing) is equably laid in crucible bottom, in order to avoid sample and earthenware
Crucible is in direct contact, conducive to hydrogen in sample decomposition and disengage；Aluminum alloy sample is fallen into graphite crucible after the completion of degassing, start into
Row hydrogen content measures, and the content of hydrogen is finally obtained from display screen.
Brush is wanted to clean upper and lower electrode tip with water before sample is added every time, being subsequently used for the white silk earned, carefully wiping is upper and lower
Electrode tip and cavity, in case previous aluminum alloy sample impacts rear primary measurement result.
The method of the measurement Dissolved H in Liquid Al-Si Alloy content of the present invention, first shears aluminium alloy, cleaning treatment, can prevent outer
Boundary's factor causes hydrogen analysis result unstable, to ensure accuracy of detection；The method of the measurement Dissolved H in Liquid Al-Si Alloy content of the present invention, is adopted
With optimal degassing power, degassing time, analysis minute, analysis power and the time of integration, can measure accurate in aluminium alloy
True hydrogen content.
Embodiment 1
Step 1, first one section of size of clip is on pre-prepd aluminum alloy sampleSample make
For sample, then one section of 0.5g of clip is used as cosolvent on remaining aluminum alloy sample；Then sample and cosolvent are passed through successively
10% sodium hydroxide solution of mass fraction, 30% nitric acid of volume fraction are respectively washed 2min；Most it is cleaned by ultrasonic 3 through absolute ethyl alcohol afterwards
Secondary, each scavenging period is 2min；
Step 1 treated sample and cosolvent are first added separately in hydrogen determinator by step 2, then in hydrogen determinator
Graphite crucible carries out degassing process twice, finally carries out analysis measurement to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.25KW, degassing time 30s, second of the work(that deaerates for the first time
Rate is 1.30KW, degassing time 65s；Analysis minute is 100s, and analysis power is 1.2KW；The time of integration is 75s.
Embodiment 2
Step 1, first one section of size of clip is on pre-prepd aluminum alloy sampleSample make
For sample, then one section of 0.5g of clip is used as cosolvent on remaining aluminum alloy sample；Then sample and cosolvent are passed through successively
10% sodium hydroxide solution of mass fraction, 30% nitric acid of volume fraction are respectively washed 2min；Most it is cleaned by ultrasonic 3 through absolute ethyl alcohol afterwards
Secondary, each scavenging period is 2min；
Step 1 treated sample and cosolvent are first added separately in hydrogen determinator by step 2, then in hydrogen determinator
Graphite crucible carries out degassing process twice, finally carries out analysis measurement to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.5KW, degassing time 30s, second of the power that deaerates for the first time
For 1.4KW, degassing time 65s；Analysis minute is 100s, and analysis power is 1.3KW；The time of integration is 80s.
Embodiment 3
Step 1, first one section of size of clip is on pre-prepd aluminum alloy sampleSample make
For sample, then one section of 0.5g of clip is used as cosolvent on remaining aluminum alloy sample；Then sample and cosolvent are passed through successively
10% sodium hydroxide solution of mass fraction, 30% nitric acid of volume fraction are respectively washed 2min；Most it is cleaned by ultrasonic 3 through absolute ethyl alcohol afterwards
Secondary, each scavenging period is 2min；
Step 1 treated sample and cosolvent are first added separately in hydrogen determinator by step 2, then in hydrogen determinator
Graphite crucible carries out degassing process twice, finally carries out analysis measurement to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.25KW, degassing time 30s, second of the work(that deaerates for the first time
Rate is 1.50KW, degassing time 65s；Analysis minute is 120s, and analysis power is 1.4KW；The time of integration is 85s.
Embodiment 4
Step 1, first one section of size of clip is on pre-prepd aluminum alloy sampleSample make
For sample, then one section of 0.5g of clip is used as cosolvent on remaining aluminum alloy sample；Then sample and cosolvent are passed through successively
10% sodium hydroxide solution of mass fraction, 30% nitric acid of volume fraction are respectively washed 2min；Most it is cleaned by ultrasonic 3 through absolute ethyl alcohol afterwards
Secondary, each scavenging period is 2min；
Step 1 treated sample and cosolvent are first added separately in hydrogen determinator by step 2, then in hydrogen determinator
Graphite crucible carries out degassing process twice, finally carries out analysis measurement to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.25KW, degassing time 30s, second of the work(that deaerates for the first time
Rate is 1.40KW, degassing time 65s；Analysis minute is 110s, and analysis power is 1.4KW；The time of integration is 75s.
Embodiment 5
Step 1, first one section of size of clip is on pre-prepd aluminum alloy sampleSample make
For sample, then one section of 0.5g of clip is used as cosolvent on remaining aluminum alloy sample；Then sample and cosolvent are passed through successively
10% sodium hydroxide solution of mass fraction, 30% nitric acid of volume fraction are respectively washed 2min；Most it is cleaned by ultrasonic 3 through absolute ethyl alcohol afterwards
Secondary, each scavenging period is 2min；
Step 1 treated sample and cosolvent are first added separately in hydrogen determinator by step 2, then in hydrogen determinator
Graphite crucible carries out degassing process twice, finally carries out analysis measurement to the hydrogen content in sample.
The analysis parameter of hydrogen determinator is：Degassing power is 6.25KW, degassing time 30s, second of the work(that deaerates for the first time
Rate is 1.50KW, degassing time 65s；Analysis minute is 100s, and analysis power is 1.2KW；The time of integration is 75s.
Protium in aluminium alloy standard substance 7B04 is measured using the assay method of the present invention, in determining work
Under the conditions of, carry out accuracy experiment using hydrogen determinator.Experimental result is shown in Table 7：
7 standard substance test result of table
The present invention carries out 10 weights using aluminium alloy 2D70 raw material as aluminum alloy sample, using the assay method of the present invention
Renaturation precision test, and compared with the standard value of other test in laboratory, experimental result is shown in Table 8：
8 aluminum alloy sample experimental result of table
The measurement result relative standard deviation of the assay method of the present invention is less than 5%, with other laboratory detection result phases
Poor 0.01 μ g/g, show that this method is accurate and reliable.
Claims (7)
1. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content, which is characterized in that include the following steps：
Step 1, first one section of clip is used as sample, then the clip on remaining aluminum alloy sample on pre-prepd aluminum alloy sample
One section is used as cosolvent；Then after obtained sample and cosolvent being distinguished cleaned dose of cleaning, sample and cosolvent are put into
It stores for use in solvent；
Step 2 will be put into the measurement that hydrogen content is carried out in hydrogen determinator through step 1 treated sample and cosolvent.
2. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as described in claim 1, which is characterized in that the aluminum alloy sample
The aluminium alloy pole of a diameter of 5.5mm~6mm made of lathe is refined；The sample mass is 2g, and size isThe cosolvent quality is 0.5g.
3. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as described in claim 1, which is characterized in that in the step 1
It is petroleum ether or ether to store solvent.
4. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as described in claim 1, which is characterized in that clear described in step 1
It washes specially：Sample and cosolvent are first cleaned into 2min through 10% sodium hydroxide solution of mass fraction, then through volume fraction 30%
Nitric acid cleans 2min, is most cleaned by ultrasonic 3 times through absolute ethyl alcohol afterwards, and each scavenging period is 2min.
5. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as described in claim 1, which is characterized in that the step 2 is specific
For：First sample and cosolvent are added separately in hydrogen determinator, then degassing process twice is carried out to the graphite crucible in hydrogen determinator,
Analysis measurement finally is carried out to the hydrogen content in sample.
6. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as claimed in claim 5, which is characterized in that point of the hydrogen determinator
Analysing parameter is：Degassing power is 6.25KW, degassing time 30s for the first time, and second of the power that deaerates is 1.30KW, degassing time
For 65s；Analysis minute is 100s~120s, and analysis power is 1.2KW~1.5KW；The time of integration is 75s~85s.
7. a kind of method measuring Dissolved H in Liquid Al-Si Alloy content as claimed in claim 5, which is characterized in that the type of the hydrogen determinator
Number be EMGA-621W.
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