阅读说明：本技术 一种金属铼中氧含量的测定方法 (Method for measuring oxygen content in metal rhenium ) 是由 谢君 侯桂臣 盛乃成 周亦胄 张典 于 2020-11-09 设计创作，主要内容包括：本发明涉及一种金属铼中氧含量的测定方法,属于金属材料气体分析领域。该测定方法采用脉冲熔融-红外吸收方法测定铼中杂质氧的含量,其流程如下：对柱状样品直切取样→超声波清洗处理→调试脉冲红外热导氧氮分析仪的工作参数→标准工作曲线的建立→对样品进行测定→挥发污染的实时校正。本发明通过的剪切工具为液压剪样机,将大块柱状铼样品直接切下小块残片,再用铁剪剪成颗粒,选定称样量0.10g～0.20g,分析功率5500W,采用镀铂镍篮作为助熔剂,结合“自动监控校正法”,建立了金属铼中氧的测试方法,可解决金属铼在分析过程中的污染干扰问题。(The invention relates to a method for measuring oxygen content in metal rhenium, and belongs to the field of gas analysis of metal materials. The determination method adopts a pulse melting-infrared absorption method to determine the content of impurity oxygen in rhenium, and comprises the following steps: sampling a columnar sample directly → ultrasonic cleaning treatment → debugging the working parameters of the pulse infrared thermal oxygen nitrogen analyzer → establishing a standard working curve → measuring the sample → correcting the volatile pollution in real time. The invention uses a hydraulic sample shearing machine as a shearing tool, directly cuts a large columnar rhenium sample into small fragments, then uses iron shears to shear the small fragments into particles, selects a sample weighing amount of 0.10-0.20 g, has an analysis power of 5500W, adopts a platinum-plated nickel basket as a fluxing agent, combines an automatic monitoring and correcting method, establishes a method for testing oxygen in metal rhenium, and can solve the problem of pollution interference of the metal rhenium in the analysis process.)

1. A method for measuring the oxygen content in metal rhenium is characterized by comprising the following steps:

(1) sampling: the large columnar rhenium sample is directly cut into small fragments by using a hydraulic sample shearing machine as a shearing tool, and then is sheared into particles by using iron shears;

(2) sample treatment: the metallic rhenium sample is placed in a container with CCl₄Cleaning the glass ground bottle in an ultrasonic cleaning machine for 2-4 minutes, taking out a sample, and air-drying;

(3) working parameters of a pulse infrared thermal conductivity oxygen nitrogen analyzer are debugged, the heating melting sample power is adjusted to 5500W, and other parameters are the same as the analysis parameters of oxygen in common steel;

(4) establishing a standard working curve: weighing three parts of the standard sample of oxygen in steel, drawing a standard curve according to the working parameters in the step (3), wherein the linear coefficient of the working curve is more than 0.999, and the sample is determined according with the requirement, otherwise, the pulse infrared thermal conductivity oxygen nitrogen analyzer is required to be recalibrated to establish a standard working curve;

(5) application of fluxing agent: adopting a platinum-plated nickel basket as a platinum-plated nickel-based fluxing agent, firstly measuring blank, and then debugging blank parameters according to the step (3); when analyzing the sample, wrapping the sample by a platinum-plated nickel basket;

(6) and (3) real-time correction: comparing the two separate analysis results, when the difference exceeds 10 wt% of the total amount, the calibration is carried out in real time by using a standard sample or an internal control standard sample.

2. The method for determining oxygen content in metal rhenium according to claim 1, characterized in that the operating parameters of the pulse infrared thermal conductivity oxynitrides analyzer are as follows: the carrier gas flow rate is 300mL/min, the degassing power is 5700W, the degassing time is 30s, the analysis power is 5500W, and the analysis time is 25 s.

3. The method for determining the oxygen content in metallic rhenium according to claim 1, characterized in that the detection results are monitored by a software program: automatically comparing the analysis results of the last two times, and reminding an operator to correct the standard sample or the internal control standard sample in real time when the deviation value exceeds 10 wt%; and after the difference caused by rhenium pollution is calculated and corrected, the result of the automatic correction of the last group of data is automatically output.

4. The method for determining oxygen content in metal rhenium according to claim 1, characterized in that an internal control steel oxygen standard is adopted to replace a commercially available steel oxygen standard, and the steel oxygen standard is as follows: gbw (e)020140(w (o) 0.014 wt%); gbw (e)020143(w (o) 0.0075 wt%); gbw (e)020137(w (o) ═ 0.0034 wt%); and correcting the sample data by adopting the standard sample data of the oxygen in the steel, and displaying and printing out the corrected analysis result on line in real time.

5. The method for determining oxygen content in metal rhenium according to claim 1, wherein the metal rhenium is 0.10g to 0.20g of granular sample, and the total weight of the platinum-nickel plating basket is 0.9 g to 1.1 g.

6. The method for determining oxygen content in metal rhenium according to claim 1, characterized in that the hydraulic shear comprises: lift hand, end cap, hydraulic cylinder body, fuel tap, valve body, end seat, tool bit, concrete structure is as follows:

the bottom of one end of the lifting hand is connected with a piston rod at the upper end of a cylinder piston in a vertically arranged hydraulic cylinder body, the valve body is arranged on a vertical surface of an end seat, a valve body piston is arranged in the valve body along the vertical direction, one end of a horizontal tool bit is connected with the center of one end of the valve body piston, and a cavity at the lower end of the cylinder piston is communicated with a cavity at the other end of the valve body piston in the valve body through an oil;

the end cap sets up in the top of valve body, and the upper end of sample installation arm links to each other with the one end of end cap, and the other end and the end seat of end cap are connected, and the lower extreme of sample installation arm is installed on the horizontal plane of end seat, and arc sample installation breach is seted up to the inboard of sample installation arm, and the other end of tool bit is seted up and is installed the arc breach corresponding with sample installation breach.

7. The method for determining oxygen content in metal rhenium according to claim 6, wherein the oil valve comprises a suction valve, a return valve and a discharge valve, one end of the suction valve and one end of the discharge valve are respectively communicated with the chamber at the lower end of the piston of the cylinder body through pipelines, the other end of the suction valve is communicated with the hydraulic oil tank through a pipeline, the other end of the discharge valve is communicated with the chamber at the other end of the piston of the valve body in the valve body through a pipeline, one end of the return valve is communicated with the hydraulic oil tank through a pipeline, and the other end of the return valve is communicated with the discharge valve and the pipeline communicated with the inner cavity of the valve body through a pipeline.

Technical Field

The invention relates to a method for measuring oxygen content in metal rhenium, and belongs to the field of gas analysis of metal materials.

Background

The aeroengine is one of the most complex and multidisciplinary integrated engineering mechanical systems in the world today, and the core component is a single crystal blade. It appears that a single thin part emits surprising power, each blade delivering horsepower equivalent to a 2.0 displacement SUV. Single crystal blades are produced without departing from a precious rare metal, rhenium. Rhenium is the latest natural element found by humans, and its content in the earth's crust is smaller than all rare earth elements and is more difficult to obtain than diamond.

The oxygen content in the purification of rhenium is a key index, the oxygen content in the rhenium is not accurately measured by a common method according to the sampling and analysis results of common samples in the early stage. And (3) controlling sample transmission, sample preparation and result normalization through test investigation, and finally establishing a standard method for measuring the oxygen content in rhenium, wherein the result is stable and accurate.

The principle of oxygen analysis in metal materials is as follows: the instrument adopts high-purity helium as carrier gas, a pulse graphite electrode furnace heats and melts a sample in a graphite crucible at high temperature with the help of a sample nickel basket fluxing agent, oxygen in the sample is separated out in a form of carbon monoxide, the carbon monoxide is carried by the carrier gas and enters an infrared detector to detect the content of the carbon monoxide, and the oxygen content value is obtained through software data processing. Then the carbon monoxide is converted into carbon dioxide by a copper oxide catalytic furnace and absorbed by an alkali asbestos absorbent.

For the conventional samples, sample preparation: the sample is loaded in a plastic self-sealing bag for transmission, the sample is taken and prepared by linear cutting, and after surface oxide skin is removed by a mechanical mode, the sample is cleaned by ultrasonic waves and dried for standby. Analysis and test aspects: the sample (without wrapping) is directly put into the sample, and is heated by a pulse electrode furnace, so that the sample is melted at high temperature. Oxygen in the sample reacts with saturated C in the graphite crucible to generate a large amount of CO and a small amount of CO₂The gas enters an infrared absorption detector, and the oxygen content in the sample is obtained.

For metallic rhenium, sample preparation aspects: the sample was packed in a valve bag, which was better than a completely sealed plastic bag, and the phenomenon of oxidative discoloration of the sample surface of the valve bag was observed. The linear cutting sampling is not available, and the linear cutting sampling can only be used for preparing samples. Analysis and test aspects: the sample (without wrapping) is directly put into the sample, and is heated by a pulse electrode furnace, so that the sample is melted at high temperature. Because the oxygen potential of the metal rhenium is lower than that of other conventional analysis samples, the rhenium sample is very volatile after being melted, volatile substances capture oxygen in carbon monoxide, and the oxygen amount reaching a detector is greatly reduced, so that the oxygen detection value is reduced, and the oxygen measurement is interfered.

Disclosure of Invention

The invention aims to provide a method for measuring the oxygen content in metal rhenium, which comprises the steps of specifying a sample to be packed in vacuum or filled with argon, directly cutting and sampling by using a special tool, and measuring the content of impurity oxygen in rhenium by adopting a pulse melting-infrared absorption method and a platinum-plated nickel basket, so that the problems of oxidation, pollution and interference caused by volatilization in the analysis process of rare earth metal rhenium in sample conveying and transportation can be solved.

The technical scheme of the invention is as follows:

a method for measuring the oxygen content in metal rhenium comprises the following steps:

(1) sampling: the large columnar rhenium sample is directly cut into small fragments by using a hydraulic sample shearing machine as a shearing tool, and then is sheared into particles by using iron shears;

(2) sample treatment: the metallic rhenium sample is placed in a container with CCl₄Cleaning the glass ground bottle in an ultrasonic cleaning machine for 2-4 minutes, taking out a sample, and air-drying;

(3) working parameters of a pulse infrared thermal conductivity oxygen nitrogen analyzer are debugged, the heating melting sample power is adjusted to 5500W, and other parameters are the same as the analysis parameters of oxygen in common steel;

(4) establishing a standard working curve: weighing three parts of the standard sample of oxygen in steel, drawing a standard curve according to the working parameters in the step (3), wherein the linear coefficient of the working curve is more than 0.999, and the sample is determined according with the requirement, otherwise, the pulse infrared thermal conductivity oxygen nitrogen analyzer is required to be recalibrated to establish a standard working curve;

(5) application of fluxing agent: adopting a platinum-plated nickel basket as a platinum-plated nickel-based fluxing agent, firstly measuring blank, and then debugging blank parameters according to the step (3); when analyzing the sample, wrapping the sample by a platinum-plated nickel basket;

(6) and (3) real-time correction: comparing the two separate analysis results, when the difference exceeds 10 wt% of the total amount, the calibration is carried out in real time by using a standard sample or an internal control standard sample.

The method for measuring the oxygen content in the metal rhenium comprises the following working parameters of a pulse infrared thermal conductivity oxygen-nitrogen analyzer: the carrier gas flow rate is 300mL/min, the degassing power is 5700W, the degassing time is 30s, the analysis power is 5500W, and the analysis time is 25 s.

The method for measuring the oxygen content in the metal rhenium monitors the detection result through a software program: automatically comparing the analysis results of the last two times, and reminding an operator to correct the standard sample or the internal control standard sample in real time when the deviation value exceeds 10 wt%; and after the difference caused by rhenium pollution is calculated and corrected, the result of the automatic correction of the last group of data is automatically output.

The method for measuring the oxygen content in the metal rhenium adopts an internal control steel oxygen standard sample to replace a commercially available steel oxygen standard sample, wherein the steel oxygen standard sample comprises the following steps: gbw (e)020140(w (o) 0.014 wt%); gbw (e)020143(w (o) 0.0075 wt%); gbw (e)020137(w (o) ═ 0.0034 wt%); and correcting the sample data by adopting the standard sample data of the oxygen in the steel, and displaying and printing out the corrected analysis result on line in real time.

According to the method for measuring the oxygen content in the metal rhenium, the metal rhenium is 0.10-0.20 g of granular samples, and the total weight of the platinum-nickel plated basket is 0.9-1.1 g.

The method for measuring the oxygen content in the metal rhenium comprises the following steps: lift hand, end cap, hydraulic cylinder body, fuel tap, valve body, end seat, tool bit, concrete structure is as follows:

the bottom of one end of the lifting hand is connected with a piston rod at the upper end of a cylinder piston in a vertically arranged hydraulic cylinder body, the valve body is arranged on a vertical surface of an end seat, a valve body piston is arranged in the valve body along the vertical direction, one end of a horizontal tool bit is connected with the center of one end of the valve body piston, and a cavity at the lower end of the cylinder piston is communicated with a cavity at the other end of the valve body piston in the valve body through an oil;

the end cap sets up in the top of valve body, and the upper end of sample installation arm links to each other with the one end of end cap, and the other end and the end seat of end cap are connected, and the lower extreme of sample installation arm is installed on the horizontal plane of end seat, and arc sample installation breach is seted up to the inboard of sample installation arm, and the other end of tool bit is seted up and is installed the arc breach corresponding with sample installation breach.

The method for measuring the oxygen content in the metal rhenium comprises the following steps that an oil valve comprises a suction valve, an oil return valve and a discharge valve, one end of the suction valve and one end of the discharge valve are respectively communicated with a cavity at the lower end of a piston of a cylinder body through pipelines, the other end of the suction valve is communicated with a hydraulic oil tank through a pipeline, the other end of the discharge valve is communicated with a cavity at the other end of the piston of a valve body in the valve body through a pipeline, one end of the oil return valve is communicated with the hydraulic oil tank through a pipeline, and the other end of the oil return valve is communicated with the discharge valve and an inner.

The design idea of the invention is as follows:

the invention controls the sample conveying process, and directly cuts and samples from the columnar rhenium block sample by a hydraulic sample shearing machine of a direct cutting sampling tool, thereby avoiding the influence of pollution which cannot be eliminated and is caused by linear cutting on oxygen analysis; the platinum-nickel-plated basket is adopted to determine the content of impurity oxygen in rhenium by a pulse melting-infrared absorption method, so that the adverse effect caused by rare earth pollution is reduced; the design is out of tolerance by 10 wt% for automatic reminding, and after the standard sample or the internal control sample is used for real-time correction, the corrected result can be automatically output.

In addition, the direct cutting sampling tool is characterized in that a large columnar sample is directly cut into small fragments by a hydraulic sample shearing machine (see figure 1), and the small fragments are sheared into particles by iron shears, so that the pollution caused by linear cutting and sawing is avoided by shearing. The platinized nickel-based fluxing agent adopts a platinized nickel basket which is characterized in that the shape is the same as that of a common nickel basket (see figure 2), and the platinized nickel basket is externally plated with platinized platinum, so that the effects of fluxing and pollution inhibition are better due to the existence of the platinum.

The invention has the advantages and beneficial effects that:

1. the invention adopts a hydraulic sample shearing machine to directly sample, and solves the problems that the residue of the existing wire-electrode cutting rhenium sample can not be completely eliminated, and the result is suddenly high and suddenly low.

2. The invention takes the platinum-plated nickel basket as a fluxing agent, adopts a pulse melting-infrared absorption instrument to carry out quantitative analysis on the oxygen content in the metal rhenium, utilizes the platinum-plated nickel basket to test under certain analysis power, can effectively inhibit the volatilization pollution of rare earth metals, and establishes a quantitative analysis method for the oxygen in the metal rhenium by matching with automatic pollution monitoring and oxygen standard sample correction in the band steel.

3. The invention has the advantages of low cost, simple operation, easy control, high test precision and accurate and reliable test result, and effectively improves the analysis precision.

Drawings

Fig. 1 is a structural schematic diagram of a hydraulic pressure sample shearing machine. In the figure, 1, a lifting hand, 2, an end cap, 3, a hydraulic cylinder body, 4, an oil valve, 5, a valve body, 6, an end seat, 7, a cutter head, 8, a sample mounting notch, 9 and a sample mounting arm.

Fig. 2 is a schematic structural diagram of a platinized nickel basket. Wherein, (a) front view, (b) back view, (c) is the F-F section view of (a), (d) top view, and (e) perspective view.

Fig. 3 is a schematic diagram of a hydraulic pressure sample shearing machine. In the figure, 1, a lifting hand, 3, a hydraulic cylinder, 41, a suction valve, 42, a return valve, 43, a discharge valve, 5, a valve body, 7, a cutter head, 10, a cylinder piston, 11, a hydraulic oil tank, 12 and a valve body piston.

Detailed Description

As shown in fig. 1 and 3, the hydraulic sample shearing machine mainly comprises: the manual device, hydraulic transmission and cut off organism triplex, by lifting hand 1, end cap 2, hydraulic cylinder body 3, fuel tap 4, valve body 5, end seat 6, tool bit 7 etc. constitute, specific structure is as follows:

the bottom of one end of the lifting hand 1 is connected with a piston rod at the upper end of a cylinder piston 10 in a hydraulic cylinder 3 which is vertically arranged, a valve body 5 is arranged on a vertical surface of an end seat 6, a valve body piston 12 is vertically arranged in the valve body 5, one end of a horizontal tool bit 7 is connected with the center of one end of the valve body piston 12, and a cavity at the lower end of the cylinder piston 10 is communicated with a cavity at the other end of the valve body piston 12 in the valve body 5 through an oil valve 4. Wherein, the valve body 5 is used for: the lifting hand 1 is lifted up and down, so that the internal pressure of the valve body 5 is increased under the reciprocating action of the cylinder piston 10 in the hydraulic cylinder 3, and the cutter head 7 is pushed forward to cut; the cylinder piston 10 and the valve body piston 12 have the following functions: under the action of the lifting up and down of the lifting hand 1, the cylinder piston 10 and the valve body piston 12 are driven to increase the internal pressure of the valve body 5, so as to provide thrust for the cutting of the cutter head 7.

The oil valve 4 comprises a suction valve 41, an oil return valve 42 and a discharge valve 43, one end of the suction valve 41 and one end of the discharge valve 43 are respectively communicated with a cavity at the lower end of the cylinder piston 10 through pipelines, the other end of the suction valve 41 is communicated with the hydraulic oil tank 11 through a pipeline, the other end of the discharge valve 43 is communicated with a cavity at the other end of the valve body piston 12 in the valve body 5 through a pipeline, one end of the oil return valve 42 is communicated with the hydraulic oil tank 11 through a pipeline, the other end of the oil return valve 42 is communicated with the discharge valve 43 and a pipeline communicated with an inner cavity of the valve body 5 through a pipeline, and the: the internal pressure of the valve body 5 is controlled, the oil valve 4 is tightly closed to help the cutter head 7 to cut forwards, and the oil valve 4 is loosened to release pressure to enable the cutter head 7 to return.

End cap 2 sets up in the top of valve body 5, and the upper end of sample installation arm 9 links to each other with the one end of end cap 2, and the other end and the end seat 6 of end cap 2 are connected, and the lower extreme of sample installation arm 9 is installed on the horizontal plane of end seat 6, and arc sample installation breach 8 is seted up to the inboard of sample installation arm 9, and the other end of tool bit 7 is seted up and is installed the arc breach corresponding with sample installation breach 8, and the effect of sample installation arm 9 and tool bit 7 is: the samples were pre-clamped as required for cutting, and then cut to size.

In a balanced system, a relatively small piston exerts a relatively small pressure on it, while a relatively large piston exerts a relatively large pressure on it, which keeps the liquid still. Thus, by the transfer of hydraulic oil, different pressures at different ends can be achieved, thus achieving a change.

As shown in fig. 1 and 3, the hydraulic sample shearing machine works as follows:

(1) before a hydraulic sample shearing machine is used, whether the structures of all parts are normal or not needs to be checked, and the situations of oil leakage, looseness and the like are ensured to be avoided;

(2) placing a material to be cut at the position of the sample mounting notch 8, and pre-clamping the sample according to the cutting requirement under the supporting action of the sample mounting arm 9;

(3) the oil valve 4 is screwed up clockwise, the lifting handle 1 is lifted up and down by utilizing the hydraulic transmission principle to drive the cylinder piston 10 and the valve body piston 12 to reciprocate, the internal pressure of the valve body 5 is continuously increased, the cutter head 7 is driven to extend outwards to cut a sample, the oil valve 4 is unscrewed counterclockwise after the sample is cut off, and the cutter head 7 gradually returns.

As shown in fig. 2, the platinum-plated nickel basket has the following structure: the shape of the nickel basket is the same as that of a common nickel basket, a nickel wire is wound into a spiral nickel basket with a large upper part and a small lower part, and the nickel basket is externally plated with metal platinum, so that the effects of fluxing and pollution inhibition are better due to the existence of the platinum.

In the specific implementation process, the method for measuring the oxygen content in the metal rhenium comprises the following steps:

1) sampling: the large columnar rhenium sample is directly cut into small fragments by a hydraulic shearing machine of a shearing tool, and then is sheared into particles by iron shears, which is completely different from the existing linear cutting sampling of all other samples.

2) Sample treatment: the metallic rhenium sample is placed in a container with CCl₄Cleaning the glass ground bottle in an ultrasonic cleaning machine for 3 minutes, taking out the sample, and air-drying;

3) working parameters of a pulse infrared thermal conductivity oxygen nitrogen analyzer are debugged, the heating melting sample power is adjusted to 5500W, and other parameters are the same as the analysis parameters of oxygen in common steel;

4) establishing a standard working curve: weighing three parts of the standard sample of oxygen in steel, drawing a standard curve according to the working parameters in the step (3), wherein the linear coefficient of the working curve is more than 0.999, and the sample is determined according with the requirement, otherwise, the pulse infrared thermal conductivity oxygen nitrogen analyzer is required to be recalibrated to establish a standard working curve;

5) application of fluxing agent: 1g of platinized nickel-based fluxing agent is adopted, a blank is firstly measured, and then blank parameters are debugged according to the step (3); when analyzing the sample, the sample is wrapped by a platinum-plated nickel basket and thrown.

6) And (3) real-time correction: comparing the two separate analysis results, when the difference exceeds 10 wt% of the total amount, the calibration is carried out in real time by using a standard sample or an internal control standard sample.

The invention adopts TC-436 pulse infrared thermal conductivity oxygen nitrogen analyzer (manufactured by American Like corporation), and the main working parameters are as follows: the carrier gas flow rate is 300mL/min, the degassing power is 5700W, the degassing time is 30s, the analysis power is 5500W, and the analysis time is 25 s.

Replacing a commercially available steel medium oxygen standard sample with an internal control steel medium oxygen standard sample, wherein the steel medium oxygen standard sample comprises the following components in percentage by weight: gbw (e)020140(w (o) 0.014 wt%); gbw (e)020143(w (o) 0.0075 wt%); gbw (e)020137(w (o) ═ 0.0034 wt%).

The present invention will be described in further detail below with reference to examples.

Examples

In this example, an internal control steel oxygen standard sample is used to replace a commercially available steel oxygen standard sample, and a standard working curve of the internal control steel oxygen standard sample is established as follows: weighing three parts of the standard sample, and drawing a standard curve according to the working parameters of the TC-436 pulse infrared thermal conductivity oxygen nitrogen analyzer, wherein the linear coefficient of the working curve is more than 0.999. In the invention, the function of establishing the standard working curve is as follows: and calibrating the detection result through a curve, and limiting the controllable range of the measurement uncertainty.

1. Samples and preparation

The sample is columnar 'large particles' of metal rhenium, the diameter is 14mm, the height is 10-30 mm, 0.10 g-0.20 g of block-shaped sample is prepared, and the block-shaped sample is cleaned by carbon tetrachloride for 3min in an ultrasonic cleaner and dried for standby.

2. Analyzing power

Rhenium is a high melting point metal whose oxide is at a high temperature for the reduction by carbonization. Therefore, the analysis power is set to 5500W, which is close to the highest heating power of the pulse infrared thermal oxygen nitrogen analyzer (which is not easy to damage).

The working parameters of the pulse infrared thermal conductivity oxygen-nitrogen analyzer are as follows: the carrier gas flow rate is 300mL/min, the degassing power is 5700W, the degassing time is 30s, the analysis power is 5500W, and the analysis time is 25 s.

3. Fluxing agent

Rhenium is an element which is an active metal and has strong oxygen-abstracting capability. When the sample is melted, the metal is volatilized and attached to the furnace wall, the residual volatile matter easily captures oxygen in CO, and the detected CO amount is reduced, so that the measured value of oxygen is reduced, and the detection of oxygen is interfered. The fluxing agent or bath material can alloy the rhenium alloy, reduce the activity of a volatile sample in a molten pool, and effectively inhibit rhenium volatilization pollution. Pt is the best flux but it is expensive and lacks recovery means. The nickel basket is a fluxing agent applied to oxygen and nitrogen analysis in titanium alloy at present, and is convenient to purchase. Here, the sample was wrapped with a platinum-plated nickel basket and then loaded together with a Pt-plated nickel basket flux.

4. Standard sample monitoring and correcting method

The infrared absorption method is a relative method, and the accuracy thereof depends on a standard substance or a standard sample. At present, a rhenium medium oxygen standard sample does not exist at home and abroad, the calibration method and the accuracy of numerical values depend on the steel medium oxygen standard sample, and the pulse infrared thermal conductivity oxygen nitrogen analyzer is monitored and corrected by applying the steel medium oxygen standard sample, so the technical means is not used by the prior people due to overhigh cost.

In this embodiment, the internal control standard sample is used to replace the standard sample sold in the market, so that the "standard sample monitoring and correcting method" enters the actual application stage. The design is finished with automatic reminding of out-of-tolerance 10 wt%, and after the standard sample or the internal control sample is used for real-time correction, the corrected result can be automatically output. If the out-of-tolerance is more than 50 wt%, the analysis is automatically reminded to be interrupted, the hearth and the electrodes are manually cleaned, the outlet antifouling cotton is replaced, the pollution interference is eliminated, and the analysis is continued when the out-of-tolerance of the calibration result of the standard sample or the internal control sample to be used is less than 10 wt%.

In the embodiment, the detection result is monitored through a software program; automatically comparing the analysis results of the last two times, and reminding an operator to correct the standard sample or the internal control standard sample in real time when the deviation value exceeds 10 wt%; and after the difference caused by rhenium pollution is calculated and corrected, the result of the automatic correction of the last group of data is automatically output.

5. Detailed description of the invention

The final implementation effect is good, the self-purification rhenium of the unit is synchronously tracked, and the result is shown in the table 1.

TABLE 1 results of Simultaneous tracing of rhenium deoxygenation purification

The implementation result shows that the determination method of the invention adopts a pulse melting-infrared absorption method to determine the content of impurity oxygen in rhenium, and the flow is as follows: sampling a columnar sample directly → ultrasonic cleaning treatment → debugging the working parameters of the pulse infrared thermal oxygen nitrogen analyzer → establishing a standard working curve → measuring the sample → correcting the volatile pollution in real time. The invention relates to a tool for sampling a columnar rhenium block direct-cutting sample particle, which selects a sample weighing amount of 0.10-0.20 g, an analysis power of 5500W, a platinum-nickel plating basket, and combines an automatic monitoring and correcting method to establish a method for testing oxygen in metal rhenium, and can solve the problem of pollution interference of the metal rhenium in the analysis process, thereby obtaining practical implementation and application.