CN117007548A - Method for measuring oxygen and nitrogen content in molybdenum product - Google Patents
Method for measuring oxygen and nitrogen content in molybdenum product Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 140
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 74
- 239000001301 oxygen Substances 0.000 title claims abstract description 74
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 72
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 71
- 239000011733 molybdenum Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000000126 substance Substances 0.000 claims abstract description 41
- 238000005259 measurement Methods 0.000 claims abstract description 37
- 238000001514 detection method Methods 0.000 claims abstract description 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 64
- 229910052759 nickel Inorganic materials 0.000 claims description 32
- 238000010008 shearing Methods 0.000 claims description 16
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000002775 capsule Substances 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 239000010955 niobium Substances 0.000 claims description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000012937 correction Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims 1
- 230000000996 additive effect Effects 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 15
- 238000012545 processing Methods 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000010301 surface-oxidation reaction Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 231100000570 acute poisoning Toxicity 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/18—Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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Abstract
The application provides a method for measuring the oxygen and nitrogen content in a molybdenum product, which comprises six steps of preparing a sample to be detected, assembling the sample, setting detection parameters, correcting blank, calibrating standard substances and measuring the oxygen and nitrogen content. The method has high processing speed, can complete the sample preparation of one sample within about 1-3 minutes, can effectively avoid the pollution and oxidation of oxygen and nitrogen components in the sample, improves the accuracy and precision of the nitrogen and oxygen content measurement result, and can especially ensure the validity of the result of the oxygen and nitrogen component analysis in the low-oxygen and low-nitrogen analysis sample. In addition, the method does not need to polish the sample on a grinder, so that the surface oxidation of the molybdenum product sample is avoided, and the accuracy and precision of the oxygen content measurement result are improved.
Description
Technical Field
The application belongs to the technical field of molybdenum chemical industry and molybdenum metal production, relates to quality control detection of molybdenum chemical industry and molybdenum metal products, and in particular relates to a method for measuring oxygen and nitrogen content in a molybdenum product.
Background
Molybdenum is an important strategic rare metal and is widely applied to industries such as metallurgy, aviation, aerospace, energy sources, chemical industry and the like. The molybdenum product mainly comprises the following components: molybdenum plate blank, molybdenum rod, molybdenum bar, molybdenum cylinder, molybdenum plug, molybdenum wire, alloy molybdenum plate blank, molybdenum cake, molybdenum electrode, molybdenum target, molybdenum plate, molybdenum belt and molybdenum special-shaped piece. The molybdenum product is used as a raw material product of customers, has higher requirements on the oxygen and nitrogen element contents, and the oxygen content and the nitrogen content directly influence the product performance, so that the control of the oxygen and nitrogen content in the molybdenum product is very important.
At present, the determination of the oxygen and nitrogen content in the molybdenum product adopts a pulse-inert gas melting method, is simple, convenient and rapid, has high sensitivity, can be used for separately or simultaneously determining oxygen, nitrogen and hydrogen, and is widely applied to metallurgical analysis. The current national standard of oxygen, nitrogen and hydrogen in molybdenum products is inert gas melting infrared absorption method-thermal conductivity method (GB/T4325.23-2013) for measuring oxygen and nitrogen content by molybdenum chemical analysis method, and the main process of the method is as follows: polishing the surface of a block sample on a grinder, processing the block sample into particles with the mass of 0.05 g-0.08 g, cleaning the particles with acetone, taking out the particles, drying with cold air, weighing the particles, loading the particles into a nickel basket, and measuring the oxygen and nitrogen content.
The method mainly has the following defects:
firstly, the surface of a molybdenum product is easily oxidized by polishing the surface on a grinder, so that the oxidation pollution of a detection sample is caused, the oxygen content measurement result is inaccurate, and the precision of the detection result is low.
Secondly, the method has long operation time for sample processing and treatment of molybdenum products, is not easy to operate, is easy to cause pollution, and is easy to cause inaccurate detection results and low precision of the detection results.
Thirdly, the method requires processing into particles with the mass of 0.05 g-0.08 g, and the difficulty of taking out processing equipment is great.
Fourth, the method requires that acetone is adopted to clean particles, oxygen and nitrogen are easy to pollute in the cleaning process, and unsafe accidents such as acute poisoning, burning explosion and the like are easy to occur when the acetone is improperly treated.
Fifth, while the procedure for determining the amount of oxygen and nitrogen in molybdenum using the inert gas melt infrared absorption method-thermal conductivity method is presented, the standard does not indicate the calibration samples and test parameter settings used in the test procedure for molybdenum product.
Disclosure of Invention
Aiming at the defects existing in the prior art, the application aims to provide a method for measuring the oxygen and nitrogen content in a molybdenum product, which solves the technical problem that the accuracy and precision of the oxygen and nitrogen content measuring result of the molybdenum product in the prior art are to be improved.
In order to solve the technical problems, the application adopts the following technical scheme:
the method for measuring the oxygen and nitrogen content in the molybdenum product specifically comprises the following steps:
step one, preparing a sample to be detected:
the method comprises the steps of preparing a molybdenum product into a sample by adopting a shredding or cutting mode, selecting the sample, clamping the sample by using a hydraulic shear, applying pressure, directly shearing from different surfaces respectively, taking a sample block in the center, obtaining a sample to be detected, and placing the sample to be detected in a sample bag for standby.
Step two, assembling a sample:
and (3) placing the block-shaped sample to be detected, which is prepared in the step (I), in a nickel bag, then closing the opening of the nickel bag, and expelling air in the nickel bag to obtain the sample to be detected, which wraps the nickel bag.
Step three, setting detection parameters:
after the parameters of the oxygen-nitrogen analyzer are set, preheating the analyzer to make each index of the analyzer reach the set value.
Step four, blank correction:
and placing the empty nickel bag into a crucible, carrying out parallel measurement for a plurality of times, replacing the crucible each time, taking the average value of the plurality of measurement results as a blank compensation value, and correcting.
Step five, calibrating a standard substance:
respectively filling a plurality of standard substances into nickel capsules, respectively measuring each nickel capsule filled with the standard substances in parallel for a plurality of times, calculating the average value of the measurement results of the plurality of times, and comparing the average value with a standard value; and if the average value accords with the standard value and does not exceed the uncertainty range given by the standard substance certificate, performing calibration.
Step six, measuring the oxygen and nitrogen content:
and (3) placing the sample to be detected wrapped with the nickel bag in the second step into a corrected oxygen-nitrogen analyzer, closing the furnace door, starting detection, and detecting each sample to be detected in parallel for multiple times to obtain a measurement result.
The application also has the following technical characteristics:
specifically, in the first step, the working force of the hydraulic shears is 2T-15T, and the shearing range is 4-22 mm.
Specifically, in the first step, the sample is a block sample with the thickness of 5-20 mm, and the sample to be detected is a block sample to be detected with the thickness of 1-5 mm.
Specifically, in the first step, the sample is a rod-shaped sample with the length of 10-50 mm, and the sample to be detected is a rod-shaped sample with the thickness of 1-5 mm.
Specifically, in the second step, the oxygen content in the nickel capsule is less than or equal to 0.0008%, the nitrogen content is less than or equal to 0.0001%, and the hydrogen content is less than or equal to 0.0001%.
Specifically, in the third step, the detection parameters are as follows: the gas purity is more than 99.99wt%, the maximum working power is 4.5-5.5 kW, the cooling time is 5s, and the comparator level is 1.00%.
Specifically, in the third step, the preheating time of the instrument is 30-60 min.
Specifically, in the fifth step, the number of times of parallel measurement is 2 to 5 times.
Specifically, in the fifth step, the standard substance is selected from the group consisting of a certified standard substance American Association AR668, a certified standard substance American LECO502-198 and a niobium standard sample GSB04-3548-2019.
Specifically, in the fifth step, the calibration is a single-point calibration or a calibration using a working curve.
Compared with the prior art, the application has the following technical effects:
the method for measuring the oxygen and nitrogen content in the molybdenum product has high processing speed, can finish the sample preparation of one sample within about 1-3 minutes, can effectively avoid the pollution and oxidation of oxygen and nitrogen components in the sample, improves the accuracy and precision of the nitrogen and oxygen content measuring result, and can particularly ensure the validity of the result of the oxygen and nitrogen component analysis in the low-oxygen and low-nitrogen analysis sample. In addition, the method does not need to polish the sample on a grinder, so that the surface oxidation of the molybdenum product sample is avoided, and the accuracy and precision of the oxygen content measurement result are improved.
The method has the characteristics of convenient measurement, high measurement speed, high accuracy of oxygen and nitrogen analysis, high precision and good reproducibility, so that the method can meet the requirements of industrial production process and rapid detection of products.
And (II) the method for measuring the oxygen and nitrogen content in the molybdenum product eliminates the influence of the adsorbed oxygen and nitrogen on the test result of the test sample while eliminating the inaccuracy of the test result caused by the oxidization problem of the sample in the sample preparation process, and further ensures the accuracy of measuring the oxygen and nitrogen content in the sample.
(III) the method for measuring the oxygen and nitrogen content in the molybdenum product has low requirements on sample processing, and even if the mass of a sample to be detected is more than 0.08g, the method still does not influence the measurement result of the nitrogen and oxygen content, so that the method is simple and convenient and has low cost, can be used for laboratory research besides industrial production, and has high applicability.
The method for measuring the oxygen and nitrogen content in the molybdenum product greatly improves the sample preparation speed in the whole measuring process without water, oil stains and organic chemical reagents, has more visual and better control on the quality judgment of the surface quality of the sample, provides powerful guarantee for the analysis of oxygen and nitrogen in the molybdenum product, improves the accuracy and precision of the analysis and detection of the oxygen and nitrogen, simultaneously avoids safety accidents caused by the use of the organic reagents, and also realizes low carbon and environmental protection.
The method for measuring the oxygen and nitrogen content in the molybdenum product of the application provides means for calibrating a sample and specific detection parameter settings for the first time, and perfects the existing method for measuring the oxygen and nitrogen content in molybdenum by an inert gas melting infrared absorption method-a thermal conductivity method.
The following examples illustrate the application in further detail.
Detailed Description
In the application, the following components are added: the content refers to mass content.
All instruments and tools of the present application are known in the art, and unless otherwise specified, for example:
the oxygen-nitrogen analyzer adopts an oxygen-nitrogen analyzer known in the prior art, in particular to an oxygen or nitrogen analysis detector by an inert gas melting infrared absorption method.
The crucible is a conventional crucible known in the art, preferably a graphite crucible.
The following specific embodiments of the present application are given according to the above technical solutions, and it should be noted that the present application is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solutions of the present application fall within the protection scope of the present application.
Example 1:
the embodiment provides a method for measuring the oxygen and nitrogen content in a molybdenum product, which specifically comprises the following steps:
step one, preparing a sample to be detected:
preparing a molybdenum product into a block sample with the thickness of 5mm by adopting a crushing or cutting mode, selecting 50g of the block sample, and clamping the block sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces respectively, taking a central sample block to obtain a block-shaped sample to be detected, wherein the thickness of the block-shaped sample to be detected is 1.2mm, the mass of the block-shaped sample to be detected is 0.067g, and placing the block-shaped sample to be detected in a clean sample bag for standby.
Step two, assembling a sample:
placing the block-shaped sample to be detected prepared in the first step in a nickel bag, wherein the content of gas elements in the nickel bag is as follows: o is less than or equal to 0.0008%, N is less than or equal to 0.0001%, and H is less than or equal to 0.0001%; and then closing the opening of the nickel bag by using pliers, and expelling air in the nickel bag to obtain a sample to be detected wrapping the nickel bag.
Step three, setting detection parameters:
parameters of the oxygen nitrogen analyzer were set as follows: the gas purity is more than 99.99wt%, the maximum working power is 4.5kW, the cooling time is 5s, and the comparator level is 1.00%; and preheating the instrument for 30min to enable various indexes of the instrument to reach set values.
Step four, blank correction:
the empty nickel capsules are placed in a crucible, the crucible is measured in parallel for three times, a new crucible is replaced each time, and the average value of the three measurement results is taken as a blank compensation value and is corrected.
Step five, calibrating a standard substance:
and selecting a standard substance, wherein the standard substance for measuring the nitrogen element content is a proven standard substance American union AR668, and the nitrogen content is 0.0031+/-0.0002%. The standard substance for measuring the content of oxygen is a certified standard substance, namely LECO502-198 in U.S. with the oxygen content of 0.0038+/-0.0005%. The oxygen and nitrogen content in the selected standard sample is slightly larger than that in the sample to be detected, but cannot exceed 1.5 times of that in the sample to be detected.
Respectively filling three standard substances into nickel capsules, respectively measuring each nickel capsule filled with the standard substances in parallel for three times, calculating the average value of the three measurement results, and comparing the average value with a standard value; and after comparison, confirming that the average value accords with the standard value, and carrying out system single-point calibration without exceeding the uncertainty range given by the standard substance certificate.
Step six, measuring the oxygen and nitrogen content:
and (3) placing the samples to be detected, which are wrapped by the nickel bags, in the second step in a corrected oxygen-nitrogen analyzer, closing the furnace door, starting detection, and detecting each sample to be detected twice in parallel, wherein the measuring results are automatically displayed by the instrument, and are shown in the table 1.
Table 1, results of measurement of example 1-
As shown in Table 1, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be met.
Example 2:
this example shows a method for determining the oxygen nitrogen content of a molybdenum article, which is substantially the same as the method of example 1, except that: step one is different.
In this embodiment, the first step is specifically as follows:
preparing a molybdenum product into a rod-shaped sample with the length of 10mm by adopting a shredding or cutting mode, selecting 20g of the rod-shaped sample, and clamping the rod-shaped sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces respectively, taking a central sample block to obtain a rod-shaped sample to be detected, wherein the thickness of the rod-shaped sample to be detected is 1.1mm, the mass of the rod-shaped sample to be detected is 0.055g, and placing the rod-shaped sample to be detected in a clean sample bag for standby.
In this example, the final measurement results are shown in table 2.
Table 2, measurement results of example 2
As shown in Table 2, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be met.
Example 3:
this example shows a method for determining the oxygen nitrogen content of a molybdenum article, which is substantially the same as the method of example 1, except that: step one is different from step five.
In this embodiment, the first step is specifically as follows:
preparing a molybdenum product into a block sample with the thickness of 11mm by adopting a crushing or cutting mode, selecting 127g of the block sample, and clamping the block sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces respectively, taking a central sample block to obtain a block-shaped sample to be detected, wherein the thickness of the block-shaped sample to be detected is 2.2mm, the mass of the block-shaped sample to be detected is 0.085g, and placing the block-shaped sample to be detected in a clean sample bag for standby.
In this embodiment, the fifth step is specifically as follows:
and selecting a standard substance, wherein the standard substance for measuring the nitrogen element content is a proven standard substance American union AR668, and the nitrogen content is 0.0031+/-0.0002%. The standard substance for measuring the oxygen content was selected from niobium standard samples (GSB 04-3548-2019) having oxygen contents of 0.073% + -0.015%, 0.0141+ -0.014% and 0.366+ -0.047%.
Respectively filling three standard substances into nickel capsules, respectively measuring each nickel capsule filled with the standard substances in parallel for three times, calculating the average value of the three measurement results, and comparing the average value with a standard value; and comparing to confirm that the average value accords with the standard value, and not exceeding the uncertainty range given by the standard substance certificate, carrying out system single-point calibration on the nitrogen element, and calibrating the oxygen element by adopting a working curve, wherein the linear correlation coefficient after calibration is 0.9996.
In this example, the final measurement results are shown in Table 3.
Table 3, results of measurement of example 3-
As shown in Table 3, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be met.
Example 4:
this example shows a method for determining the oxygen nitrogen content of a molybdenum article, which is substantially the same as the method of example 1, except that: step one is different from step five.
In this embodiment, the first step is specifically as follows:
preparing a molybdenum product into a rod-shaped sample with the length of 22mm by adopting a shredding or cutting mode, selecting 235g of the rod-shaped sample, and clamping the rod-shaped sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces, taking a central sample block to obtain a rod-shaped sample to be detected, wherein the thickness of the rod-shaped sample to be detected is 2.7mm, the mass of the rod-shaped sample to be detected is 0.1003g, and placing the rod-shaped sample to be detected in a clean sample bag for later use.
In this embodiment, the fifth step is specifically as follows:
and selecting a standard substance, wherein the standard substance for measuring the nitrogen element content is a proven standard substance American union AR668, and the nitrogen content is 0.0031+/-0.0002%. The standard substance for measuring the oxygen content was selected from niobium standard samples (GSB 04-3548-2019) having oxygen contents of 0.073% + -0.015%, 0.0141+ -0.014% and 0.366+ -0.047%.
Respectively filling three standard substances into nickel capsules, respectively measuring each nickel capsule filled with the standard substances in parallel for three times, calculating the average value of the three measurement results, and comparing the average value with a standard value; and comparing to confirm that the average value accords with the standard value, and carrying out system single-point calibration on the nitrogen element without exceeding the uncertainty range given by the standard substance certificate, and calibrating the oxygen element by adopting a working curve, wherein the linear correlation coefficient after calibration is 0.9996.
In this example, the final measurement results are shown in Table 4.
Table 4, measurement results of example 4
As shown in Table 4, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be met.
Example 5:
this example shows a method for determining the oxygen nitrogen content of a molybdenum article, which is substantially the same as the method of example 1, except that: step one is different.
In this embodiment, the first step is specifically as follows:
preparing a molybdenum product into a block sample with the thickness of 16mm by adopting a crushing or cutting mode, selecting 323g of the block sample, and clamping the block sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces, taking a central sample block to obtain a block-shaped sample to be detected, wherein the thickness of the block-shaped sample to be detected is 4.8mm, the mass of the block-shaped sample to be detected is 0.1052g, and placing the block-shaped sample to be detected in a clean sample bag for later use.
In this example, the final measurement results are shown in Table 5.
Table 5, measurement results of example 5
As shown in Table 5, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be satisfied.
Example 6:
this example shows a method for determining the oxygen nitrogen content of a molybdenum article, which is substantially the same as the method of example 1, except that: step one is different.
In this embodiment, the first step is specifically as follows:
preparing a molybdenum product into a rod-shaped sample with the length of 49mm by adopting a shredding or cutting mode, selecting 431g of the rod-shaped sample, and clamping the rod-shaped sample by using a hydraulic shear, wherein the working output of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm; and (3) manually applying pressure, directly shearing from different surfaces respectively, taking a central sample block to obtain a rod-shaped sample to be detected, wherein the thickness of the rod-shaped sample to be detected is 4.5mm, the mass of the rod-shaped sample to be detected is 0.1013g, and placing the rod-shaped sample to be detected in a clean sample bag for standby.
In this example, the final measurement results are shown in Table 6.
Table 6, measurement results of example 6
As shown in Table 6, the results of two parallel measurement of the oxygen and nitrogen contents in the molybdenum product meet the allowable difference in the GB/T4325.23-2013 rule, and the analysis and detection requirements can be met.
From the results of examples 1 to 6, it is apparent that the method of the present application was used to measure the oxygen and nitrogen content of the molybdenum product, and the measurement difference of the results was 0.01% or less, with high accuracy and precision.
Claims (10)
1. The method for measuring the oxygen and nitrogen content in the molybdenum product is characterized by comprising the following steps of:
step one, preparing a sample to be detected:
preparing a molybdenum product into a sample by adopting a crushing or cutting mode, selecting the sample, clamping the sample by using a hydraulic shear, applying pressure, directly shearing from different surfaces respectively, taking a sample block in the center to obtain a sample to be detected, and placing the sample to be detected in a sample bag for later use;
step two, assembling a sample:
placing the block-shaped sample to be detected, which is prepared in the step one, in a nickel bag, then closing the opening of the nickel bag, and expelling air in the nickel bag to obtain the sample to be detected, which wraps the nickel bag;
step three, setting detection parameters:
after the parameters of the oxygen-nitrogen analyzer are set, preheating the analyzer to enable various indexes of the analyzer to reach set values;
step four, blank correction:
placing the empty nickel bag into a crucible, measuring in parallel for a plurality of times, replacing the crucible each time, taking the average value of the measuring results of the plurality of times as a blank compensation value, and correcting;
step five, calibrating a standard substance:
respectively filling a plurality of standard substances into nickel capsules, respectively measuring each nickel capsule filled with the standard substances in parallel for a plurality of times, calculating the average value of the measurement results of the plurality of times, and comparing the average value with a standard value; if the average value accords with the standard value and does not exceed the uncertainty range given by the standard substance certificate, calibrating;
step six, measuring the oxygen and nitrogen content:
and (3) placing the sample to be detected wrapped with the nickel bag in the second step into a corrected oxygen-nitrogen analyzer, closing the furnace door, starting detection, and detecting each sample to be detected in parallel for multiple times to obtain a measurement result.
2. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the first step, the working force of the hydraulic shear is 2T-15T, and the shearing range is 4-22 mm.
3. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the first step, the sample is a block sample with a thickness of 5-20 mm, and the sample to be detected is a block sample to be detected with a thickness of 1-5 mm.
4. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the first step, the sample is a rod-shaped sample with a length of 10-50 mm, and the sample to be detected is a rod-shaped sample to be detected with a thickness of 1-5 mm.
5. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the second step, the oxygen content in the nickel capsule is not more than 0.0008%, the nitrogen content is not more than 0.0001%, and the hydrogen content is not more than 0.0001%.
6. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the third step, the detection parameters are as follows: the gas purity is more than 99.99wt%, the maximum working power is 4.5-5.5 kW, the cooling time is 5s, and the comparator level is 1.00%.
7. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the third step, the preheating time of the instrument is 30 min-60 min.
8. The method for measuring the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the fifth step, the number of parallel measurements is 2 to 5.
9. The method for determining the oxygen and nitrogen content of a molybdenum product according to claim 1, wherein in the fifth step, the standard substance is selected from the group consisting of a certified standard substance american additive AR668, a certified standard substance american LECO502-198, and a niobium standard sample GSB04-3548-2019.
10. The method of determining the oxygen and nitrogen content of a molybdenum article according to claim 1, wherein in step five, the calibration is a single point calibration or a calibration using a working curve.
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