CN117589725A - Method for identifying complete dissolution of metal sample - Google Patents
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- CN117589725A CN117589725A CN202311573303.8A CN202311573303A CN117589725A CN 117589725 A CN117589725 A CN 117589725A CN 202311573303 A CN202311573303 A CN 202311573303A CN 117589725 A CN117589725 A CN 117589725A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 109
- 239000002184 metal Substances 0.000 title claims abstract description 109
- 238000004090 dissolution Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000002834 transmittance Methods 0.000 claims abstract description 92
- 230000003068 static effect Effects 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 10
- 229910001309 Ferromolybdenum Inorganic materials 0.000 claims description 7
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 85
- 238000010438 heat treatment Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 238000005070 sampling Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910001339 C alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004836 empirical method Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0205—Investigating particle size or size distribution by optical means, e.g. by light scattering, diffraction, holography or imaging
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for identifying complete dissolution of a metal sample, and belongs to the technical field of detection. The method for identifying the complete dissolution of the metal sample comprises the following steps: A. placing the solution of the metal sample to be tested into a transparent container, horizontally passing the solution in a static state by using a parallel light source, and automatically adjusting the wavelength of the light source within the range of 200nm-2500nm to ensure that the horizontal light transmittance reaches the maximum value, wherein the wavelength is denoted as lambda max The method comprises the steps of carrying out a first treatment on the surface of the B. The solution is circulated, and lambda is used after the solution is static max Measuring the horizontal light transmittance TH and the vertical light transmittance TV; C. and identifying the dissolution state of the metal sample. The invention can rapidly and accurately identify whether the metal sample is completely dissolved by the acid liquor, reduces human error and improves the accuracy of the measurement result. The invention can simultaneously distinguish whether the impurity exists in the solution, and reduce the experimental instrumentIs a safety hazard.
Description
Technical Field
The invention relates to a method for identifying complete dissolution of a metal sample, and belongs to the technical field of detection.
Background
In the field of chemical analysis, the content of trace elements in a metal sample can be obtained by utilizing instruments such as inductively coupled plasma atomic emission spectroscopy (ICP-OES), inductively coupled plasma mass spectrometer (ICP-MS) and the like, so that the content of trace elements in the metal sample can be accurately detected, and a higher requirement is provided for pretreatment of the sample, and the metal sample is required to be completely dissolved by acid liquor and has no impurities. The existing method for identifying whether the metal sample is completely dissolved by the acid liquor is an empirical method, and experimenters roughly and qualitatively judge whether solid particles exist in a transparent reactor (such as a flat-bottom flask and the like) or not and the form of bubbles generated in the solution by visual observation, so that the method has great human errors and experimental hidden dangers. On the one hand, the insufficient complete dissolution of the metal sample will lead to lower test results; on the other hand, the solid particles of the metal sample which are not fully dissolved have serious influence on experimental equipment (such as blockage of an instrument sampling system and the like). Based on the above problems, a method for identifying complete dissolution of a metal sample has been proposed.
Disclosure of Invention
The invention aims to provide a method for identifying complete dissolution of a metal sample.
To achieve the object of the present invention, the method for identifying complete dissolution of a metal sample comprises:
A. placing the solution of the metal sample to be tested into a transparent container, horizontally passing the solution in a static state by using a parallel light source, and automatically adjusting the wavelength of the light source within the range of 200nm-2500nm to ensure that the horizontal light transmittance reaches the maximum value, wherein the wavelength is denoted as lambda max ；
B. The solution is circulated, and lambda is used after the solution is static max Measuring the horizontal light transmittance TH and the vertical light transmittance TV;
C. identifying the dissolved state of a metal sample
(1) The granularity of the metal sample before dissolution is less than or equal to 0.1mm:
if the average value of TV is within the TH confidence interval mu-sigma to mu+sigma, the metal sample can be determined to be completely dissolved; if the TV average value is outside a TH confidence interval mu-sigma to mu+sigma, determining that the metal sample is not completely dissolved, wherein mu is the average value, sigma is the standard deviation, and the confidence level is 0.683;
(2) particle size of the metal sample before dissolution is more than 0.1mm: TC=TV-TH, the distribution frequency peak height of TC is within the confidence interval 0-sigma, and the complete dissolution of the metal sample can be determined; the distribution frequency peak height of TC is outside the confidence interval 0-sigma, the metal sample can be determined to be incompletely dissolved, wherein the average value is zero, sigma is the standard deviation, and the confidence level is 0.683;
the TH confidence interval mu-sigma to mu+sigma, and the mu value and the sigma value are determined by carrying out normal distribution fitting on TH;
TC confidence interval 0-sigma, through carrying on normal distribution fitting to TH confirm sigma value.
In one embodiment, the method of preparing the solution of step a comprises dissolving a metal sample to be tested in an acid.
In one embodiment, the metal sample to be tested is dissolved in an acid and heated to dissolve.
Heating can accelerate the dissolution of the metal.
The method of the present invention is applicable to all metal samples, and in one embodiment, the metal is at least one of medium and low alloy, high temperature alloy, titanium alloy and ferromolybdenum.
In one specific embodiment, the intensity of the light source in the step A is fixed, and the intensity of the light source ranges from 2500lm to 3000lm.
In one specific embodiment, the step B is repeated, and the number of the measuring points of TH and TV is respectively more than or equal to 1000. I.e. the number of data points contained on the spot during a single measurement.
In one embodiment, the method further comprises step D:
c, determining that the metal sample is not completely dissolved, continuing to dissolve the metal sample, and repeating the steps B and C to determine whether the metal sample is completely dissolved; if the steps B and C are repeated for more than 5 times, judging that the metal sample is still not completely dissolved according to the step C, and determining that impurities exist in the solution.
For the sample for which it is determined in step C that the metal sample is not completely dissolved, the dissolution is continued, and the dissolution may be a conventional dissolution method of the metal sample, such as dissolution by adding an acid, and acceleration of dissolution by heating.
In one embodiment, the method further comprises step E: and D, if the impurities exist in the solution, filtering, and repeating the steps B and C until the step C is used for determining that the average value of the TV is within a confidence interval mu-sigma to mu+sigma of TH or the distribution frequency peak height of TC is within a confidence interval 0-sigma.
The beneficial effects are that:
the invention adopts a mode of comparing the horizontal light transmittance and the vertical light transmittance to identify whether the metal sample is completely dissolved, replaces the conventional visual identification method, and has the following advantages:
1. the invention can rapidly and accurately identify whether the metal sample is completely dissolved by the acid liquor, reduces human error and improves the accuracy of the measurement result.
2. The invention can simultaneously distinguish whether impurities exist in the solution, and reduce the potential safety hazard of experimental instruments.
Drawings
FIG. 1 is a flow chart of a method for identifying complete dissolution of a metal sample according to the present invention;
FIG. 2 is a schematic diagram of powder sample discrimination;
FIG. 3 is a schematic diagram of the discrimination of a pellet sample.
FIGS. 4-8 show the results of sampling measurements at different dissolution times for examples 1-5, respectively.
Detailed Description
To achieve the object of the present invention, the method for identifying complete dissolution of a metal sample comprises:
A. placing the solution of the metal sample to be tested into a transparent container, horizontally passing the solution in a static state by using a parallel light source, and automatically adjusting the wavelength of the light source within the range of 200nm-2500nm to ensure that the horizontal light transmittance reaches the maximum value, wherein the wavelength is denoted as lambda max ；
B. The solution is circulated, and lambda is used after the solution is static max Measuring the horizontal light transmittance TH and the vertical light transmittance TV;
C. identifying the dissolved state of a metal sample
(1) The granularity of the metal sample before dissolution is less than or equal to 0.1mm:
if the average value of TV is within the TH confidence interval mu-sigma to mu+sigma, the metal sample can be determined to be completely dissolved; if the TV average value is outside a TH confidence interval mu-sigma to mu+sigma, determining that the metal sample is not completely dissolved, wherein mu is the average value, sigma is the standard deviation, and the confidence level is 0.683;
(2) particle size of the metal sample before dissolution is more than 0.1mm: TC=TV-TH, the distribution frequency peak height of TC is within the confidence interval 0-sigma, and the complete dissolution of the metal sample can be determined; the distribution frequency peak height of TC is outside the confidence interval 0-sigma, the metal sample can be determined to be incompletely dissolved, wherein the average value is zero, sigma is the standard deviation, and the confidence level is 0.683;
the TH confidence interval mu-sigma to mu+sigma, and the mu value and the sigma value are determined by carrying out normal distribution fitting on TH;
TC confidence interval 0-sigma, through carrying on normal distribution fitting to TH confirm sigma value.
In one embodiment, the method of preparing the solution of step a comprises dissolving a metal sample to be tested in an acid.
In one embodiment, the metal sample to be tested is dissolved in an acid and heated to dissolve.
Heating can accelerate the dissolution of the metal.
The method of the present invention is applicable to all metal samples, and in one embodiment, the metal is at least one of medium and low alloy, high temperature alloy, titanium alloy and ferromolybdenum.
In one specific embodiment, the intensity of the light source in the step A is fixed, and the intensity of the light source ranges from 2500lm to 3000lm.
In one specific embodiment, the step B is repeated, and the number of the measuring points of TH and TV is respectively more than or equal to 1000. I.e. the number of data points contained on the spot during a single measurement.
In one embodiment, the method further comprises step D:
c, determining that the metal sample is not completely dissolved, continuing to dissolve the metal sample, and repeating the steps B and C to determine whether the metal sample is completely dissolved; if the steps B and C are repeated for more than 5 times, judging that the metal sample is still not completely dissolved according to the step C, and determining that impurities exist in the solution.
For the sample for which it is determined in step C that the metal sample is not completely dissolved, the dissolution is continued, and the dissolution may be a conventional dissolution method of the metal sample, such as dissolution by adding an acid, and acceleration of dissolution by heating.
In one embodiment, the method further comprises step E: and D, if the impurities exist in the solution, filtering, and repeating the steps B and C until the step C is used for determining that the average value of the TV is within a confidence interval mu-sigma to mu+sigma of TH or the distribution frequency peak height of TC is within a confidence interval 0-sigma.
In one embodiment, the method is:
1. dissolution of metal sample
By using an analytical balance, accurately weighing a certain mass (for example, 0.2000 g+/-0.0005 g) of a metal sample, placing the metal sample into a transparent reactor (for example, a flat-bottom flask), adding a certain volume of acid liquor with known concentration (for example, 20mL of 1.19g/mL hydrochloric acid, 2mL of 1.42g/mL nitric acid and the like), placing the metal sample on a heating table for heating, and determining the heating temperature (for example, high-temperature alloy 100 ℃ and titanium alloy 150 ℃ and the like) according to the material quality of the metal sample so as to accelerate the dissolution of the metal sample.
2. Light source parameter adjustment
A beam of parallel light source with fixed intensity horizontally passes through the solution in a static state, the wavelength of the light source is automatically adjusted according to the horizontal light Transmittance (TH), and the wavelength is adjusted from 200nm to 2500nm, so that the horizontal light Transmittance (TH) reaches the maximum value.
3. Determination of transmittance of circulating solution
And (3) circulating the solution in the reactor, and repeating the measurement of the horizontal light Transmittance (TH) and the vertical light Transmittance (TV) for a plurality of times (the number of data points contained in the light spot in single measurement is more than or equal to 1000) after the solution is slowly stationary.
4. Identifying the dissolved state of a metal sample
4.1 different metal sample states, adopting different identification methods:
(1) Powder sample (particle size of sample particle. Ltoreq.0.1 mm): by comparing the vertical light transmittance data with the horizontal light transmittance data when the solution in the measuring reactor in the step 3 is in a static state after circulating movement, if the average value of the vertical light Transmittance (TV) is within the confidence interval [ mu-sigma, mu+sigma ] (mu is the average value, sigma is the standard deviation and the confidence level is 0.683) of the horizontal light Transmittance (TH), the material of the metal sample can be determined to be completely dissolved. If the vertical light Transmittance (TV) average is outside the horizontal light Transmittance (TH) confidence interval [ mu-sigma, mu+sigma ], it can be determined that the metal sample is not completely dissolved.
(2) Particle size of the sample > 0.1mm: and 3, subtracting the horizontal light Transmittance (TH) data from the vertical light Transmittance (TV) data when the solution in the reactor is in a static state after the solution in the step 3 performs circular motion to obtain residual light transmittance data (TC), and determining that the metal sample material is completely dissolved if the distribution frequency peak height of the residual light Transmittance (TC) is within a confidence interval [0, sigma ] (the average value is zero, sigma is the standard deviation and the confidence level is 0.683). If the distribution frequency peak height of the residual light Transmittance (TC) is outside the confidence interval [0, sigma ] (the average value is zero, sigma is the standard deviation, and the confidence level is 0.683), the metal sample material can be determined to be not completely dissolved.
4.2 treatment of incompletely dissolved Metal samples
And (3) continuously heating and dissolving the metal sample in the reactor for the metal sample which is not completely dissolved, measuring the vertical light Transmittance (TV) at the horizontal light Transmittance (TH) according to the steps 2 and 3, and judging whether the metal sample is completely dissolved or not according to the step 4.1. If the above steps 2 and 3 are repeated several times (> 5 times), the average value of the vertical light Transmittance (TV) is still outside the confidence interval [ mu-sigma, mu+sigma ] of the horizontal light Transmittance (TH) or the distribution frequency peak height of the residual light Transmittance (TC) is outside the confidence interval [0, sigma ], the impurities in the solution can be determined, and the filtering treatment is required until the step 4.1 is performed to determine that the average value of the vertical light Transmittance (TV) is inside the confidence interval [ mu-sigma, mu+sigma ] of the horizontal light Transmittance (TH) or the distribution frequency peak height of the residual light Transmittance (TC) is inside the confidence interval [0, sigma ].
The above-mentioned confidence intervals [ mu-sigma, mu + sigma ] of the horizontal light Transmittance (TH), the mu value and sigma value are determined by normal distribution fitting to the horizontal light Transmittance (TH).
The residual light Transmittance (TC) confidence interval [0, σ ] described above, the σ value is determined by normal distribution fitting to the horizontal light Transmittance (TH).
The following describes the invention in more detail with reference to examples, which are not intended to limit the invention thereto.
Examples 1 to 5
1. Experimental sample
Examples 1-5 respectively adopted blocky medium-low alloy, flaky high alloy, flaky titanium alloy and ferromolybdenum powder, wherein the diameters of ferromolybdenum powder sample particles are less than or equal to 0.1mm, and the particle sizes of other samples are more than 0.1mm.
2. The experiment is carried out by weighing 0.1000+/-0.0010 g, cutting a small sample for the block-shaped and sheet-shaped samples, weighing, trimming for multiple times, and weighing to obtain the sample with the weight of 0.1000+/-0.0010 g.
3. Solvent(s)
3.1, the low alloy, high alloy and ferromolybdenum are mixed with 20ml of salt nitric acid, and the volume ratio of hydrochloric acid to nitric acid is 5:4.
3.2 the superalloy is dissolved in 20ml of hydrochloric acid, and nitric acid is added dropwise after 10 minutes, wherein the consumption of nitric acid is less than 5ml.
3.3 titanium alloy was dissolved with 20ml hydrochloric acid.
4. Experimental environment
The table was heated to 100℃and a fume hood.
5. Experimental method
1. Dissolution of metal sample
And (3) respectively placing the accurately weighed metal samples into transparent flat-bottomed flasks, respectively adding the solvents, placing the solutions on a heating table for heating so as to accelerate the dissolution of the metal samples, and sampling and detecting the samples at different time.
2. Light source parameter adjustment
A beam of parallel light source with fixed intensity of 3000lm horizontally passes through the solution in a static state, the wavelength of the light source is automatically adjusted according to the horizontal light Transmittance (TH), and the wavelength is adjusted from 200nm to 2500nm, so that the horizontal light Transmittance (TH) reaches the maximum value.
3. Determination of transmittance of circulating solution
The solution in the reactor is circulated, and after the solution is slowly stationary, the horizontal light Transmittance (TH) and the vertical light Transmittance (TV) are measured repeatedly for 5 times (1100 measuring points, namely 1100 data points contained on a light spot in single measurement).
4. Identifying the dissolved state of a metal sample
4.1 different metal sample states, adopting different identification methods:
(1) Powder sample: by comparing the vertical light transmittance data with the horizontal light transmittance data when the solution in the measuring reactor in the step 3 is in a static state after circulating movement, if the average value of the vertical light Transmittance (TV) is within the confidence interval [ mu-sigma, mu+sigma ] (mu is the average value, sigma is the standard deviation and the confidence level is 0.683) of the horizontal light Transmittance (TH), the material of the metal sample can be determined to be completely dissolved. If the vertical light Transmittance (TV) average is outside the horizontal light Transmittance (TH) confidence interval [ mu-sigma, mu+sigma ], it can be determined that the metal sample is not completely dissolved.
(2) Samples with particle sizes greater than 0.1mm: and 3, subtracting the horizontal light Transmittance (TH) data from the vertical light Transmittance (TV) data when the solution in the reactor is in a static state after the solution in the step 3 performs circular motion to obtain residual light transmittance data (TC), and determining that the metal sample material is completely dissolved if the distribution frequency peak height of the residual light Transmittance (TC) is within a confidence interval [0, sigma ] (the average value is zero, sigma is the standard deviation and the confidence level is 0.683). If the distribution frequency peak height of the residual light Transmittance (TC) is outside the confidence interval [0, sigma ] (the average value is zero, sigma is the standard deviation, and the confidence level is 0.683), the metal sample material can be determined to be not completely dissolved.
4.2 treatment of incompletely dissolved Metal samples
And (3) continuously heating and dissolving the metal sample in the reactor for the metal sample which is not completely dissolved, measuring the vertical light Transmittance (TV) at the horizontal light Transmittance (TH) according to the steps 2 and 3, and judging whether the metal sample is completely dissolved or not according to the step 4.1. If the above steps 2 and 3 are repeated several times (> 5 times), the average value of the vertical light Transmittance (TV) is still outside the confidence interval [ mu-sigma, mu+sigma ] of the horizontal light Transmittance (TH) or the distribution frequency peak height of the residual light Transmittance (TC) is outside the confidence interval [0, sigma ], the impurities in the solution can be determined, and the filtering treatment is required until the step 4.1 is performed to determine that the average value of the vertical light Transmittance (TV) is inside the confidence interval [ mu-sigma, mu+sigma ] of the horizontal light Transmittance (TH) or the distribution frequency peak height of the residual light Transmittance (TC) is inside the confidence interval [0, sigma ].
The above-mentioned confidence intervals [ mu-sigma, mu + sigma ] of the horizontal light Transmittance (TH), the mu value and sigma value are determined by normal distribution fitting to the horizontal light Transmittance (TH).
The residual light Transmittance (TC) confidence interval [0, σ ] described above, the σ value is determined by normal distribution fitting to the horizontal light Transmittance (TH).
Examples 1-5 the results of sampling measurements at different dissolution times are detailed in FIGS. 4-8. As can be seen from fig. 4-8, the different samples can be completely dissolved with increasing dissolution time, and the bulk medium-low alloy, high alloy scraps, flaky superalloy, flaky titanium alloy and ferromolybdenum powder are completely dissolved at 36min, 29min, 36min and 4.5min respectively.
Claims (8)
1. A method for identifying complete dissolution of a metal specimen, the method comprising:
A. placing the solution of the metal sample to be tested into a transparent container, horizontally passing the solution in a static state by using a parallel light source, and automatically adjusting the wavelength of the light source within the range of 200nm-2500nm to ensure that the horizontal light transmittance reaches the maximumThe wavelength at this time is denoted as lambda max ；
B. The solution is circulated, and lambda is used after the solution is static max Measuring the horizontal light transmittance TH and the vertical light transmittance TV;
C. identifying the dissolved state of a metal sample
(1) The granularity of the metal sample before dissolution is less than or equal to 0.1mm:
if the average value of TV is within the TH confidence interval mu-sigma to mu+sigma, the metal sample can be determined to be completely dissolved; if the TV average value is outside a TH confidence interval mu-sigma to mu+sigma, determining that the metal sample is not completely dissolved, wherein mu is the average value, sigma is the standard deviation, and the confidence level is 0.683;
(2) particle size of the metal sample before dissolution is more than 0.1mm: TC=TV-TH, the distribution frequency peak height of TC is within the confidence interval 0-sigma, and the complete dissolution of the metal sample can be determined; the distribution frequency peak height of TC is outside the confidence interval 0-sigma, the metal sample can be determined to be incompletely dissolved, wherein the average value is zero, sigma is the standard deviation, and the confidence level is 0.683;
the TH confidence interval mu-sigma to mu+sigma, and the mu value and the sigma value are determined by carrying out normal distribution fitting on TH;
TC confidence interval 0-sigma, through carrying on normal distribution fitting to TH confirm sigma value.
2. The method for identifying complete dissolution of a metal specimen according to claim 1, wherein the method for preparing the solution in step a comprises dissolving the metal specimen to be tested in an acid.
3. The method for identifying complete dissolution of a metal specimen according to claim 2, wherein the metal specimen to be measured is dissolved in an acid and heated for dissolution.
4. The method of claim 1 or 2, wherein the metal is at least one of medium and low alloy, high temperature alloy, titanium alloy, and ferromolybdenum.
5. The method for identifying complete dissolution of a metal specimen according to claim 1 or 2, wherein the intensity of the light source in step a is fixed, and the intensity of the light source ranges from 2500lm to 3000lm.
6. The method for identifying complete dissolution of a metal specimen according to claim 1 or 2, wherein the number of points at TH and TV is equal to or greater than 1000, respectively, by repeating the step B.
7. The method of identifying complete dissolution of a metal specimen according to claim 1 or 2, further comprising step D:
c, determining that the metal sample is not completely dissolved, continuing to dissolve the metal sample, and repeating the steps B and C to determine whether the metal sample is completely dissolved; if the steps B and C are repeated for more than 5 times, judging that the metal sample is still not completely dissolved according to the step C, and determining that impurities exist in the solution.
8. The method of identifying complete dissolution of a metal specimen according to claim 7, further comprising step E: and D, if the impurities exist in the solution, filtering, and repeating the steps B and C until the step C is used for determining that the average value of the TV is within a confidence interval mu-sigma to mu+sigma of TH or the distribution frequency peak height of TC is within a confidence interval 0-sigma.
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