Sample preparation method and detection method of glow discharge mass spectrometry titanium powder

Abstract

The invention relates to a glow discharge mass spectrometry titanium powder sample preparation method and a glow discharge mass spectrometry titanium powder detection method.The sample preparation method comprises the steps that a concave indium material to be treated is sequentially subjected to first acid pickling, first rinsing and first alcohol washing, and the concave indium material is obtained; and adding titanium powder into the concave indium material until the groove is filled, and then pressing to obtain the to-be-detected sample. According to the sample preparation method provided by the invention, sample preparation during glow discharge mass spectrometry detection of the titanium powder can be realized, the sample preparation process is efficient and rapid, meanwhile, a relatively strong signal can be obtained when the obtained sample is detected, the sensitivity is high, and the detection accuracy is high. And the detection result has good accuracy and precision.

Description

Technical Field

[0001] The invention relates to the field of detection and analysis, and in particular to a sample preparation method and a detection method for glow discharge mass spectrometry titanium powder. Background Art

[0002] At present, titanium powder is a widely used metal powder. It is an additive for powder metallurgy and alloy materials. It is also an important raw material for metal ceramics, surface coating agents, aluminum alloy additives, electric vacuum getters, spraying and plating. It is also used in aerospace, spraying, metallurgy, fireworks and other industries.

[0003] Material purity has an important influence on material properties, so the purity of titanium powder often needs to be tested before use.

[0004] For example, CN104807952A discloses a method for detecting the purity of titanium dioxide, comprising the following steps:

[0005] Step 1: weigh 1g of titanium dioxide powder, add 10mL of 70wt% concentrated sulfuric acid and 10g of ammonium nitrate, and heat while stirring until the solution becomes transparent, wherein the particle size of titanium dioxide is 20-100nm, and the titanium dioxide is pre-dried at a temperature greater than 800°C for 1 hour; Step 2: add 50mL of distilled water, 15mL of concentrated hydrochloric acid, and 1.5g of aluminum sheet; Step 3: then add an excess of saturated sodium bicarbonate solution to make the solution neutral; Step 4: quickly titrate the solution in step 3 with 0.1mol / L of ammonium ferric sulfate until the purple color disappears, then add 2-4mL of ammonium thiocyanate solution as an indicator, continue to titrate, and the solution becomes light red, and the purity of titanium dioxide is calculated based on the consumption of ammonium ferric sulfate.

[0006] However, the prior art still has the defects of low detection accuracy and low sensitivity in the process of detecting the purity of titanium powder. Summary of the invention

[0007] In view of the problems existing in the prior art, the purpose of the present invention is to provide a sample preparation method and a detection method for glow discharge mass spectrometry titanium powder to solve the defects of low detection accuracy and low sensitivity in the process of purity detection of titanium powder.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a method for preparing a sample of titanium powder for glow discharge mass spectrometry, the method comprising:

[0010] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0011] Titanium powder is added to the concave indium material until the groove is filled, and then pressed to obtain the sample to be tested.

[0012] The sample preparation method provided by the present invention can realize the sample preparation for glow discharge mass spectrometry detection of titanium powder. The sample preparation process is efficient and rapid. At the same time, when the obtained sample is detected, a strong signal can be obtained, the sensitivity is high, and the detection result has good accuracy and precision.

[0013] As a preferred technical solution of the present invention, the maximum equivalent circular diameter of the concave shape in the concave indium material is 0.7-0.8 mm.

[0014] Preferably, the depth of the concave shape in the concave indium material is 0.3-0.4 mm.

[0015] As a preferred technical solution of the present invention, the acid solution used in the first pickling includes a nitric acid solution.

[0016] Preferably, the mass concentration of the acid solution used in the first pickling is 50-65%.

[0017] Preferably, the first pickling time is 3-5 minutes.

[0018] As a preferred technical solution of the present invention, the medium used in the first rinsing includes water.

[0019] Preferably, the first rinsing time is ≥5 min.

[0020] Preferably, the first acid wash and first rinse cycles are performed at least 3 times.

[0021] Preferably, the medium used in the first alcohol wash comprises one or a combination of at least two of methanol, ethanol or propanol.

[0022] Preferably, the time of the first alcohol washing is ≥5 min.

[0023] As a preferred technical solution of the present invention, the material adding device used in adding titanium powder to the concave indium material until the groove is filled is sequentially subjected to mixed acid washing, a second rinsing and a second alcohol washing.

[0024] As a preferred technical solution of the present invention, the mixed acid used in the mixed pickling comprises concentrated nitric acid with a mass ratio of 1:(1-1.2) and hydrofluoric acid with a mass concentration of 30-50%.

[0025] Preferably, the mixed pickling time is 3-5 minutes.

[0026] Preferably, the second rinsing medium comprises water.

[0027] Preferably, the second rinsing time is ≥5 min.

[0028] Preferably, the second rinsing is performed at least 3 times.

[0029] Preferably, the medium used in the second alcohol wash comprises one or a combination of at least two of methanol, ethanol or propanol.

[0030] Preferably, the second alcohol washing time is ≥10 min.

[0031] As a preferred technical solution of the present invention, the pressing pressure is 10-15 MPa.

[0032] Preferably, the holding time of the pressing is 10-12 minutes.

[0033] In a second aspect, the present invention provides a method for detecting titanium powder by glow discharge mass spectrometry, the detection method comprising performing glow discharge mass spectrometry detection on the sample to be tested obtained in the first aspect to obtain titanium powder detection data.

[0034] As a preferred technical solution of the present invention, in the glow discharge mass spectrometry detection, sputtering is started after cooling for 10-15 minutes.

[0035] As a preferred technical solution of the present invention, the sputtering voltage in the glow discharge mass spectrometry detection is 1.5-2 kV.

[0036] Preferably, the sputtering current in the glow discharge mass spectrometry detection is 3-5 mA.

[0037] Preferably, the instrument resolution in the glow discharge mass spectrometry detection is 3600-4000.

[0038] Compared with the prior art solutions, the present invention has the following beneficial effects:

[0039] The preparation method provided by the present invention can complete the sample preparation of titanium powder, and the introduction of impurities is avoided as much as possible during the sample preparation process, thereby shortening the analysis time and ensuring the accuracy of the data; using the above test parameters, a stronger signal can be obtained with high sensitivity; the detection result has good accuracy and precision, the detection accuracy deviation is ≤0.005%, and the relative standard deviation is ≤0.000748%. DETAILED DESCRIPTION

[0040] To better illustrate the present invention and facilitate understanding of the technical solution of the present invention, typical but non-limiting embodiments of the present invention are as follows:

[0041] This embodiment provides a method for preparing a sample of titanium powder for glow discharge mass spectrometry, the method comprising:

[0042] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0043] Titanium powder is added to the concave indium material until the groove is filled, and then pressed to obtain the sample to be tested.

[0044] Specifically, the maximum equivalent circular diameter of the concave shape in the concave indium material is 0.7-0.8 mm, for example, it can be 0.7 mm, 0.71 mm, 0.72 mm, 0.73 mm, 0.74 mm, 0.75 mm, 0.76 mm, 0.77 mm, 0.78 mm, 0.79 mm or 0.8 mm, etc., but is not limited to the listed values, and other values ​​not listed within the range also meet the requirements.

[0045] Specifically, the depth of the concave shape in the concave indium material is 0.3-0.4 mm, for example, it can be 0.3 mm, 0.31 mm, 0.32 mm, 0.33 mm, 0.34 mm, 0.35 mm, 0.36 mm, 0.37 mm, 0.38 mm, 0.39 mm or 0.4 mm, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0046] In the present invention, the concave shape of the concave indium material can be a cylinder, a cone, a hemisphere, etc. If it is a cone, the maximum equivalent circular diameter of the concave shape is the bottom circular diameter of the cone, and the depth of the concave shape is the height of the cone.

[0047] Specifically, the acid solution used in the first pickling includes a nitric acid solution.

[0048] Specifically, the mass concentration of the acid solution used in the first pickling is 50-65%, for example, it can be 50%, 52%, 54%, 56%, 58%, 60%, 62%, 64% or 65%, etc., but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0049] In the present invention, the concave indium material can be kept immersed in the acid solution for cleaning during the pickling process without any restriction on the solid-liquid ratio.

[0050] Specifically, the first pickling time is 3-5 min, for example, it can be 3 min, 3.2 min, 3.4 min, 3.6 min, 3.8 min, 4 min, 4.2 min, 4.4 min, 4.6 min, 4.8 min or 5 min, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0051] Specifically, the medium used in the first rinsing includes water.

[0052] Specifically, the time for the first rinsing is ≥5 min, for example, it can be 5 min, 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 50 min or 60 min, etc., but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0053] Specifically, the first pickling and first rinsing cycles are performed at least 3 times; that is, pickling is performed once and then rinsing is performed, then pickling is performed and then rinsing is performed, and then pickling is performed and then rinsing is performed, which is performed 3 times, and more times can be deduced in the same way, and then the first alcohol wash is performed.

[0054] Specifically, the medium used in the first alcohol wash includes one or a combination of at least two of methanol, ethanol or propanol;

[0055] Specifically, the time for the first alcohol wash is ≥5 min, for example, it can be 5 min, 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 50 min or 60 min, etc., but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0056] In the present invention, titanium powder is added to the concave indium material until the groove is filled, and the material adding device used is sequentially subjected to mixed acid washing, a second rinsing and a second alcohol washing.

[0057] In the present invention, the material adding device used includes a medicine spoon and other equipment commonly used in the art for adding powder.

[0058] Specifically, the mixed acid used in the mixed pickling includes concentrated nitric acid with a mass ratio of 1:(1-1.2) and hydrofluoric acid with a mass concentration of 30-50%, for example, it can be 1:1, 1:1.02, 1:1.04, 1:1.06, 1:1.08, 1:1.1, 1:1.12, 1:1.14, 1:1.16, 1:1.18 or 1:1.2, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0059] Specifically, the mixed pickling time is 3-5 min, for example, it can be 3 min, 3.2 min, 3.4 min, 3.6 min, 3.8 min, 4 min, 4.2 min, 4.4 min, 4.6 min, 4.8 min or 5 min, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0060] Specifically, the second rinsing medium includes water;

[0061] Specifically, the second rinsing time is ≥5 min, for example, it can be 5 min, 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 50 min or 60 min, etc., but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0062] Specifically, the second rinsing is performed at least 3 times, for example, 3 times, 4 times or 5 times, etc., but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0063] Specifically, the medium used in the second alcohol wash includes one or a combination of at least two of methanol, ethanol or propanol;

[0064] Specifically, the time for the second alcohol wash is ≥10 min, for example, it can be 10 min, 15 min, 20 min, 25 min, 30 min, 35 min, 40 min, 50 min or 60 min, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0065] Specifically, the pressing pressure is 10-15MPa, for example, it can be 10MPa, 10.5MPa, 11MPa, 11.5MPa, 12MPa, 12.5MPa, 13MPa, 13.5MPa, 14MPa, 14.5MPa or 15MPa, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0066] Specifically, the holding time of the pressing is 10-12min, for example, it can be 10min, 10.2min, 10.4min, 10.6min, 10.8min, 11min, 11.2min, 11.4min, 11.6min, 11.8min or 12min, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0067] In the present invention, the pressing method includes cold pressing, etc., which is a commonly used pressing method in the art.

[0068] Furthermore, the present invention provides a method for detecting titanium powder by glow discharge mass spectrometry, the method comprising performing glow discharge mass spectrometry detection on the sample to be detected to obtain titanium powder detection data.

[0069] Specifically, in the glow discharge mass spectrometry detection, sputtering is started after cooling for 10-15 minutes, for example, it can be 10 minutes, 10.5 minutes, 11 minutes, 11.5 minutes, 12 minutes, 12.5 minutes, 13 minutes, 13.5 minutes, 14 minutes, 14.5 minutes or 15 minutes, but is not limited to the listed values, and other values ​​not listed in the range also meet the requirements.

[0070] Specifically, the sputtering voltage in the glow discharge mass spectrometry detection is 1.5-2kV, for example, it can be 1.5kV, 1.55kV, 1.6kV, 1.65kV, 1.7kV, 1.75kV, 1.8kV, 1.85kV, 1.9kV, 1.95kV or 2kV, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0071] Specifically, the sputtering current in the glow discharge mass spectrometry detection is 3-5 mA, for example, it can be 3 mA, 3.2 mA, 3.4 mA, 3.6 mA, 3.8 mA, 4 mA, 4.2 mA, 4.4 mA, 4.6 mA, 4.8 mA or 5 mA, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0072] Specifically, the instrument resolution in the glow discharge mass spectrometry detection is 3600-4000, for example, it can be 3600, 3650, 3700, 3750, 3800, 3850, 3900, 3950 or 4000, but is not limited to the listed values, and other unlisted values ​​within the range also meet the requirements.

[0073] Further, in order to illustrate the excellent effect of the method for preparing a sample of titanium powder for glow discharge mass spectrometry provided by the present invention, a corresponding description is given using an actual embodiment, as follows:

[0074] Example 1

[0075] This embodiment provides a sample preparation and detection process of titanium powder for glow discharge mass spectrometry, which is as follows:

[0076] Sample preparation methods include:

[0077] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0078] Add titanium powder to the concave indium material until the groove is filled, and then press it to obtain a sample to be tested;

[0079] Among them, the maximum circular diameter of the concave shape (conical concave shape) in the concave indium material is 0.74mm; the depth of the concave shape in the concave indium material is 0.36mm; the acid solution used in the first pickling is a nitric acid solution; the mass concentration of the acid solution used in the first pickling is 55%; the time of the first pickling is 4.5min; the medium used in the first rinsing is water; the time of the first rinsing is 5min; the first pickling and the first rinsing are cycled 3 times; the medium used in the first alcohol washing is ethanol; the time of the first alcohol washing is 8min;

[0080] The material adding apparatus used in adding titanium powder to the concave indium material until the groove is filled performs mixed pickling, second rinsing and second alcohol washing in sequence; the mixed acid used in the mixed pickling is concentrated nitric acid with a mass ratio of 1:1.1 and hydrofluoric acid with a mass concentration of 40%; the time of the mixed pickling is 3.5 minutes; the medium used in the second rinsing is water; the time of the second rinsing is 8 minutes; the second rinse is performed 4 times; the medium used in the second alcohol washing is propylene glycol; the time of the second alcohol washing is 15 minutes.

[0081] The pressing pressure is 14 MPa; the holding time of the pressing is 12 min;

[0082] Detection methods include:

[0083] The sample to be tested is subjected to glow discharge mass spectrometry detection to obtain titanium powder detection data;

[0084] In the glow discharge mass spectrometry detection, sputtering is started after cooling for 14 minutes;

[0085] The sputtering voltage in the glow discharge mass spectrometry detection is 1.8 kV;

[0086] The sputtering current in the glow discharge mass spectrometry detection is 4 mA;

[0087] The instrument resolution in the glow discharge mass spectrometry detection is 3800.

[0088] Example 2

[0089] This embodiment provides a sample preparation and detection process of titanium powder for glow discharge mass spectrometry, which is as follows:

[0090] Sample preparation methods include:

[0091] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0092] Add titanium powder to the concave indium material until the groove is filled, and then press it to obtain a sample to be tested;

[0093] Among them, the circular diameter of the concave shape (cylindrical concave shape) in the concave indium material is 0.77mm; the depth of the concave shape in the concave indium material is 0.33mm; the acid solution used in the first pickling is a nitric acid solution; the mass concentration of the acid solution used in the first pickling is 60%; the time of the first pickling is 4min; the medium used in the first rinsing is water; the time of the first rinsing is 8min; the first pickling and the first rinsing cycle are performed 4 times; the medium used in the first alcohol washing is ethanol; the time of the first alcohol washing is 10min;

[0094] The material adding apparatus used in adding titanium powder to the concave indium material until the groove is filled performs mixed pickling, second rinsing and second alcohol washing in sequence; the mixed acid used in the mixed pickling is concentrated nitric acid with a mass ratio of 1:1.2 and hydrofluoric acid with a mass concentration of 45%; the time of the mixed pickling is 4 minutes; the medium used in the second rinsing is water; the time of the second rinsing is 10 minutes; the second rinse is performed 3 times; the medium used in the second alcohol washing is methanol; the time of the second alcohol washing is 10 minutes.

[0095] The pressing pressure is 12 MPa; the holding time of the pressing is 11 min;

[0096] Detection methods include:

[0097] The sample to be tested is subjected to glow discharge mass spectrometry detection to obtain titanium powder detection data;

[0098] In the glow discharge mass spectrometry detection, sputtering is started after cooling for 12 minutes;

[0099] The sputtering voltage in the glow discharge mass spectrometry detection is 1.7 kV;

[0100] The sputtering current in the glow discharge mass spectrometry detection is 3.5 mA;

[0101] The instrument resolution in the glow discharge mass spectrometry detection is 3700.

[0102] Example 3

[0103] This embodiment provides a sample preparation and detection process of titanium powder for glow discharge mass spectrometry, which is as follows:

[0104] Sample preparation methods include:

[0105] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0106] Add titanium powder to the concave indium material until the groove is filled, and then press it to obtain a sample to be tested;

[0107] Among them, the bottom circle diameter of the concave shape (conical concave shape) in the concave indium material is 0.8mm; the depth of the concave shape in the concave indium material is 0.3mm; the acid solution used in the first pickling is a nitric acid solution; the mass concentration of the acid solution used in the first pickling is 50%; the time of the first pickling is 5min; the medium used in the first rinsing is water; the time of the first rinsing is 20min; the first pickling and the first rinsing are cycled 3 times; the medium used in the first alcohol washing is ethanol; the time of the first alcohol washing is 15min;

[0108] The material adding apparatus used in adding titanium powder to the concave indium material until the groove is filled performs mixed pickling, second rinsing and second alcohol washing in sequence; the mixed acid used in the mixed pickling is concentrated nitric acid with a mass ratio of 1:1.2 and hydrofluoric acid with a mass concentration of 30%; the time of the mixed pickling is 5 minutes; the medium used in the second rinsing is water; the time of the second rinsing is 15 minutes; the second rinse is performed 3 times; the medium used in the second alcohol washing is ethanol; the time of the second alcohol washing is 10 minutes.

[0109] The pressing pressure is 15 MPa; the holding time of the pressing is 10 min;

[0110] Detection methods include:

[0111] The sample to be tested is subjected to glow discharge mass spectrometry detection to obtain titanium powder detection data;

[0112] In the glow discharge mass spectrometry detection, sputtering is started after cooling for 10 minutes;

[0113] The sputtering voltage in the glow discharge mass spectrometry detection is 1.5 kV;

[0114] The sputtering current in the glow discharge mass spectrometry detection is 3 mA;

[0115] The instrument resolution in the glow discharge mass spectrometry detection is 4000.

[0116] Example 4

[0117] This embodiment provides a sample preparation and detection process of titanium powder for glow discharge mass spectrometry, which is as follows:

[0118] Sample preparation methods include:

[0119] The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material;

[0120] Add titanium powder to the concave indium material until the groove is filled, and then press it to obtain a sample to be tested;

[0121] Among them, the bottom circle diameter of the concave shape (conical concave shape) in the concave indium material is 0.7mm; the depth of the concave shape in the concave indium material is 0.4mm; the acid solution used in the first pickling is a nitric acid solution; the mass concentration of the acid solution used in the first pickling is 65%; the time of the first pickling is 3min; the medium used in the first rinsing is water; the time of the first rinsing is 15min; the first pickling and the first rinsing are cycled 5 times; the medium used in the first alcohol washing is ethanol; the time of the first alcohol washing is 10min;

[0122] The material adding apparatus used in adding titanium powder to the concave indium material until the groove is filled performs mixed pickling, second rinsing and second alcohol washing in sequence; the mixed acid used in the mixed pickling is concentrated nitric acid with a mass ratio of 1:1 and hydrofluoric acid with a mass concentration of 50%; the time of the mixed pickling is 3 minutes; the medium used in the second rinsing is water; the time of the second rinsing is 10 minutes; the second rinse is performed 5 times; the medium used in the second alcohol washing is propylene glycol; the time of the second alcohol washing is 20 minutes.

[0123] The pressing pressure is 10 MPa; the holding time of the pressing is 12 min;

[0124] Detection methods include:

[0125] The sample to be tested is subjected to glow discharge mass spectrometry detection to obtain titanium powder detection data;

[0126] In the glow discharge mass spectrometry detection, sputtering is started after cooling for 15 minutes;

[0127] The sputtering voltage in the glow discharge mass spectrometry detection is 2 kV;

[0128] The sputtering current in the glow discharge mass spectrometry detection is 5 mA;

[0129] The instrument resolution in the glow discharge mass spectrometry detection is 3600.

[0130] Comparative Example 1

[0131] The only difference from Example 1 is that titanium powder is directly used for glow discharge mass spectrometry detection.

[0132] Comparative Example 2

[0133] The only difference from Example 1 is that the first acid wash is not performed.

[0134] Comparative Example 3

[0135] The only difference from Example 1 is that mixed pickling is not performed.

[0136] Comparative Example 4

[0137] The only difference from Example 1 is that the sputtering voltage is 2.5 kV.

[0138] Comparative Example 5

[0139] The only difference from Example 1 is that the sputtering voltage is 1 kV.

[0140] Comparative Example 6

[0141] The only difference from Example 1 is that the sputtering current is 2 mA.

[0142] Comparative Example 7

[0143] The only difference from Example 1 is that the sputtering current is 7 mA.

[0144] Test and results:

[0145] 1. Accuracy experiment

[0146] The accuracy of the detection methods provided in Examples 1-4 and Comparative Examples 1-7 was evaluated by comparing the measured values ​​of standard sample A with the certified values.

[0147] The content of the standard sample and the test results are shown in Table 1

[0148] Table 1

[0149]

[0150]

[0151] 2. Precision experiment

[0152] The detection methods provided in Examples 1-4 and Comparative Examples 1-7 were evaluated through precision tests, and the unknown sample 1# was tested repeatedly 5 times.

[0153] The test results are shown in Table 2.

[0154] Table 2

[0155]

[0156]

[0157] According to the results of the above embodiments and comparative examples, the sample preparation method provided by the present invention can be used to prepare samples for glow discharge mass spectrometry detection of titanium powder. The sample preparation process is efficient and rapid. At the same time, a strong signal can be obtained when the obtained sample is detected. The sensitivity is high, and the detection results have good accuracy and precision.

[0158] It is stated 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 rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the components selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0159] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0160] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0161] In addition, various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A method for preparing a sample of titanium powder for glow discharge mass spectrometry, characterized in that: The sample preparation method comprises: The concave indium material to be processed is sequentially subjected to a first acid wash, a first rinse and a first alcohol wash to obtain a concave indium material; Titanium powder is added to the concave indium material until the groove is filled, and then pressed to obtain the sample to be tested.

2. The sample preparation method according to claim 1, characterized in that: The maximum equivalent circular diameter of the concave shape in the concave indium material is 0.7-0.8 mm; Preferably, the depth of the concave shape in the concave indium material is 0.3-0.4 mm.

3. The sample preparation method according to claim 1 or 2, characterized in that: The acid solution used in the first pickling comprises a nitric acid solution; Preferably, the mass concentration of the acid solution used in the first pickling is 50-65%; Preferably, the first pickling time is 3-5 minutes.

4. The sample preparation method according to any one of claims 1 to 3, characterized in that: The medium used in the first rinsing includes water; Preferably, the first rinsing time is ≥5 min; Preferably, the first pickling and first rinsing cycles are performed at least 3 times; Preferably, the medium used in the first alcohol wash comprises one or a combination of at least two of methanol, ethanol or propanol; Preferably, the time of the first alcohol washing is ≥5 min.

5. The sample preparation method according to any one of claims 1 to 4, characterized in that: The material adding device used in the process of adding titanium powder to the concave indium material until the concave groove is filled is sequentially subjected to mixed acid washing, a second rinsing and a second alcohol washing.

6. The sample preparation method according to claim 5, characterized in that: The mixed acid used in the mixed pickling comprises concentrated nitric acid with a mass ratio of 1:(1-1.2) and hydrofluoric acid with a mass concentration of 30-50%; Preferably, the mixed pickling time is 3-5min; Preferably, the second rinsing medium comprises water; Preferably, the second rinsing time is ≥5 min; Preferably, the second rinsing is performed at least 3 times; Preferably, the medium used in the second alcohol wash comprises one or a combination of at least two of methanol, ethanol or propanol; Preferably, the second alcohol washing time is ≥10 min.

7. The sample preparation method according to any one of claims 1 to 6, characterized in that: The pressing pressure is 10-15MPa; Preferably, the holding time of the pressing is 10-12 minutes.

8. A method for detecting titanium powder by glow discharge mass spectrometry, characterized in that: The detection method comprises performing glow discharge mass spectrometry detection on the sample to be tested as described in any one of claims 1 to 7 to obtain titanium powder detection data.

9. The detection method according to claim 8, characterized in that: In the glow discharge mass spectrometry detection, sputtering is started after cooling for 10-15 minutes.

10. The detection method according to claim 8 or 9, characterized in that: The sputtering voltage in the glow discharge mass spectrometry detection is 1.5-2 kV; Preferably, the sputtering current in the glow discharge mass spectrometry detection is 3-5 mA; Preferably, the instrument resolution in the glow discharge mass spectrometry detection is 3600-4000.

Images