CN210487653U - Device for preparing spectral analysis sample - Google Patents
Device for preparing spectral analysis sample Download PDFInfo
- Publication number
- CN210487653U CN210487653U CN201921185803.3U CN201921185803U CN210487653U CN 210487653 U CN210487653 U CN 210487653U CN 201921185803 U CN201921185803 U CN 201921185803U CN 210487653 U CN210487653 U CN 210487653U
- Authority
- CN
- China
- Prior art keywords
- hearth
- swinging
- swing
- preparing
- analysis sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The utility model discloses a device for preparing a spectrum analysis sample, which comprises a hearth structure and a sample melting machine structure; the hearth structure comprises a hearth shell, wherein a vacuum cavity for placing the fusion machine structure is formed in the hearth shell, the top of the hearth shell is connected with a hearth cover plate, and a swing bearing seat, a vacuum exhaust port, an argon gas charging port, a swing motor base, a high-frequency cable sleeve and a vacuum exhaust port are arranged on one side surface of the hearth shell; the sample melting machine structure comprises a fixed support, a swinging machine base, a swinging fixed support and a swinging mechanism, wherein one end of the swinging machine base is connected with the fixed support, the other end of the swinging machine base is erected on the swinging fixed support and is connected with the swinging mechanism, a rotating motor is arranged on the swinging machine base, an output shaft of the rotating motor is connected with a driving wheel, two driven wheels are sequentially meshed through the driving wheel, one driven wheel is provided with a high-frequency coil, and the other driven wheel is provided with a crucible. The utility model discloses utilize the direct casting of high frequency induction molten metal material to prepare spectral analysis sample, can solve prior art's defect.
Description
Technical Field
The present invention relates to sample preparation devices, and more particularly, to a device for preparing a spectroscopic sample.
Background
The X-ray fluorescence and photoelectric direct-reading spectral analysis has the advantages of rapidness, convenience, accuracy, high precision and the like, and with the development of instruments and software technologies, how to exert the advantages of spectral analysis becomes a key point in sample preparation. The requirements for analyzing samples are that the surface is smooth, no pollution is caused, the elements are uniformly distributed, no particle effect and mineral effect are caused, the stability is realized, and the accuracy of the analysis result can be ensured only by keeping the physical forms of the standard sample and the test sample consistent. At present, the sample preparation method for the spectral analysis of the metal sample mainly comprises the following steps:
1) a block sample method, wherein a sample is cut and polished;
2) powder tabletting method, for example, after alloy materials (ferrosilicon, ferromanganese, ferromolybdenum, ferrochromium alloy and the like) are crushed, ground and tabletted, detection is carried out, but the defects of the method are that the particle effect and the mineral effect are difficult to completely eliminate, matched standard articles are difficult to find, and the analysis accuracy is poor;
3) the glass bead melting method is characterized in that a powder metal sample, an oxidant and a solvent (sodium tetraborate, lithium tetraborate or a mixture of lithium tetraborate and lithium metaborate) are melted in a platinum crucible to form glass beads, and the glass bead melting method has the advantages that the glass bead melting method can effectively overcome the particle effect and the mineral effect, but has the defects of complex operation process, high risk of corrosion to the platinum crucible and long sample preparation time;
4) the solution method is to process a metal sample into solution, and has the advantages of effectively overcoming the particle effect and the mineral effect, and uniformly distributing elements, but has the defects of needing to configure a special instrument, low safety and reliability, needing to use a large amount of acid and alkali, and polluting the environment;
5) the centrifugal casting method has the advantages that the sample preparation time is short, the particle effect and the mineral effect of the sample are eliminated, but the defects are that equipment needs to be imported, the price is high (about 60 ten thousand RMB) and a ceramic crucible special for consumables of the sample is also high (one needs 400 yuan RMB), so that most enterprises cannot bear the production cost. Although the existing sample machines are made in China at present, special crucibles are also needed.
SUMMERY OF THE UTILITY MODEL
To the above-mentioned defect that exists among the prior art, the utility model aims at providing an equipment for preparing spectral analysis sample utilizes the direct casting of high frequency induction molten metal material to prepare spectral analysis sample, can solve the defect among the prior art.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
an apparatus for preparing a spectral analysis sample comprises a hearth structure and a sample melting machine structure arranged in the hearth structure;
the hearth structure comprises a hearth shell which is arranged into a box body shape, a vacuum cavity for placing the sample melting machine structure is arranged in the hearth shell, a water cooling jacket is arranged on the outer side surface of the vacuum cavity corresponding to the hearth shell, a hearth cover plate is connected to the top of the hearth shell, and a swing bearing seat, a vacuum relief port, an argon gas charging port, a swing motor seat, a high-frequency cable sleeve and a vacuum exhaust port are arranged on one side surface of the hearth shell;
the sample melting machine structure comprises a fixed support, a swinging machine base, a swinging fixed support and a swinging mechanism, wherein the swinging machine base is horizontally arranged, one end of the swinging machine base is connected with the fixed support, the other end of the swinging machine base is erected on the swinging fixed support and is connected with the swinging mechanism, a rotating motor is arranged on the swinging machine base, an output shaft of the rotating motor is connected with a driving wheel, two driven wheels are sequentially meshed through the driving wheel to form a rotating transmission gear set, one driven wheel is provided with a high-frequency coil, and the other driven wheel is provided with a crucible.
The hearth shell is connected with the hearth cover plate through a hinge, and the hearth cover plate is further provided with a cover plate handle.
And the hearth cover plate is also provided with a quartz glass temperature measuring hole and a quartz glass observation hole.
And a cover plate opening supporting positioning rod is arranged between the hearth shell and the hearth cover plate.
And a bearing seat is also arranged at one end of the swinging machine seat connected with the fixed support.
The high-frequency coil is connected with a coil height adjusting support through an insulating and heat-insulating support, and the coil height adjusting support is fixed on the swing machine base.
And a clamping regulator is arranged on the other driven wheel, a ceramic crucible support is arranged on the clamping regulator, and the crucible is arranged on the ceramic crucible support.
And a coil fixing clamp is also arranged at one end of the swinging base connected with the swinging mechanism.
The swing mechanism comprises a swing bearing seat fixed on a swing fixing support, the swing bearing seat is connected with a first driving wheel, the first driving wheel is connected with a second driving wheel through a swing driving belt, the second driving wheel is connected with the end portion of a swing machine base, the first driving wheel is further connected with a swing motor, an angle sensor is further arranged between the first driving wheel and the swing motor, and a tensioning wheel is further arranged on the swing driving belt.
The crucible is made of corundum materials, and a graphite heating sleeve is additionally sleeved on the outer side of the crucible.
In the technical scheme, the utility model provides an equipment for preparing spectral analysis sample can prepare stably, the element distributes evenly, no particle effect and mineral effect, can be used for spectral analysis's cubic sample, can improve the efficiency of analysis greatly, and the sample that uses conventional wet chemistry analytical method to analyze a multielement is from 5 to 7 days, shortens to 1 day, even to 2 hours, does not use chemical reagent such as acid-base, greatly reduced analysis's cost is favorable to improving the environment.
Drawings
FIG. 1 is a schematic view of the structure of a furnace chamber in the apparatus of the present invention;
FIG. 2 is a schematic view of the structure of the sample melting furnace in the apparatus of the present invention.
Detailed Description
The technical solution of the present invention will be further explained with reference to the accompanying drawings and examples.
Please refer to fig. 1 to 2, the present invention provides an apparatus for preparing a spectrum analysis sample, which includes a furnace structure and a sample melting machine structure disposed in the furnace structure.
Preferably, the hearth structure comprises a hearth shell 1 which is arranged in a box shape, a vacuum cavity 2 for placing a sample melting machine structure is arranged in the hearth shell, a water cooling jacket 3 is arranged on the outer side surface of the vacuum cavity 2 corresponding to the hearth shell 1, a hearth cover plate 4 is connected to the top of the hearth shell 1, and a swing bearing seat 5, a vacuum relief port 6, an argon gas charging port 7, a swing motor seat 8, a high-frequency cable sleeve 9 and a vacuum pumping port 10 are arranged on one side surface of the hearth shell 1.
Preferably, the hearth shell 1 is connected with the hearth cover plate 4 through a hinge, and the hearth cover plate 4 is further provided with a cover plate handle 11, so that the hearth cover plate 4 can be opened and closed conveniently.
Preferably, still be equipped with quartz glass temperature measurement hole 12 and quartz glass observation hole 13 on the furnace apron 4, be used for observing the utility model discloses the temperature condition of equipment at the during operation, and the condition when its internal work moves.
Preferably, a cover plate opening supporting positioning rod 14 is further arranged between the hearth shell 1 and the hearth cover plate 4 and used for supporting and positioning after the hearth cover plate 4 is opened, so that the hearth cover plate 4 is prevented from returning to be closed.
Preferably, the top of the hearth shell 1 is further provided with a circle of sealing ring 15 for increasing the sealing degree between the hearth shell 1 and the hearth cover plate 4 during operation.
Preferably, the sample melting machine structure comprises a fixed support 16, a swinging base 17, a swinging fixed support 18 and a swinging mechanism, wherein the swinging base 17 is horizontally arranged, one end of the swinging base 17 is connected with the fixed support 16, the other end of the swinging base is erected on the swinging fixed support 18 and then connected with the swinging mechanism, a rotating motor 19 is arranged on the swinging base 17, an output shaft of the rotating motor 19 is connected with a driving wheel 20, two driven wheels 21 and 22 are sequentially meshed through the driving wheel 20 to form a rotating transmission gear set, a high-frequency coil 23 is arranged on one driven wheel 21, and a crucible 24 is arranged on the other driven wheel 22.
Preferably, a bearing seat 25 is further disposed at an end of the swing base 17 connected to the fixed bracket 16, so that the swing base 17 is rotatably connected to the fixed bracket 16.
Preferably, the high-frequency coil 23 is connected with a coil height adjusting bracket 27 through an insulating and heat-insulating bracket 26, and the coil height adjusting bracket 27 is fixed on the swinging base 17.
Preferably, the other driven wheel 22 is provided with a clamping adjuster 28, the clamping adjuster 28 is provided with a ceramic crucible support 29, and the crucible 24 is arranged on the ceramic crucible support 29.
Preferably, a coil fixing clip 30 is further disposed on one end of the swing base 17 connected to the swing mechanism.
Preferably, the swing mechanism includes a swing bearing block 31 fixed on the swing fixing support 18, the swing bearing block 31 is connected with a first driving wheel 32, the first driving wheel 32 is connected with a second driving wheel 34 through a swing driving belt 33, the second driving wheel 34 is connected with the end of the swing base 17, the first driving wheel 32 is further connected with a swing motor 35, an angle sensor 36 is further arranged between the first driving wheel 32 and the swing motor 35, and a tension wheel 37 is further arranged on the outer side surface of the swing driving belt 33.
Preferably, the crucible 24 is made of corundum, so that the cost is low, and a graphite heating sleeve is additionally sleeved on the outer side of the crucible, so that the uniformity of the melting temperature and the heating speed of a sample are ensured, and the defect of uneven high-frequency heating is overcome.
Preferably, the upper portion of vacuum chamber 2 is equipped with the rectangle flange, and the flange inlays on furnace shell 1, sways frame 17 and adopts four screw fixation on two reinforcing plates on the bottom plate of vacuum chamber 1, has still set up two cylindrical support of placing the mould seat on the bottom plate of vacuum chamber 2, and two moulds can be placed on mould seat upper portion, and crucible 24 just in time will dissolve the appearance and pour into two moulds when empting, and the mould adopts two open-close type structures, can open after the cooling and take out and melt the appearance.
The utility model solves the oxidation and volatilization problems of alloy samples through the mode of adding inert gas (argon) into vacuum. The whole furnace body is cooled by water, so that the operation safety is guaranteed. The frequency is adopted as a high-frequency power supply, and a power supply is provided for a small experimental furnace. Through the whole swing of the swing base 17 and the design that each sample rotates independently, the uniformity and the repeatability of the molten sample are guaranteed, and compared with a direct casting structure, the device is simple in structure and convenient to operate.
The equipment of the utility model is used for detecting the X-ray fluorescence spectrum analysis of the element components in the silicon iron and the silicon-manganese-iron alloy.
Example 1
And (3) carrying out X-ray fluorescence spectrum analysis on Si, Mn, Fe, P, Al, Cr and Cu in the ferrosilicon alloy.
The standard blocks were prepared as follows:
1) weighing 5.000g of a ferrosilicon standard sample and 40.00g of a pure iron cosolvent and putting into a crucible;
2) the crucible is placed on a ceramic crucible support of a fusion machine structure;
3) closing the furnace hearth cover plate, vacuumizing to set parameters, and then turning to argon protection;
4) after the mixture is statically melted for 5 minutes under certain heating power, the crucible is tilted and rotated for 5 minutes, and then the mixture is automatically cast into a copper mold, and the prepared standard sample blocks are numbered.
Test sample block preparation.
The test comprises the steps of measuring the X-ray fluorescence intensity of SiK α, MnK α, FeK α, PK α, AlK α, CrK α and CuK α of a standard sample block by using an X-ray fluorescence spectrometer, drawing a calibration curve by using the concentration and the intensity, measuring the intensity of each element in the sample under the same condition, and calculating the content of Si, Mn, Fe, P, Al, Cr and Cu in the sample according to the corresponding calibration curve.
Adopt the utility model discloses the analysis result and the standard value contrast of equipment system appearance piece see table 1 below, can see out the uniformity of measured value and standard value from table 1's the degree of accuracy result.
TABLE 1
Example 2
And (3) carrying out X-ray fluorescence spectrum analysis on Si, Mn and P in the ferro-silico-manganese alloy.
The standard blocks were prepared as follows:
1) weighing 8.000g of a ferro-silico-manganese alloy standard sample and 40.00g of a pure iron cosolvent, and putting the standard sample and the pure iron cosolvent into a crucible;
2) the crucible is placed on a ceramic crucible support of a fusion machine structure;
3) closing the furnace hearth cover plate, vacuumizing to set parameters, and then turning to argon protection;
4) after the mixture is statically melted for 5 minutes under certain heating power, the crucible is tilted and rotated for 5 minutes, and then the mixture is automatically cast into a copper mold, and the prepared standard sample blocks are numbered.
Test sample block preparation.
And (3) testing, namely measuring the X-ray fluorescence intensity of SiK α, MnK α and PK α of the standard sample block by using an X-ray fluorescence spectrometer, drawing a calibration curve by using the concentration and the intensity, measuring the intensity of each element in the sample under the same condition, and calculating the content of Si, Mn and P in the sample according to the corresponding calibration curve.
Adopt the utility model discloses the analysis result and the standard value contrast of equipment system appearance piece see table 2 below, can see the uniformity of measured value and standard value from the degree of accuracy result of table 2.
TABLE 2
As can be seen from the comparison of the accuracy data in tables 1 and 2, the X-fluorescence analysis value is identical to the standard value, which indicates that the sample prepared by the device of the utility model is accurate and reliable.
It will be appreciated by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be used as limitations of the present invention, and that changes and modifications to the above described embodiments will fall within the scope of the claims of the present invention as long as they are within the spirit and scope of the present invention.
Claims (10)
1. An apparatus for preparing a spectroscopic analysis sample, characterized by: comprises a hearth structure and a sample melting machine structure arranged in the hearth structure;
the hearth structure comprises a hearth shell which is arranged into a box body shape, a vacuum cavity for placing the sample melting machine structure is arranged in the hearth shell, a water cooling jacket is arranged on the outer side surface of the vacuum cavity corresponding to the hearth shell, a hearth cover plate is connected to the top of the hearth shell, and a swing bearing seat, a vacuum relief port, an argon gas charging port, a swing motor seat, a high-frequency cable sleeve and a vacuum exhaust port are arranged on one side surface of the hearth shell;
the sample melting machine structure comprises a fixed support, a swinging machine base, a swinging fixed support and a swinging mechanism, wherein the swinging machine base is horizontally arranged, one end of the swinging machine base is connected with the fixed support, the other end of the swinging machine base is erected on the swinging fixed support and is connected with the swinging mechanism, a rotating motor is arranged on the swinging machine base, an output shaft of the rotating motor is connected with a driving wheel, two driven wheels are sequentially meshed through the driving wheel to form a rotating transmission gear set, one driven wheel is provided with a high-frequency coil, and the other driven wheel is provided with a crucible.
2. An apparatus for preparing a spectroscopic analysis sample according to claim 1 wherein: the hearth shell is connected with the hearth cover plate through a hinge, and the hearth cover plate is further provided with a cover plate handle.
3. An apparatus for preparing a spectroscopic analysis sample according to claim 2 wherein: and the hearth cover plate is also provided with a quartz glass temperature measuring hole and a quartz glass observation hole.
4. An apparatus for preparing a spectroscopic analysis sample according to claim 2 wherein: and a cover plate opening supporting positioning rod is arranged between the hearth shell and the hearth cover plate.
5. An apparatus for preparing a spectroscopic analysis sample according to claim 1 wherein: and a bearing seat is also arranged at one end of the swinging machine seat connected with the fixed support.
6. An apparatus for preparing a spectroscopic analysis sample according to claim 1 wherein: the high-frequency coil is connected with a coil height adjusting support through an insulating and heat-insulating support, and the coil height adjusting support is fixed on the swing machine base.
7. An apparatus for preparing a spectroscopic analysis sample according to claim 1 wherein: and a clamping regulator is arranged on the other driven wheel, a ceramic crucible support is arranged on the clamping regulator, and the crucible is arranged on the ceramic crucible support.
8. An apparatus for preparing a spectroscopic analysis sample according to claim 1 wherein: and a coil fixing clamp is also arranged at one end of the swinging base connected with the swinging mechanism.
9. An apparatus for preparing a spectroscopic analysis sample according to claim 8 wherein: the swing mechanism comprises a swing bearing seat fixed on a swing fixing support, the swing bearing seat is connected with a first driving wheel, the first driving wheel is connected with a second driving wheel through a swing driving belt, the second driving wheel is connected with the end portion of a swing machine base, the first driving wheel is further connected with a swing motor, an angle sensor is further arranged between the first driving wheel and the swing motor, and a tensioning wheel is further arranged on the swing driving belt.
10. An apparatus for preparing a spectroscopic analysis sample according to claim 8 wherein: the crucible is made of corundum materials, and a graphite heating sleeve is additionally sleeved on the outer side of the crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921185803.3U CN210487653U (en) | 2019-07-25 | 2019-07-25 | Device for preparing spectral analysis sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921185803.3U CN210487653U (en) | 2019-07-25 | 2019-07-25 | Device for preparing spectral analysis sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210487653U true CN210487653U (en) | 2020-05-08 |
Family
ID=70532856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921185803.3U Active CN210487653U (en) | 2019-07-25 | 2019-07-25 | Device for preparing spectral analysis sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210487653U (en) |
-
2019
- 2019-07-25 CN CN201921185803.3U patent/CN210487653U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100394161C (en) | Method and apparatus for quantitative determination of hydrogen content in casting aluminum alloy liquation | |
| CN113324828A (en) | Remelting and ingot casting sample preparation and component detection method for ferroalloy | |
| CN102426122A (en) | Sample preparation method by fusing medium-carbon ferrochrome and high-carbon ferrochrome | |
| CN101526488A (en) | Method for analyzing components of iron ore by using X-ray fluorescence spectrum | |
| CN210487653U (en) | Device for preparing spectral analysis sample | |
| CN105588781B (en) | A kind of device and method for measuring field trash rate of dissolution in metallurgy clinker | |
| CN108254234A (en) | A kind of preparation method of stainless steel smelting process control standard specimen | |
| CN108918563A (en) | Preparation method for the sample of manganese silicon phosphorus content in X-ray fluorescence method measurement silicomangan | |
| CN207197692U (en) | A kind of vacuum melting furnace multi-functional continuous temperature measurement and sampler | |
| CN114486967B (en) | Method for measuring calcium, silicon, magnesium and iron in submerged arc slag by X fluorescence | |
| CN105784529B (en) | The manufacture craft of plastics ball indentation hardness calibrated bolck | |
| CN106896099A (en) | A kind of device and method of laser detection solid material composition | |
| CN110646452A (en) | Method for measuring major elements in ferrochrome alloy by X fluorescence fuse link method | |
| CN106338534A (en) | Method for rapidly measuring content of calcium fluoride in fluorite by X-ray fluorescence spectrometer | |
| CN109001654B (en) | Manufacturing method of relative magnetic permeability standard steel of non-magnetic drill collar | |
| CN112213342A (en) | Portable analysis and detection system for content of elements in ore | |
| CN117782769A (en) | Device and method for manufacturing high-carbon ferrochrome spectrum sample | |
| CN113447330A (en) | Method for determining content of impurity components in white corundum by X-ray fluorescence spectrometry | |
| CN112461878A (en) | Method for determining content of ferronickel in carbonyl ferronickel alloy powder | |
| JP3308276B2 (en) | Non-contact continuous temperature measurement method for solidification of alloys | |
| CN115639233B (en) | Method for analyzing lanthanum and cerium content in blast furnace molten iron | |
| CN206563712U (en) | A kind of device of laser detection solid material composition | |
| CN206670973U (en) | A kind of aluminum matrix composite melt sampler | |
| CN109668872A (en) | A kind of direct-reading spectrometer surveys the analysis method of nitrogen in steel online | |
| CN103264150B (en) | Pig iron spectral analysis sample centrifugal casting device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |