A chemical determination device and method for iron content in silicon-aluminum alloy

Abstract

The present invention relates to the field of metal content detection, and specifically discloses a chemical determination device and method for the iron content of silicon-aluminum alloy, comprising the following steps: S1: sample dissolution, weighing 0.1g silicon-aluminum alloy in a 100ml plastic beaker, adding 1ml nitric acid to soak the sample, adding 4-6ml hydrofluoric acid in small amounts and multiple times, adding 5ml potassium nitrate solution after the yellow smoke disappears, filtering and precipitating, and adding 3ml saturated boric acid solution to the filtrate; S2: standard curve drawing, according to the content of iron element in the sample to be tested, configuring a series of high and low ranges of gradient standard solutions, and drawing high and low range standard curves according to the absorbance and concentration of different standard solutions. The chemical determination method for the iron content of silicon-aluminum alloy uses nitric acid and hydrofluoric acid to decompose the silicon-aluminum alloy sample, which is not only simple to operate, but also relatively less in the use of drugs and equipment, and has a wide range of application, and is suitable for the detection of high, medium and low iron contents in silicon-aluminum alloys, so it is more suitable for non-batch detection.

Description

Technical Field

[0001] The present invention relates to the technical field of iron content detection, and in particular to a device and method for chemically determining the iron content of a silicon-aluminum alloy. Background Art

[0002] At present, there is no unified national standard or industry standard for the determination of iron in silicon-aluminum alloys. The existing methods are mainly based on the combination of microwave digestion and ICP-OES and alkali dissolution at high temperature combined with o-phenanthroline spectrophotometry. Among them, the combination of microwave digestion and ICP-OES has a low detection limit and high sensitivity, but the equipment is expensive and suitable for large-scale detection. The cost is high when a small amount is detected; the high-temperature alkali dissolution combined with o-phenanthroline spectrophotometry has simple equipment and low cost, but the pre-treatment steps are cumbersome, the detection process is poor, and the detection efficiency is low. In addition, some existing technologies use 6% hydrochloric acid to heat and dissolve the iron in silicon-aluminum alloys for a long time. This method is only applicable to the detection of low-content (less than 10%) iron. It is not only time-consuming, but also has a narrow scope of application and is not conducive to the detection of high iron content (>10%).

[0003] Therefore, it is necessary to propose a chemical determination device and method for the iron content of silicon-aluminum alloy to solve the above problems. Summary of the invention

[0004] The main purpose of the present invention is to provide a chemical determination device and method for the iron content of silicon-aluminum alloy, which can effectively solve the problems in the background technology.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A method for chemically determining the iron content of a silicon-aluminum alloy comprises the following steps:

[0007] S1: Sample dissolution, weigh 0.1g of silicon aluminum alloy into a 100ml plastic beaker, add 1ml nitric acid to soak the sample, then add 4-6ml hydrofluoric acid in small amounts and multiple times, add 5ml potassium nitrate solution after the yellow smoke disappears, filter the precipitate, add 3ml saturated boric acid solution to the filtrate, let it stand for 3 minutes, then transfer to a 100ml volumetric flask, make up to volume, shake well, and set aside;

[0008] S2: Standard curve drawing: according to the content of iron in the sample to be tested, a series of gradient standard solutions with different high and low ranges are prepared, and high and low range standard curves are drawn according to the absorbance and concentration of different standard solutions;

[0009] S3: 1-5 ml of filtrate is taken into a 50 ml volumetric flask according to the iron content in the sample to be tested, and diluted to about 15 ml with water, and then 2.5 ml of hydroxylamine hydrochloride solution is added, and the mixture is shaken for a while, and then 1 ml of tartaric acid solution is added, and then an appropriate amount of sodium acetate solution is added to adjust the pH to 3-6, and then 2 ml of 1-1-phenanthroline ethanol solution is added, and the mixture is diluted to the scale with water and shaken. After 15 minutes, the absorbance is measured at a wavelength of 510 nm with the reagent blank as a reference, and the concentration of ferric oxide is found from the standard curve, and the result is calculated.

[0010] Preferably, in step S2, when configuring a series of high and low ranges of gradient standard solutions and drawing high and low range standard curves according to the absorbance and concentration of different standard solutions, take 0 ml, 0.5 ml, 1 ml, 1.5 ml, 2 ml, 2.5 ml, and 3 ml of ferric oxide standard solution, respectively, and place them in 50 ml volumetric flasks, dilute them with water to about 15 ml, add 2.5 ml of hydroxylamine hydrochloride solution, shake and let stand for a while, add 1 ml of tartaric acid solution, add an appropriate amount of sodium acetate solution to adjust pH = 3-6, add 2 ml of o-phenanthroline ethanol solution, dilute with water to the scale, shake well, and after 15 minutes, use the reagent blank solution as a control, measure its absorbance at a wavelength of 510 nanometers, and draw a standard curve with ferric oxide concentration as the horizontal coordinate and absorbance as the vertical coordinate.

[0011] Preferably, in step S3, the formula for calculating the result is:

[0012]

[0013] In the formula:

[0014] X is the iron content in the sample, %;

[0015] C is the concentration of ferric oxide in the test solution obtained from the standard curve, μg / mL;

[0016] C0 is the concentration of ferric oxide in the blank solution accompanying the sample obtained from the standard curve, μg / mL;

[0017] V is the constant volume of the sample on the machine, mL;

[0018] f is the dilution factor of the sample solution;

[0019] m is the weight of the sample, g;

[0020] 159.69 is the molecular weight of ferric oxide.

[0021] Also included is an embodiment, which is a chemical determination device for the iron content of silicon-aluminum alloy, which is applied to the shaking step in the chemical determination method for the iron content of silicon-aluminum alloy, including a shell, a shaking component is arranged in the shell, and the shaking component includes a rotating disk arranged on the inner side of the shell, and the inner upper end of the shell is provided with a fixing frame located on the top of the rotating disk, and the middle part of the fixing frame is provided with a rotating sleeve, and a first universal ball is movably arranged on the inner side of the rotating sleeve, and a shaking seat for fixing a container is fixedly arranged on the upper end of the first universal ball, and an inner rod body is movably connected to the bottom of the first universal ball, and the outer side of the lower end of the inner rod body The movable sleeve is provided with an outer cylinder, a slide groove is radially arranged at one end of the top of the rotating disk, a slide seat is movably connected with the inner side of the slide groove along the radial direction of the rotating disk, the lower end of the outer cylinder is movably connected with the upper end of the slide seat, a driving arm extending to the outside of the rotating disk is arranged on the side of the slide seat away from the axis of the rotating disk, an elastic member is arranged between the side of the slide seat close to the axis of the rotating disk and the inner wall of the slide groove, a driving plate corresponding to the driving arm is arranged on the inner wall of the outer shell, and guide slopes with a smooth transition with the inner wall of the outer shell are arranged at both ends of the driving plate, and a second driving source for driving the rotating disk to rotate is arranged below the rotating disk.

[0022] Preferably, columns corresponding to the fixing frame are evenly arranged on the periphery of the top of the rotating disk, and a rotating ring is fixedly arranged on the top of a plurality of the columns, and the upper end of the rotating ring is rotatably connected to the bottom of the fixing frame.

[0023] Preferably, a limit assembly for limiting the fixing frame is provided on the side of the fixing frame, and the limit assembly includes guide arms evenly arranged on the circumferential side walls of the fixing frame, and the inner wall of the outer shell is provided with guide grooves corresponding to the guide arms one by one, and one end of the guide arm away from the fixing frame extends to the inner side of the guide groove and cooperates with the guide groove sliding guide.

[0024] Preferably, a lifting frame is provided at the inner lower end of the shell, the second driving source is fixedly mounted on the lifting frame, and the second driving source is a motor.

[0025] Preferably, the top of the shaking seat is open for placing containers, the circumferential side wall of the shaking seat is evenly threaded with a screw, the length direction of the screw is consistent with the radial direction of the shaking seat, one end of the screw extends to the inner side of the shaking seat and is rotatably provided with an arc-shaped clamp, which is used to clamp the container.

[0026] Preferably, a first driving source for driving the lifting frame to rise and fall is provided under the lifting frame, and a conical guide cylinder is provided on the top of the driving plate. The interior of the guide cylinder smoothly transitions with the inner side of the driving plate, and the inner diameter of the guide cylinder increases successively from top to bottom, and is configured so that when the driving arm corresponds to the inner wall of the upper end of the guide cylinder, the outer cylinder body and the inner rod body are in a vertical state, and the top opening of the shaking seat faces upward.

[0027] Preferably, the container is a beaker, a volumetric flask or a test tube.

[0028] Compared with the prior art, the present invention provides a device and method for chemically determining the iron content of silicon-aluminum alloy, which has the following beneficial effects:

[0029] 1. This chemical determination method for iron content in silicon-aluminum alloy uses nitric acid and hydrofluoric acid to decompose silicon-aluminum alloy samples. It is not only easy to operate, but also uses relatively few drugs and equipment. It also has a wide range of applications, high detection efficiency, and high accuracy. It is suitable for the detection of high, medium, and low iron contents in silicon-aluminum alloys, and is therefore more suitable for non-batch detection.

[0030] 2. The chemical determination device for the iron content in silicon-aluminum alloy can continuously change the shaking path during the shaking process through a shaking component specially designed for the chemical determination method for the iron content in silicon-aluminum alloy, thereby changing the problem of poor shaking effect caused by the unchanged conventional shaking path, avoiding the inertial motion of the solution following the unchanged shaking path, and more effectively breaking the local concentration difference in the solution to promote the uniform distribution of the solute in the solvent; by setting the first driving source and cooperating with the guide cylinder, the container can be ensured to be vertically upward when disassembling and assembling the container, and the container is tilted and hidden in the shell during shaking, which not only increases safety, but also facilitates shaking, is easy to use, and increases practicality. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the structure of the device for chemical determination of iron content in silicon-aluminum alloy of the present invention;

[0032] Figure 2 It is a schematic cross-sectional structure diagram of a chemical determination device for iron content in silicon-aluminum alloy according to the present invention;

[0033] Figure 3 It is a schematic diagram of the structure of the chemical determination device for iron content in silicon-aluminum alloy of the present invention in a disassembled state;

[0034] Figure 4 It is a schematic diagram of the overall structure of the guide cylinder, the drive plate, the fixing frame and the lifting frame in the chemical determination device for the iron content of the silicon-aluminum alloy of the present invention;

[0035] Figure 5 The present invention Figure 4 Schematic diagram of the structure when the foundation is disassembled;

[0036] Figure 6 The present invention Figure 5 A structural diagram from another perspective based on the above;

[0037] Figure 7 It is a schematic diagram of the overall structure of the fixed frame and the rotating disk in the chemical determination device for the iron content of the silicon-aluminum alloy of the present invention;

[0038] Figure 8 The present invention Figure 7 A structural diagram from another perspective based on the above;

[0039] Fig. 9 It is a schematic diagram of the structure of the device for chemical determination of iron content in silicon-aluminum alloy of the present invention, in which the driving arm, the slide seat, the outer cylinder and the rotating disk are separated;

[0040] Fig.10 It is a schematic diagram of the overall structure of the guide cylinder and the drive plate in the chemical determination device for the iron content of silicon-aluminum alloy of the present invention.

[0041] In the figure: 1. shell; 2. base; 3. top cover; 4. guide cylinder; 5. drive plate; 6. shaking seat; 7. connecting seat; 8. lifting frame; 9. guide groove; 10. first drive source; 11. guide column; 12. second drive source; 13. guide arm; 14. fixed frame; 15. swivel; 16. column; 17. rotating disk; 18. clamping plate; 19. screw; 20. rotating sleeve; 21. first universal ball; 22. drive arm; 23. outer cylinder; 24. inner rod; 25. slide seat; 26. second universal ball; 27. elastic member; 28. slide groove; 29. ​​guide rail; 30. guide slope. DETAILED DESCRIPTION

[0042] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0043] A chemical determination method for the iron content of silicon-aluminum alloy. It should be noted that this method stipulates the determination of the iron content by o-phenanthroline spectrophotometry; this method is applicable to the determination of iron in silicon-aluminum alloy;

[0044] For the principle:

[0045] The silicon in the sample reacts with potassium fluoride and nitric acid to form potassium fluorosilicate precipitate, and the filtrate is used for the determination of iron. Under the condition of pH = 2-6, divalent iron ions and o-phenanthroline generate a very stable red complex. The molar absorption coefficient of the complex at a wavelength of 505nm is 505 = 1.1×104. In a volume of 100mL, divalent iron ions conform to Beer's law in the range of 0-1000g, and the photometric determination of iron is carried out by the change in absorbance.

[0046] Divalent iron ions and o-phenanthroline can show color in the pH range of 2-6, and their color is independent of pH. However, in order to minimize the influence of other ions and improve the selectivity of the method, color is usually developed in a slightly acidic (around pH 5) solution.

[0047] The trivalent iron ion also forms a 3:1 light blue complex with o-phenanthroline, so the trivalent iron ion is reduced to divalent iron ion by hydroxylamine hydrochloride before color development.

[0048] For reagent preparation:

[0049] Unless otherwise specified, the reagents used in this method are of high purity and the water is first-grade water specified in GB / T6682. The specific reagents are:

[0050] Nitric acid (=1.42 g / mL);

[0051] Hydrofluoric acid (=1.15 g / mL);

[0052] Potassium nitrate-nitric acid solution (200g / L): weigh 20g potassium nitrate and dissolve it in nitric acid, dilute it to 100mL with nitric acid, shake well, and store it in a brown reagent bottle;

[0053] Saturated potassium nitrate solution.

[0054] 1-Phenanthroline ethanol solution (4 g / L): weigh 0.4 g of 1-Phenanthroline and dissolve it in ethanol. Dilute it to 100 mL with ethanol, shake well, and set aside.

[0055] Hydroxylamine hydrochloride solution (50g / L aqueous solution): weigh 5g of hydroxylamine hydrochloride into a volumetric flask and dilute to 100mL with distilled water. Shake well and prepare before use.

[0056] Tartaric acid solution (50 g / L aqueous solution): weigh 5 g of tartaric acid into a volumetric flask and dilute to 100 mL with distilled water. Shake well and set aside.

[0057] Sodium acetate solution (250g / L aqueous solution): weigh 25g of sodium acetate into a volumetric flask and dilute it to 100mL with distilled water. Shake well and set aside.

[0058] Saturated boric acid solution (4g / L): weigh about 0.4g of boric acid into a volumetric flask and dilute to 100mL with distilled water. Shake well and set aside.

[0059] Iron standard solution (0.1 mg / mL) was purchased directly from a national standard substance with a certificate.

[0060] For instruments and equipment: double beam UV-visible spectrophotometer: model T10CS; analytical balance: sensitivity 0.1 mg; chemical determination device for iron content of silicon-aluminum alloy, used for the shaking step.

[0061] There are at least two implementation examples for the operation steps:

[0062] Example 1

[0063] 1. Sample pretreatment

[0064] During sample preparation, the samples were crushed to 200 mesh as much as possible.

[0065] 2. Sample dissolution

[0066] Weigh 0.1g of primary silicon-aluminum alloy 1 into a 100mL plastic beaker, add 1mL of nitric acid to wet the sample, then add 15mL of potassium nitrate-nitric acid solution (200g / L), shake gently, slowly add 4mL of hydrofluoric acid in small amounts several times, add 5mL of saturated potassium nitrate solution after the yellow smoke disappears, let it stand for 20min, then dry filter and precipitate, add 3mL of saturated boric acid solution (4g / L) to the filtrate, shake well, let it stand for 3 minutes, then transfer to a 100mL volumetric flask and make up to volume for testing.

[0067] 3. Preparation of standard curve

[0068] Pipette 0mL, 0.5mL, 1mL, 1.5mL, 2mL, 2.5mL, and 3mL of ferric oxide standard solution (100μg / mL) into 50mL volumetric flasks respectively, dilute with water to about 15mL, add 2.5mL of hydroxylamine hydrochloride solution (50g / L aqueous solution), shake well and let stand for a while, add 1mL of tartaric acid solution (50g / L aqueous solution), add 10mL of sodium acetate solution (250g / L aqueous solution) to adjust pH=5, add 2mL of o-phenanthroline ethanol solution (4g / L), dilute to the scale with water, shake well, after 15 minutes, use the reagent blank solution as a reference, measure its absorbance at a wavelength of 510nm, and draw a standard curve with ferric oxide concentration as the horizontal axis and absorbance as the vertical axis.

[0069] The following table shows the concentration and absorbance data of different series of standard solutions of ferric oxide

[0070]

[0071] 4. Sample measurement

[0072] Pipette 4mL of filtrate into a 50mL volumetric flask, dilute with water to about 15mL, add 2.5mL of hydroxylamine hydrochloride solution, shake well and let stand for a while, add 1mL of tartaric acid solution, add about 11mL of sodium acetate solution to adjust pH to 5, add 2mL of o-phenanthroline ethanol solution, dilute with water to the scale, shake well, after 15 minutes, use the reagent blank solution as a reference, measure its absorbance at a wavelength of 510nm, measure its absorbance, find out the concentration of ferric oxide from the standard curve, and calculate the result.

[0073] 5. Result calculation

[0074] The calculation formula for the iron content in the sample is: ;

[0075] In the formula: X is the iron content in the sample, %; C is the concentration of ferric oxide in the test solution obtained from the standard curve, μg / mL; C0 is the concentration of ferric oxide in the blank solution accompanying the sample obtained from the standard curve, μg / mL; V is the fixed volume of the sample on the machine, mL; f is the dilution factor of the sample solution; m is the weighed mass of the sample, g; 159.69 is the molecular weight of ferric oxide.

[0076] Precision and repeatability

[0077]

[0078] Example 2

[0079] 1. Sample pretreatment

[0080] During sample preparation, the samples were crushed to 200 mesh as much as possible.

[0081] 2. Sample dissolution

[0082] Weigh 0.1g of primary silicon-aluminum alloy 2 into a 100mL plastic beaker, add 1mL of nitric acid to wet the sample, then add 15mL of potassium nitrate-nitric acid solution (200g / L), shake gently, slowly add 5mL of hydrofluoric acid in small amounts several times, add 5mL of saturated potassium nitrate solution after the yellow smoke disappears, let it stand for 20min, then dry filter the precipitate, add 3mL of saturated boric acid solution (4g / L) to the filtrate, shake well, let it stand for 3 minutes, then transfer to a 100mL volumetric flask and make up to volume for testing.

[0083] 3. Preparation of standard curve

[0084] Pipette 0mL, 0.5mL, 1mL, 1.5mL, 2mL, 2.5mL, and 3mL of ferric oxide standard solution (100μg / mL) into 50mL volumetric flasks respectively, dilute with water to about 15mL, add 2.5mL of hydroxylamine hydrochloride solution (50g / L aqueous solution), shake well and let stand for a while, add 1mL of tartaric acid solution (50g / L aqueous solution), add 10mL of sodium acetate solution (250g / L aqueous solution) to adjust pH=5, add 2mL of o-phenanthroline ethanol solution (4g / L), dilute to the scale with water, shake well, after 15 minutes, use the reagent blank solution as a reference, measure its absorbance at a wavelength of 510nm, and draw a standard curve with ferric oxide concentration as the horizontal axis and absorbance as the vertical axis.

[0085] The following table shows the concentration and absorbance data of different series of standard solutions of ferric oxide

[0086]

[0087] 4. Sample measurement

[0088] Pipette 1mL of the filtrate into a 50mL volumetric flask, dilute with water to about 15mL, add 2.5mL of hydroxylamine hydrochloride solution, shake well and let stand for a while, add 1mL of tartaric acid solution, add about 7.5mL of sodium acetate solution to adjust pH to 5, add 2mL of o-phenanthroline ethanol solution, dilute with water to the scale, shake well, after 15 minutes, use the reagent blank solution as a reference, measure its absorbance at a wavelength of 510nm, measure its absorbance, find out the concentration of ferric oxide from the standard curve, and calculate the result.

[0089] Result calculation

[0090] The calculation formula for the iron content in the sample is: ;

[0091] In the formula: X is the iron content in the sample, %; C is the concentration of ferric oxide in the test solution obtained from the standard curve, μg / mL; C0 is the concentration of ferric oxide in the blank solution accompanying the sample obtained from the standard curve, μg / mL; V is the fixed volume of the sample on the machine, mL; f is the dilution factor of the sample solution; m is the weighed mass of the sample, g; 159.69 is the molecular weight of ferric oxide.

[0092] Precision and repeatability

[0093]

[0094] It should be noted that the absolute difference between two independent measurement results obtained under repeatability conditions shall not exceed 5% of the arithmetic mean.

[0095] In addition, if Figure 1-Figure 10As shown, it also includes a chemical determination device for the iron content of silicon-aluminum alloy, which is applied to the shaking step in the above-mentioned chemical determination method for the iron content of silicon-aluminum alloy, including a shell 1, a top cover 3 is arranged on the top of the shell 1, a base 2 is arranged on the bottom, a shaking assembly is arranged in the shell 1, and the shaking assembly includes a rotating disk 17 arranged on the inner side of the shell 1, a fixing frame 14 located on the top of the rotating disk 17 is arranged on the inner upper end of the inner side of the shell 1, a rotating sleeve 20 is arranged in the middle of the fixing frame 14, a first universal ball 21 is movably arranged on the inner side of the rotating sleeve 20, and a shaking seat 6 for fixing a container is fixedly arranged on the upper end of the first universal ball 21, and the container is a beaker, a volumetric flask or a test tube in the above-mentioned method, a connecting seat 7 is fixedly arranged on the bottom of the first universal ball 21, and the lower end of the connecting seat 7 is movably connected to an inner rod body 24, and an outer cylinder body 23 is movably sleeved on the outer side of the lower end of the inner rod body 24, and a slide groove 28 is radially arranged on one end of the top of the rotating disk 17. A guide rail 29 is provided on the side wall of the inner cavity, and the slide 25 is slidably guided with the guide rail 29. The slide 25 is movably connected to the inner side of the slide groove 28 along the radial direction of the rotating disk 17. The lower end of the outer cylinder 23 is movably connected to the upper end of the slide 25. A driving arm 22 extending to the outside of the rotating disk 17 is provided on the side of the slide 25 away from the axis of the rotating disk 17. An elastic member 27 is provided between the side of the slide 25 close to the axis of the rotating disk 17 and the inner wall of the slide groove 28. The elastic member 27 is preferably a spring. A driving plate 5 corresponding to the driving arm 22 is provided on the inner wall of the outer shell 1, and guide slopes 30 with a smooth transition to the inner wall of the outer shell 1 are provided at both ends of the driving plate 5. A second universal ball 26 for rolling cooperation with the side wall of the driving plate 5 and the inner wall of the outer shell 1 is movably provided on the end of the driving arm 22 away from the slide 25. A second driving source 12 for driving the rotating disk 17 to rotate is provided below the rotating disk 17. The second driving source 12 is preferably a motor.

[0096] like Figure 2 , Figure 4-Figure 8 As shown, in order to achieve that the fixed frame 14 can follow the lifting and lowering of the rotating disk 17 and will not follow the rotation of the rotating disk 17, columns 16 corresponding to the fixed frame 14 are evenly arranged on the outer periphery of the top of the rotating disk 17, and a swivel 15 is fixedly arranged on the top of multiple columns 16. The upper end of the swivel 15 is rotatably connected to the bottom of the fixed frame 14, and the side of the fixed frame 14 is provided with a limiting component for limiting the fixed frame 14. The limiting component includes guide arms 13 evenly arranged on the circumferential side walls of the fixed frame 14, and the inner wall of the outer shell 1 is provided with guide grooves 9 corresponding to the guide arms 13 one by one, and the end of the guide arm 13 away from the fixed frame 14 extends to the inner side of the guide groove 9 and cooperates with the guide groove 9 for sliding guidance.

[0097] Further, such as Figure 7As shown, as an embodiment, the top of the shaking seat 6 is open and used to place the container. The circumferential side wall of the shaking seat 6 is evenly threaded with a screw 19. The length direction of the screw 19 is consistent with the radial direction of the shaking seat 6. One end of the screw 19 extends to the inner side of the shaking seat 6 and is rotatably provided with an arc-shaped clamp 18, which is used to clamp the container.

[0098] like Figure 2 , Figure 4-Figure 6 As shown, in order to realize the lifting and lowering of the rotating disk 17 and the fixed frame 14, a lifting frame 8 is arranged at the lower inner end of the shell 1, and the second driving source 12 is fixedly installed on the lifting frame 8. A first driving source 10 for driving the lifting and lowering of the lifting frame 8 is arranged below the lifting frame 8, and the first driving source 10 is installed on the base 2. In order to increase the stability of the lifting frame 8, a guide column 11 is arranged on the outer periphery of the bottom of the lifting frame 8, and the guide column 11 cooperates with the movable guide at the upper end of the base 2. In order to facilitate the taking and placing of the container, a conical guide cylinder 4 is arranged on the top of the driving plate 5. The second universal ball 26 is also used for rolling cooperation with the inner wall of the guide cylinder 4 to reduce friction. The inside of the guide cylinder 4 and the inner side of the driving plate 5 are smoothly transitioned, and the inner diameter of the guide cylinder 4 increases successively from top to bottom, and it is configured that when the driving arm 22 corresponds to the inner wall of the upper end of the guide cylinder 4, the outer cylinder body 23 and the inner rod body 24 are in a vertical state, and the top opening of the shaking seat 6 faces upward.

[0099] As for the working principle of the chemical determination device for the iron content of silicon-aluminum alloy, when the solution needs to be shaken during use, the container containing the solution is placed in the opening at the top of the shaking seat 6, the sealing cover is fixed on the top of the container, and the clamping plate 18 is driven to move by screwing the screw 19 to achieve clamping of the container, and then the first driving source 10 is controlled to drive the lifting frame 8 to move downward, and the lifting frame 8 drives the rotating disk 17, the fixed frame 14 and the container as a whole to move downward, and under the action of the guide tube 4, the elastic member 27 is gradually reset, the driving arm 22 is gradually moved outward, and then the sliding seat 25 is gradually moved outward, the outer cylinder body 23 and the inner rod body 24 are tilted as a whole, and the first universal ball 21 will drive the container to tilt through the shaking seat 6 until the driving arm 22 corresponds to the driving plate 5, and the top cover 3 is covered before shaking, and the second driving source 10 is controlled. The source 12 drives the connecting seat 7 to rotate. Due to the restriction of the guide arm 13 and the guide groove 9, the fixed frame 14 remains stationary. The rotating disk 17 drives the first universal ball 21 to rotate continuously through the outer cylinder 23 and the inner rod 24. Under the action of the driving plate 5 and the guide slope 30, the driving arm 22 moves back and forth, and the outer cylinder 23 and the inner rod 24 continuously change their inclination angles and extend and retract, so that the first universal ball 21 drives the shaking seat 6 to change its inclination angle continuously and shake back and forth, thereby achieving shaking. After the end, the top cover 3 is opened, and the first driving source 10 drives the lifting frame 8, the rotating disk 17, and the fixed frame 14 to move upward as a whole. The driving arm 22 is gradually pushed inward by the inner wall of the guide cylinder 4, and the outer cylinder 23 and the inner rod 24 are gradually vertical. Finally, the container extends from the upper end of the outer shell 1 and can be removed.

[0100] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited by the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A chemical determination method for iron content in silicon aluminum alloy, characterized in that: The following steps are involved: S1: Sample dissolution, weigh 0.1g of silicon aluminum alloy into a 100ml plastic beaker, add 1ml nitric acid to soak the sample, then add 4-6ml hydrofluoric acid in small amounts and multiple times, add 5ml potassium nitrate solution after the yellow smoke disappears, filter the precipitate, add 3ml saturated boric acid solution to the filtrate, let it stand for 3 minutes, then transfer to a 100ml volumetric flask, make up to volume, shake well, and set aside; S2: Standard curve drawing: according to the content of iron in the sample to be tested, a series of gradient standard solutions with different high and low ranges are prepared, and high and low range standard curves are drawn according to the absorbance and concentration of different standard solutions; S3: o-phenanthroline spectrophotometric method for testing iron, according to the iron content in the sample to be tested, 1-5 ml of the filtrate is taken and placed in a 50 ml volumetric flask, diluted with water to about 15 ml, 2.5 ml of hydroxylamine hydrochloride solution is added, shaken and left for a while, 1 ml of tartaric acid solution is added, and an appropriate amount of sodium acetate solution is added to adjust the pH to 3-6, 2 ml of o-phenanthroline ethanol solution is added, diluted with water to the scale and shaken, after 15 minutes, the reagent blank is used as a reference, and the absorbance is measured at a wavelength of 510 nm, the concentration of ferric oxide is found from the standard curve, and the result is calculated; The device for shaking in steps S1-S3 comprises a housing (1), a shaking assembly is arranged in the housing (1), the shaking assembly comprises a rotating disk (17) arranged inside the housing (1), a fixing frame (14) located on the top of the rotating disk (17) is arranged at the inner upper end of the housing (1), a rotating sleeve (20) is arranged in the middle of the fixing frame (14), a first universal ball (21) is movably arranged inside the rotating sleeve (20), a shaking seat (6) for fixing the container is fixedly arranged at the upper end of the first universal ball (21), an inner rod body (24) is movably connected to the bottom of the first universal ball (21), an outer cylinder body (23) is movably sleeved on the outer side of the lower end of the inner rod body (24), a sliding groove (28) is arranged at one end of the top of the rotating disk (17) along the radial direction, and the sliding groove (28) is arranged at the inner side of the rotating sleeve (20). A slide seat (25) is movably connected to the inner side of the groove (28) along the radial direction of the rotating disk (17); the lower end of the outer cylinder (23) is movably connected to the upper end of the slide seat (25); a driving arm (22) extending to the outside of the rotating disk (17) is provided on the side of the slide seat (25) away from the axis of the rotating disk (17); an elastic member (27) is provided between the side of the slide seat (25) close to the axis of the rotating disk (17) and the inner wall of the slide groove (28); a driving plate (5) corresponding to the driving arm (22) is provided on the inner wall of the outer shell (1); and guide slopes (30) that smoothly transition to the inner wall of the outer shell (1) are provided at both ends of the driving plate (5); and a second driving source (12) for driving the rotating disk (17) to rotate is provided below the rotating disk (17); The top of the mixing seat (6) is open and is used to place the container. The circumferential side wall of the mixing seat (6) is evenly threaded with a screw (19). The length direction of the screw (19) is consistent with the radial direction of the mixing seat (6). One end of the screw (19) extends to the inner side of the mixing seat (6) and is rotatably provided with an arc-shaped clamping plate (18). The clamping plate (18) is used to clamp the container. A first driving source (10) for driving the lifting frame (8) to move upward and downward is arranged below the lifting frame (8), and a conical guide tube (4) is arranged on the top of the driving plate (5), the interior of the guide tube (4) and the inner side of the driving plate (5) are smoothly transitioned, and the inner diameter of the guide tube (4) increases from top to bottom, and is configured such that when the driving arm (22) corresponds to the inner wall of the upper end of the guide tube (4), the outer tube body (23) and the inner rod body (24) are in a vertical state, and the top opening of the shaking seat (6) faces upward.

2. The method for chemical determination of iron content in silicon aluminum alloy according to claim 1, characterized in that: In step S2, when configuring a series of high and low range gradient standard solutions and drawing high and low range standard curves according to the absorbance and concentration of different standard solutions, take 0 ml, 0.5 ml, 1 ml, 1.5 ml, 2 ml, 2.5 ml, and 3 ml of ferric oxide standard solution, respectively place them in 50 ml volumetric flasks, dilute with water to about 15 ml, add 2.5 ml of hydroxylamine hydrochloride solution, shake and let stand for a while, add 1 ml of tartaric acid solution, add an appropriate amount of sodium acetate solution to adjust pH=3-6, add 2 ml of o-phenanthroline ethanol solution, dilute with water to the scale, shake, after 15 minutes, use the reagent blank solution as a control, measure its absorbance at a wavelength of 510 nanometers, and draw a standard curve with the concentration of ferric oxide as the horizontal coordinate and the absorbance as the vertical coordinate.

3. The method for chemical determination of iron content in silicon aluminum alloy according to claim 1, characterized in that: In step S3, the result calculation formula is: In the formula: X is the iron content in the sample, %; C is the concentration of ferric oxide in the test solution obtained from the standard curve, μg / mL; C0 is the concentration of ferric oxide in the blank solution accompanying the sample obtained from the standard curve, μg / mL; V is the constant volume of the sample on the machine, mL; f is the dilution factor of the sample solution; m is the weight of the sample, g; 159.69 is the molecular weight of ferric oxide.

4. The method for chemical determination of iron content in silicon aluminum alloy according to claim 1, characterized in that: The top periphery of the rotating disk (17) is evenly provided with upright posts (16) corresponding to the fixed frame (14), and a rotating ring (15) is fixedly provided on the top of the plurality of upright posts (16), and the upper end of the rotating ring (15) is rotatably connected to the bottom of the fixed frame (14).

5. A chemical determination method of iron content in silicon aluminum alloy according to claim 4, characterized in that: A limiting assembly for limiting the fixing frame (14) is arranged on the side of the fixing frame (14), the limiting assembly comprising guide arms (13) uniformly arranged on the circumferential side wall of the fixing frame (14), the inner wall of the housing (1) is provided with guide grooves (9) corresponding to the guide arms (13), and one end of the guide arm (13) away from the fixing frame (14) extends along the inner side of the guide groove (9) and cooperates with the guide groove (9) for sliding guidance.

6. The method for chemical determination of iron content in silicon aluminum alloy according to claim 1, characterized in that: A lifting frame (8) is provided at the inner lower end of the housing (1), and the second driving source (12) is fixedly mounted on the lifting frame (8), and the second driving source (12) is a motor.

7. The method for chemical determination of iron content in silicon aluminum alloy according to claim 1, characterized in that: The container is a beaker, a volumetric flask or a test tube.

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