CN102393387A - Method for analyzing surface silver coating components of high-temperature alloy GH4169 part - Google Patents
Method for analyzing surface silver coating components of high-temperature alloy GH4169 part Download PDFInfo
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- CN102393387A CN102393387A CN2011103560853A CN201110356085A CN102393387A CN 102393387 A CN102393387 A CN 102393387A CN 2011103560853 A CN2011103560853 A CN 2011103560853A CN 201110356085 A CN201110356085 A CN 201110356085A CN 102393387 A CN102393387 A CN 102393387A
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Abstract
The invention provides a method for analyzing the surface silver coating components of a high-temperature alloy GH4169 part. According to the invention, first, a part test piece is cleaned; a surface silver coating is dissolved, and a sufficient amount of dilute hydrochloric acid is added to the solution, such that a precipitate is formed; after the volume is metered, the supernatant is adopted as a sample solution; a blank contrast solution and a calibration solution are prepared; and the sample solution, the blank contrast solution and the calibration solution are detected by using an inductively coupled plasma atomic emission spectrometer, such that the component contents of the surface silver coating of the part test piece are obtained. According to the invention, various elements can be detected simultaneously with a single time of sample pretreatment. Further, the single time of sample pretreatment is more convenient than pretreatment processes of existing methods.
Description
Technical field
The present invention relates to the material tests technical field, be specially a kind of method of analyzing high temperature alloy GH4169 piece surface silver coating composition.
Background technology
Silver is stable as a kind of chemical property, and the difficult metal that reacts with air has well anti-oxidant, anticorrosive effect.And the ductility of silver is good, is conduction, the fabulous metal of heat conduction.Therefore play good conduction, anti-oxidation, anticorrosion, anti and effect attractive in appearance in that piece surface is silver-plated.Analyze the composition of piece surface silver coating, can consider silver-plated effect, whether whether the silver-colored purity that detects silver coating reach requirement or in silver-plated process, have other materials to sneak into silver coating, thereby the control silver coating can farthest be brought into play above-mentioned effect.
Existing silver coating analytical approach has atomic absorption method, AAS; When these methods are the chemical constitution of piece surface silver coating of high temperature alloy GH4169 at analysis of material; Need measure respectively each element in the silver coating; When measuring different element, need the different processing procedure in early stage of experience, cause analytic process loaded down with trivial details.
Summary of the invention
The technical matters that solves
For solving the problem that prior art exists, the present invention proposes a kind of method of analyzing high temperature alloy GH4169 piece surface silver coating composition.
Technical scheme
Technical scheme of the present invention is:
Said a kind of method of analyzing high temperature alloy GH4169 piece surface silver coating composition is characterized in that: may further comprise the steps:
Step 1: the part test piece was immersed in the salpeter solution of 1+9 to 1,+12 5 to 10 minutes; Part test piece top layer dirt is cleared up; Then the part test piece is pulled out, behind distilled water flushing, with ether part test piece surface is cleaned again; After the cleaning part test piece dried and weigh, obtain weight M gram;
Step 2: the part test piece that will pass through after step 1 is handled is immersed in the salpeter solution of 1+2 to 1+5; Treat after the dissolving of part test piece surface silver layer the part test piece to be taken out; With distilled water the part test piece is fully washed, and washing lotion is collected, after the flushing part test piece oven dry is weighed; Obtain weight m gram, and then the silver layer weight that obtains dissolving is the M-m=G gram;
Step 3: the washing lotion heating with step 2 is collected, when washing lotion is just seethed with excitement, stop heating, in washing lotion, add capacity watery hydrochloric acid, form the AgCl post precipitation, once more to the washing lotion heating, make the AgCl deposition stop heating after the cohesion fully;
Step 4: will pass through after washing lotion after step 3 is handled naturally cools to room temperature; Washing lotion is moved in first volumetric flask; And with the container that holds washing lotion in the distilled water cleaning step 33 to 5 times, obtain new washing lotion and also move in first volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare the standard blank solution of sample solution, No. 1 calibration solutions and No. 2 calibration solutions respectively;
Said No. 1 calibration solutions process for preparation is: take by weighing the fine silver mark steel of weight between 95%G to 1.05%G, with the salpeter solution of 1+1 to 1+3 fine silver is marked the steel dissolving, fine silver is marked the heating of steel lysate; When fine silver mark steel lysate has just seethed with excitement; Stop heating, in fine silver mark steel lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To the heating of fine silver mark steel lysate, make the AgCl deposition stop heating after the cohesion fully once more; After fine silver marked the steel lysate and naturally cool to room temperature; Fine silver is marked the steel lysate to be moved in second volumetric flask; And clean the container 3 to 5 times hold fine silver mark steel lysate with distilled water, and obtain washing lotion and also move in second volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solutions; The second volumetric flask volume is identical with the first volumetric flask volume;
Said No. 2 calibration solutions process for preparation are: take by weighing the purity of weight between 95%G to 1.05%G greater than 99.99% high fine silver; Salpeter solution with 1+1 to 1+3 dissolves high fine silver, and in high fine silver lysate, adding concentration is the ferrous solution 0.2mL to 0.4mL of 1mg/mL, then with high fine silver lysate heating; When high fine silver lysate has just seethed with excitement; Stop heating, in high fine silver lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To high fine silver lysate heating, make the AgCl deposition stop heating after the cohesion fully once more; After high fine silver lysate naturally cooled to room temperature; High fine silver lysate is moved in the 3rd volumetric flask; And clean the container 3 to 5 times hold high fine silver lysate with distilled water, and obtain washing lotion and also move in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solutions; The 3rd volumetric flask volume is identical with the first volumetric flask volume;
Step 6: in the sample message file with the constant volume input inductance coupled plasma Atomic Emission Spectrometer AES of first volumetric flask in dissolving silver layer weight G in the step 2 and the step 4; With inductively coupled plasma atomic emission spectrometer start after stable at least 1 hour; The standard blank solution of analytical sample solution, No. 1 calibration solutions, No. 2 calibration solutions and sample solution successively; Then by the percentage composition of plumbous each element of bismuth of copper iron in the inductively coupled plasma atomic emission spectrometer output element test piece surface silver layer, the percentage composition by plumbous each element of bismuth of copper iron calculates silver content in the part test piece surface silver layer again.
Beneficial effect
It is that the chemical constitution of the piece surface silver coating of high temperature alloy GH4169 is measured to material that the present invention adopts inductively coupled plasma atomic emission spectrometer (ICP); Only once early stage, sample preparation can be measured each element simultaneously; And once early stage the sample preparation process also the processing procedure in early stage in than existing methods is more easy; Overcome in the existing method and need measure respectively each element in the silver coating; When measuring different element, need the different processing procedure in early stage of experience, cause the loaded down with trivial details problem of analytic process.
Embodiment
Below in conjunction with specific embodiment the present invention is described:
Embodiment 1:
Present embodiment is that the piece surface silver coating composition of high temperature alloy GH4169 is analyzed to material, mainly analyzes four constituent contents of the plumbous bismuth of copper iron in the silver coating, calculates the content of silver in the silver coating then.
The method step of present embodiment is following:
Step 1: the part test piece was immersed in the pure salpeter solution of top grade of 1+9 5 minutes; Part test piece top layer dirt is cleared up; Then the part test piece is pulled out, behind distilled water flushing, with ether part test piece surface is cleaned again; After the cleaning part test piece dried and weigh, obtain weight M=30.25 gram;
Step 2: the part test piece that will pass through after step 1 is handled is immersed in the salpeter solution of 1+2; Treat after the dissolving of part test piece surface silver layer the part test piece to be taken out; With distilled water the part test piece is fully washed, and washing lotion is collected, after the flushing part test piece oven dry is weighed; Obtain weight m=12.38 gram, and then the silver layer weight that obtains dissolving is the M-m=G=17.87 gram;
Step 3: the washing lotion that step 2 is collected places on the electric furnace and heats, and when washing lotion is just seethed with excitement, stops heating, in washing lotion, adds the pure watery hydrochloric acid of capacity top grade, forms the AgCl post precipitation, once more to the washing lotion heating, makes the AgCl deposition stop heating after the cohesion fully;
Step 4: will pass through after washing lotion after step 3 is handled naturally cools to room temperature; Washing lotion is moved in first volumetric flask of 200mL; And with the container that holds washing lotion in the distilled water cleaning step 33 times, obtain new washing lotion and also move in first volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare the standard blank solution of sample solution, No. 1 calibration solutions and No. 2 calibration solutions respectively;
Said No. 1 calibration solutions process for preparation is: take by weighing the fine silver mark steel of 18.00 grams, with the salpeter solution of 1+1 fine silver is marked the steel dissolving, fine silver is marked the heating of steel lysate; When fine silver mark steel lysate has just seethed with excitement; Stop heating, in fine silver mark steel lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To the heating of fine silver mark steel lysate, make the AgCl deposition stop heating after the cohesion fully once more; After fine silver marked the steel lysate and naturally cool to room temperature; Fine silver is marked in second volumetric flask that the steel lysate moves to 200mL; And clean the container 3 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in second volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solutions;
Said No. 2 calibration solutions process for preparation are: the purity that takes by weighing 18.00 grams is greater than 99.99% high fine silver, with the salpeter solution of 1+1 high fine silver dissolved, and adding concentration is the ferrous solution 0.3mL of 1mg/mL in high fine silver lysate; Then, when high fine silver lysate has just seethed with excitement, stop heating with high fine silver lysate heating; In high fine silver lysate, add capacity watery hydrochloric acid; Form the AgCl post precipitation,, make the AgCl deposition stop heating after the cohesion fully once more to high fine silver lysate heating; After high fine silver lysate naturally cooled to room temperature; High fine silver lysate is moved in the 3rd volumetric flask of 200mL; And clean the container 3 times hold high fine silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solutions;
The process for preparation of the standard blank solution of sample solution is: get with step 2 in the identical 1+2 salpeter solution of salpeter solution volume; And stop heating after being heated to firm boiling; Again to wherein add with step 3 in the watery hydrochloric acid of watery hydrochloric acid equivalent; Gained solution moves in the 4th volumetric flask of 200mL after naturally cooling to room temperature, and cleans the container 3 times hold gained solution with distilled water, and the washing lotion that obtains also moves in the 4th volumetric flask; Be settled to shake up behind the scale mark and leave standstill, get in the 4th volumetric flask solution as the standard blank solution of sample solution;
Step 6: in the sample message file with the constant volume 200mL input inductance coupled plasma Atomic Emission Spectrometer AES of first volumetric flask in the dissolving silver layer weight in the step 2 17.87 gram and the step 4, with inductively coupled plasma atomic emission spectrometer start shooting stablize 1 hour after, instrument parameter be set be: radio-frequency power 1350W; Plasma gas flow rate 15L/min; Secondary air amount 0.2L/min, carrier gas flux 1L/min, observed altitude 15mm; Sample flow rate 1.5ml/min; 40 seconds time delay of reading, point 3 points, each element analysis spectrum line sees the following form:
| Analytical element | Fe | Bi | Cu | Pb |
| Wavelength (nm) | 238.204 | 223.061 | 224.700 | 217.000 |
Then adopt inductively coupled plasma atomic emission spectrometer standard blank solution, No. 1 calibration solutions, No. 2 calibration solutions and the sample solution of analytical sample solution successively; Obtain the spectral intensity of plumbous each element of bismuth of copper iron in standard blank solution, calibration solutions and the style solution respectively; And by the percentage composition of plumbous each element of bismuth of copper iron in the inductively coupled plasma atomic emission spectrometer output element test piece surface silver layer; The result is Fe 0.00002% (Wt%); Cu0.00004% (Wt%); Pb 0.00090% (Wt%), Bi 0.00010% (Wt%) is calculated by the percentage composition of plumbous each element of bismuth of copper iron that silver content is 99.999% (Wt%) in the part test piece surface silver layer again.
Embodiment 2:
Present embodiment is that the piece surface silver coating composition of high temperature alloy GH4169 is analyzed to material, mainly analyzes four constituent contents of the plumbous bismuth of copper iron in the silver coating, calculates the content of silver in the silver coating then.
The method step of present embodiment is following:
Step 1: the part test piece was immersed in the pure salpeter solution of top grade of 1,+10 8 minutes; Part test piece top layer dirt is cleared up; Then the part test piece is pulled out, behind distilled water flushing, with ether part test piece surface is cleaned again; After the cleaning part test piece dried and weigh, obtain weight M=35.31 gram;
Step 2: the part test piece that will pass through after step 1 is handled is immersed in the salpeter solution of 1+3; Treat after the dissolving of part test piece surface silver layer the part test piece to be taken out; With distilled water the part test piece is fully washed, and washing lotion is collected, after the flushing part test piece oven dry is weighed; Obtain weight m=20.22 gram, and then the silver layer weight that obtains dissolving is the M-m=G=15.09 gram;
Step 3: the washing lotion that step 2 is collected places on the electric furnace and heats, and when washing lotion is just seethed with excitement, stops heating, in washing lotion, adds the pure watery hydrochloric acid of capacity top grade, forms the AgCl post precipitation, once more to the washing lotion heating, makes the AgCl deposition stop heating after the cohesion fully;
Step 4: will pass through after washing lotion after step 3 is handled naturally cools to room temperature; Washing lotion is moved in first volumetric flask of 200mL; And with the container that holds washing lotion in the distilled water cleaning step 34 times, obtain new washing lotion and also move in first volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare the standard blank solution of sample solution, No. 1 calibration solutions and No. 2 calibration solutions respectively;
Said No. 1 calibration solutions process for preparation is: take by weighing the fine silver mark steel of 15.00 grams, with the salpeter solution of 1+2 fine silver is marked the steel dissolving, fine silver is marked the heating of steel lysate; When fine silver mark steel lysate has just seethed with excitement; Stop heating, in fine silver mark steel lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To the heating of fine silver mark steel lysate, make the AgCl deposition stop heating after the cohesion fully once more; After fine silver marked the steel lysate and naturally cool to room temperature; Fine silver is marked in second volumetric flask that the steel lysate moves to 200mL; And clean the container 4 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in second volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solutions;
Said No. 2 calibration solutions process for preparation are: the purity that takes by weighing 15.00 grams is greater than 99.99% high fine silver, with the salpeter solution of 1+2 high fine silver dissolved, and adding concentration is the ferrous solution 0.2mL of 1mg/mL in high fine silver lysate; Then, when high fine silver lysate has just seethed with excitement, stop heating with high fine silver lysate heating; In high fine silver lysate, add capacity watery hydrochloric acid; Form the AgCl post precipitation,, make the AgCl deposition stop heating after the cohesion fully once more to high fine silver lysate heating; After high fine silver lysate naturally cooled to room temperature; High fine silver lysate is moved in the 3rd volumetric flask of 200mL; And clean the container 4 times hold high fine silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solutions;
The process for preparation of the standard blank solution of sample solution is: get with step 2 in the identical 1+3 salpeter solution of salpeter solution volume; And stop heating after being heated to firm boiling; Again to wherein add with step 3 in the watery hydrochloric acid of watery hydrochloric acid equivalent; Gained solution moves in the 4th volumetric flask of 200mL after naturally cooling to room temperature, and cleans the container 4 times hold gained solution with distilled water, and the washing lotion that obtains also moves in the 4th volumetric flask; Be settled to shake up behind the scale mark and leave standstill, get in the 4th volumetric flask solution as the standard blank solution of sample solution;
Step 6: in the sample message file with the constant volume 200mL input inductance coupled plasma Atomic Emission Spectrometer AES of first volumetric flask in the dissolving silver layer weight in the step 2 15.09 gram and the step 4, with inductively coupled plasma atomic emission spectrometer start shooting stablize 1 hour after, instrument parameter be set be: radio-frequency power 1350W; Plasma gas flow rate 15L/min; Secondary air amount 0.2L/min, carrier gas flux 1L/min, observed altitude 15mm; Sample flow rate 1.5ml/min; 40 seconds time delay of reading, point 3 points, each element analysis spectrum line sees the following form:
| Analytical element | Fe | Bi | Cu | Pb |
| Wavelength (nm) | 238.204 | 223.061 | 224.700 | 217.000 |
Then adopt inductively coupled plasma atomic emission spectrometer standard blank solution, No. 1 calibration solutions, No. 2 calibration solutions and the sample solution of analytical sample solution successively; Obtain the spectral intensity of plumbous each element of bismuth of copper iron in standard blank solution, calibration solutions and the style solution respectively; And by the percentage composition of plumbous each element of bismuth of copper iron in the inductively coupled plasma atomic emission spectrometer output element test piece surface silver layer; The result is Fe 0.00006% (Wt%); Cu0.00005% (Wt%); Pb 0.00063% (Wt%), Bi 0.00015% (Wt%) is calculated by the percentage composition of plumbous each element of bismuth of copper iron that silver content is 99.999% (Wt%) in the part test piece surface silver layer again.
Embodiment 3:
Present embodiment is that the piece surface silver coating composition of high temperature alloy GH4169 is analyzed to material, mainly analyzes four constituent contents of the plumbous bismuth of copper iron in the silver coating, calculates the content of silver in the silver coating then.
The method step of present embodiment is following:
Step 1: the part test piece was immersed in the pure salpeter solution of top grade of 1,+12 10 minutes; Part test piece top layer dirt is cleared up; Then the part test piece is pulled out, behind distilled water flushing, with ether part test piece surface is cleaned again; After the cleaning part test piece dried and weigh, obtain weight M=28.69 gram;
Step 2: the part test piece that will pass through after step 1 is handled is immersed in the salpeter solution of 1+5; Treat after the dissolving of part test piece surface silver layer the part test piece to be taken out; With distilled water the part test piece is fully washed, and washing lotion is collected, after the flushing part test piece oven dry is weighed; Obtain weight m=17.10 gram, and then the silver layer weight that obtains dissolving is the M-m=G=11.59 gram;
Step 3: the washing lotion that step 2 is collected places on the electric furnace and heats, and when washing lotion is just seethed with excitement, stops heating, in washing lotion, adds the pure watery hydrochloric acid of capacity top grade, forms the AgCl post precipitation, once more to the washing lotion heating, makes the AgCl deposition stop heating after the cohesion fully;
Step 4: will pass through after washing lotion after step 3 is handled naturally cools to room temperature; Washing lotion is moved in first volumetric flask of 200mL; And with the container that holds washing lotion in the distilled water cleaning step 35 times, obtain new washing lotion and also move in first volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare the standard blank solution of sample solution, No. 1 calibration solutions and No. 2 calibration solutions respectively;
Said No. 1 calibration solutions process for preparation is: take by weighing the fine silver mark steel of 12.00 grams, with the salpeter solution of 1+3 fine silver is marked the steel dissolving, fine silver is marked the heating of steel lysate; When fine silver mark steel lysate has just seethed with excitement; Stop heating, in fine silver mark steel lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To the heating of fine silver mark steel lysate, make the AgCl deposition stop heating after the cohesion fully once more; After fine silver marked the steel lysate and naturally cool to room temperature; Fine silver is marked in second volumetric flask that the steel lysate moves to 200mL; And clean the container 5 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in second volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solutions;
Said No. 2 calibration solutions process for preparation are: the purity that takes by weighing 12.00 grams is greater than 99.99% high fine silver, with the salpeter solution of 1+3 high fine silver dissolved, and adding concentration is the ferrous solution 0.4mL of 1mg/mL in high fine silver lysate; Then, when high fine silver lysate has just seethed with excitement, stop heating with high fine silver lysate heating; In high fine silver lysate, add capacity watery hydrochloric acid; Form the AgCl post precipitation,, make the AgCl deposition stop heating after the cohesion fully once more to high fine silver lysate heating; After high fine silver lysate naturally cooled to room temperature; High fine silver lysate is moved in the 3rd volumetric flask of 200mL; And clean the container 5 times hold high fine silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solutions;
The process for preparation of the standard blank solution of sample solution is: get with step 2 in the identical 1+5 salpeter solution of salpeter solution volume; And stop heating after being heated to firm boiling; Again to wherein add with step 3 in the watery hydrochloric acid of watery hydrochloric acid equivalent; Gained solution moves in the 4th volumetric flask of 200mL after naturally cooling to room temperature, and cleans the container 5 times hold gained solution with distilled water, and the washing lotion that obtains also moves in the 4th volumetric flask; Be settled to shake up behind the scale mark and leave standstill, get in the 4th volumetric flask solution as the standard blank solution of sample solution;
Step 6: in the sample message file with the constant volume 200mL input inductance coupled plasma Atomic Emission Spectrometer AES of first volumetric flask in the dissolving silver layer weight in the step 2 11.59 gram and the step 4, with inductively coupled plasma atomic emission spectrometer start shooting stablize 1 hour after, instrument parameter be set be: radio-frequency power 1350W; Plasma gas flow rate 15L/min; Secondary air amount 0.2L/min, carrier gas flux 1L/min, observed altitude 15mm; Sample flow rate 1.5ml/min; 40 seconds time delay of reading, point 3 points, each element analysis spectrum line sees the following form:
| Analytical element | Fe | Bi | Cu | Pb |
| Wavelength (nm) | 238.204 | 223.061 | 224.700 | 217.000 |
Then adopt inductively coupled plasma atomic emission spectrometer standard blank solution, No. 1 calibration solutions, No. 2 calibration solutions and the sample solution of analytical sample solution successively; Obtain the spectral intensity of plumbous each element of bismuth of copper iron in standard blank solution, calibration solutions and the style solution respectively; And by the percentage composition of plumbous each element of bismuth of copper iron in the inductively coupled plasma atomic emission spectrometer output element test piece surface silver layer; The result is Fe 0.00007% (Wt%); Cu0.00009% (Wt%); Pb 0.00044% (Wt%), Bi 0.00021% (Wt%) is calculated by the percentage composition of plumbous each element of bismuth of copper iron that silver content is 99.999% (Wt%) in the part test piece surface silver layer again.
Claims (1)
1. method of analyzing high temperature alloy GH4169 piece surface silver coating composition is characterized in that: may further comprise the steps:
Step 1: the part test piece was immersed in the salpeter solution of 1+9 to 1,+12 5 to 10 minutes; Part test piece top layer dirt is cleared up; Then the part test piece is pulled out, behind distilled water flushing, with ether part test piece surface is cleaned again; After the cleaning part test piece dried and weigh, obtain weight M gram;
Step 2: the part test piece that will pass through after step 1 is handled is immersed in the salpeter solution of 1+2 to 1+5; Treat after the dissolving of part test piece surface silver layer the part test piece to be taken out; With distilled water the part test piece is fully washed, and washing lotion is collected, after the flushing part test piece oven dry is weighed; Obtain weight m gram, and then the silver layer weight that obtains dissolving is the M-m=G gram;
Step 3: the washing lotion heating with step 2 is collected, when washing lotion is just seethed with excitement, stop heating, in washing lotion, add capacity watery hydrochloric acid, form the AgCl post precipitation, once more to the washing lotion heating, make the AgCl deposition stop heating after the cohesion fully;
Step 4: will pass through after washing lotion after step 3 is handled naturally cools to room temperature; Washing lotion is moved in first volumetric flask; And with the container that holds washing lotion in the distilled water cleaning step 33 to 5 times, obtain new washing lotion and also move in first volumetric flask, be settled to shake up behind the scale mark and leave standstill; Make the AgCl deposition be deposited on first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare the standard blank solution of sample solution, No. 1 calibration solutions and No. 2 calibration solutions respectively;
Said No. 1 calibration solutions process for preparation is: take by weighing the fine silver mark steel of weight between 95%G to 1.05%G, with the salpeter solution of 1+1 to 1+3 fine silver is marked the steel dissolving, fine silver is marked the heating of steel lysate; When fine silver mark steel lysate has just seethed with excitement; Stop heating, in fine silver mark steel lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To the heating of fine silver mark steel lysate, make the AgCl deposition stop heating after the cohesion fully once more; After fine silver marked the steel lysate and naturally cool to room temperature; Fine silver is marked the steel lysate to be moved in second volumetric flask; And clean the container 3 to 5 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in second volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solutions; The second volumetric flask volume is identical with the first volumetric flask volume;
Said No. 2 calibration solutions process for preparation are: take by weighing the purity of weight between 95%G to 1.05%G greater than 99.99% high fine silver; Salpeter solution with 1+1 to 1+3 dissolves high fine silver, and in high fine silver lysate, adding concentration is the ferrous solution 0.2mL to 0.4mL of 1mg/mL, then with high fine silver lysate heating; When high fine silver lysate has just seethed with excitement; Stop heating, in high fine silver lysate, add capacity watery hydrochloric acid, form the AgCl post precipitation; To high fine silver lysate heating, make the AgCl deposition stop heating after the cohesion fully once more; After high fine silver lysate naturally cooled to room temperature; High fine silver lysate is moved in the 3rd volumetric flask; And clean the container 3 to 5 times hold high fine silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, is settled to shake up behind the scale mark to leave standstill; Make the AgCl deposition be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solutions; The 3rd volumetric flask volume is identical with the first volumetric flask volume;
Step 6: in the sample message file with the constant volume input inductance coupled plasma Atomic Emission Spectrometer AES of first volumetric flask in dissolving silver layer weight G in the step 2 and the step 4; With inductively coupled plasma atomic emission spectrometer start after stable at least 1 hour; The standard blank solution of analytical sample solution, No. 1 calibration solutions, No. 2 calibration solutions and sample solution successively; Then by the percentage composition of plumbous each element of bismuth of copper iron in the inductively coupled plasma atomic emission spectrometer output element test piece surface silver layer, the percentage composition by plumbous each element of bismuth of copper iron calculates silver content in the part test piece surface silver layer again.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278488A (en) * | 2013-05-24 | 2013-09-04 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for quickly semi-quantifying GH4169 alloy trace elements |
| CN104155267A (en) * | 2014-07-27 | 2014-11-19 | 中国人民解放军第五七一九工厂 | Method for chemically analyzing content of boron nitride in nickel-based powder material |
| CN104237209A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Method for synchronously detecting copper, bismuth, iron, lead, tellurium, selenium, antimony and palladium in electrolytic silver through ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105067590A (en) * | 2015-07-16 | 2015-11-18 | 西安航空动力股份有限公司 | Method for measuring content of lead and bismuth elements in depollution solution |
| CN107525700A (en) * | 2017-07-24 | 2017-12-29 | 浙江大学 | The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050170518A1 (en) * | 2003-12-12 | 2005-08-04 | L'oreal | Method for the preparation of a sample for analysis, sample prepared, and method of analysis, and sample analyzed |
| US20070292991A1 (en) * | 2006-06-20 | 2007-12-20 | Lisa Edith Helberg | Method for quantification of analytes in a titanium, tin or silcon tetrachloride sample |
| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| CN101315316A (en) * | 2008-07-01 | 2008-12-03 | 攀钢集团研究院有限公司 | Digestion method and detection method of titanium-rich material |
| CN101609047A (en) * | 2009-06-24 | 2009-12-23 | 谱尼测试科技（北京）有限公司 | The assay method of antimony in a kind of electric equipment products |
-
2011
- 2011-11-10 CN CN 201110356085 patent/CN102393387B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050170518A1 (en) * | 2003-12-12 | 2005-08-04 | L'oreal | Method for the preparation of a sample for analysis, sample prepared, and method of analysis, and sample analyzed |
| US20070292991A1 (en) * | 2006-06-20 | 2007-12-20 | Lisa Edith Helberg | Method for quantification of analytes in a titanium, tin or silcon tetrachloride sample |
| CN101315316A (en) * | 2008-07-01 | 2008-12-03 | 攀钢集团研究院有限公司 | Digestion method and detection method of titanium-rich material |
| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| CN101609047A (en) * | 2009-06-24 | 2009-12-23 | 谱尼测试科技（北京）有限公司 | The assay method of antimony in a kind of electric equipment products |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278488A (en) * | 2013-05-24 | 2013-09-04 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for quickly semi-quantifying GH4169 alloy trace elements |
| CN104155267A (en) * | 2014-07-27 | 2014-11-19 | 中国人民解放军第五七一九工厂 | Method for chemically analyzing content of boron nitride in nickel-based powder material |
| CN104237209A (en) * | 2014-10-16 | 2014-12-24 | 云南驰宏锌锗股份有限公司 | Method for synchronously detecting copper, bismuth, iron, lead, tellurium, selenium, antimony and palladium in electrolytic silver through ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105067590A (en) * | 2015-07-16 | 2015-11-18 | 西安航空动力股份有限公司 | Method for measuring content of lead and bismuth elements in depollution solution |
| CN107525700A (en) * | 2017-07-24 | 2017-12-29 | 浙江大学 | The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact |
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