Method for digesting WMo alloy and application of method in ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer) test of WMo alloy

Abstract

The invention provides a method for digesting a WMo alloy and application of the method in ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer) testing of the WMo alloy. The method comprises the following steps: mixing WMo alloy, HF, HNO3 and HCl, and carrying out digestion treatment to obtain a digestion solution; wherein the volume ratio of the HF to the HNO3 to the HCl is (3 to 6): (1.5 to 2.5): (0.5 to 1). According to the method provided by the invention, not only can single metal be dissolved, but also WMo alloy can be directly dissolved, the effect of full dissolution can be achieved, and the detection standard of ICP-OES on a machine is achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of element detection, and particularly relates to a method for digesting a WMo alloy and an application of the method in ICP-OES testing of the WMo alloy. Background Art

[0002] Tungsten-molybdenum alloy refers to an alloy composed of tungsten and molybdenum, which can be used in high-temperature environments without being easily melted, and is suitable for high-temperature application scenarios such as heating elements of high-temperature furnaces. The tungsten content in commonly used tungsten-molybdenum alloys is 30% to 50% (mass). At room temperature, WMo alloy has high strength and hardness. This high strength and hardness enable the alloy to be used to manufacture wear-resistant parts, such as the cutter head part of high-speed cutting tools, which can maintain a good shape and the sharpness of the cutting edge when processing high-hardness materials. Secondly, WMo alloy can effectively conduct heat and has advantages in applications with high heat dissipation requirements. In addition, the thermal expansion coefficient of WMo alloy is low, a feature that enables the alloy to maintain relative dimensional stability in environments with large temperature changes.

[0003] The commonly used WMo testing equipment is ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometer). ICP-OES has less interference, stable signal, and simple operation. Before testing, it only needs to be dissolved with acid and then tested on the machine. However, there are currently only methods for dissolving single metals of W and Mo, and no method for dissolving WMo alloys.

[0004] Therefore, it is urgent to design a dissolution method for WMo alloy so as to detect both W and Mo elements at the same time. Summary of the invention

[0005] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for dissolving WMo alloy and its application in ICP-OES testing of WMo alloy. The method provided by the present invention can not only dissolve a single metal, but also directly dissolve WMo alloy, and can achieve a sufficient dissolution effect to meet the detection standard of ICP-OES.

[0006] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a method for digesting a WMo alloy, the method comprising the following steps:

[0008] WMo alloy, HF, HNO 3 and HCl, and perform digestion treatment to obtain a digestion solution;

[0009] Among them, HF, HNO 3 The volume ratio of HCl is (3-6):(1.5-2.5):(0.5-1).

[0010] The present invention uses a specific combination of three acid solutions, so that it can not only dissolve a single metal, but also directly dissolve the WMo alloy, and can achieve a full dissolution effect to meet the detection standard of the ICP-OES machine.

[0011] In the present invention, HF, HNO 3 The volume ratio of HF to HCl is (3-6):(1.5-2.5):(0.5-1). The volume ratio of the three can be any ratio that satisfies this range. For example, the volume of HF can be any ratio within the range of 3-6, such as 3, 4, 5, 5.5 or 6, etc., and the volume of HNO 3 The volume ratio of HF and HNO can be any ratio in the range of 1.5-2.5, such as 1.5, 1.75, 2, 2.25 or 2.5, and the volume ratio of HCl can be any ratio in the range of 0.5-1, such as 0.5, 0.6, 0.7, 0.8, 0.9 or 1. Within the above suitable volume ratio range, the WMo alloy can be dissolved quickly. 3 If the volume ratio of HNO is too large or too small, the WMo alloy will not be completely dissolved. 3 If the volume ratio of HCl is too large or too small, a precipitate will form.

[0012] Preferably, the concentration of HF is 38-42wt%, for example, 38wt%, 39wt%, 40wt%, 41wt% or 42wt%, etc. The above concentration of HF is used in the present invention to accelerate the dissolution of WMo alloy.

[0013] Preferably, the HNO 3 The concentration of HNO is 65-68wt%, for example, 65wt%, 66wt%, 67wt% or 68wt%. 3 It helps to accelerate the dissolution of WMo alloy.

[0014] Preferably, the concentration of HCl is 36.5-38.5 wt%, for example, 36.5 wt%, 37.5 wt% or 38.5 wt%, etc. The use of HCl of the above concentration in the present invention is conducive to the dissolution of precipitation.

[0015] Preferably, the HF, HNO 3 The total volume of HCl is V 酸 The mass of the WMo alloy is recorded as M, M:V 酸=(0.05-0.2)g:(2.5-4)mL, the mass volume ratio of the two can be any ratio that satisfies this range. For example, the mass of the WMo alloy can be any ratio within the range of (0.05-0.2)g, such as 0.05g, 0.1g, 0.15g or 0.2g, etc., and the mass volume ratio of HF and HNO 3 The total volume of HF, HNO and HCl can be any ratio within the range of (2.5-4) mL, for example, 2.5 mL, 3 mL, 3.5 mL or 4 mL. The present invention defines the mass of WMo alloy and the mass of HF, HNO 3 When the total volume of HCl is within the above range, the alloy can be fully dissolved, making the subsequent element detection more accurate.

[0016] Preferably, the digestion process is accompanied by stirring, and the purpose of stirring is to make the WMo alloy dissolve more thoroughly.

[0017] Preferably, the stirring rate is 800-1200 rpm, for example, 800 rpm, 900 rpm, 1000 rpm, 1100 rpm or 1200 rpm.

[0018] Preferably, the temperature of the digestion treatment is 60-80°C, for example, 60°C, 65°C, 70°C, 75°C or 80°C.

[0019] In the present invention, a suitable digestion temperature is helpful to fully and quickly dissolve the WMo alloy. If the temperature of the digestion treatment is too low, the dissolution is incomplete; if the temperature of the digestion treatment is too high, the test element volatilizes.

[0020] Preferably, the digestion treatment time is 20-40 min, for example, it can be 20 min, 25 min, 30 min, 35 min or 40 min.

[0021] In the present invention, the appropriate digestion treatment time can fully and quickly dissolve the WMo alloy. If the digestion treatment time is too short, the dissolution is incomplete; if the digestion treatment time is too long, the test element volatilizes.

[0022] Preferably, the method comprises the following steps:

[0023] (1) Mix HF and HNO in a volume ratio of (3-6):(1.5-2.5):(0.5-1) 3 and HCl to obtain a composite acid solution.

[0024] Among them, the concentration of HF is 38-42wt%, HNO 3 The concentration of is 65-68wt%, and the concentration of HCl is 36.5-38.5wt%.

[0025] (2) The WMo alloy and the composite acid solution are stirred and mixed according to a mass volume ratio of (0.05-0.2) g:(2.5-4) mL, and digested on a graphite heater at 60-80° C. for 20-40 min to obtain a clear and transparent digestion solution.

[0026] In a second aspect, the present invention provides an application of the method described in the first aspect in ICP-OES testing of WMo alloy.

[0027] Preferably, the specific steps of the application include:

[0028] The digestion solution was fixed to volume, and then the fixed-volume digestion solution was placed in an ICP-OES device to simultaneously detect the W element and the Mo element.

[0029] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] The present invention uses a specific combination of three acid solutions, so that it can not only dissolve a single metal, but also directly dissolve the WMo alloy, and can achieve a full dissolution effect to meet the detection standard of the ICP-OES machine. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is a process flow chart for digesting WMo alloy provided in Example 1 of the present invention. DETAILED DESCRIPTION

[0033] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0034] It should be noted that the composition contents of the WMo alloy used in the following embodiments are as follows:

[0035] W is 75 wt% and Mo is 25 wt%.

[0036] Example 1

[0037] This embodiment provides a method for digesting WMo alloy, and its process flow chart is as follows: Figure 1 As shown, the method comprises the following steps:

[0038] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3and HCl to obtain a composite acid solution.

[0039] The concentration of HF is 40wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0040] (2) The WMo alloy and the composite acid solution were stirred and mixed in a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 15 min to obtain a clear and transparent digestion solution.

[0041] Example 2

[0042] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0043] (1) Mix HF and HNO in a volume ratio of 5:2:0.5. 3 and HCl to obtain a composite acid solution.

[0044] The concentration of HF is 41wt%, HNO 3 The concentration of N is 67 wt %, and the concentration of HCl is 37 wt %.

[0045] (2) The WMo alloy and the composite acid solution were stirred and mixed at a mass volume ratio of 0.1 g:3 mL, and digested on a graphite heater at 50° C. for 30 min to obtain a clear and transparent digestion solution.

[0046] Example 3

[0047] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0048] (1) Mix HF and HNO in a volume ratio of 4:2.5:1. 3 and HCl to obtain a composite acid solution.

[0049] Among them, the concentration of HF is 39wt%, HNO 3 The concentration of is 66.5 wt %, and the concentration of HCl is 38 wt %.

[0050] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:2.5 mL, and digested on a graphite heater at 70° C. for 20 min to obtain a clear and transparent digestion solution.

[0051] Example 4

[0052] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0053] (1) Mix HF and HNO in a volume ratio of 3:1.5:1. 3 and HCl to obtain a composite acid solution.

[0054] The concentration of HF is 38 wt%, HNO 3 The concentration of is 65 wt %, and the concentration of HCl is 36.5 wt %.

[0055] (2) The WMo alloy and the composite acid solution were stirred and mixed at a mass volume ratio of 0.1 g:4 mL, and digested on a graphite heater at 80° C. for 15 min to obtain a clear and transparent digestion solution.

[0056] Example 5

[0057] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0058] (1) Mix HF and HNO in a volume ratio of 6:2.5:1. 3 and HCl to obtain a composite acid solution.

[0059] Among them, the concentration of HF is 42wt%, HNO 3 The concentration of is 68 wt %, and the concentration of HCl is 38.5 wt %.

[0060] (2) The WMo alloy and the composite acid solution were stirred and mixed in a mass volume ratio of 0.2 g:2.5 mL, and digested on a graphite heater at 100° C. for 15 min to obtain a clear and transparent digestion solution.

[0061] Example 6

[0062] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0063] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0064] The concentration of HF is 36wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0065] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0066] Example 7

[0067] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0068] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0069] The concentration of HF is 45wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0070] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0071] Example 8

[0072] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0073] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0074] The concentration of HF is 40wt%, HNO 3 The concentration of is 63 wt %, and the concentration of HCl is 37.5 wt %.

[0075] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0076] Example 9

[0077] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0078] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0079] The concentration of HF is 40wt%, HNO 3 The concentration of is 70 wt %, and the concentration of HCl is 37.5 wt %.

[0080] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0081] Example 10

[0082] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0083] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0084] The concentration of HF is 40wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 36 wt %.

[0085] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0086] Embodiment 11

[0087] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0088] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0089] The concentration of HF is 40wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 39 wt %.

[0090] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0091] Example 12

[0092] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0093] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0094] The concentration of HF is 40wt%, HNO 3 The concentration of is 33 wt %, and the concentration of HCl is 37.5 wt %.

[0095] (2) The WMo alloy and the composite acid solution were stirred and mixed in a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 40° C. for 15 min to obtain a clear and transparent digestion solution.

[0096] Example 13

[0097] This embodiment provides a method for digesting WMo alloy, the method comprising the following steps:

[0098] (1) Mix HF and HNO in a volume ratio of 4:2:1. 3 and HCl to obtain a composite acid solution.

[0099] The concentration of HF is 40wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0100] (2) The WMo alloy and the composite acid solution were stirred and mixed in a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 90° C. for 30 min to obtain a clear and transparent digestion solution.

[0101] Comparative Example 1

[0102] This comparative example provides a method for digesting WMo alloy, which comprises the following steps:

[0103] (1) Mix HF and HNO in a volume ratio of 1:1:1. 3 and HCl to obtain a composite acid solution.

[0104] The concentration of HF is 40wt%, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0105] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0106] Comparative Example 2

[0107] This comparative example provides a method for digesting WMo alloy, which comprises the following steps:

[0108] (1) Mix HF and HNO in a volume ratio of 6:1:0.1. 3 and HCl to obtain a composite acid solution.

[0109] The concentration of HF is 40wt%, HNO 3The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0110] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0111] Comparative Example 3

[0112] This comparative example provides a method for digesting WMo alloy, which comprises the following steps:

[0113] (1) Mix HF and HNO in a volume ratio of 4:2 3 Mix well to obtain a composite acid solution.

[0114] The concentration of HF is 40wt%, HNO 3 The concentration is 33wt%.

[0115] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0116] Comparative Example 4

[0117] This comparative example provides a method for digesting WMo alloy, which comprises the following steps:

[0118] (1) HF and HCl are mixed uniformly in a volume ratio of 4:1 to obtain a composite acid solution.

[0119] The concentration of HF is 40 wt % and the concentration of HCl is 37.5 wt %.

[0120] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0121] Comparative Example 5

[0122] This comparative example provides a method for digesting WMo alloy, which comprises the following steps:

[0123] (1) Add HNO with a volume ratio of 2:1 3 and HCl to obtain a composite acid solution.

[0124] Among them, HNO 3 The concentration of is 66 wt %, and the concentration of HCl is 37.5 wt %.

[0125] (2) The WMo alloy and the composite acid solution were stirred and mixed according to a mass volume ratio of 0.1 g:3.5 mL, and digested on a graphite heater at 70° C. for 30 min to obtain a clear and transparent digestion solution.

[0126] Performance Testing

[0127] The digestion solutions provided in the above examples and comparative examples were placed in a volumetric flask, fixed to 100 mL, diluted 100 times, and then placed in an ICP-OES device to simultaneously detect W and Mo elements. The detection results are shown in Table 1.

[0128] Table 1

[0129]

[0130] analyze:

[0131] As can be seen from the above table, the present invention uses the specific combination of three acid solutions, so that it can not only dissolve a single metal, but also directly dissolve the WMo alloy, and can achieve a sufficient dissolution effect to meet the detection standards of the ICP-OES machine.

[0132] It can be seen from Example 1 and Examples 6-7 that if the concentration of HF is too low, it will lead to incomplete dissolution and affect the detection results; if the concentration of HF is too high, it will cause great damage to the equipment.

[0133] It can be seen from Examples 1 and 8-9 that if HNO 3 If the concentration of HNO is too low, it will lead to incomplete dissolution and affect the test results. 3 If the concentration is too high, it will lead to incomplete dissolution and affect the test results.

[0134] It can be seen from Example 1 and Examples 10-11 that if the concentration of HCl is too low, precipitation will occur, affecting the detection result; if the concentration of HCl is too high, the detected content of the Mo element will be too high, affecting the detection result.

[0135] It can be seen from Examples 1 and 12-13 that if the temperature of the digestion treatment is too low, the precipitate will not dissolve, affecting the test results; if the temperature of the digestion treatment is too high, it will cause element loss, affecting the test results;

[0136] It can be seen from Example 1 and Comparative Examples 1-2 that if HF, HNO 3 If the ratio of HF, HNO 3 If the ratio to HCl is too large, it will damage the equipment and the detected element content will be too high.

[0137] It can be seen from Example 1 and Comparative Examples 3-5 that if only HF and HNO 3 , it will cause precipitation; if only HF and HCl are used, the WMo alloy will not dissolve; if only HNO 3 and HCl, the WMo alloy will not dissolve.

[0138] The applicant declares that the present invention illustrates the process method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned process steps, that is, it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials 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.

Claims

1. A method for digesting WMo alloy, characterized in that: The method The following steps are involved: The WMo alloy, HF, HNO3 and HCl are mixed and digested to obtain a digestion solution; Among them, the volume ratio of HF, HNO3 and HCl is (3-6):(1.5-2.5):(0.5-1).

2. The method according to claim 1, characterized in that The concentration of HF is 38-42wt%; Preferably, the concentration of HNO3 is 65-68wt%; Preferably, the concentration of HCl is 36.5-38.5 wt %.

3. The method according to claim 1 or 2, characterized in that: The total volume of HF, HNO3 and HCl is denoted as V 酸 The mass of the WMo alloy is recorded as M, M:V 酸 =(0.05-0.2)g:(2.5-4)mL.

4. The method according to any one of claims 1 to 3, characterized in that: The digestion process is accompanied by stirring; Preferably, the stirring rate is 800-1200 rpm.

5. The method according to any one of claims 1 to 4, characterized in that: The temperature of the digestion treatment is 60-80°C.

6. The method according to any one of claims 1 to 5, characterized in that: The digestion treatment time is 20-40 minutes.

7. The method according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: (1) mixing HF, HNO3 and HCl in a volume ratio of (3-6):(1.5-2.5):(0.5-1) to obtain a composite acid solution; Wherein, the concentration of HF is 38-42wt%, the concentration of HNO3 is 65-68wt%, and the concentration of HCl is 36.5-38.5wt%; (2) The WMo alloy and the composite acid solution are stirred and mixed according to a mass volume ratio of (0.05-0.2) g:(2.5-4) mL, and digested on a graphite heater at 60-80° C. for 20-40 min to obtain a clear and transparent digestion solution.

8. Use of the method according to any one of claims 1 to 7 in ICP-OES testing of WMo alloy.

9. The use according to claim 8, characterized in that: The specific steps of the application include: The digestion solution was fixed to volume, and then the fixed-volume digestion solution was placed in an ICP-OES device to simultaneously detect the W element and the Mo element.

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