CN108562560A - A kind of method of aluminium content in measurement titanium alloy - Google Patents
A kind of method of aluminium content in measurement titanium alloy Download PDFInfo
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Abstract
The invention discloses a kind of method of aluminium content in measurement titanium alloy, the assay method includes the following steps：1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；3）Control sample correction：By analyzing the standard sample of known content, it is corrected according to the deviation of analysis result and standard value, obtains correction coefficient；4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut, and is polished titanium alloy sample surface, waits for that surfacing is smooth spare；5）Analysis measures：It titanium alloy sample, is analyzed using photoelectric emission spectrograph, the average value of analysis result to be obtained, analysis terminates.The present invention measures aluminium content in titanium alloy, and by the verification repeatedly of standard sample, measurement result has good stability, reproducibility and accuracy.
Description
Technical field
The invention belongs to chemical analysis test technical fields, and in particular to a method of measuring aluminium content in titanium alloy.
Background technology
Titanium alloy has intensity height and density is small, and mechanical performance and toughness, etch resistant properties are fine, in the sixties in last century
Phase is just used in industry, and titanium alloy material is used to make the electrode of electrolytic industry, the condenser in power station, benzin
The heater and environment pollution control device etc. of refining and sea water desalination.With the needs that aerospace industry develops, make titanium work
Industry is developed with every year on average about 8% growth rate.Mainly production titanium ingot, titanium volume, the titanium alloy production mostly of current Tai Ye companies
Product can be by high-end fields such as products application to aerospace, medical treatment nowadays in order to keep on improving titanium products quality, this is just
New requirement is proposed to the detection work of various chemical compositions in titanium alloy, aluminium and v element are the constant members in titanium alloy
Element, chemical composition content is relatively high, is the quality control index of titanium alloy product.
The aluminium content in titanium alloy is measured at present, and main method is to measure titanium with reference to plasma atomic emission spectrometry to close
Research in gold in terms of multielement, and rarely photoelectric emission spectrograph measures the paper and patent of aluminium content in titanium alloy,
More without national standard.Moreover plasma atomic emission spectrometer and photoelectric emission spectrograph are two distinct types of set
Standby, analysis sample state, analysis condition, operating process are all different, and can be sayed without what similitude.
Therefore, a kind of method measuring aluminium content in titanium alloy is invented, by a large amount of experiment, Reusability standard specimen is tested
Card, constantly gropes and studies, it is established that reliable analyzing detecting method realizes quick, the accurate survey to aluminium content in titanium alloy
It is fixed, it is innovation and technological break-through of the photoelectric emission spectrograph in titanium alloy sample detection method, has filled up photoemission spectrum
Technological gap of the instrument in titanium alloy sample detection method.
Invention content
The purpose of the present invention is to provide a kind of methods of aluminium content in measurement titanium alloy.
The object of the present invention is achieved like this, includes the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut, is polished titanium alloy sample surface with belt sander, waits for that surface is flat
It is whole smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation,
Excitation position, the average value of analysis result to be obtained are needed to change when repetitive operation, analysis terminates；The photoelectric emission spectrograph
Operating condition be：
。
Compared with prior art, beneficial effects of the present invention：
1）The present invention measures aluminium content in titanium alloy, and by the verification repeatedly of standard sample, measurement result has good stabilization
Property, reproducibility and accuracy.
2）The method of the present invention is reliable, practical, can meet aluminum content tests needs in daily titanium alloy.
3）The analysis method that the present invention uses does not use any chemical reagents, and analysis cost is low, environmentally safe, can
Multielement simultaneous determination, it is easier, while the time can be saved.
4）The analysis method that the present invention uses need not claim sample, molten sample process, shorten analytical cycle, improve analysis
Efficiency alleviates the labor intensity of analysis operation personnel, reduces the harmful effect to environment and operating personnel.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated, but is not limited in any way to the present invention,
Based on present invention teach that made by it is any transform or replace, all belong to the scope of protection of the present invention.
The method of aluminium content, includes the following steps in measurement titanium alloy of the present invention：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut, is polished titanium alloy sample surface with belt sander, waits for that surface is flat
It is whole smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation,
Excitation position, the average value of analysis result to be obtained are needed to change when repetitive operation, analysis terminates；The photoelectric emission spectrograph
Operating condition be：
。
Element wavelength to be measured：
。
Step（1）Described in a trace behaviour alternatively steel sample trace is carried out to spectrometer at Fe287.2nm spectral lines
Operation, final choice 292 are used as trace value.
Step（2）Described in normalizing operation be to use Ti323.2nm as internal standard channel, with RTi11/29, BST-5A,
Tri- Sample of Ti Alloy of BST-81 are standardized operation, obtain standardization correction coefficient alpha=0.89554 of Al elements, β=
0.00932 and κ=1.0000.
Step（3）Described in known content standard sample be Sample of Ti Alloy TC11, obtain Al elements correction system
Number AC=0.00000, MC=1.0000.
Step（4）Described in belt sander granularity be 60 ~ 80 mesh.
Step（4）Described in titanium alloy sample to be measured cutting specification be high 2.5 ~ 4cm, 12 ~ 30mm of diameter.
Step（4）Described in be cut into and cut using wire cutting machine.
The photoelectric emission spectrograph is PDA-8000 photoelectric emission spectrographs.
Step（5）Described in repetitive operation number be not less than 1 time.
Embodiment 1
The method of aluminium content, includes the following steps in a kind of measurement titanium alloy：
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N, middle section
Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
1）Trace
When inspection apparatus state, if trace is wanted in photoelectric emission spectrograph prompt, trace operation is carried out, turntable is passed through
Travelling slit position, adjustment each element peak position deviation, then with the accuracy of sample survey trace numerical value, only retouched in time
Mark operates, and just can guarantee the accuracy and reliability of aluminium content in titanium alloy sample.The present embodiment selects a steel sample,
At Fe287.2nm spectral lines, trace operation is carried out to spectrometer, final choice 292 is used as trace value.
2）Standardization
Elemental profiles in titanium alloy can at any time, environmental change, will produce deviation after repeatedly analyze, need selection three
A Sample of Ti Alloy is standardized operation, recalculates standardization correction coefficient alpha, β and κ values, it is ensured that analysis result accurately may be used
It leans on.The present embodiment uses Ti323.2nm as internal standard channel, and with RTi11/29, tri- Sample of Ti Alloy of BST-5A, BST-81 carry out
Normalizing operation obtains standardization correction coefficient alpha=0.89554, β=0.00932 and κ=1.0000 of Al elements.
3）Control sample correction
By analyzing the standard sample of known content, it is corrected according to the deviation of analysis result and standard value, obtains correction system
Number, to reduce analytical error；After instrument has carried out trace and normalizing operation, analytical error feelings bigger than normal are there is also
Condition will then carry out control sample correction work.The present embodiment selects Sample of Ti Alloy TC11 to control sample correcting sample, obtains Al elements
Control sample correction coefficient AC=0.00000, MC=1.0000.
4）It is prepared by sample pretreating：By titanium alloy sample to be measured（Sample of Ti Alloy TC4）Cutting, uses belt sander（Belt sander
Granularity is 60 mesh）It polishes titanium alloy sample surface, waits for that surfacing is smooth spare.
5）Analysis measures：The present embodiment selects Sample of Ti Alloy TC4 to carry out analysis verification work, is placed on photoemission light
On the excitation bench of spectrometer, sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode
Point, repetitive operation 11 times, when repetitive operation, need to change excitation position, the average value of analysis result to be obtained, and analysis terminates；It is described
The operating condition of photoelectric emission spectrograph be：
。
The data of acquisition are as shown in the table：（n=11）
。
As can be seen from the above table, Al elements average value and standard value error very little, RSD are less than 1%, and analysis result has very well
Precision, illustrate that the method for the present invention is accurate and reliable.
Embodiment 2
A titanium for choosing the production of Yunnan Tai Ye companies adds up to sample 1#, it is cut into diameter 15mm with wire cutting machine, height
The square of 35mm carries out being polishing to any surface finish smoothly for use with sample grinding machine.
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N,
Middle section's Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
Control sample correction：By analyzing the standard sample of known content, it is corrected, is obtained according to the deviation of analysis result and standard value
Obtain correction coefficient；
Analysis measures：The titanium alloy sample smooth any surface finish is polishing to, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation,
Excitation position is needed to change when repetitive operation, and the average value for showing analysis result on computers, analysis is waited to terminate；The photoelectricity hair
The operating condition for penetrating spectrometer is：
This operating procedure repeats 11 times.
Obtained analysis result see the table below：
。
As can be seen from the above table, Al elements average value and standard value error very little, RSD are less than 1%, and analysis result has very well
Precision, illustrate that the method for the present invention is accurate and reliable.
Embodiment 3
The method of aluminium content, includes the following steps in a kind of measurement titanium alloy：
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N, middle section
Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
Include the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured to be cut using wire cutting machine, the specification of cutting is high 2.5cm,
Diameter 12mm, uses belt sander（The granularity of belt sander is 80 mesh）It polishes titanium alloy sample surface, waits for that surfacing is smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation 1
Secondary, when repetitive operation, needs to change excitation position, the average value of analysis result to be obtained, and analysis terminates；The photoemission light
The operating condition of spectrometer is：
。
Embodiment 4
The method of aluminium content, includes the following steps in a kind of measurement titanium alloy：
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N, middle section
Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
Include the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut using wire cutting machine, the specification of cutting is high 4cm, directly
Diameter 30mm, uses belt sander（The granularity of belt sander is 70 mesh）It polishes titanium alloy sample surface, waits for that surfacing is smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation 2
Secondary, when repetitive operation, needs to change excitation position, the average value of analysis result to be obtained, and analysis terminates；The photoemission light
The operating condition of spectrometer is：
。
Embodiment 5
The method of aluminium content, includes the following steps in a kind of measurement titanium alloy：
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N, middle section
Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
Include the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut using wire cutting machine, the specification of cutting is high 3cm, directly
Diameter 20mm, uses belt sander（The granularity of belt sander is 60 mesh）It polishes titanium alloy sample surface, waits for that surfacing is smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation 5
Secondary, when repetitive operation, needs to change excitation position, the average value of analysis result to be obtained, and analysis terminates；The photoemission light
The operating condition of spectrometer is：
。
Embodiment 6
The method of aluminium content, includes the following steps in a kind of measurement titanium alloy：
Key instrument:1. photoelectric emission spectrograph:PDA-8000, Japanese Shimadzu Corporation;2. argon gas evolution device:CZA-4N, middle section
Puri;3. regulated power supply:YQS-10KB AC purified voltage stabilized power sources.
Include the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured to be cut using wire cutting machine, the specification of cutting is high 3.5cm,
Diameter 25mm, uses belt sander（The granularity of belt sander is 80 mesh）It polishes titanium alloy sample surface, waits for that surfacing is smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation 20
Secondary, when repetitive operation, needs to change excitation position, the average value of analysis result to be obtained, and analysis terminates；The photoemission light
The operating condition of spectrometer is：
。
Claims (9)
1. a kind of method measuring aluminium content in titanium alloy, it is characterised in that include the following steps：
1）Trace：Start spectrometer analysis software, trace operation is carried out to photoelectric emission spectrograph；
2）Standardization：Three Sample of Ti Alloy are selected to be standardized operation, normalized correction coefficient alpha, β and κ values；
3）Control sample correction：By the standard sample of analysis known content, it is corrected according to the deviation of analysis result and standard value,
Obtain correction coefficient；
4）It is prepared by sample pretreating：Titanium alloy sample to be measured is cut, is polished titanium alloy sample surface with belt sander, waits for that surface is flat
It is whole smooth spare；
5）Analysis measures：By step（4）The titanium alloy sample of processing, is placed on the excitation bench of photoelectric emission spectrograph,
Sample stage hole is covered, closed safe door starts to excite, and safety door is opened after analysis, scrubs electrode tip, repeats operation,
Excitation position, the average value of analysis result to be obtained are needed to change when repetitive operation, analysis terminates；The photoelectric emission spectrograph
Operating condition be：
。
2. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（1）Described in retouch
Alternatively a steel sample carries out trace operation, final choice 292 is used as and retouches to mark behaviour at Fe287.2nm spectral lines to spectrometer
Mark value.
3. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（2）Described in mark
Standardization operation is uses Ti323.2nm as internal standard channel, and with RTi11/29, tri- Sample of Ti Alloy of BST-5A, BST-81 carry out
Normalizing operation obtains standardization correction coefficient alpha=0.89554, β=0.00932 and κ=1.0000 of Al elements.
4. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（3）Described in
Know that the standard sample of content is Sample of Ti Alloy TC11, obtains correction coefficient AC=0.00000 of Al elements, MC=1.0000.
5. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（4）Described in sand
Granularity with machine is 60 ~ 80 mesh.
6. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（4）Described in wait for
The specification for surveying titanium alloy sample cutting is high 2.5 ~ 4cm, 12 ~ 30mm of diameter.
7. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（4）Described in cut
It is segmented into and is cut using wire cutting machine.
8. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that the photoemission light
Spectrometer is PDA-8000 photoelectric emission spectrographs.
9. the method according to claim 1 for measuring aluminium content in titanium alloy, it is characterised in that step（5）Described in weight
The number operated again is not less than 1 time.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109752366A (en) * | 2019-03-01 | 2019-05-14 | 本钢板材股份有限公司 | Method that is a kind of while measuring multielement content in potassium steel |
| CN110146491A (en) * | 2019-06-14 | 2019-08-20 | 山西八达镁业有限公司 | A method of verifying alloying component testing result accuracy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109752366A (en) * | 2019-03-01 | 2019-05-14 | 本钢板材股份有限公司 | Method that is a kind of while measuring multielement content in potassium steel |
| CN110146491A (en) * | 2019-06-14 | 2019-08-20 | 山西八达镁业有限公司 | A method of verifying alloying component testing result accuracy |
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Application publication date: 20180921 |