CN113804672A - Method for simultaneously measuring multiple elements of trace elements in copper-chromium electrical contact material - Google Patents
Method for simultaneously measuring multiple elements of trace elements in copper-chromium electrical contact material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 48
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000011573 trace mineral Substances 0.000 title claims abstract description 29
- 235000013619 trace mineral Nutrition 0.000 title claims abstract description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 32
- 239000011651 chromium Substances 0.000 claims abstract description 32
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000010949 copper Substances 0.000 claims abstract description 27
- 229910052802 copper Inorganic materials 0.000 claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- 239000012086 standard solution Substances 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 239000011133 lead Substances 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 16
- 239000010941 cobalt Substances 0.000 claims abstract description 16
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011777 magnesium Substances 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011575 calcium Substances 0.000 claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 14
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 10
- 238000005485 electric heating Methods 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- 230000003595 spectral effect Effects 0.000 claims abstract description 7
- 238000003705 background correction Methods 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 25
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 25
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 25
- 238000012360 testing method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
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- 238000009835 boiling Methods 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 230000010354 integration Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 5
- 230000029087 digestion Effects 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012085 test solution Substances 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 229910000599 Cr alloy Inorganic materials 0.000 description 5
- 239000000788 chromium alloy Substances 0.000 description 5
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 238000009614 chemical analysis method Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001061225 Arcos Species 0.000 description 1
- OYPRJOBELJOOCE-BKFZFHPZSA-N Calcium-45 Chemical compound [45Ca] OYPRJOBELJOOCE-BKFZFHPZSA-N 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000001803 electron scattering Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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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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Abstract
A method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material comprises the following specific steps: preparing a mixed standard solution, preparing a working curve solution, digesting a sample, and measuring on a computer; the method is characterized in that dilute hydrochloric acid and hydrogen peroxide are adopted to digest a sample on an electric heating plate, the problem that a copper-chromium electrical contact material is difficult to dissolve completely is solved, high-purity copper and high-purity chromium are used for carrying out matrix matching to manufacture a working curve, the interference of high-content chromium to elements to be detected is solved, an optimal analysis line of each element is selected on an inductively coupled plasma emission spectrometer, background correction is carried out, the contents of 10 trace elements such as aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead in the copper-chromium electrical contact material are measured simultaneously according to the linear relation between the spectral line intensity and the element content, the detection period is short, the operation process is simple, the reagent consumption is low, the method is suitable for batch detection, and the vacancy of a method for simultaneously measuring and analyzing a plurality of trace elements in the copper-chromium electrical contact material is filled.
Description
Technical Field
The invention relates to the field of chemical analysis, in particular to a method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material.
Background
The high-chromium-content copper-chromium alloy has the characteristics of excellent electric conductivity, heat conduction, voltage resistance, arc ablation resistance, on-off current performance, oxygen absorption and the like, so that the high-chromium-content copper-chromium alloy is widely applied to a medium-high voltage vacuum arc extinguishing chamber as a contact material. According to different proportions of copper and chromium elements, the common copper and chromium electrical contact materials at present comprise six materials including CuCr25, CuCr30, CuCr35, CuCr40, CuCr45 and CuCr 50.
The chemical composition of the copper-chromium electrical contact material is crucial to the material performance, and besides the two main components of copper and chromium, other trace elements also have different influences on the material performance. Such as: in the smelting process, impurity elements are introduced due to insufficient purity of raw material metal chromium and pollution of crucible materials, so that the pressure resistance and the breaking performance of the materials are reduced, and the operation of a power grid is threatened; the aging process points out that when the influence of nickel, iron and cobalt on the performance of the CuCr50 electrical contact material is researched in the text of 'preparation and performance research of Cu-based electrical contact material': fe. The addition of Co and Ni is helpful for improving the wettability of Cu and Cr, promoting the infiltration, and helping the uniform distribution of material structure, and improving the density, hardness and bending strength of the material, but the addition of Fe, Co and Ni can also cause the lattice distortion of Cu, increase the probability of electron scattering, and increase the resistivity of the material.
The chemical analysis method of copper and chromium elements in the copper-chromium electrical contact material is already specified in the mechanical industry standard JB/T8443 "chemical analysis method of copper-chromium contact material". But few researches are currently carried out on a chemical analysis method of trace elements in the copper-chromium electrical contact material. GB/T5121.27-2008 & lt & ltchemical analysis method for copper and copper alloy & gt part 27 & lt/27 & gt, inductively coupled plasma atomic emission spectrometry & gt discloses a method for simultaneously determining multiple elements in a copper alloy by using an inductively coupled plasma emission spectrometer, but due to the introduction of high-content chromium in a copper-chromium electrical contact material, a sample cannot be completely dissolved by using the GB/T5121.27-2008 method, and meanwhile, the accuracy of a result is insufficient due to matrix mismatching, so that the method is not suitable for analysis of the copper-chromium electrical contact material. Zhejiang metallurgy, 1994, No. 4, pages 26-30, discloses a method for determining trace aluminum in a copper-chromium alloy by a chromium azure S colorimetric method; a method for measuring trace elements in a copper-chromium binary alloy by using an atomic absorption spectrometry is disclosed on pages 37 to 39 of a large-scale forging and casting No.3May 2008, and the measurement of trace elements such as iron and lead is researched; the method for measuring the trace amount of zinc and manganese atoms in the copper-chromium alloy by the absorption method is disclosed in the electronic alloy literature 1989 (03) pages 62 to 63. The analytical methods described in the above-mentioned articles employ spectrophotometry or atomic absorption spectroscopy, respectively, and have the following disadvantages: 1, the analysis of element types by a spectrophotometry and an atomic absorption spectrometry is limited, and the current research is limited to five elements of lead, iron, aluminum, zinc and manganese; 2. the spectrophotometry and the atomic absorption spectrometry are single-element measurement, the detection efficiency is low, the detection period is long, and the method is not suitable for batch detection; 3. meanwhile, the spectrophotometry method uses more chemical reagents and more dosage, which is not beneficial to environmental protection.
In summary, no method capable of simultaneously and efficiently measuring multiple trace elements in the copper-chromium electrical contact material is found at present. The method for simultaneously measuring multiple trace elements in the copper-chromium electrical contact material is efficient, rapid, accurate and low in cost, and has important significance for process improvement, material performance research and product quality control.
In view of the above, a method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material has been developed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material, adopts dilute hydrochloric acid and hydrogen peroxide to digest a sample on an electric heating plate, solves the problem that the copper-chromium electrical contact material is difficult to dissolve completely, uses high-purity copper and high-purity chromium to carry out matrix matching to manufacture a working curve, solves the interference of high-content chromium on elements to be measured, selecting the optimal analysis line of each element on an inductively coupled plasma emission spectrometer, performing background correction, according to the linear relation between the spectral line intensity and the element content, the content of 10 trace elements of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead in the copper-chromium electrical contact material is measured simultaneously, the detection period is short, the operation process is simple, the reagent consumption is low, the method is suitable for batch detection, and the vacancy of the method for simultaneously measuring and analyzing a plurality of trace elements in the copper-chromium electrical contact material is filled.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material comprises the following specific steps: preparing a mixed standard solution, preparing a working curve solution, digesting a sample, and measuring on a computer.
Preparing a mixed standard solution:
sucking 2.50mL of each of ten single element national standard solutions with the concentration of 1000 mug/mL of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead by using a liquid transfer gun, putting the solutions into a 100mL volumetric flask, adding 7.5mL of high-grade pure hydrochloric acid, uniformly mixing and fixing the volume, wherein each of the mixed standard solutions contains 25 mug/mL of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead;
preparing a working curve solution:
selecting high-purity copper and high-purity chromium with the element content to be detected not more than 0.0003% as matrixes, weighing 5 parts of the high-purity copper and the high-purity chromium matrixes in parallel, respectively placing the high-purity copper and the high-purity chromium matrixes in 5 250mL polytetrafluoroethylene beakers, wherein 0.125g-0.250g of high-purity chromium and 0.250g-0.375g of high-purity copper in each polytetrafluoroethylene beaker, and the ratio of the high-purity chromium to the high-purity copper is consistent with the ratio of copper to chromium in the copper-chromium electrical contact material; adding 10-20 mL of hydrochloric acid (1+1) into a polytetrafluoroethylene beaker, placing the polytetrafluoroethylene beaker on an electric heating plate, heating the polytetrafluoroethylene beaker at a low temperature until no bubbles emerge, adding 2-5 mL of hydrogen peroxide (30%), heating the polytetrafluoroethylene beaker until the sample is completely dissolved, boiling the mixture to remove the excessive hydrogen peroxide, taking down the polytetrafluoroethylene beaker, cooling the polytetrafluoroethylene beaker to room temperature, washing the wall of the polytetrafluoroethylene beaker by using water, adding 1.0mL, 2.0mL, 5.0mL and 10.0mL of mixed standard solution into four of the 5 beakers by using a pipette gun respectively, adding the mixed standard solution into the other beaker without adding the mixed standard solution, fixing the volume to 100mL, and uniformly mixing the solutions for later use.
Digestion of the sample: weighing 0.50g of sample by using an electronic balance, accurately weighing the sample to 0.0001g, placing the sample in a 250mL polytetrafluoroethylene beaker, adding 10mL-20mL of hydrochloric acid (1+1), placing the sample on an electric heating plate, heating the sample at a low temperature until no bubbles emerge, adding 2mL-5mL of hydrogen peroxide (30%), heating the sample until the sample is completely dissolved, boiling the sample to remove the excessive hydrogen peroxide, taking down the sample, cooling the sample to room temperature, washing the wall of the beaker by using water, transferring the solution in the beaker into a 100mL volumetric flask, diluting the solution to a scale, and uniformly mixing the solution to be detected;
testing on a machine: performing working curve fitting on the inductively coupled plasma emission spectrometer by using the working curve solution prepared in the step 2, wherein the linear correlation coefficient of the fitted working curve is not less than 0.999, selecting the optimal wavelength of each element on the instrument, determining the test solution with the constant volume in the step 3, checking the background of the spectral line of each element, performing background correction at a proper position, simultaneously performing a blank test according to the steps, subtracting a reagent blank value, and automatically and simultaneously giving the content of each element to be measured by a computer;
the measurement parameters of the inductively coupled plasma emission spectrometer are as follows: adopting a vertical observation mode, the plasma power is 1200W-1500W, the flow rate of atomizing gas is 0.5L/min-1.2L/min, the cooling air flow rate is 10L/min-15L/min, the auxiliary air flow rate is 1.0L/min-2.0L/min, the flushing pump speed and the analysis pump speed are both 20-50rpm, the flushing time is 30-50s, the integration time is 10s-50s, and the integration times are 2-4 times.
The invention has the beneficial effects that: according to the invention, dilute hydrochloric acid and hydrogen peroxide are adopted to digest a sample on an electric heating plate, so that the problem that a copper-chromium electrical contact material is difficult to dissolve completely is solved, a working curve is made by matching high-purity copper and high-purity chromium with a substrate, the interference of high-content chromium to an element to be detected is solved, an optimal analysis line of each element is selected on an inductively coupled plasma emission spectrometer, background correction is carried out, and the content of 10 trace elements of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead in the copper-chromium electrical contact material is determined simultaneously according to the linear relation between the spectral line intensity and the element content; aiming at the defects of the existing method for detecting trace elements in the copper-chromium electrical contact material, the invention provides a method for detecting the trace elements in the copper-chromium electrical contact material, which can simultaneously detect multiple elements, has the advantages of fewer operation steps, good digestion effect and less reagent consumption, compared with the existing method for detecting the trace elements in the copper-chromium alloy material, the method for detecting the trace elements in the copper-chromium electrical contact material can simultaneously detect ten elements of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead with the chromium content of 4-52 percent, has short detection period, simple operation process and less reagent consumption, is suitable for batch detection, and fills the gap of a method for simultaneously detecting and analyzing the trace elements in the copper-chromium electrical contact material.
Detailed Description
The present invention will be described in further detail with reference to the following examples and embodiments:
example 1
The analysis process of the content of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead in the CuCr50 electrical contact material comprises the following steps: preparing a mixed standard solution:
sucking 2.50mL of each of ten single element national standard solutions with the concentration of 1000 mug/mL of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead by using a liquid transfer gun, putting the solutions into a 100mL volumetric flask, adding 7.5mL of hydrochloric acid (super pure), uniformly mixing and fixing the volume, wherein the mixed standard solution contains 25 mug/mL of each of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead;
preparing a working curve solution: selecting high-purity copper and high-purity chromium with the element content to be detected not more than 0.0003% as matrixes, weighing 5 parts of the high-purity copper and the high-purity chromium matrixes in parallel, respectively placing the 5 parts of the high-purity copper and the high-purity chromium matrixes in 5 250mL of polytetrafluoroethylene beakers, wherein each part of the high-purity copper and the high-purity chromium matrix consists of 0.025g to 0.250g to 0.475g of high-purity copper, adding 15mL of hydrochloric acid (1+1) into each polytetrafluoroethylene beaker, placing the polytetrafluoroethylene beaker on an electric heating plate, heating the polytetrafluoroethylene beaker at a low temperature until no bubbles emerge, adding 3mL of hydrogen peroxide (30%), heating the sample until the sample is completely dissolved, boiling the sample to remove the excessive hydrogen peroxide, taking the sample down and cooling the sample to room temperature, washing the wall of the cup with water, respectively adding 1.0mL, 2.0mL, 5.0mL and 10.0mL of mixed standard solutions into four of the 5 beakers by using a liquid-moving gun, keeping the volume, not adding the mixed standard solutions into the other beakers, and uniformly mixing the sample for later use;
digestion of the sample: weighing two CuCr50 electric contact material samples, namely a parallel sample No. 1#0.5013g and a parallel sample No. 2#0.4996g in parallel by using an electronic balance, respectively placing the samples in two 250mL polytetrafluoroethylene beakers, adding 15mL hydrochloric acid (1+1), placing the samples on an electric heating plate, heating at a low temperature until no bubbles emerge, adding 3mL hydrogen peroxide (30%), heating until the samples are completely dissolved, boiling to remove excessive hydrogen peroxide, taking down and cooling to room temperature, washing the wall of the beaker with water, transferring the solution in the beaker into a 100mL volumetric flask, diluting to a scale, uniformly mixing to be detected;
testing on a machine: the instrument measurement parameters were set as follows: adopting a German Schucker ARCOS type inductively coupled plasma emission spectrometer, and adopting a vertical observation mode, wherein the plasma power is 1400W, the atomization airflow rate is 1.0L/min, the cooling airflow rate is 13L/min, the auxiliary airflow rate is 1.5L/min, the flushing pump speed and the analysis pump speed are both 30rpm, the flushing time is 40s, the integration time is 28s, and the integration time is 2 times;
performing working curve fitting on an inductively coupled plasma emission spectrometer by using the working curve solution prepared in the step 2, wherein the linear correlation coefficient of the fitted working curve is not less than 0.999, the interference of chromium to the spectrum of other elements to be detected is very obvious, the interference condition and the sensitivity of the elements to be detected are comprehensively considered, the optimal spectral line of each element is selected according to the table 1, the test solution with the constant volume in the step 3 is measured, the background of each element spectral line is checked, the background correction is performed at the proper position, a blank test is simultaneously performed according to the steps, the blank value of a reagent is subtracted, the content of each element to be detected is automatically and simultaneously given by a computer, and finally, the detection result of each trace element of the CuCr50 electrical contact material is as follows: 0.021% of aluminum, 0.025% of iron, 0.0018% of nickel, 0.0012% of cobalt, 0.018% of calcium, 0.012% of magnesium, 0.0008% of manganese, 0.0048% of zinc, 0.026% of silicon and 0.0010% of lead;
TABLE 1 analysis lines of elements to be tested
And (3) precision test: in this embodiment, 6 parts of the CuCr50 electrical contact material was weighed in parallel, ten elements of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon, and lead were measured according to the method of the present invention, and the results of the method precision test were shown in table 2:
TABLE 2 precision test data
The data in Table 2 show that the relative standard deviation of the method is 2.16-7.00%, and the method has better precision;
and (3) accuracy test: the CuCr50 electrical contact material in the embodiment is selected, the standard solution is quantitatively added, the accuracy of the standard recovery test verification method is carried out, and the test results are shown in Table 3:
TABLE 3 spiking recovery test
| Element(s) | Known amount of% | Amount of addition% | Measured value% | Percent recovery rate% |
| Aluminum (Al) | 0.021 | 0.020 | 0.040 | 97.56 |
| Iron (Fe) | 0.025 | 0.020 | 0.044 | 97.78 |
| Nickel (Ni) | 0.0018 | 0.0010 | 0.0030 | 107.14 |
| Cobalt (Co) | 0.0012 | 0.0010 | 0.0021 | 95.45 |
| Calcium (Ca) | 0.018 | 0.010 | 0.028 | 100.00 |
| Magnesium (Mg) | 0.012 | 0.010 | 0.023 | 104.55 |
| Manganese (Mn) | 0.0009 | 0.0010 | 0.0018 | 94.74 |
| Zinc (Zn) | 0.0048 | 0.0050 | 0.01 | 102.04 |
| Silicon (Si) | 0.026 | 0.020 | 0.047 | 102.17 |
| Lead (Pb) | 0.0011 | 0.0010 | 0.0020 | 95.24 |
The data in Table 3 show that the recovery rate of the standard addition by the method is 94.74-107.14%, and the method has better accuracy;
the above embodiments show that the method of the present invention can completely realize the simultaneous determination of ten elements of the copper-chromium electrical contact material aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon, and lead, and precision tests and accuracy tests show that the method has good accuracy and precision. The method also has the advantages of simplicity, rapidness, simple and convenient operation and low material cost, fills the gap of a method for simultaneously determining and analyzing a plurality of trace elements in the copper-chromium electrical contact material, and is suitable for batch detection of the trace elements in the material.
Claims (3)
1. A method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material is characterized by comprising the following steps: the method comprises the following specific steps: preparing a mixed standard solution, preparing a working curve solution, digesting a sample, and measuring on a computer.
2. The method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material as claimed in claim 1, wherein:
preparing a mixed standard solution:
sucking 2.50mL of each of ten single element national standard solutions with the concentration of 1000 mug/mL of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead by using a liquid transfer gun, putting the solutions into a 100mL volumetric flask, adding 7.5mL of high-grade pure hydrochloric acid, uniformly mixing and fixing the volume, wherein each of the mixed standard solutions contains 25 mug/mL of aluminum, iron, nickel, cobalt, calcium, magnesium, manganese, zinc, silicon and lead;
preparing a working curve solution:
selecting high-purity copper and high-purity chromium with the element content to be detected not more than 0.0003% as matrixes, weighing 5 parts of the high-purity copper and the high-purity chromium matrixes in parallel, respectively placing the high-purity copper and the high-purity chromium matrixes in 5 250mL polytetrafluoroethylene beakers, wherein 0.125g-0.250g of high-purity chromium and 0.250g-0.375g of high-purity copper in each polytetrafluoroethylene beaker, and the ratio of the high-purity chromium to the high-purity copper is consistent with the ratio of copper to chromium in the copper-chromium electrical contact material; adding 10-20 mL of hydrochloric acid (1+1) into a polytetrafluoroethylene beaker, placing the polytetrafluoroethylene beaker on an electric heating plate, heating the polytetrafluoroethylene beaker at a low temperature until no bubbles emerge, adding 2-5 mL of hydrogen peroxide (30%), heating the polytetrafluoroethylene beaker until the sample is completely dissolved, boiling the mixture to remove the excessive hydrogen peroxide, taking down the polytetrafluoroethylene beaker, cooling the polytetrafluoroethylene beaker to room temperature, washing the wall of the polytetrafluoroethylene beaker by using water, adding 1.0mL, 2.0mL, 5.0mL and 10.0mL of mixed standard solution into four of the 5 beakers by using a pipette gun respectively, adding the mixed standard solution into the other beaker without adding the mixed standard solution, fixing the volume to 100mL, and uniformly mixing the solutions for later use.
3. The method for simultaneously measuring multiple elements of trace elements in a copper-chromium electrical contact material as claimed in claim 1, wherein:
digestion of the sample: weighing 0.50g of sample by using an electronic balance, accurately weighing the sample to 0.0001g, placing the sample in a 250mL polytetrafluoroethylene beaker, adding 10mL-20mL of hydrochloric acid (1+1), placing the sample on an electric heating plate, heating the sample at a low temperature until no bubbles emerge, adding 2mL-5mL of hydrogen peroxide (30%), heating the sample until the sample is completely dissolved, boiling the sample to remove the excessive hydrogen peroxide, taking down the sample, cooling the sample to room temperature, washing the wall of the beaker by using water, transferring the solution in the beaker into a 100mL volumetric flask, diluting the solution to a scale, and uniformly mixing the solution to be detected;
testing on a machine: performing working curve fitting on the inductively coupled plasma emission spectrometer by using the working curve solution prepared in the step 2, wherein the linear correlation coefficient of the fitted working curve is not less than 0.999, selecting the optimal wavelength of each element on the instrument, determining the test solution with the constant volume in the step 3, checking the background of the spectral line of each element, performing background correction at a proper position, simultaneously performing a blank test according to the steps, subtracting a reagent blank value, and automatically and simultaneously giving the content of each element to be measured by a computer;
the measurement parameters of the inductively coupled plasma emission spectrometer are as follows: adopting a vertical observation mode, the plasma power is 1200W-1500W, the flow rate of atomizing gas is 0.5L/min-1.2L/min, the cooling air flow rate is 10L/min-15L/min, the auxiliary air flow rate is 1.0L/min-2.0L/min, the flushing pump speed and the analysis pump speed are both 20-50rpm, the flushing time is 30-50s, the integration time is 10s-50s, and the integration times are 2-4 times.
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