CN113237945A - Sample preparation method of high-purity indium in glow discharge mass spectrum - Google Patents
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- 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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Abstract
The invention relates to a sample preparation method of high-purity indium in glow discharge mass spectrometry, which comprises the following steps: firstly, tabletting a high-purity indium sample to obtain a high-purity indium sheet; and carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected. According to the sample preparation method of high-purity indium in the glow discharge mass spectrum, provided by the invention, the high-purity indium sample is subjected to tabletting and puncturing, and meanwhile, a specific three-step acid treatment process is adopted, so that the detection signal in the glow discharge mass spectrum is obviously enhanced, the detection signal is stable, the deviation in multiple detections is obviously reduced, and the detection precision is obviously improved.
Description
Technical Field
The invention relates to the field of glow discharge, in particular to a sample preparation method of high-purity indium in glow discharge mass spectrometry.
Background
Glow discharge mass spectrometry is an analysis method for mass spectrometry by connecting a glow discharge source as an ion source with a mass spectrometer, and has good analysis capability on solid metal samples.
For example, CN109192649A discloses a glow discharge mass spectrometer apparatus which can increase the intensity of an ion beam extracted without significantly changing the apparatus structure and driving conditions of a conventional glow discharge system, and which can achieve higher analysis accuracy. A circular and flat plate-shaped 1 st magnet is disposed between a flat plate-shaped solid sample and a plunger for holding the solid sample, a ring-shaped 2 nd magnet is disposed on an ion extraction side of a unit body forming a discharge region, the 2 nd magnet is disposed coaxially with the 1 st magnet so as to surround the discharge region, and the 1 st magnet and the 2 nd magnet are disposed so that magnetization directions are parallel to a direction in which an ion beam is extracted and magnetic poles face opposite directions to each other, whereby when glow discharge is generated in the discharge region, the intensity of the extracted ion beam is increased by a magnetic field formed by the 1 st magnet and the 2 nd magnet.
For example, CN112067391A discloses a device and a method for preparing a glow discharge sputtering sample for microscopic characterization of a material, the device comprises a glow discharge sputtering unit, a glow discharge energy supply source, an automatic gas circuit control unit, a spectrometer and a computer; the structure of the glow discharge sputtering unit is optimized through simulation so as to be more suitable for sample preparation, and a magnetic field is applied to glow plasma so as to realize uniform sample sputtering in a large-size range on the surface of a sample; the spectrometer is used for monitoring element spectrum signals in the sputtering depth direction of the sample so as to realize the accurate preparation of different layer tissue structures; and realizing the correspondence between the spatial coordinates of the sample preparation surface and the tissue structure by combining the acquisition of the sample position mark and the accurate spatial coordinate (x, y, z) information. The preparation method can realize the mm-cm level large-size flat preparation of the sample, has no damage to the tissue structure of the material, can prepare the sample layer by layer along the depth direction of the surface of the sample, and has the advantages of quick preparation and low cost.
However, in the prior art, when glow discharge is used for detecting a high-purity indium (not less than 5N) sample, the problems of poor detection signal, unstable signal and larger deviation of the detection result occur.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a sample preparation method for high-purity indium in glow discharge mass spectrometry, which solves the problems of poor detection signal, unstable signal and large deviation of detection result in the existing glow discharge mass spectrometry detection by adopting a specific sample treatment mode and a multi-stage acid treatment process, and realizes high-efficiency and high-precision detection of a high-purity indium sample.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a sample preparation method of high-purity indium in glow discharge mass spectrometry, which comprises the following steps:
firstly, tabletting a high-purity indium sample to obtain a high-purity indium sheet;
and carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected.
According to the sample preparation method of high-purity indium in the glow discharge mass spectrum, provided by the invention, the high-purity indium sample is subjected to tabletting and puncturing, and meanwhile, a specific three-step acid treatment process is adopted, so that the detection signal in the glow discharge mass spectrum is obviously enhanced, the detection signal is stable, the deviation in multiple detections is obviously reduced, and the detection precision is obviously improved.
In a preferred embodiment of the present invention, the tabletting treatment is performed by compressing a sample of high purity indium into a sheet having a thickness of 2 to 4mm, and may be, for example, 2mm, 2.1mm, 2.2mm, 2.3mm, 2.4mm, 2.5mm, 2.6mm, 2.7mm, 2.8mm, 2.9mm, 3mm, 3.1mm, 3.2mm, 3.3mm, 3.4mm, 3.5mm, 3.6mm, 3.7mm, 3.8mm, 3.9mm or 4mm, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, the punching process is performed by forming a hole of 0.01 to 0.2mm in the surface of the high purity indium sheet, and may be performed by, for example, 0.01mm, 0.02mm, 0.03mm, 0.04mm, 0.05mm, 0.07mm, 0.08mm, 0.09mm, 0.1mm, 0.11mm, 0.12mm, 0.13mm, 0.14mm, 0.15mm, 0.16mm, 0.17mm, 0.18mm, 0.19mm, or 0.2mm, but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
Preferably, the holes are uniformly distributed on the surface of the high-purity indium sheet.
Preferably, the distance between adjacent holes is 0.5-0.6mm, such as 0.5mm, 0.51mm, 0.52mm, 0.53mm, 0.54mm, 0.55mm, 0.56mm, 0.57mm, 0.58mm, 0.59mm or 0.6mm, but not limited to the values recited, and other values not recited in this range are equally applicable.
In a preferred embodiment of the present invention, the acid used in the first acid treatment is a mixed acid.
Preferably, the mixed acid is a mixed acid of nitric acid and hydrofluoric acid.
Preferably, the volume ratio of nitric acid to hydrofluoric acid in the mixed acid is (1-1.2):1, and may be, for example, 1:1, 1.01:1, 1.02:1, 1.03:1, 1.04:1, 1.05:1, 1.06:1, 1.07:1, 1.08:1, 1.09:1, 1:1.1, 1:1.11, 1:1.12, 1:1.13, 1:1.14, 1:1.15, 1:1.16, 1:1.17, 1:1.18, 1:1.19, or 1:1.2, and the like, but is not limited to the recited values, and other values not recited in this range are equally applicable.
In a preferred embodiment of the present invention, the time of the first acid treatment is 5 to 6min, for example, 5min, 5.1min, 5.2min, 5.3min, 5.4min, 5.5min, 5.6min, 5.7min, 5.8min, 5.9min, or 6min, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
In a preferred embodiment of the present invention, the acid used in the second acid treatment is nitric acid.
Preferably, the second acid treatment time is 3 to 4min, and may be, for example, 3min, 3.1min, 3.2min, 3.3min, 3.4min, 3.5min, 3.6min, 3.7min, 3.8min, 3.9min, or 4min, but is not limited to the values recited, and other values not recited in this range are also applicable.
Preferably, the second acid treatment is performed at least 2 times, for example, 2, 3, 4, or 5 times, etc., but is not limited to the recited values, and other values not recited within this range are equally applicable.
As a preferable embodiment of the present invention, the third acid treatment includes a nitric acid treatment and a mixed acid treatment which are sequentially performed.
Preferably, the nitric acid treatment is carried out for 2 to 3min, and may be, for example, 2min, 2.1min, 2.2min, 2.3min, 2.4min, 2.5min, 2.6min, 2.7min, 2.8min, 2.9min or 3min, but not limited to the values listed, and other values not listed in the range are also applicable.
In a preferred embodiment of the present invention, the acid used in the mixed acid treatment is a mixed acid of nitric acid and hydrofluoric acid in a volume ratio of 1 (0.7-0.9), and examples thereof include 1:0.7, 1:0.71, 1:0.72, 1:0.73, 1:0.74, 1:0.75, 1:0.76, 1:0.77, 1:0.78, 1:0.79, 1:0.8, 1:0.81, 1:0.82, 1:0.83, 1:0.84, 1:0.85, 1:0.86, 1:0.87, 1:0.88, 1:0.89, and 1:0.9, but are not limited thereto, and other values not listed in the range are also applicable.
Preferably, the time of the mixed acid treatment is 20 to 30 seconds, for example, 20s, 21s, 22s, 23s, 24s, 25s, 26s, 27s, 28s, 29s, or 30s, etc., but is not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred embodiment of the present invention, the rinsing includes water washing and ethanol washing performed in this order.
Preferably, the water wash is performed at least 3 times, for example, 3, 4, 5, or 6 times, etc., but is not limited to the recited values, and other values not recited within this range are equally applicable.
The frequency of the ethanol washing is not particularly limited, and can be reasonably set according to the washing process, so that no obvious water residue is left on the surface after the ethanol washing.
As a preferable embodiment of the present invention, the sample preparation method includes: firstly, tabletting a high-purity indium sample to obtain a high-purity indium sheet;
carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected;
the tabletting treatment is to press the high-purity indium sample into a thin sheet with the thickness of 2-4 mm;
the punching treatment is to arrange 0.01-0.2mm holes on the surface of the high-purity indium sheet, the holes are uniformly distributed on the surface of the high-purity indium sheet, and the distance between every two adjacent holes is 0.5-0.6 mm;
the acid used in the first acid treatment is mixed acid, the mixed acid is mixed acid of nitric acid and hydrofluoric acid, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is (1-1.2):1, and the time of the first acid treatment is 5-6 min;
the acid used in the second acid treatment is nitric acid, the time of the second acid treatment is 3-4min, and the second acid treatment is carried out at least 2 times;
the third acid treatment comprises nitric acid treatment and mixed acid treatment which are sequentially carried out, wherein the nitric acid treatment time is 2-3min, the acid adopted in the mixed acid treatment is the mixed acid of nitric acid and hydrofluoric acid with the volume ratio of 1 (0.7-0.9), and the mixed acid treatment time is 20-30 s;
the rinsing comprises water washing and ethanol washing which are carried out in sequence, wherein the water washing is carried out for at least 3 times.
In the invention, the reagents are all analytical pure reagents.
Compared with the prior art, the invention at least has the following beneficial effects:
according to the sample preparation method of high-purity indium in the glow discharge mass spectrum, provided by the invention, the high-purity indium sample is subjected to tabletting and puncturing, and meanwhile, a specific three-step acid treatment process is adopted, so that the detection signal in the glow discharge mass spectrum is obviously enhanced, the detection signal is stable, the deviation in multiple detections is obviously reduced, and the detection precision is obviously improved.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a sample preparation method of high-purity indium in glow discharge mass spectrometry, which comprises the steps of firstly carrying out tabletting treatment on a high-purity indium sample to obtain a high-purity indium sheet;
carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected;
the tabletting treatment is to press a high-purity indium sample into a thin sheet with the thickness of 3 mm;
the punching treatment is to arrange 0.1mm holes on the surface of the high-purity indium sheet;
the acid used in the first acid treatment is mixed acid, the mixed acid is mixed acid of nitric acid and hydrofluoric acid, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is 1.1:1, and the time of the first acid treatment is 5.5 min;
the acid used in the second acid treatment is nitric acid, the time of the second acid treatment is 3.5min, and the second acid treatment is carried out for 2 times;
the third acid treatment comprises nitric acid treatment and mixed acid treatment which are sequentially carried out, wherein the nitric acid treatment time is 2.5min, the acid adopted in the mixed acid treatment is the mixed acid of nitric acid and hydrofluoric acid with the volume ratio of 1:0.8, and the mixed acid treatment time is 25 s;
the rinsing comprises water washing and ethanol washing which are sequentially carried out, wherein the water washing is carried out for 3 times.
Example 2
The embodiment provides a sample preparation method of high-purity indium in glow discharge mass spectrometry, which comprises the steps of firstly carrying out tabletting treatment on a high-purity indium sample to obtain a high-purity indium sheet;
carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected;
the tabletting treatment is to press a high-purity indium sample into a sheet with the thickness of 2 mm;
the punching treatment is to arrange 0.2mm holes on the surface of the high-purity indium sheet;
the acid used in the first acid treatment is mixed acid, the mixed acid is mixed acid of nitric acid and hydrofluoric acid, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is 1:1, and the time of the first acid treatment is 6 min;
the acid used in the second acid treatment is nitric acid, the time of the second acid treatment is 3min, and the second acid treatment is carried out for 2 times;
the third acid treatment comprises nitric acid treatment and mixed acid treatment which are sequentially carried out, wherein the nitric acid treatment time is 3min, the acid adopted in the mixed acid treatment is the mixed acid of nitric acid and hydrofluoric acid with the volume ratio of 1:0.9, and the mixed acid treatment time is 30 s;
the rinsing comprises water washing and ethanol washing which are sequentially carried out, wherein the water washing is carried out for 3 times.
Example 3
The embodiment provides a sample preparation method of high-purity indium in glow discharge mass spectrometry, which comprises the steps of firstly carrying out tabletting treatment on a high-purity indium sample to obtain a high-purity indium sheet;
carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected;
the tabletting treatment is to press a high-purity indium sample into a thin sheet with the thickness of 4 mm;
the punching treatment is to arrange 0.01mm holes on the surface of the high-purity indium sheet;
the acid used in the first acid treatment is mixed acid, the mixed acid is mixed acid of nitric acid and hydrofluoric acid, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is 1.2:1, and the time of the first acid treatment is 5 min;
the acid used in the second acid treatment is nitric acid, the time of the second acid treatment is 4min, and the second acid treatment is carried out for 3 times;
the third acid treatment comprises nitric acid treatment and mixed acid treatment which are sequentially carried out, wherein the nitric acid treatment time is 2min, the acid adopted in the mixed acid treatment is the mixed acid of nitric acid and hydrofluoric acid with the volume ratio of 1:0.7, and the mixed acid treatment time is 20 s;
the rinsing comprises water washing and ethanol washing which are sequentially carried out, wherein the water washing is carried out for 3 times.
Comparative example 1
The difference from example 1 is only that the high purity indium sheet was not subjected to the piercing treatment.
Comparative example 2
The difference from example 1 is only that the diameter of the hole on the surface of the high purity indium sheet is 1 mm.
Comparative example 3
The difference from example 1 is only that the diameter of the hole on the surface of the high purity indium sheet is 0.001 mm.
Comparative example 4
The only difference from example 1 is that the first acid treatment was not performed.
Comparative example 5
The only difference from example 1 is that no second acid treatment was performed.
Comparative example 6
The only difference from example 1 is that the third acid treatment was not performed.
Comparative example 7
The only difference from example 1 is that the mixed acid in the first acid treatment was replaced with nitric acid.
Comparative example 8
The only difference from example 1 is that nitric acid in the second acid treatment is replaced with a mixed acid.
Comparative example 9
The only difference from example 1 is that the nitric acid treatment and the mixed acid treatment, which are sequentially performed in the third acid treatment, are replaced with the mixed acid treatment and the nitric acid treatment, which are sequentially performed.
Glow discharge mass spectrometry detection is carried out on the samples obtained in the above examples and comparative examples under the conditions of 1.2KV and 2mA current, and the detection results are detailed in Table 1.
TABLE 1
The duplicate tests in the above table are performed to test 10 samples from the same batch, i.e., 10 samples are obtained from one sample preparation.
According to the results of the embodiment and the comparative example, the high-efficiency detection of the high-purity indium sample is realized under the specific sample treatment means and the specific acid treatment, namely the sample preparation method of the high-purity indium in the glow discharge mass spectrum provided by the invention has the advantages that the high-purity indium sample is subjected to tabletting and pricking, and meanwhile, the specific three-step acid treatment process is adopted, so that the detection signal in the glow discharge mass spectrum is obviously enhanced, the detection signal is stable, the deviation in multiple detections is obviously reduced, and the detection precision is obviously improved.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A sample preparation method of high-purity indium in glow discharge mass spectrometry is characterized by comprising the following steps:
firstly, tabletting a high-purity indium sample to obtain a high-purity indium sheet;
and carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected.
2. A sample preparation method as claimed in claim 1, wherein the tabletting process is carried out by compressing a sample of high purity indium into a thin sheet having a thickness of 2-4 mm.
3. The sample preparation method as claimed in claim 1 or 2, wherein the punching treatment is to arrange 0.01-0.2mm holes on the surface of the high-purity indium sheet;
preferably, the holes are uniformly distributed on the surface of the high-purity indium sheet;
preferably, the distance between adjacent holes is 0.5-0.6 mm.
4. A sample preparation method as claimed in any one of claims 1 to 3, wherein the acid used in the first acid treatment is a mixed acid;
preferably, the mixed acid is a mixed acid of nitric acid and hydrofluoric acid;
preferably, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is (1-1.2): 1.
5. A sample preparation method as claimed in any one of claims 1 to 4, wherein the time of the first acid treatment is 5 to 6 min.
6. A sample preparation method as claimed in any one of claims 1 to 5, wherein the acid used in the second acid treatment is nitric acid;
preferably, the time for treating the second acid is 3-4 min;
preferably, the second acid treatment is performed at least 2 times.
7. The production method according to any one of claims 1 to 6, wherein the third acid treatment comprises a nitric acid treatment and a mixed acid treatment which are performed in this order;
preferably, the nitric acid treatment time is 2-3 min.
8. The preparation method according to claim 7, wherein the acid used in the mixed acid treatment is a mixed acid of nitric acid and hydrofluoric acid in a volume ratio of 1 (0.7-0.9);
preferably, the time of the mixed acid treatment is 20 to 30 s.
9. The production method according to any one of claims 1 to 8, wherein the rinsing comprises water washing and ethanol washing which are carried out in this order;
preferably, the water washing is performed at least 3 times.
10. The method of any one of claims 1 to 9, wherein the sample preparation method comprises:
firstly, tabletting a high-purity indium sample to obtain a high-purity indium sheet;
carrying out punching treatment on the high-purity indium sheet, and then sequentially carrying out first acid treatment, second acid treatment, third acid treatment and rinsing to obtain a high-purity indium sample to be detected;
the tabletting treatment is to press the high-purity indium sample into a thin sheet with the thickness of 2-4 mm;
the punching treatment is to arrange 0.01-0.2mm holes on the surface of the high-purity indium sheet, the holes are uniformly distributed on the surface of the high-purity indium sheet, and the distance between every two adjacent holes is 0.5-0.6 mm;
the acid used in the first acid treatment is mixed acid, the mixed acid is mixed acid of nitric acid and hydrofluoric acid, the volume ratio of the nitric acid to the hydrofluoric acid in the mixed acid is (1-1.2):1, and the time of the first acid treatment is 5-6 min;
the acid used in the second acid treatment is nitric acid, the time of the second acid treatment is 3-4min, and the second acid treatment is carried out at least 2 times;
the third acid treatment comprises nitric acid treatment and mixed acid treatment which are sequentially carried out, wherein the nitric acid treatment time is 2-3min, the acid adopted in the mixed acid treatment is the mixed acid of nitric acid and hydrofluoric acid with the volume ratio of 1 (0.7-0.9), and the mixed acid treatment time is 20-30 s;
the rinsing comprises water washing and ethanol washing which are carried out in sequence, wherein the water washing is carried out for at least 3 times.
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| CN115436460A (en) * | 2022-09-29 | 2022-12-06 | 宁波江丰电子材料股份有限公司 | Glow discharge mass spectrum detection method for tantalum powder |
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