CN113029730A - Mixed acid solution for dissolving copper-phosphorus alloy sample and preparation method and application thereof - Google Patents
Mixed acid solution for dissolving copper-phosphorus alloy sample and preparation method and application thereof Download PDFInfo
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- 239000002253 acid Substances 0.000 title claims abstract description 75
- 229910001096 P alloy Inorganic materials 0.000 title claims abstract description 47
- RIRXDDRGHVUXNJ-UHFFFAOYSA-N [Cu].[P] Chemical compound [Cu].[P] RIRXDDRGHVUXNJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 54
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 15
- 239000011574 phosphorus Substances 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims description 16
- 230000010355 oscillation Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 18
- 238000001514 detection method Methods 0.000 abstract description 17
- 238000004090 dissolution Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 122
- 230000000052 comparative effect Effects 0.000 description 18
- 239000002245 particle Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 4
- 229910003470 tongbaite Inorganic materials 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000000120 microwave digestion Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Life Sciences & Earth Sciences (AREA)
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- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
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Abstract
The invention provides a mixed acid solution for dissolving a copper-phosphorus alloy sample, and a preparation method and application thereof, wherein the mixed acid solution comprises a nitric acid solution and a hydrofluoric acid solution; the concentration of the nitric acid solution is 62-68 wt%; the concentration of the hydrofluoric acid solution is 32-40 wt%; the volume ratio of the nitric acid solution to the hydrofluoric acid solution is 1 (1-3). The preparation method comprises the following steps: and (3) mixing the nitric acid solution and the hydrofluoric acid solution according to the volume ratio of 1 (1-3), and uniformly oscillating to obtain the mixed acid solution. The application comprises the following steps: and mixing the copper-phosphorus alloy sample with the mixed acid solution, heating and oscillating to obtain a solution dissolved with copper and phosphorus. The invention improves the dissolving efficiency of the copper-phosphorus alloy, shortens the dissolving time, and realizes the complete dissolution of the copper-phosphorus alloy in the mixed acid solution, thereby meeting the subsequent ICP-OES detection standard.
Description
Technical Field
The invention belongs to the technical field of sample treatment, relates to a mixed acid solution for dissolving an alloy sample, and particularly relates to a mixed acid solution for dissolving a copper-phosphorus alloy sample, and a preparation method and application thereof.
Background
The copper-phosphorus alloy is mainly used for a copper interconnection line seed layer, wherein the content of copper metal plays a decisive role in relevant performance, so that accurate knowledge of the content is necessary. A commonly used device for testing the content of copper and phosphorus is an inductively coupled plasma emission spectrometer (ICP-OES), the device has the advantages of less interference, stable signal and simple operation, and a sample can be tested on a machine only by dissolving the sample with acid liquor before testing. ICP-OES is mainly used to detect most metallic elements and some non-metallic elements. However, the existing dissolving method only has single element of copper and phosphorus, and is not suitable for the dissolving method of copper-phosphorus alloy.
CN 101303307A discloses an analysis and detection method for impurity elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten and the like in chromium carbide, wherein a chromium carbide sample is placed in a sample dissolving cup, hydrofluoric acid, sulfuric acid and nitric acid are sequentially added into the sample dissolving cup, the mixture is uniformly mixed, and the mixture is placed in a closed high-pressure tank; placing the high-pressure tank in a microwave digestion instrument for microwave digestion twice; taking out the high-pressure tank from the microwave digestion instrument for cooling, transferring the dissolved chromium carbide test solution into a volumetric flask for diluting to a scale, and uniformly mixing; preparing a mixed standard solution series of aluminum, calcium, iron, molybdenum, niobium, titanium and tungsten matched with a chromium matrix; and simultaneously measuring the emission intensity of elements such as aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten and the like on an inductively coupled plasma atomic emission spectrometer by using the blank and chromium carbide test solution and the prepared series of mixed standard solutions, and checking a standard working curve or calculating and analyzing a result by using a linear equation. However, the method has complicated operation steps and is not suitable for the efficient dissolution of the copper-phosphorus alloy.
Therefore, how to provide a mixed acid solution for dissolving a copper phosphorus alloy sample, improve the dissolving efficiency of the copper phosphorus alloy, shorten the dissolving time, and realize the complete dissolution of the copper phosphorus alloy in the mixed acid solution, so that the subsequent ICP-OES detection standard is met, and the problem which needs to be solved by technical personnel in the field at present is solved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a mixed acid solution for dissolving a copper-phosphorus alloy sample, and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a mixed acid solution for dissolving a copper-phosphorus alloy sample, wherein the mixed acid solution comprises a nitric acid solution and a hydrofluoric acid solution.
The nitric acid solution has a concentration of 62 to 68 wt.%, and may be, for example, 62 wt.%, 63 wt.%, 64 wt.%, 65 wt.%, 66 wt.%, 67 wt.% or 68 wt.%, but is not limited to the recited values, and other values not recited within the range of values are also applicable.
The hydrofluoric acid solution has a concentration of 32 to 40 wt%, and may be, for example, 32 wt%, 33 wt%, 34 wt%, 35 wt%, 36 wt%, 37 wt%, 38 wt%, 39 wt% or 40 wt%, but is not limited to the recited values, and other values not recited within the range of values are also applicable.
The volume ratio of the nitric acid solution to the hydrofluoric acid solution is 1 (1-3), and may be, for example, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, or 1:3, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
According to the invention, the concentration and the proportion of each component in the mixed acid solution are reasonably designed, the copper-phosphorus alloy sample is efficiently dissolved by utilizing the synergistic effect between the nitric acid solution and the hydrofluoric acid solution, and compared with the traditional single acid solution, the copper-phosphorus alloy can be completely dissolved in the mixed acid solution, so that the subsequent ICP-OES detection standard is met.
Preferably, the nitric acid solution has a concentration of 64 to 66 wt.%, for example 64 wt.%, 64.2 wt.%, 64.4 wt.%, 64.6 wt.%, 64.8 wt.%, 65 wt.%, 65.2 wt.%, 65.4 wt.%, 65.6 wt.%, 65.8 wt.% or 66 wt.%, but is not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the hydrofluoric acid solution has a concentration of 35-37 wt%, for example 35 wt%, 35.2 wt%, 35.4 wt%, 35.6 wt%, 35.8 wt%, 36 wt%, 36.2 wt%, 36.4 wt%, 36.6 wt%, 36.8 wt% or 37 wt%, but is not limited to the recited values, and other values not recited within the range are equally applicable.
In a second aspect, the present invention provides a method for preparing the mixed acid solution according to the first aspect, the method comprising: and (3) mixing the nitric acid solution and the hydrofluoric acid solution according to the volume ratio of 1 (1-3), and uniformly oscillating to obtain the mixed acid solution.
In the present invention, the nitric acid solution and the hydrofluoric acid solution may be mixed in a volume ratio of 1 (1-3), and may be, for example, 1:1, 1:1.2, 1:1.4, 1:1.6, 1:1.8, 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8 or 1:3, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable.
The mixing of the present invention may be performed by pouring the nitric acid solution into the hydrofluoric acid solution, or by pouring the hydrofluoric acid solution into the nitric acid solution, or by pouring the two solutions into a container at the same time, as long as the purpose of sufficient mixing is achieved, and therefore, the specific mixing method is not particularly limited herein.
In a third aspect, the present invention provides a use of the mixed acid solution of the first aspect, the use comprising: and mixing the copper-phosphorus alloy sample with the mixed acid solution, heating and oscillating to obtain a solution dissolved with copper and phosphorus.
In the invention, the application realizes the complete dissolution of the copper-phosphorus alloy in the mixed acid solution, thereby achieving the subsequent ICP-OES detection standard.
Preferably, the liquid-solid ratio of the mixture is (25-35) mL/g, for example, 25mL/g, 26mL/g, 27mL/g, 28mL/g, 29mL/g, 30mL/g, 31mL/g, 32mL/g, 33mL/g, 34mL/g, or 35mL/g, but not limited to the values listed, and other values not listed in this range are equally applicable.
In the present invention, the liquid-solid ratio of the mixing needs to be kept within a reasonable range. When the liquid-solid ratio is less than 25mL/g, the copper-phosphorus alloy dissolution process is slow, and the situation that particles still exist after the oscillation is ended occasionally occurs; when the liquid-solid ratio is more than 35mL/g, the copper-phosphorus alloy can be quickly dissolved, but the waste of the mixed acid solution is caused to a certain extent.
Preferably, the heating temperature is 90-100 ℃, for example 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
In the present invention, the heating temperature is kept within a reasonable range. When the heating temperature is lower than 90 ℃, the copper-phosphorus alloy dissolution process is slow, and the situation that particles still exist after the oscillation is ended occasionally occurs; when the heating temperature is higher than 100 ℃, the water in the mixed acid solution begins to evaporate and run off, and the nitric acid and the hydrofluoric acid are volatilized in a large amount, so that the resource waste is caused and the health of operators is harmed.
Preferably, the speed of oscillation is 50 to 100rps, for example 50rps, 55rps, 60rps, 65rps, 70rps, 75rps, 80rps, 85rps, 90rps, 95rps or 100rps, but is not limited to the recited values, and other values not recited in this range are equally applicable.
Preferably, the period of oscillation is 10-30min, for example 10min, 12min, 14min, 16min, 18min, 20min, 22min, 24min, 26min, 28min or 30min, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable technical solution of the third aspect of the present invention, the applying includes: mixing a copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of (25-35) mL/g, heating at 90-100 ℃, and oscillating at a speed of 50-100rps for 10-30min to obtain a solution dissolved with copper and phosphorus.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through reasonably designing the concentration and the proportion of each component in the mixed acid solution, the copper-phosphorus alloy sample is dissolved by utilizing the synergistic effect between the nitric acid solution and the hydrofluoric acid solution, the dissolving efficiency is improved, the dissolving time is shortened, and compared with the traditional single acid solution, the copper-phosphorus alloy can be completely dissolved in the mixed acid solution, so that the subsequent ICP-OES detection standard is met.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a 65 wt% nitric acid solution and a 36 wt% hydrofluoric acid solution according to a volume ratio of 1:2, and uniformly oscillating to obtain a mixed acid solution.
Example 2
The embodiment provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a nitric acid solution with the concentration of 64 wt% and a hydrofluoric acid solution with the concentration of 35 wt% according to the volume ratio of 1:1.5, and uniformly oscillating to obtain a mixed acid solution.
Example 3
The embodiment provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a nitric acid solution with the concentration of 66 wt% and a hydrofluoric acid solution with the concentration of 37 wt% according to the volume ratio of 1:2.5, and uniformly oscillating to obtain a mixed acid solution.
Example 4
The embodiment provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a nitric acid solution with the concentration of 62 wt% and a hydrofluoric acid solution with the concentration of 32 wt% according to the volume ratio of 1:1, and uniformly oscillating to obtain a mixed acid solution.
Example 5
The embodiment provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a nitric acid solution with the concentration of 68 wt% and a hydrofluoric acid solution with the concentration of 40 wt% according to the volume ratio of 1:3, and uniformly oscillating to obtain a mixed acid solution.
Comparative example 1
The comparative example provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a 65 wt% nitric acid solution and a 36 wt% sulfuric acid solution according to a volume ratio of 1:2, and uniformly oscillating to obtain a mixed acid solution.
Comparative example 2
The comparative example provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a 65 wt% nitric acid solution and a 36 wt% hydrochloric acid solution according to a volume ratio of 1:2, and uniformly oscillating to obtain a mixed acid solution.
Comparative example 3
The comparative example provides a mixed acid solution for dissolving a copper-phosphorus alloy sample and a preparation method thereof, wherein the preparation method comprises the following steps: mixing 65 wt% sulfuric acid solution and 36 wt% hydrochloric acid solution according to a volume ratio of 1:2, and uniformly oscillating to obtain mixed acid solution.
Application example 1
The present application example provides an application of the mixed acid solution obtained in example 1, where the application is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 30mL/g, heating at 95 ℃ and oscillating at a speed of 75rps for 20min to obtain a solution dissolved with copper and phosphorus.
After the application example is oscillated, the obtained solution is in a clear and transparent state, and the detection standard of subsequent ICP-OES is met.
Application example 2
The present application example provides an application of the mixed acid solution obtained in example 2, where the application is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 27mL/g, heating at 93 ℃ and oscillating at a speed of 60rps for 15min to obtain a solution dissolved with copper and phosphorus.
After the application example is oscillated, the obtained solution is in a clear and transparent state, and the detection standard of subsequent ICP-OES is met.
Application example 3
The present application example provides an application of the mixed acid solution obtained in example 3, where the application is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 33mL/g, heating at 97 ℃ and oscillating at a speed of 90rps for 25min to obtain a solution dissolved with copper and phosphorus.
After the application example is oscillated, the obtained solution is in a clear and transparent state, and the detection standard of subsequent ICP-OES is met.
Application example 4
The present application example provides an application of the mixed acid solution obtained in example 4, where the application is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 25mL/g, heating at 90 ℃ and oscillating at a speed of 50rps for 10min to obtain a solution in which copper and phosphorus are dissolved.
After the application example is oscillated, the obtained solution is in a clear and transparent state, and the detection standard of subsequent ICP-OES is met.
Application example 5
The present application example provides an application of the mixed acid solution obtained in example 5, where the application is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to the liquid-solid ratio of 35mL/g, heating at 100 ℃ and oscillating at the speed of 100rps for 30min to obtain a solution dissolved with copper and phosphorus.
After the application example is oscillated, the obtained solution is in a clear and transparent state, and the detection standard of subsequent ICP-OES is met.
Application example 6
This application example provides an application of the mixed acid solution obtained in example 1, and the application is the same as application example 1 except that the liquid-solid ratio of the copper-phosphorus alloy sample to the mixed acid solution is changed to 20mL/g, and therefore, the details are not repeated herein.
After the oscillation of the application example is finished, the obtained solution is in a clear and transparent state, but a few particles still exist at the bottom after standing, and the detection standard of the subsequent ICP-OES is basically met.
Application example 7
This application example provides an application of the mixed acid solution obtained in example 1, and the conditions other than the heating temperature being reduced to 85 ℃ are the same as those in application example 1, and therefore, the details are not described herein.
After the oscillation of the application example is finished, the obtained solution is in a clear and transparent state, but a few particles still exist at the bottom after standing, and the detection standard of the subsequent ICP-OES is basically met.
Comparative application example 1
This comparative application example provides an application of the mixed acid solution obtained in comparative example 1, which is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 30mL/g, heating at 95 ℃ and oscillating at a speed of 75rps for 20min to obtain a solution dissolved with copper and phosphorus.
After the oscillation of the comparative application example is finished, the obtained solution is in a turbid state with particles and does not meet the detection standard of subsequent ICP-OES.
Comparative application example 2
This comparative application example provides an application of the mixed acid solution obtained in comparative example 2, which is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 30mL/g, heating at 95 ℃ and oscillating at a speed of 75rps for 20min to obtain a solution dissolved with copper and phosphorus.
After the oscillation of the comparative application example is finished, the obtained solution is in a turbid state with particles and does not meet the detection standard of subsequent ICP-OES.
Comparative application example 3
This comparative application example provides an application of the mixed acid solution obtained in comparative example 3, which is: and mixing the copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of 30mL/g, heating at 95 ℃ and oscillating at a speed of 75rps for 20min to obtain a solution dissolved with copper and phosphorus.
After the oscillation of the comparative application example is finished, the obtained solution is in a turbid state with particles and does not meet the detection standard of subsequent ICP-OES.
Therefore, the concentration and the proportion of each component in the mixed acid solution are reasonably designed, the copper-phosphorus alloy sample is dissolved by utilizing the synergistic effect between the nitric acid solution and the hydrofluoric acid solution, the dissolving efficiency is improved, the dissolving time is shortened, and compared with the traditional single acid solution, the copper-phosphorus alloy can be completely dissolved in the mixed acid solution, so that the subsequent ICP-OES detection standard is met.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A mixed acid solution for dissolving a copper-phosphorus alloy sample is characterized by comprising a nitric acid solution and a hydrofluoric acid solution;
the concentration of the nitric acid solution is 62-68 wt%;
the concentration of the hydrofluoric acid solution is 32-40 wt%;
the volume ratio of the nitric acid solution to the hydrofluoric acid solution is 1 (1-3).
2. The mixed acid solution as set forth in claim 1, wherein the concentration of the nitric acid solution is 64 to 66 wt%.
3. The mixed acid solution according to claim 1 or 2, wherein the concentration of the hydrofluoric acid solution is 35 to 37 wt%.
4. A method for preparing the mixed acid solution according to any one of claims 1 to 3, comprising: and (3) mixing the nitric acid solution and the hydrofluoric acid solution according to the volume ratio of 1 (1-3), and uniformly oscillating to obtain the mixed acid solution.
5. Use of the mixed acid solution according to any of claims 1 to 3, comprising: and mixing the copper-phosphorus alloy sample with the mixed acid solution, heating and oscillating to obtain a solution dissolved with copper and phosphorus.
6. The use of claim 5, wherein the combined liquid-to-solid ratio is (25-35) mL/g.
7. Use according to claim 5 or 6, wherein the heating temperature is 90-100 ℃.
8. Use according to any of claims 5-7, wherein the speed of oscillation is 50-100 rps.
9. Use according to any one of claims 5 to 8, wherein the oscillation time is 10-30 min.
10. The application according to any of claims 5-9, characterized in that the application comprises: mixing a copper-phosphorus alloy sample with a mixed acid solution according to a liquid-solid ratio of (25-35) mL/g, heating at 90-100 ℃, and oscillating at a speed of 50-100rps for 10-30min to obtain a solution dissolved with copper and phosphorus.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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