CN113063642A - CrSi alloy sample preparation method suitable for ICP-OES - Google Patents
CrSi alloy sample preparation method suitable for ICP-OES Download PDFInfo
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- CN113063642A CN113063642A CN202110315789.XA CN202110315789A CN113063642A CN 113063642 A CN113063642 A CN 113063642A CN 202110315789 A CN202110315789 A CN 202110315789A CN 113063642 A CN113063642 A CN 113063642A
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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
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
Abstract
The invention provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and mixed acid, heating to 90-100 ℃, and preserving heat, wherein the total time of heating and heat preservation is 40-60min, so as to obtain a sample solution; the mixed acid is hydrochloric acid and hydrofluoric acid which are composed of (1-3) to (1-3) in volume ratio, the concentration of the hydrochloric acid is 36-38 wt%, and the concentration of the hydrofluoric acid is 35-38 wt%. The CrSi alloy sample preparation method provided by the invention can completely dissolve the CrSi alloy target material within 40-60min, has high dissolution efficiency, and fills up the sample preparation blank when the CrSi alloy target material is subjected to ICP-OES test.
Description
Technical Field
The invention belongs to the technical field of semiconductors, relates to a method for analyzing a CrSi alloy, and particularly relates to a CrSi alloy sample preparation method suitable for ICP-OES.
Background
The CrSi alloy target material has great significance in optical coating. The high-precision film resistor has higher stability and radiation resistance intensity, so the high-precision film resistor is widely applied to the fields of aviation, aerospace, communication, automotive electronics, medical equipment, smart phones, navigation systems and the like. In the thin film resistor, the thin film formed by the chromium-silicon alloy has good stability and small resistance temperature coefficient, the thin film characteristic can be improved by adopting a sputtering mode, and the excellent thin film resistor is manufactured, so that the performance of the hybrid integrated circuit is improved. The contents of Cr and Si in the CrSi alloy target play a decisive role in relevant performance, so that the contents of Cr and Si need to be accurately analyzed.
An inductively coupled plasma emission spectrometer (ICP-OES) is a common device for testing the components of the CrSi alloy target, the interference of the inductively coupled plasma emission spectrum on the CrSi alloy target in the test is less, the test signal is stable, the operation is simple, but the CrSi alloy target needs to be dissolved before the test.
Chen Lei in Special Steel Technology (2014),20(79) 44-46 published an article entitled ICP-OES method for determining chromium in titanium alloys by treating samples with: weighing 0.1g of sample and a 200mL conical flask, adding 10mL of sulfuric acid, heating at low temperature to dissolve, adding 3-4 drops of nitric acid to oxidize low-valence titanium into high-valence titanium, moving to high temperature and emitting slight smoke, taking down and cooling to room temperature, and transferring the solution to a 200mL volumetric flask for dilution. The above method enables the testing of chromium in titanium alloys, but does not disclose any method of dissolving both Cr and Si.
CN 103411960A discloses a method for measuring the content of multiple elements in high-silicon low-alloy steel by an ICP spectrometer, which comprises the following steps: (i) preparing a sample solution by using a sample to be tested; (ii) preparing a working curve solution by using a high-purity iron and nitric acid solution and a national standard solution of silicon, manganese, nickel, chromium and copper elements; (iii) and (3) spectral determination: and selecting the optimal analysis spectral lines of the silicon, manganese, nickel, chromium and copper elements by using an ICP (inductively coupled plasma) spectrometer, sequentially measuring the spectral intensity of each element in the working curve solution, drawing the working curve of each element, measuring the spectral intensity of the silicon, manganese, nickel, chromium and copper elements in the sample solution, and obtaining the content of each element from the working curve. The method analyzes various elements, but does not relate to the dissolution of raw materials, and whether the raw materials can be sufficiently dissolved directly influences the accuracy of the final determination.
CN 107764802A discloses a method for measuring trace aluminum, chromium, copper, manganese, nickel and silicon elements in pure iron, which comprises the steps of adopting a purification reagent, weighing a sample in a plastic bottle, dropwise adding hydrochloric acid and nitric acid to dissolve the sample, adding water to dilute the solution in the plastic bottle until the net weight of the solution is 50g, adding a working curve series solution by adopting a standard, deducting a background on an inductively coupled plasma atomic emission spectrometer, measuring the content of analytical elements in the sample with the standard added working curve, calculating the real content of the analytical elements in the working curve series solution, establishing a working curve without deducting the background, and measuring the content of the trace aluminum, chromium, copper, manganese, nickel and silicon elements in the pure iron. The method can detect trace elements, but when the method is used for detecting the CrSi alloy target, the dissolution efficiency is low, and the detection efficiency of the CrSi alloy target is difficult to guarantee.
Therefore, a CrSi alloy sample preparation method suitable for ICP-OES is needed, the CrSi alloy target can be smoothly dissolved, and the sample preparation efficiency is ensured.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the CrSi alloy sample preparation method suitable for ICP-OES, the CrSi alloy sample preparation method can completely dissolve the CrSi alloy target material within 40-60min, the dissolution efficiency is high, and the sample preparation blank when the CrSi alloy target material is subjected to ICP-OES test is filled.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and mixed acid, heating to 90-100 ℃, and preserving heat, wherein the total time of heating and heat preservation is 40-60min, so as to obtain a sample solution;
the mixed acid is hydrochloric acid and hydrofluoric acid which are composed of (1-3) to (1-3) in volume ratio, the concentration of the hydrochloric acid is 36-38 wt%, and the concentration of the hydrofluoric acid is 35-38 wt%.
According to the invention, the CrSi alloy target is dissolved by using the mixed acid of hydrochloric acid and hydrofluoric acid, the CrSi alloy target can be completely dissolved within 40-60min, the required time is short, and the obtained sample solution has an accurate result when being measured.
The concentration of hydrochloric acid in the mixed acid according to the invention is 36 to 38 wt.%, and can be, for example, 36 wt.%, 36.5 wt.%, 37 wt.%, 37.5 wt.% or 38 wt.%, but is not limited to the values listed, and other values not listed in the numerical ranges are equally applicable.
The concentration of hydrofluoric acid in the mixed acid according to the invention is 35-38 wt%, and may be, for example, 35 wt%, 35.5 wt%, 36 wt%, 36.5 wt%, 37 wt%, 37.5 wt%, or 38 wt%, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
The volume ratio of hydrochloric acid to hydrofluoric acid in the mixed acid of the present invention is (1-3): 1-3, and may be, for example, 1:1, 1:2, 1:3, 3:2 or 3:1, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
When the CrSi alloy target is dissolved by using the mixed acid, the dissolution is carried out at 90 to 100 ℃, for example, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃, but the present invention is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the solid-to-liquid ratio of the CrSi alloy target material to the mixed acid is 1 (70-90), and can be, for example, 1:70, 1:72, 1:75, 1:78, 1:80, 1:82, 1:85, 1:88 or 1:90, but is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable; the unit of the solid-liquid ratio is g/mL.
Preferably, the Cr content of the CrSi alloy target material is 83 to 86 wt%, for example, 83 wt%, 83.5 wt%, 84 wt%, 84.5 wt%, 85 wt%, 85.5 wt%, or 86 wt%, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the heating and holding are accompanied by stirring and/or sonication.
According to the invention, through the setting of stirring and/or ultrasound, the CrSi alloy target material can be completely dissolved within 40-60 min.
Preferably, the stirring includes a first stirring and a second stirring which are performed sequentially.
Preferably, the first stirring speed is 200-400r/min, such as 200r/min, 250r/min, 300r/min, 350r/min or 400r/min, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the second stirring speed is 400-600r/min, such as 400r/min, 450r/min, 500r/min, 550r/min or 600r/min, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the ultrasound comprises a first ultrasound and a second ultrasound performed sequentially.
Preferably, the power of the first ultrasonic wave is 200-400W, such as 200W, 250W, 300W, 350W or 400W, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the power of the second ultrasonic wave is 500-800W, such as 500W, 550W, 600W, 650W, 700W, 750W or 800W, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the first sonication is accompanied by a first agitation and the second sonication is accompanied by a second agitation.
Preferably, the first stirring time is 20-30min, such as 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min or 30min, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the second stirring time is 20-30min, such as 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min or 30min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the heating time is 30-40min, for example 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min or 40min, but is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the incubation time is 10-30min, for example 10min, 12min, 15min, 16min, 18min, 20min, 21min, 24min, 25min, 26min, 27min, 28min or 30min, but is not limited to the values recited, and other values not listed in the range of values are equally applicable.
As a preferred technical scheme of the CrSi alloy sample preparation method, the CrSi alloy sample preparation method comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 90-100 ℃, and preserving heat, wherein the heating time is 30-40min, the heat preservation time is 10-30min, and the total heating and heat preservation time is 40-60min to obtain a sample solution;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed by (1-3) to (1-3) in volume ratio, the concentration of the hydrochloric acid is 36-38 wt%, and the concentration of the hydrofluoric acid is 35-38 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1 (70-90), and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 200-400r/min, and the time is 20-30 min; the rotation speed of the second stirring is 400-;
the power of the first ultrasonic wave is 200-400W, and the power of the second ultrasonic wave is 500-800W.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
(1) the sample preparation method provided by the invention is simple to operate, can realize the rapid dissolution of the CrSi alloy target material, and fills the blank of sample preparation when the CrSi alloy target material is subjected to ICP-OES test;
(2) when the sample solution obtained by the sample preparation method is used for ICP-OES testing, the testing accuracy is high, errors caused by the use of mixed acid can be avoided, and the accuracy is high.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 2
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 83 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:3, the concentration of the hydrochloric acid is 36 wt%, and the concentration of the hydrofluoric acid is 38 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:75, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 350r/min, and the time is 22 min; the rotation speed of the second stirring is 550r/min, and the time is 28 min;
the power of the first ultrasonic wave is 250W, and the power of the second ultrasonic wave is 550W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 3
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 86 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 3:1, the concentration of the hydrochloric acid is 38 wt%, and the concentration of the hydrofluoric acid is 35 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:85, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 250r/min, and the time is 28 min; the rotation speed of the second stirring is 450r/min, and the time is 22 min;
the power of the first ultrasonic wave is 350W, and the power of the second ultrasonic wave is 750W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 4
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:70, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 200r/min, and the time is 30 min; the rotation speed of the second stirring is 400r/min, and the time is 20 min;
the power of the first ultrasonic wave is 200W, and the power of the second ultrasonic wave is 500W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 5
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:90, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 400r/min, and the time is 20 min; the rotation speed of the second stirring is 600r/min, and the time is 30 min;
the power of the first ultrasonic wave is 400W, and the power of the second ultrasonic wave is 800W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 6
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 90 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 30min, and the total heating and heat preservation time is 60min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 30 min; the rotation speed of the second stirring is 500r/min, and the time is 30 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 7
This example provides a sample preparation method of CrSi alloy suitable for ICP-OES, which is the same as example 6 except that the heating time is 40min and the heat preservation time is 20 min.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 8
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 100 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 10min, and the total heating and heat preservation time is 40min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 20 min; the rotation speed of the second stirring is 500r/min, and the time is 20 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the embodiment is clear and free of impurities, and the CrSi alloy target material is completely dissolved.
Example 9
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring is carried out during the heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min.
The sample solution obtained in this example is clear and free of impurities, and realizes complete dissolution of the CrSi alloy target, but the time for obtaining the clear and free of impurities in this example is slightly later than that in example 1.
Example 10
The embodiment provides a CrSi alloy sample preparation method suitable for ICP-OES, which comprises the following steps: mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution; the mass percentage of Cr in the CrSi alloy target material is 85 wt%;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
the heating and the heat preservation are accompanied by ultrasound; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the time of the first ultrasonic is 25 min; the time of the second ultrasonic is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in this example is clear and free of impurities, and realizes complete dissolution of the CrSi alloy target, but the time for obtaining the clear and free of impurities in this example is slightly later than that in example 1.
Comparative example 1
The comparative example provides a CrSi alloy sample preparation method, which comprises the following steps:
mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution;
the mixed acid is nitric acid and hydrofluoric acid which are formed in a volume ratio of 1:1, the concentration of the nitric acid is 37 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the comparative example contains solid residues, so that the CrSi alloy target cannot be completely dissolved, and the sample solution cannot be used for ICP-OES detection.
Comparative example 2
The comparative example provides a CrSi alloy sample preparation method, which comprises the following steps:
mixing a CrSi alloy target material and a mixed acid, heating to 95 ℃, and preserving heat, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution;
the mixed acid is hydrochloric acid and nitric acid which are formed in a volume ratio of 1:1, the concentration of the hydrochloric acid is 37 wt%, and the concentration of the nitric acid is 36 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the comparative example contains solid residues, so that the CrSi alloy target cannot be completely dissolved, and the sample solution cannot be used for ICP-OES detection.
Comparative example 3
The comparative example provides a CrSi alloy sample preparation method, which comprises the following steps:
mixing a CrSi alloy target material and hydrochloric acid, heating to 95 ℃, and keeping the temperature, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution;
the concentration of the hydrochloric acid is 37 wt%; the solid-liquid ratio of the CrSi alloy target material to hydrochloric acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the comparative example contains solid residues, so that the CrSi alloy target cannot be completely dissolved, and the sample solution cannot be used for ICP-OES detection.
Comparative example 4
The comparative example provides a CrSi alloy sample preparation method, which comprises the following steps:
mixing a CrSi alloy target material and hydrofluoric acid, heating to 95 ℃, and keeping the temperature, wherein the heating time is 30min, the heat preservation time is 20min, and the total heating and heat preservation time is 50min to obtain a sample solution;
the concentration of the hydrofluoric acid is 36 wt%; the solid-liquid ratio of the CrSi alloy target material to hydrofluoric acid is 1:80, and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 300r/min, and the time is 25 min; the rotation speed of the second stirring is 500r/min, and the time is 25 min;
the power of the first ultrasonic wave is 300W, and the power of the second ultrasonic wave is 600W.
The sample solution obtained in the comparative example contains solid residues, so that the CrSi alloy target cannot be completely dissolved, and the sample solution cannot be used for ICP-OES detection.
In conclusion, the sample preparation method provided by the invention is simple to operate, can realize the rapid dissolution of the CrSi alloy target material, and fills the sample preparation blank when the CrSi alloy target material is subjected to ICP-OES test; when the sample solution obtained by the sample preparation method is used for ICP-OES testing, the testing accuracy is high, errors caused by the use of mixed acid can be avoided, and the accuracy is high.
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 CrSi alloy sample preparation method suitable for ICP-OES is characterized by comprising the following steps: mixing a CrSi alloy target material and mixed acid, heating to 90-100 ℃, and preserving heat, wherein the total time of heating and heat preservation is 40-60min, so as to obtain a sample solution;
the mixed acid is hydrochloric acid and hydrofluoric acid which are composed of (1-3) to (1-3) in volume ratio, the concentration of the hydrochloric acid is 36-38 wt%, and the concentration of the hydrofluoric acid is 35-38 wt%.
2. The CrSi alloy sample preparation method according to claim 1, wherein a solid-to-liquid ratio of the CrSi alloy target material to the mixed acid is 1 (70-90), and a unit of the solid-to-liquid ratio is g/mL.
3. The CrSi alloy sample preparation method according to claim 1 or 2, wherein the mass percentage of Cr in the CrSi alloy target material is 83 to 86 wt%.
4. A CrSi alloy sample preparation method according to any one of claims 1 to 3, wherein said heating and holding are accompanied by stirring and/or sonication.
5. A CrSi alloy sample preparation method according to claim 4, wherein the stirring comprises a first stirring and a second stirring which are performed in this order;
preferably, the rotating speed of the first stirring is 200-400 r/min;
preferably, the rotation speed of the second stirring is 400-600 r/min.
6. The CrSi alloy sample preparation method according to claim 4 or 5, wherein the ultrasonication comprises a first ultrasonication and a second ultrasonication which are sequentially performed;
preferably, the power of the first ultrasonic wave is 200-;
preferably, the power of the second ultrasonic wave is 500-.
7. A CrSi alloy sample preparation method according to claim 6, wherein said first ultrasonic treatment is performed with first stirring, and said second ultrasonic treatment is performed with second stirring.
8. A CrSi alloy sample preparation method according to claim 7, characterized in that the time of the first stirring is 20-30 min;
preferably, the time of the second stirring is 20 to 30 min.
9. A CrSi alloy sample preparation method according to any one of claims 1 to 8, wherein the heating time is 30 to 40 min;
preferably, the time for heat preservation is 10-30 min.
10. A CrSi alloy sample preparation method according to any one of claims 1 to 9, comprising the steps of: mixing a CrSi alloy target material and a mixed acid, heating to 90-100 ℃, and preserving heat, wherein the heating time is 30-40min, the heat preservation time is 10-30min, and the total heating and heat preservation time is 40-60min to obtain a sample solution;
the mixed acid is hydrochloric acid and hydrofluoric acid which are formed by (1-3) to (1-3) in volume ratio, the concentration of the hydrochloric acid is 36-38 wt%, and the concentration of the hydrofluoric acid is 35-38 wt%;
the solid-liquid ratio of the CrSi alloy target material to the mixed acid is 1 (70-90), and the unit of the solid-liquid ratio is g/mL;
stirring and ultrasound are accompanied during heating and heat preservation; the stirring comprises a first stirring and a second stirring which are sequentially carried out; the ultrasound comprises a first ultrasound and a second ultrasound which are carried out in sequence; the first ultrasonic is carried out along with first stirring, and the second ultrasonic is carried out along with second stirring;
the rotating speed of the first stirring is 200-400r/min, and the time is 20-30 min; the rotation speed of the second stirring is 400-;
the power of the first ultrasonic wave is 200-400W, and the power of the second ultrasonic wave is 500-800W.
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