CN102393387B - 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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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 surface silver coating components of high-temperature alloy GH 4169 part.
Background technology
Silver is as a kind of stable chemical nature, 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, prevent adhesion 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 have other materials to sneak into silver coating in silver-plated process, thereby the control silver coating can farthest be brought into play above-mentioned effect.
Existing silver coating analytical approach has atomic absorption method, spectrophotometric method, when these methods are the chemical constitution of piece surface silver coating of high temperature alloy GH4169 at analysis of material, need to 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
The problem that exists for solving prior art, the present invention proposes a kind of method of analyzing surface silver coating components of high-temperature alloy GH 4169 part.
Technical scheme
Technical scheme of the present invention is:
Described a kind of method of analyzing surface silver coating components of high-temperature alloy GH 4169 part 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 after will processing through step 1 is immersed in the salpeter solution of 1+2 to 1+5, after the dissolving of part test piece surface silver layer, the part test piece is taken out, with distilled water the part test piece is fully washed, and washing lotion 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: with the washing lotion heating that step 2 is collected, when washing lotion was just seethed with excitement, stopped heating added capacity watery hydrochloric acid in washing lotion, after the formation AgCl precipitation, again to the washing lotion heating, made the fully rear stopped heating of cohesion of AgCl precipitation;
Step 4: after the washing lotion after will processing through step 3 naturally cools to room temperature, washing lotion is moved in the first volumetric flask, and with the container that holds washing lotion in the distilled water cleaning step 33 to 5 times, obtaining new washing lotion also moves in the first volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare respectively the standard blank solution of sample solution, No. 1 calibration solution and No. 2 calibration solution;
Described No. 1 calibration solution preparation process is: take by weighing the fine silver mark steel of weight between 95%G to 1.05%G, salpeter solution with 1+1 to 1+3 dissolves fine silver mark steel, fine silver mark steel lysate is heated, when fine silver mark steel lysate has just seethed with excitement, stopped heating adds capacity watery hydrochloric acid in fine silver mark steel lysate, after the formation AgCl precipitation, again to the heating of fine silver mark steel lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After fine silver mark steel lysate naturally cooled to room temperature, fine silver mark steel lysate is moved in the second volumetric flask, and clean the container 3 to 5 times hold fine silver mark steel lysate with distilled water, obtaining washing lotion also moves in the second volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solution; The second volumetric flask volume is identical with the first volumetric flask volume;
Described No. 2 calibration solution preparation processes are: take by weighing the purity of weight between 95%G to 1.05%G greater than 99.99% high purity silver, salpeter solution with 1+1 to 1+3 dissolves high purity silver, adding concentration in the high purity silver lysate is the ferrous solution 0.2mL to 0.4mL of 1mg/mL, then the high purity silver lysate is heated, when the high purity silver lysate has just seethed with excitement, stopped heating, in the high purity silver lysate, add capacity watery hydrochloric acid, after forming the AgCl precipitation, again to the heating of high purity silver lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After the high purity silver lysate naturally cooled to room temperature, the high purity silver lysate is moved in the 3rd volumetric flask, and clean the container 3 to 5 times hold the high purity silver lysate with distilled water, obtaining washing lotion also moves in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solution; The 3rd volumetric flask volume is identical with the first volumetric flask volume;
Step 6: the constant volume of the first volumetric flask in the dissolving silver layer weight G in the step 2 and the step 4 is inputted in the sample message file of inductively coupled plasma atomic emission spectrometer, with inductively coupled plasma atomic emission spectrometer start after stable at least 1 hour, the standard blank solution of analytical sample solution successively, No. 1 calibration solution, calibrate solution and sample solution No. 2, 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 simultaneously to each element, and once early stage the sample preparation process also the processing procedure in early stage in than existing methods is more easy, having overcome needs in the existing method each element in the silver coating is measured respectively, 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, and then four constituent contents of the plumbous bismuth of copper iron in the Main Analysis silver coating calculate the content of silver in the silver coating.
The method step of present embodiment is as follows:
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 after will processing through step 1 is immersed in the salpeter solution of 1+2, after the dissolving of part test piece surface silver layer, the part test piece is taken out, with distilled water the part test piece is fully washed, and washing lotion 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 was just seethed with excitement, stopped heating added the pure watery hydrochloric acid of capacity top grade in washing lotion, form the AgCl precipitation after, again to the washing lotion heating, make fully stopped heating after the cohesion of AgCl precipitation;
Step 4: after the washing lotion after will processing through step 3 naturally cools to room temperature, washing lotion is moved in the first volumetric flask of 200mL, and with the container that holds washing lotion in the distilled water cleaning step 33 times, obtaining new washing lotion also moves in the first volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare respectively the standard blank solution of sample solution, No. 1 calibration solution and No. 2 calibration solution;
Described No. 1 calibration solution preparation process is: the fine silver mark steel that takes by weighing 18.00 grams, salpeter solution with 1+1 dissolves fine silver mark steel, fine silver mark steel lysate is heated, when fine silver mark steel lysate has just seethed with excitement, stopped heating adds capacity watery hydrochloric acid in fine silver mark steel lysate, after the formation AgCl precipitation, again to the heating of fine silver mark steel lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After fine silver mark steel lysate naturally cooled to room temperature, fine silver mark steel lysate is moved in the second volumetric flask of 200mL, and clean the container 3 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in the second volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solution;
Described No. 2 calibration solution preparation processes are: the purity that take by weighing 18.00 grams are greater than 99.99% high purity silver, salpeter solution with 1+1 dissolves high purity silver, adding concentration in the high purity silver lysate is the ferrous solution 0.3mL of 1mg/mL, then the high purity silver lysate is heated, when the high purity silver lysate has just seethed with excitement, stopped heating, in the high purity silver lysate, add capacity watery hydrochloric acid, after the formation AgCl precipitation, again to the heating of high purity silver lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After the high purity silver lysate naturally cooled to room temperature, the high purity silver lysate is moved in the 3rd volumetric flask of 200mL, and clean the container 3 times hold the high purity silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solution;
The process for preparation of the standard blank solution of sample solution is: get the 1+2 salpeter solution identical with salpeter solution volume in the step 2, and be heated to stopped heating after the 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 clean the container 3 times hold gained solution with distilled water, 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 inductively coupled plasma atomic emission spectrometer of the first volumetric flask in dissolving silver layer weight 17.87 grams in the step 2 and the step 4, after inductively coupled plasma atomic emission spectrometer start stablized 1 hour, instrument parameter is set is: radio-frequency power 1350W, plasma gas flow rate 15L/min, assisted gas flow 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 the successively standard blank solution of analytical sample solution of inductively coupled plasma atomic emission spectrometer, No. 1 calibration solution, calibrate solution and sample solution No. 2, obtain respectively the standard blank solution, the spectral intensity of plumbous each element of bismuth of copper iron in calibration solution and the style solution, 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, and then four constituent contents of the plumbous bismuth of copper iron in the Main Analysis silver coating calculate the content of silver in the silver coating.
The method step of present embodiment is as follows:
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 after will processing through step 1 is immersed in the salpeter solution of 1+3, after the dissolving of part test piece surface silver layer, the part test piece is taken out, with distilled water the part test piece is fully washed, and washing lotion 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 was just seethed with excitement, stopped heating added the pure watery hydrochloric acid of capacity top grade in washing lotion, form the AgCl precipitation after, again to the washing lotion heating, make fully stopped heating after the cohesion of AgCl precipitation;
Step 4: after the washing lotion after will processing through step 3 naturally cools to room temperature, washing lotion is moved in the first volumetric flask of 200mL, and with the container that holds washing lotion in the distilled water cleaning step 34 times, obtaining new washing lotion also moves in the first volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare respectively the standard blank solution of sample solution, No. 1 calibration solution and No. 2 calibration solution;
Described No. 1 calibration solution preparation process is: the fine silver mark steel that takes by weighing 15.00 grams, salpeter solution with 1+2 dissolves fine silver mark steel, fine silver mark steel lysate is heated, when fine silver mark steel lysate has just seethed with excitement, stopped heating adds capacity watery hydrochloric acid in fine silver mark steel lysate, after the formation AgCl precipitation, again to the heating of fine silver mark steel lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After fine silver mark steel lysate naturally cooled to room temperature, fine silver mark steel lysate is moved in the second volumetric flask of 200mL, and clean the container 4 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in the second volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solution;
Described No. 2 calibration solution preparation processes are: the purity that take by weighing 15.00 grams are greater than 99.99% high purity silver, salpeter solution with 1+2 dissolves high purity silver, adding concentration in the high purity silver lysate is the ferrous solution 0.2mL of 1mg/mL, then the high purity silver lysate is heated, when the high purity silver lysate has just seethed with excitement, stopped heating, in the high purity silver lysate, add capacity watery hydrochloric acid, after the formation AgCl precipitation, again to the heating of high purity silver lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After the high purity silver lysate naturally cooled to room temperature, the high purity silver lysate is moved in the 3rd volumetric flask of 200mL, and clean the container 4 times hold the high purity silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solution;
The process for preparation of the standard blank solution of sample solution is: get the 1+3 salpeter solution identical with salpeter solution volume in the step 2, and be heated to stopped heating after the 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 clean the container 4 times hold gained solution with distilled water, 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 inductively coupled plasma atomic emission spectrometer of the first volumetric flask in dissolving silver layer weight 15.09 grams in the step 2 and the step 4, after inductively coupled plasma atomic emission spectrometer start stablized 1 hour, instrument parameter is set is: radio-frequency power 1350W, plasma gas flow rate 15L/min, assisted gas flow 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 the successively standard blank solution of analytical sample solution of inductively coupled plasma atomic emission spectrometer, No. 1 calibration solution, calibrate solution and sample solution No. 2, obtain respectively the standard blank solution, the spectral intensity of plumbous each element of bismuth of copper iron in calibration solution and the style solution, 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, and then four constituent contents of the plumbous bismuth of copper iron in the Main Analysis silver coating calculate the content of silver in the silver coating.
The method step of present embodiment is as follows:
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 after will processing through step 1 is immersed in the salpeter solution of 1+5, after the dissolving of part test piece surface silver layer, the part test piece is taken out, with distilled water the part test piece is fully washed, and washing lotion 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 was just seethed with excitement, stopped heating added the pure watery hydrochloric acid of capacity top grade in washing lotion, form the AgCl precipitation after, again to the washing lotion heating, make fully stopped heating after the cohesion of AgCl precipitation;
Step 4: after the washing lotion after will processing through step 3 naturally cools to room temperature, washing lotion is moved in the first volumetric flask of 200mL, and with the container that holds washing lotion in the distilled water cleaning step 35 times, obtaining new washing lotion also moves in the first volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare respectively the standard blank solution of sample solution, No. 1 calibration solution and No. 2 calibration solution;
Described No. 1 calibration solution preparation process is: the fine silver mark steel that takes by weighing 12.00 grams, salpeter solution with 1+3 dissolves fine silver mark steel, fine silver mark steel lysate is heated, when fine silver mark steel lysate has just seethed with excitement, stopped heating adds capacity watery hydrochloric acid in fine silver mark steel lysate, after the formation AgCl precipitation, again to the heating of fine silver mark steel lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After fine silver mark steel lysate naturally cooled to room temperature, fine silver mark steel lysate is moved in the second volumetric flask of 200mL, and clean the container 5 times hold fine silver mark steel lysate with distilled water, the washing lotion that obtains also moves in the second volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solution;
Described No. 2 calibration solution preparation processes are: the purity that take by weighing 12.00 grams are greater than 99.99% high purity silver, salpeter solution with 1+3 dissolves high purity silver, adding concentration in the high purity silver lysate is the ferrous solution 0.4mL of 1mg/mL, then the high purity silver lysate is heated, when the high purity silver lysate has just seethed with excitement, stopped heating, in the high purity silver lysate, add capacity watery hydrochloric acid, after the formation AgCl precipitation, again to the heating of high purity silver lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After the high purity silver lysate naturally cooled to room temperature, the high purity silver lysate is moved in the 3rd volumetric flask of 200mL, and clean the container 5 times hold the high purity silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solution;
The process for preparation of the standard blank solution of sample solution is: get the 1+5 salpeter solution identical with salpeter solution volume in the step 2, and be heated to stopped heating after the 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 clean the container 5 times hold gained solution with distilled water, 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 inductively coupled plasma atomic emission spectrometer of the first volumetric flask in dissolving silver layer weight 11.59 grams in the step 2 and the step 4, after inductively coupled plasma atomic emission spectrometer start stablized 1 hour, instrument parameter is set is: radio-frequency power 1350W, plasma gas flow rate 15L/min, assisted gas flow 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 the successively standard blank solution of analytical sample solution of inductively coupled plasma atomic emission spectrometer, No. 1 calibration solution, calibrate solution and sample solution No. 2, obtain respectively the standard blank solution, the spectral intensity of plumbous each element of bismuth of copper iron in calibration solution and the style solution, 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 surface silver coating components of high-temperature alloy GH 4169 part 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 after will processing through step 1 is immersed in the salpeter solution of 1+2 to 1+5, after the dissolving of part test piece surface silver layer, the part test piece is taken out, with distilled water the part test piece is fully washed, and washing lotion 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: with the washing lotion heating that step 2 is collected, when washing lotion was just seethed with excitement, stopped heating added capacity watery hydrochloric acid in washing lotion, after the formation AgCl precipitation, again to the washing lotion heating, made the fully rear stopped heating of cohesion of AgCl precipitation;
Step 4: after the washing lotion after will processing through step 3 naturally cools to room temperature, washing lotion is moved in the first volumetric flask, and with the container that holds washing lotion in the distilled water cleaning step 33 to 5 times, obtaining new washing lotion also moves in the first volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the first volumetric flask bottom fully, get the first volumetric flask upper clear supernate as sample solution;
Step 5: prepare respectively the standard blank solution of sample solution, No. 1 calibration solution and No. 2 calibration solution;
Described No. 1 calibration solution preparation process is: take by weighing the fine silver mark steel of weight between 95%G to 1.05%G, salpeter solution with 1+1 to 1+3 dissolves fine silver mark steel, fine silver mark steel lysate is heated, when fine silver mark steel lysate has just seethed with excitement, stopped heating adds capacity watery hydrochloric acid in fine silver mark steel lysate, after the formation AgCl precipitation, again to the heating of fine silver mark steel lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After fine silver mark steel lysate naturally cooled to room temperature, fine silver mark steel lysate is moved in the 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 the second volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the second volumetric flask bottom fully, get the second volumetric flask upper clear supernate as No. 1 calibration solution; The second volumetric flask volume is identical with the first volumetric flask volume;
Described No. 2 calibration solution preparation processes are: take by weighing the purity of weight between 95%G to 1.05%G greater than 99.99% high purity silver, salpeter solution with 1+1 to 1+3 dissolves high purity silver, adding concentration in the high purity silver lysate is the ferrous solution 0.2mL to 0.4mL of 1mg/mL, then the high purity silver lysate is heated, when the high purity silver lysate has just seethed with excitement, stopped heating, in the high purity silver lysate, add capacity watery hydrochloric acid, after forming the AgCl precipitation, again to the heating of high purity silver lysate, make the fully rear stopped heating of cohesion of AgCl precipitation; After the high purity silver lysate naturally cooled to room temperature, the high purity silver lysate is moved in the 3rd volumetric flask, and clean the container 3 to 5 times hold the high purity silver lysate with distilled water, the washing lotion that obtains also moves in the 3rd volumetric flask, be settled to shake up behind the scale mark and leave standstill, make the AgCl precipitation be deposited on the 3rd volumetric flask bottom fully, get the 3rd volumetric flask upper clear supernate as No. 2 calibration solution; The 3rd volumetric flask volume is identical with the first volumetric flask volume;
The process for preparation of the standard blank solution of described sample solution is: get with step 2 in the salpeter solution volume is identical, concentration is identical salpeter solution, and be heated to stopped heating after the 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 clean the container 3～5 times hold gained solution with distilled water, 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: the constant volume of the first volumetric flask in the dissolving silver layer weight G in the step 2 and the step 4 is inputted in the sample message file of inductively coupled plasma atomic emission spectrometer, with inductively coupled plasma atomic emission spectrometer start after stable at least 1 hour, the standard blank solution of analytical sample solution successively, No. 1 calibration solution, calibrate solution and sample solution No. 2, 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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| 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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| 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 |
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| 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 |
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