Infrared carbon and sulfur analyzer for measuring trace carbon
By introducing the automatic adjustment of crucible position and multi-stage sealing structure in the carbon-sulfur analyzer, the problem of poor combustion caused by manual loading is solved, and higher detection accuracy and combustion efficiency are achieved.
Patent Information
- Application Number
- CN202421636184.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-10
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2034-07-10
AI Technical Summary
During the loading process of existing carbon-sulfur analyzers, it is difficult to adjust the crucible position due to the narrow manual clamping, resulting in poor combustion effect and affecting the detection accuracy.
The feeding protection structure and multi-stage sealing structure that automatically adjust the crucible position are adopted to ensure the accurate positioning and sealing of the crucible in the combustion chamber, thereby improving the combustion effect.
By automatically adjusting the crucible position and sealing structure, the accuracy of carbon content detection and combustion efficiency are improved, external air interference is reduced, and the accuracy of test results is ensured.
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Figure CN223320371U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to a carbon-sulfur analyzer, in particular to an infrared carbon-sulfur analyzer for determining trace carbon. Background Art
[0002] The carbon and sulfur analyzer uses a high-performance lithium tantalate pyroelectric infrared sensor and full-range high-frequency combustion technology to measure the carbon and sulfur content in ferrous metals, non-ferrous metals, rare earth metals, inorganic substances, mineral porcelain and other substances. The principle of the carbon and sulfur analyzer is to place the sample in a high-temperature furnace for oxygen combustion to generate and release CO2 and SO2 gases, thereby separating carbon and sulfur elements from metal elements and their compounds, measuring the gas content of CO2 and SO2, and then converting the specific content of the components in the sample to obtain the measurement results.
[0003] In the existing technology, before analysis, the sample to be tested needs to be placed in a crucible, and the crucible is placed on a push-pull seat by a clamp. The crucible is pushed to the heating zone by the push-pull seat, and the material in the crucible is heated and burned by the heater. During the manual clamping stage, since it is clamped manually and the loading area is relatively narrow to improve the fit, it is difficult to manually adjust the position of the crucible after loading. The overall sealing of the crucible after it is sent to the loading area will also affect the accuracy of carbon detection, thereby affecting the combustion effect. If the heat dissipation effect during combustion is not good, it is also easy to cause subtle effects on the entire sampling and combustion process. Utility Model Content
[0004] The utility model provides an infrared carbon-sulfur analyzer for trace carbon determination, which can automatically adjust the position of the crucible after manual loading and can perform local sealing after the crucible reaches the specified position, thereby improving the overall combustion effect and further improving the detection accuracy of the carbon content, and can effectively solve the above-mentioned problems.
[0005] The utility model is achieved in this way:
[0006] An infrared carbon-sulfur analyzer for trace carbon determination comprises a cabinet, wherein an analysis chamber, a plurality of switches, and detection instruments are provided within the cabinet; a high-frequency furnace is provided on the cabinet, wherein the high-frequency furnace comprises a combustion chamber for heating; a loading rod for placing a crucible is provided below the combustion chamber; and the carbon-sulfur analyzer further comprises:
[0007] The feeding protection structure, the feeding rod is fixed in a lower power box, a hydraulic push rod is provided in the lower power box, the feeding rod is hollow, the feeding protection structure includes a carrying piece arranged at the top edge of the feeding rod, one end of the carrying piece is movably connected to the inner wall of the feeding rod through a movable shaft, the bottom of the carrying piece is driven by a bottom flipping assembly, the movable shaft and the bottom flipping assembly are both provided on an electric push rod, when the crucible needs to be loaded, the bottom flipping assembly drives the carrying piece to flip and tilt along the movable shaft, after the crucible is placed on the carrying piece, the bottom flipping assembly resets and drives the carrying piece to return to a horizontal position, and the electric push rod drives the movable shaft and the bottom flipping assembly to move downward until the carrying piece is retracted into the inner side of the feeding rod;
[0008] A multi-stage sealing structure, wherein a matching cylinder is connected to the bottom of the combustion chamber, and the multi-stage sealing structure comprises a first matching guard plate arranged above the feeding rod, a second matching guard plate is arranged on the inner side of the matching cylinder, and a sealing ring is arranged at the lower end of the matching cylinder. When the hydraulic push rod drives the feeding rod to move upward, the first matching guard plate and the second matching guard plate form a circular closed surface, and the inner side of the sealing ring is clamped on the outer side of the feeding rod.
[0009] As a further improvement, the carrier plate includes a placement plate connected to the movable shaft, a fixed plate is provided on the placement plate, the diameter of the fixed plate is smaller than the diameter of the placement plate, and the crucible is located on the fixed plate.
[0010] As a further improvement, the movable shaft includes a hinged shaft hinged on the side of the placement plate, the bottom of the hinged shaft is fixed on an extension rod, the extension rod is attached to the inner wall of the loading rod, and the bottom of the extension rod is connected to the electric push rod.
[0011] As a further improvement, the bottom flip assembly includes an upper movable button seat arranged at the bottom of the carrier plate, a flip motor is connected below the upper movable button seat, and the bottom of the flip motor is connected to a lower movable button seat connected to the electric push rod.
[0012] As a further improvement, a heat insulation block is provided between the movable shaft, the bottom flip assembly and the electric push rod, and the extension rod and the lower movable button seat are both fixed on the heat insulation block.
[0013] As a further improvement, a heat dissipation casing is provided on the outside of the combustion chamber, and the heat dissipation casing includes an inner fixing frame fixedly connected to the outside of the combustion chamber, an outer fixing frame is provided on the outside of the inner fixing frame, and the outer fixing frame is spaced apart from the inner fixing frame. A first heat dissipation area is provided on the front of the outer fixing frame, and a second heat dissipation area is provided on both sides of the outer fixing frame.
[0014] The utility model also provides a method for measuring trace carbon in a gold target material using a carbon-sulfur analyzer, which uses the above-mentioned infrared carbon-sulfur analyzer for trace carbon determination, comprising the following steps:
[0015] S1: Crucible pretreatment: Place the crucible with the opening facing upward in the muffle furnace at 1100°C for 2-4 hours. When the temperature drops below 200°C, remove the crucible and store it in a desiccator.
[0016] S2: Sample processing: Cut the sample into small pieces, add nitric acid and heat to boil on a hot plate, wash with distilled water and dry for later use;
[0017] S3: Carbon and sulfur analyzer detection: Weigh the sample in S2 and place it in a crucible. Use tweezers to clamp the crucible into the loading rod, push the loading rod into the combustion chamber for combustion, and the generated CO2 enters the analysis chamber for analysis.
[0018] As a further improvement, the S3 specifically includes:
[0019] S31: Before clamping the crucible to the loading rod, first control the bottom flip assembly to drive the carrier to flip sideways, so that the experimenter can better locate the position of the crucible when placing the material;
[0020] S32: After the crucible is in place, the bottom flip assembly is reset, the carrier is reset to a horizontal position, and the electric push rod drives the carrier to retract, so that the entire carrier and the crucible are retracted to the inside of the loading rod;
[0021] S33: The entire feeding rod is pushed upward by the hydraulic push rod, so that the first matching guard plate and the second matching guard plate on the feeding rod form a complete sealing ring structure, forming a double-layer sealing limit with the sealing ring at the bottom.
[0022] The beneficial effects of the utility model are:
[0023] In the existing feeding structure of carbon-sulfur analyzers, the experimenter often clamps the crucible to the position of the feeding rod through the experimental clamp, and then directly pushes the feeding rod to the heated area for heating. However, with this feeding method, due to the narrow feeding position, it is difficult for the experimenter to adjust the position of the crucible. If the crucible is not placed in a good position during feeding, it will affect the subsequent combustion effect. Therefore, this case adds a feeding protection structure. First, during the placement stage of the crucible, the bottom flip assembly drives the movable carrier to tilt, allowing the experimenter to be more flexible when loading on one side. It is easy to add and even easier to put the crucible in the correct position. After the crucible is fixed, the movable shaft of the fixed carrier and the bottom flip assembly are pulled down by the electric push rod, thereby driving the crucible on the carrier to shrink downward. Even if the position of the crucible is a little deviated at this time, it will be corrected to the correct position due to touching the inner wall of the loading rod downward. If the crucible is already placed in the correct position, there will be no interference during the shrinking process, so that the crucible can reach the accurate position, and the combustion efficiency can be guaranteed during combustion, thereby improving the detection accuracy of carbon content.
[0024] Since the carrier plate needs to be tilted, in order to improve the fixing effect of the crucible, the carrier plate is divided into two parts. One part is a placement plate used to isolate heat from dissipating. The placement plate can prevent the heat during combustion from dissipating downward and affecting the bottom flipping component; the other part is used to fix the crucible, so that the crucible is stuck on the fixing plate, thereby preventing it from tipping over when tilting to load materials, and also preventing it from tilting during the reset stage.
[0025] In order to achieve the rotation effect of the carrier plate and support it, a movable shaft is set on the side of the carrier plate, and a rotatably installed hinge shaft is set at one end of the movable shaft, so that the carrier plate can achieve unilateral rotation and tilt, allowing it to tilt toward the feeding side. After the carrier plate is reset, the extension rod can provide longitudinal support to the carrier plate, thereby achieving the effect of tilted feeding and stable combustion.
[0026] After the crucible reaches the designated position, the sample in the crucible is fully burned by the heater in the combustion chamber. During this period, in order to reduce the interference of external air and facilitate the collection of gas, a certain degree of sealing is required. In the existing structure, only the fit between the crucible itself and the combustion chamber is relied upon, but this fit is likely to cause external air to interfere with the combustion process. Therefore, the utility model sets a multi-stage sealing structure on the basis of the feeding protection structure. When the crucible rises with the feeding rod, the first matching guard plate on the feeding rod will rise accordingly. After the feeding rod is in place, the first matching guard plate will be embedded in the matching tube , and the second matching guard plate in the matching cylinder forms a complete circular closed structure, and the feeding rod and the crucible are within the coverage of this circular closed structure, so that when the sample on the crucible is processed, the CO2 generated will only run upwards, and at the same time, the external air will not be able to enter the internal interference of the combustion chamber, and a sealing ring is also provided at the bottom of the entire matching cylinder. The sealing ring can squeeze the outer wall of the feeding rod, thereby holding the feeding rod tightly and isolating it from the external space. At the same time, since the sealing ring is provided at the lower end of the circular closed structure, it will not be affected by high temperature, thereby avoiding its softening and deformation due to the effect of high temperature. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 The utility model is a three-dimensional structural schematic diagram of an infrared carbon-sulfur analyzer for determining trace carbon.
[0028] Figure 2 This utility model Figure 1 Schematic diagram of the top view structure.
[0029] Figure 3 This utility model Figure 2 Cross-section view at AA in the middle.
[0030] Figure 4 It is a structural schematic diagram of the feeding protection structure of the utility model.
[0031] Figure 5 This utility model Figure 4 A top view of the structure.
[0032] Figure 6 This utility model Figure 5 Cross-section view at the middle BB.
[0033] Figure 7 It is an isometric side cross-sectional view (back view) of the heat dissipation housing of the present invention.
[0034] In the picture:
[0035] Cabinet 10, high-frequency furnace 20, combustion chamber 21, loading rod 22, lower power box 23, hydraulic push rod 24, matching cylinder 25, loading protection structure 30, load-bearing plate 31, placement plate 311, fixed plate 312, movable shaft 32, hinge shaft 321, extension rod 322, bottom flip assembly 33, upper movable button seat 331, flip motor 332, lower movable button seat 333, electric push rod 34, insulation block 35, multi-stage sealing structure 40, first matching guard plate 41, second matching guard plate 42, sealing ring 43, heat dissipation casing 50, inner fixing frame 51, first heat dissipation area 52, outer fixing frame 53, second heat dissipation area 54. DETAILED DESCRIPTION
[0036] All embodiments of the present invention fall within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but rather merely represents selected embodiments of the present invention. All other embodiments derived by persons of ordinary skill in the art based on the embodiments of the present invention without inventive effort fall within the scope of protection of the present invention.
[0037] In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as referring to the purpose, technical solutions and advantages of the methods. To be clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work indicate or imply relative importance or implicitly indicate the number of indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.
[0038] Reference Figures 1 to 7As shown, an infrared carbon-sulfur analyzer for trace carbon determination comprises a cabinet 10, wherein the cabinet 10 is provided with an analysis chamber, a plurality of switches and detection instruments, a high-frequency furnace 20 is provided on the cabinet 10, and the high-frequency furnace 20 comprises a combustion chamber 21 for heating, and a loading rod 22 for placing a crucible is provided below the combustion chamber 21, and the carbon-sulfur analyzer further comprises: a loading protection structure 30, wherein the loading rod 22 is fixed in a lower power box 23, and a hydraulic push rod 24 is provided in the lower power box 23, and the loading rod 22 is hollow, and the loading protection structure 30 comprises a bearing plate 31 provided on the top edge of the loading rod 22, and one end of the bearing plate 31 is movably connected to the inner wall of the loading rod 22 through a movable shaft 32, and the bottom of the bearing plate 31 is driven by a bottom flip assembly 33, and the movable shaft 32 and the bottom flip assembly 33 are both provided on an electric push rod 34. When the crucible needs to be loaded, the bottom flipping assembly 33 drives the supporting plate 31 to flip and tilt along the movable shaft 32. After the crucible is placed on the supporting plate 31, the bottom flipping assembly 33 is reset and drives the supporting plate 31 to return to a horizontal position, and the electric push rod 34 drives the movable shaft 32 and the bottom flipping assembly 33 to move downward until the supporting plate 31 is retracted into the inner side of the loading rod 22; a multi-stage sealing structure 40, a matching cylinder 25 is connected to the bottom of the combustion chamber 21, and the multi-stage sealing structure 40 includes a first matching guard plate 41 arranged above the loading rod 22, and a second matching guard plate 42 is arranged on the inner side of the matching cylinder 25, and a sealing ring 43 is arranged at the lower end of the matching cylinder 25. When the hydraulic push rod 24 drives the loading rod 22 to move upward, the first matching guard plate 41 and the second matching guard plate 42 form a circular closed surface, and the inner side of the sealing ring 43 is clamped on the outer side of the loading rod 22.
[0039] The carbon and sulfur analyzer in this embodiment is only used to detect CO2 in the sample, but in actual use, different modes can be set to analyze other components, such as SO2.
[0040] In the existing feeding structure of the carbon-sulfur analyzer, the experimenter often clamps the crucible to the position of the feeding rod 22 through the experimental clamp, and then directly pushes the feeding rod 22 to the heated area for heating. However, with such a feeding method, it is difficult for the experimenter to adjust the position of the crucible due to the narrow feeding position. If the crucible is not placed in a good position during feeding, it will affect the subsequent combustion effect. Therefore, in this case, an additional feeding protection structure 30 is added. First, during the placement stage of the crucible, the bottom flip assembly 33 is used to drive the movable carrier 31 to tilt, so that the experimenter can be more comfortable when feeding on one side. It is easy to put the crucible in the correct position. After the crucible is fixed, the movable shaft 32 of the fixed carrier plate 31 and the bottom flip assembly 33 are pulled downward by the electric push rod 34, thereby driving the crucible on the carrier plate 31 to retract downward. Even if the position of the crucible is a little deviated at this time, it will be corrected to the correct position due to touching the inner wall of the loading rod 22 downward. If the crucible is already placed in the correct position, there will be no interference during the retraction process, so that the crucible can reach the correct position, and the combustion efficiency can be guaranteed during combustion, thereby improving the detection accuracy of the carbon content.
[0041] Since the carrier plate 31 needs to be tilted, in order to improve the fixing effect of the crucible, specifically, the carrier plate 31 includes a placement plate 311 connected to the movable shaft 32, and a fixing plate 312 is provided on the placement plate 311. The diameter of the fixing plate 312 is smaller than the diameter of the placement plate 311. The crucible is located on the fixing plate 312, and the carrier plate 31 is divided into two parts. One part is the placement plate 311 for isolating heat overflow. The placement plate 311 can prevent the heat during combustion from overflowing downward and affecting the bottom flipping component 33, and the other part is used to fix the crucible, so that the crucible is stuck on the fixing plate 312, thereby preventing it from tipping over when tilting to load materials, and also avoiding it from tilting during the reset stage.
[0042] In order to realize the rotation effect of the supporting plate 31 and support it, a movable shaft 32 is set on the side of the supporting plate 31, and the movable shaft 32 includes a hinge shaft 321 hinged on the side of the placement plate 311, and the bottom of the hinge shaft 321 is fixed on an extension rod 322, and the extension rod 322 is attached to the inner wall of the loading rod 22, and the bottom of the extension rod 322 is connected to the electric push rod 34. A rotatably mounted hinge shaft 321 is set at one end of the movable shaft 32, so that the supporting plate 31 can realize unilateral rotation and tilting, and tilt it toward the loading side. After the supporting plate 31 is reset, the extension rod 322 can play a longitudinal support effect on the supporting plate 31, thereby realizing the effect of loading tilt and stable combustion.
[0043] Since the movable shaft 32 is a unilaterally rotatable structure, the corresponding bottom flipping assembly 33 also needs to be set as a movable structure. Specifically, the bottom flipping assembly 33 includes an upper movable button seat 331 arranged at the bottom of the supporting plate 31, and a flipping motor 332 is connected to the bottom of the upper movable button seat 331. The bottom of the flipping motor 332 is connected to the lower movable button seat 333 connected to the electric push rod 34. When the supporting plate 31 needs to be rotated, the flipping motor 332 is used to flip the supporting plate 31 upward, so that the supporting plate 31 is flipped upward with the hinge shaft 321 as the fulcrum. When the supporting plate 31 is in the reset state, the flipping motor 332 and the extension rod 322 are used for bilateral support, making the supporting plate 31 more stable.
[0044] In order to further reduce the impact of heat during combustion on the electric push rod 34, an insulation block 35 is provided between the movable shaft 32, the bottom flip assembly 33 and the electric push rod 34, and the extension rod 322 and the lower movable button seat 333 are both fixed on the insulation block 35. The insulation block 35 adapted to the inner wall of the loading rod 22 can greatly prevent heat from penetrating into the area of the electric push rod 34, thereby preventing the electric push rod 34 from being affected.
[0045] During the combustion process in the combustion chamber 21, a certain amount of heat is generated, which needs to be discharged. However, if the entire combustion chamber 21 is dissipated in one direction, the location is prone to overheating. Therefore, in this embodiment, a heat dissipation housing 50 is provided on the outside of the combustion chamber 21. The heat dissipation housing 50 includes an inner fixing frame 51 fixedly connected to the outside of the combustion chamber 21. An outer fixing frame 53 is provided on the outside of the inner fixing frame 51. The outer fixing frame 53 is spaced apart from the inner fixing frame 51. A first heat dissipation area 52 is provided on the front of the outer fixing frame 53. A second heat dissipation area 54 is provided on both sides of the outer fixing frame 53. A channel is formed between the outer fixing frame 53 and the inner fixing frame 51. A hole is opened in the position corresponding to the first heat dissipation area 52 in the inner fixing frame 51. The heat in the inner fixing frame 51 is discharged to the first heat dissipation area 52 through the hole. Part of the heat discharged from the first heat dissipation area 52 will overflow to the second heat dissipation area 54 through the channel. Since the second heat dissipation area 54 is not directly connected to the combustion chamber 21, the overall sealing will not be greatly affected, thereby achieving multi-directional exhaust without causing too much impact.
[0046] After the crucible reaches the designated position, the sample in the crucible is fully burned by the heater in the combustion chamber 21. During this period, in order to reduce the interference of external air and facilitate the collection of gas, a certain degree of sealing is required. In the existing structure, only the fit between the crucible itself and the combustion chamber 21 is relied upon. However, this fit can easily cause external air to interfere with the combustion process. Therefore, the present invention provides a multi-stage sealing structure 40 based on the feeding protection structure 30. When the crucible rises with the feeding rod 22, the first matching guard plate 41 on the feeding rod 22 will rise accordingly. After the feeding rod 22 is in place, the first matching guard plate 41 will be embedded in the matching tube 25. , and the second matching guard plate 42 in the matching cylinder 25 form a complete circular closed structure, and the loading rod 22 and the crucible are within the coverage of this circular closed structure, so that when the sample on the crucible is processed, the generated CO2 will only run upwards, and at the same time, the external air cannot enter the internal interference of the combustion chamber 21, and a sealing ring 43 is also provided at the bottom of the entire matching cylinder 25. The sealing ring 43 can squeeze the outer wall of the loading rod 22, thereby tightly holding the loading rod 22 and isolating it from the external space. At the same time, since the sealing ring 43 is provided at the lower end of the circular closed structure, it will not be affected by high temperature, thereby avoiding its softening and deformation due to the effect of high temperature.
[0047] In another embodiment of the present invention, a method for measuring trace carbon in a gold target using a carbon-sulfur analyzer is provided. The method uses the carbon-sulfur analyzer described above, and includes the following steps:
[0048] S1: Crucible pretreatment: Place the crucible with the opening facing upward in the muffle furnace at 1100°C for 2-4 hours. When the temperature drops below 200°C, remove the crucible and store it in a desiccator.
[0049] S2: Sample processing: Cut the sample into 1g, add nitric acid (1+1), and heat to boil on a hot plate. Rinse with distilled water and dry for later use.
[0050] S3: Carbon-sulfur analyzer detection: Weigh the sample in S2 and place it in a crucible. Use tweezers to clamp the crucible into the loading rod 22, and push the loading rod 22 into the combustion chamber 21 for combustion. The generated CO2 enters the analysis chamber for analysis.
[0051] Furthermore, the S3 specifically includes:
[0052] S31: Before clamping the crucible to the loading rod 22, the bottom flip assembly 33 is controlled to drive the carrier 31 to flip sideways, so that the experimenter can better locate the position of the crucible when placing the material;
[0053] S32: After the crucible is in place, the bottom flip assembly 33 is reset, the carrier 31 is reset to a horizontal position, and the electric push rod 34 drives the carrier 31 to retract, so that the entire carrier 31 and the crucible are retracted to the inner side of the loading rod 22;
[0054] S33: The entire loading rod 22 is pushed upward by the hydraulic push rod 24, so that the first matching guard plate 41 and the second matching guard plate 42 on the loading rod 22 form a complete sealing ring structure, forming a double-layer sealing limit with the sealing ring 43 at the bottom.
[0055] In this example, 1 g of high-purity gold and 0.2 g of a steel sample were weighed, and carbon content was measured twice at 1050°C, 1100°C, 1150°C, and 1200°C, respectively, to investigate the effect of the measurement temperature on carbon determination. The test results are shown in Table 1 below.
[0056] Table 1
[0057]
[0058]
[0059] As shown in Table 1, the samples burned incompletely at 1050°C and 1100°C, resulting in low results. However, the samples burned completely at 1150°C and 1200°C, resulting in good results. However, since 1200°C is close to the melting point of the crucible, which can easily cause the crucible to bend and deform, 1150°C was used as the measurement temperature.
[0060] Contamination from machining metal debris, lubricating oil, and other contaminants, as well as transportation and storage, can have a significant impact on the accuracy and stability of the measurement results. This study examined the carbon content of carbon-free high-purity gold samples measured at 1150°C after storage for a period of time, followed by cleaning with nitric acid and hydrochloric acid, and baking at different temperatures. The carbon content results for samples treated in different ways are shown in Table 2 below.
[0061] Table 2
[0062]
[0063] Table 2 shows that the carbon content is lower after heating and cleaning with nitric acid (1+1). Using nitric acid solution (1+1) to heat and clean the sample has a relatively ideal surface decontamination effect. This method selects nitric acid (1+1) heating and cleaning as the sample treatment method.
[0064] The air contains carbon dioxide and dust particles, which will have a great impact on the accuracy and stability of the measurement results. Take a blank high-purity gold sample, place it in the air, and measure the carbon results after different periods of time. The results are shown in Table 3.
[0065] Table 3
[0066]
[0067] As shown in Table 3, the sample contained approximately 0.00004% carbon after being exposed to air for 5 minutes, and reached 0.000146% carbon after 3 days. Exposure of the sample to air resulted in an increase in carbon content, which had a significant impact on the determination of trace carbon in high-purity gold.
[0068] To this end, in this example, the carbon content of carbon-free high-purity gold samples measured at 1150°C was investigated in a ziplock bag, a weighing bottle, a vacuumed aluminum foil bag, and a weighing bottle placed in an aluminum foil bag under vacuum. The carbon content measurement results of the samples under different storage methods are shown in Table 4.
[0069] Table 4
[0070]
[0071] As shown in Table 4, the effect of placing a weighing bottle in an aluminum foil bag for vacuum storage of samples is ideal. However, the weighing bottle is prone to breakage during vacuuming, and a thickened weighing bottle can be used. Taking all factors into consideration, this experiment chose to place a weighing bottle in an aluminum foil bag for vacuum storage of samples.
[0072] High-purity gold samples were weighed, with sample weights of 0.5 g, 1.5 g, and 2.0 g, and carbon was determined three times. The effect of sample weight on carbon determination was investigated. The test results are shown in Table 5.
[0073] Table 5
[0074]
[0075] As shown in Table 5, all samples can be completely burned. When the sample size is small, the results are less stable. When the sample size is more than 1g, the results are stable and meet the analysis requirements. Taking all factors into consideration, the sample size is 1g.
[0076] It can be seen from this that the method of this embodiment uses an appropriate sample amount and the most appropriate processing temperature to reasonably process and preserve the sample, thereby improving the completeness of sample combustion and further improving the precision of carbon detection.
[0077] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that the present invention is susceptible to various modifications and variations. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.
Claims
1. An infrared carbon-sulfur analyzer for trace carbon determination, characterized in that: The invention comprises a cabinet (10), wherein an analysis chamber, a plurality of switches and detection instruments are arranged in the cabinet (10), a high-frequency furnace (20) is arranged on the cabinet (10), the high-frequency furnace (20) comprises a combustion chamber (21) for heating, a loading rod (22) for placing a crucible is arranged below the combustion chamber (21), and further comprises: A feeding protection structure (30), wherein the feeding rod (22) is fixed in a lower power box (23), a hydraulic push rod (24) is provided in the lower power box (23), the feeding rod (22) is hollow, the feeding protection structure (30) comprises a supporting plate (31) provided on the top edge of the feeding rod (22), one end of the supporting plate (31) is movably connected to the inner wall of the feeding rod (22) through a movable shaft (32), the bottom of the supporting plate (31) is driven by a bottom flipping assembly (33), and the movable shaft (32) and the bottom flipping assembly (33) are both provided on an electric push rod (34).
2. The infrared carbon-sulfur analyzer for trace carbon determination according to claim 1, characterized in that: The carrier plate (31) includes a placement plate (311) connected to a movable shaft (32). A fixing plate (312) is provided on the placement plate (311). The diameter of the fixing plate (312) is smaller than the diameter of the placement plate (311). The crucible is located on the fixing plate (312).
3. The infrared carbon-sulfur analyzer for trace carbon determination according to claim 2, characterized in that: The movable shaft (32) includes a hinge shaft (321) hinged to the side of the placement plate (311), the bottom of the hinge shaft (321) is fixed on an extension rod (322), the extension rod (322) is attached to the inner wall of the loading rod (22), and the bottom of the extension rod (322) is connected to the electric push rod (34).
4. The infrared carbon-sulfur analyzer for trace carbon determination according to claim 3, characterized in that: The bottom flip assembly (33) comprises an upper movable button seat (331) arranged at the bottom of the carrier plate (31), a flip motor (332) is connected below the upper movable button seat (331), and a lower movable button seat (333) connected to the electric push rod (34) is connected to the bottom of the flip motor (332).
5. The infrared carbon-sulfur analyzer for trace carbon determination according to claim 4, characterized in that: A heat insulation block (35) is provided between the movable shaft (32), the bottom flip assembly (33) and the electric push rod (34), and the extension rod (322) and the lower movable button seat (333) are both fixed on the heat insulation block (35).
6. The infrared carbon-sulfur analyzer for trace carbon determination according to claim 1, characterized in that: A heat dissipation housing (50) is sleeved on the outer side of the combustion chamber (21), and the heat dissipation housing (50) includes an inner fixing frame (51) fixedly connected to the outer side of the combustion chamber (21), an outer fixing frame (53) is arranged on the outer side of the inner fixing frame (51), and the outer fixing frame (53) is spaced apart from the inner fixing frame (51), a first heat dissipation area (52) is opened on the front side of the outer fixing frame (53), and second heat dissipation areas (54) are arranged on both sides of the outer fixing frame (53).