CN106568676A - Method for measuring content of trace hydrogen in low alloy steel - Google Patents
Method for measuring content of trace hydrogen in low alloy steel Download PDFInfo
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- CN106568676A CN106568676A CN201510664526.4A CN201510664526A CN106568676A CN 106568676 A CN106568676 A CN 106568676A CN 201510664526 A CN201510664526 A CN 201510664526A CN 106568676 A CN106568676 A CN 106568676A
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Abstract
The invention relates to a method for measuring the content of trace hydrogen in low alloy steel. According to the method, a hydrogen analyzer is adopted, an inert gas pulse heating-thermal conductivity method is used to measure the content of trace hydrogen (less than 0.0002%) in low alloy steel, and the method comprises the following steps: preparing experiment conditions, preparing a sample, carrying out a blank experiment, calibrating a hydrogen analyzer, and measuring the hydrogen content of the sample. The provided method improves the accuracy of the measurement results and solves the problem that the content of trace hydrogen (less than 0.0002%) in low alloy steel is difficult to measure.
Description
Technical field
The invention belongs to analysis and testing technology field, and in particular to trace hydrogen contains in a kind of low-alloy steel
The assay method of amount.
Background technology
Hydrogen is in a metal an inconstant element, with height motility.It is a large amount of non-equilibrium when introducing
Amount hydrogen will produce shattered crack and defect in metal, and the intensity of steel is higher, and hydrogen embrittlement is more sensitive.Cause
This, now many aeronautical products propose to compare strict requirements to hydrogen content, for this purpose, Accurate Determining
The content of trace hydrogen is most important in low-alloy steel.The analysis of hydrogen content in general material is generally adopted
Inert purge gas pulses heating-thermal conductivity method, the method has simple to operate, accurately and rapidly feature.
But there is presently no the specific standards that trace hydrogen content in low-alloy steel is detected using the method.Simultaneously
Through patent retrieval, at present still not using inert purge gas pulses heating-thermal conductivity method measure low-alloy steel
The method of middle trace hydrogen.Because trace hydrogen content standard requires to be less than 0.0002% in low-alloy steel, protect
Card has low and stable blank and guarantees that the release completely of hydrogen is particularly important.Therefore, how accurately to survey
The content for determining trace hydrogen in low-alloy steel is a current difficult problem.
The content of the invention
The purpose of the present invention is：A kind of assay method of trace hydrogen content in low-alloy steel is proposed, is grasped
Make simple, accurate, quick, with high accuracy, solve the low-alloy steel that background technology is present
A measure difficult problem for middle trace hydrogen content.Low-alloy is determined using inert purge gas pulses heating-thermal conductivity method
The exact level of trace hydrogen in steel, meets the dividing less than 0.0002% that aeronautical product is proposed to hydrogen content
Analysis is required.
The technical scheme is that：A kind of method of trace hydrogen content in measure low-alloy steel, its
It is characterised by：Determined in low-alloy steel using hydrogen analyzer application inert purge gas pulses heating-thermal conductivity method
Trace hydrogen content less than 0.0002%.
Comprise the following steps that：
Step 1：Experimental condition prepares
Step by step 1.1:Apparatus selection
Determine the equipment that hydrogen analyzer is trace hydrogen content in detection low-alloy steel, the setting of the equipment
Parameter is：Degassing power 3700W～4200W, time：60s, analyzes power 2250W～2750W,
Most short analysis time：80s, deaerate mode：Double degassings, flow：140ml/min～160ml/min,
Measurement pressure：14psi～16psi, inlet pressure：36psi～44psi；
Step by step 1.2：The preparation of main agents and material
Ether or acetone：Analysis is pure,
Hydrogen content standard substance in steel：
U.S. LECO501-529, hydrogen content is：0.00058% ± 0.00008%
U.S. LECO502-457, hydrogen content is：0.00009% ± 0.00004%
Graphite crucible:Spectroscopic pure, high-temperature crucibles；
Step 2：Prepare sample
Cut after sample using water-cooled cutting machine or equivalent means, sample smart car is made Pole of the length more than 30mm, with file or 150#Fine sandpaper grinds new surface, uses wire nipper
Sample is cut to into the analysis sample of 0.500g～1.000g, after being cleaned with ether or acetone,
Dry for standby under low temperature；
Step 3：Blank assay
According to the working condition that hydrogen analyzer is selected, blank analysis is done with empty high-temperature crucibles, at least analyzed
3 times, hydrogen blank averages are input in system；The hydrogen content measured value of empty high-temperature crucibles is less than
0.00004%；
Step 4：Hydrogen analyzer is calibrated
Step by step 4.1：Calibrated using hydrogen content standard substance in steel
Hydrogen content standard substance in steel is put into into hydrogen analyzer, by the working condition that hydrogen analyzer is selected
Hydrogen content standard substance in steel is measured, 3 standard substances are at least analyzed, hydrogen content mark is obtained
The average measurement of quasi- material, if the average measurement is consistent with the standard value of standard substance, in card
In the range of the tolerance that book is provided, then step by step 4.2 are carried out, otherwise, according to hydrogen in known steel
The standard value of content standard material is calibrated to hydrogen analyzer so as to which deviation is in permitting that certificate is given
Perhaps in deviation range；
Step by step 4.2：Determine hydrogen content standard substance in steel and determine calibration
Hydrogen content standard substance in steel is put into into hydrogen analyzer, by the working condition that hydrogen analyzer is selected
Hydrogen content standard substance in steel is measured, the measured value of hydrogen content standard substance is obtained, the survey
Definite value should be in the range of the tolerance that certificate is given, now, and hydrogen analyzer calibration is completed；
Step 5：Determine the hydrogen content in sample
The sample of 0.500g～1.000g steps 2 is weighed, 0.0001g is accurate to, sample is put into into hydrogen point
Analyzer, the working condition selected by hydrogen analyzer is measured to hydrogen content, and the measured value for obtaining is straight
Connect in the results window for being displayed in screen.
It is an advantage of the invention that：The accuracy of measurement result is improve, is solved in low-alloy steel and is less than
A measure difficult problem for 0.0002% trace hydrogen content.Specifically：
(1) using double degassings, it is ensured that obtain low and stable blank value；
(2) determine the best operating condition of hydrogen analyzer, so that hydrogen content discharges completely in material, carry
The high accuracy of measurement result.
Specific embodiment：
Embodiment 1：The analysis of hydrogen content standard substance LECO502-457 in steel
Step 1：Experimental condition prepares
Step by step 1.1:Apparatus selection
Determine the equipment that hydrogen analyzer is trace hydrogen content in examination criteria material LECO502-457,
The setup parameter of the equipment is：Degassing power 3900W, time：60s, analyzes power 2500W,
Most short analysis time：80s, deaerate mode：Double degassings, flow：150ml/min, measures pressure：
15psi, inlet pressure：40psi.
Step by step 1.2：The preparation of main agents and material：
Ether or acetone：Analysis is pure,
Hydrogen content standard substance in steel：
U.S. LECO501-529, hydrogen content is：0.00058% ± 0.00008%
U.S. LECO502-457, hydrogen content is：0.00009% ± 0.00004%
Graphite crucible:Spectroscopic pure, high-temperature crucibles；
Step 2：Prepare sample
After being cleaned with ether or acetone, dry for standby at low temperature；
Step 3：Blank assay
According to the working condition that hydrogen analyzer is selected, blank analysis is done with empty crucible, analyzed 3 times, will
Hydrogen blank averages 0.000015% are input in system.The hydrogen content measured value of empty crucible is less than
0.00004%, meet analysis and require；
Step 4：Hydrogen analyzer is calibrated
Step by step 4.1：Calibrated using hydrogen content standard substance in steel
Hydrogen content standard substance LECO501-529 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance in steel is measured, analyze 3 standard substances, obtain hydrogen
The average measurement 0.00057% of content standard material, the value is consistent with the standard value of standard substance,
In the range of the tolerance that certificate is given, then step by step 4.2 can be carried out；
Step by step 4.2：Determine hydrogen content standard substance in steel and determine calibration
Hydrogen content standard substance LECO502-457 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance in steel is measured, obtain hydrogen content standard substance in steel
Measured value 0.000092%, the measured value in steel in the range of hydrogen content standard substance tolerance,
Now, hydrogen analyzer calibration is completed；
Step 5：Determine the hydrogen content of hydrogen content standard substance LECO502-457 in steel
The LECO502-457 of 0.500g～1.000g steps 2 is weighed, 0.0001g is accurate to, by standard
Material LECO502-457 is put into hydrogen analyzer, and the working condition selected by hydrogen analyzer is entered to hydrogen content
Row is determined, and the measured value for obtaining is directly displayed in the results window of screen, and analysis result is shown in Table 1, by
The result of table 1 is visible, and the measured value of standard substance is kissed and preferable with admitted value, and relative standard deviation is less than
5%, the method veracity and precision is higher.
Embodiment 2：The analysis of hydrogen content in low-alloy steel 18Cr2Ni4WA
Step 1：Experimental condition prepares
Step by step 1.1:Apparatus selection
Determine that hydrogen analyzer is the equipment for detecting trace hydrogen content in low-alloy steel 18Cr2Ni4WA, should
The setup parameter of equipment is：Degassing power 3950W, time：60s, analyzes power 2550W, most
Short analysis time：80s, deaerate mode：Double degassings, flow：150ml/min, measures pressure：15psi,
Inlet pressure：40psi.
Step by step 1.2：The preparation of main agents and material
Ether or acetone：Analysis is pure,
Hydrogen content standard substance in steel：
U.S. LECO501-529, hydrogen content is：0.00058% ± 0.00008%
U.S. LECO502-457, hydrogen content is：0.00009% ± 0.00004%
Graphite crucible:Spectroscopic pure, high-temperature crucibles；
Step 2：Prepare sample
Cut after sample using water-cooled cutting machine or equivalent means, sample smart car is made Pole of the length more than 30mm, with file or fine sandpaper (150#) new surface is ground, with cutting
Sample is cut to line tweezer the analysis sample of 0.500g～1.000g, after being cleaned with ether or acetone,
Dry for standby at low temperature；
Step 3：Blank assay
According to the working condition that hydrogen analyzer is selected, blank analysis is done with empty crucible, analyzed 3 times, will
Hydrogen blank averages 0.000018% are input in system.The hydrogen content measured value of empty crucible is less than
0.00004%, meet analysis and require；
Step 4：Hydrogen analyzer is calibrated
Step by step 4.1：Calibrated using hydrogen content standard substance in steel
Hydrogen content standard substance LECO501-529 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance in steel is measured, analyze 3 standard substances, obtain hydrogen
The average measurement of content standard material is 0.000555%, according to hydrogen content reference material in known steel
The standard value 0.00058% of matter is calibrated to hydrogen analyzer, its deviation hydrogen content reference material in steel
In the range of matter tolerance；
Step by step 4.2：Determine hydrogen content standard substance in steel and determine calibration
Hydrogen content standard substance LECO502-457 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance LECO502-457 in steel is measured, obtain hydrogen content mark
The measured value of quasi- material is 0.000097%, measured value hydrogen content standard substance tolerance in steel
In the range of, now, hydrogen analyzer calibration is completed；
Step 5：Determine the hydrogen content in 18Cr2Ni4WA
The sample of 0.500g～1.000g steps 2 is weighed, 0.0001g is accurate to, sample is put into into hydrogen point
Analyzer, the working condition selected by hydrogen analyzer is measured to hydrogen content, obtains hydrogen in sample and contains
The measured value of amount, with the accuracy and practicality of evaluation methodology, analysis result is shown in Table 2, is tied by table 2
Really visible, the relative standard deviation of hydrogen content is less than 6% in low-alloy steel 18Cr2Ni4WA, the method
Veracity and precision is higher.
Embodiment 3：The analysis of hydrogen content in low-alloy steel 30CrMnSiNi2A
Step 1：Experimental condition prepares
Step by step 1.1:Apparatus selection
Determine that hydrogen analyzer is the equipment for detecting trace hydrogen content in low-alloy steel 30CrMnSiNi2A,
The setup parameter of the equipment is：Degassing power 3800W, time：60s, analyzes power 2450W,
Most short analysis time：80s, deaerate mode：Double degassings, flow：150ml/min, measures pressure：
15psi, inlet pressure：40psi.
Step by step 1.2：The preparation of main agents and material
Ether or acetone：Analysis is pure,
Hydrogen content standard substance in steel：
U.S. LECO501-529, hydrogen content is：0.00058% ± 0.00008%
U.S. LECO502-457, hydrogen content is：0.00009% ± 0.00004%
Graphite crucible:Spectroscopic pure, high-temperature crucibles；
Step 2：Prepare sample
Cut after sample using water-cooled cutting machine or equivalent means, sample smart car is made Pole of the length more than 30mm, with file or fine sandpaper (150#) new surface is ground, with cutting
Sample is cut to line tweezer the analysis sample of 0.500g～1.000g, after being cleaned with ether or acetone,
Dry for standby at low temperature；
Step 3：Blank assay
According to the working condition that hydrogen analyzer is selected, blank analysis is done with empty crucible, analyzed 3 times, will
Hydrogen blank averages 0.000014% are input in system.The hydrogen content measured value of empty crucible is less than
0.00004%, meet analysis and require；
Step 4：Hydrogen analyzer is calibrated
Step by step 4.1：Calibrated using hydrogen content standard substance in steel
Hydrogen content standard substance LECO501-529 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance in steel is measured, analyze 3 standard substances, obtain hydrogen
The average measurement of content standard material is 0.000540%, according to hydrogen content reference material in known steel
The standard value 0.00058% of matter is calibrated to hydrogen analyzer, its deviation hydrogen content reference material in steel
In the range of matter tolerance；
Step by step 4.2：Determine hydrogen content standard substance in steel and determine calibration
Hydrogen content standard substance LECO502-457 in steel is put into into hydrogen analyzer, is selected by hydrogen analyzer
Working condition hydrogen content standard substance LECO502-457 in steel is measured, obtain hydrogen content mark
The measured value of quasi- material is 0.000094%, measured value hydrogen content standard substance tolerance in steel
In the range of, now, hydrogen analyzer calibration is completed；
Step 5：Determine the hydrogen content in 30CrMnSiNi2A
The sample of 0.500g～1.000g steps 2 is weighed, 0.0001g is accurate to, sample is put into into hydrogen point
Analyzer, the working condition selected by hydrogen analyzer is measured to hydrogen content, obtains hydrogen in sample and contains
The measured value of amount, with the accuracy and practicality of evaluation methodology, analysis result is shown in Table 3, is tied by table 3
Really visible, the relative standard deviation of hydrogen content is less than 5% in low-alloy steel 30CrMnSiNi2A, the party
Method veracity and precision is higher.
The standard substance analysis result (n=8) of table 1
The actual sample analysis result (n=8) of table 2
The actual sample analysis result (n=8) of table 3
Claims (1)
1. a kind of method for determining trace hydrogen content in low-alloy steel, comprises the steps：
Step 1：Experimental condition prepares
Step by step 1.1:Apparatus selection
Determine the equipment that hydrogen analyzer is trace hydrogen content in detection low-alloy steel, the setting of the equipment
Parameter is：Degassing power 3700W～4200W, time：60s, analyzes power 2250W～2750W,
Most short analysis time：80s, deaerate mode：Double degassings, flow：140ml/min～160ml/min,
Measurement pressure：14psi～16psi, inlet pressure：36psi～44psi；
Step by step 1.2：The preparation of main agents and material
Ether or acetone：Analysis is pure,
Hydrogen content standard substance in steel：
U.S. LECO501-529, hydrogen content is：0.00058% ± 0.00008%
U.S. LECO502-457, hydrogen content is：0.00009% ± 0.00004%
Graphite crucible:Spectroscopic pure, high-temperature crucibles；
Step 2：Prepare sample
Cut after sample using water-cooled cutting machine or equivalent means, sample smart car is made Pole of the length more than 30mm, with file or 150#Fine sandpaper grinds new surface, uses wire nipper
Sample is cut to into the analysis sample of 0.500g～1.000g, after being cleaned with ether or acetone,
Dry for standby under low temperature；
Step 3：Blank assay
According to the working condition that hydrogen analyzer is selected, blank analysis is done with empty high-temperature crucibles, at least analyzed
3 times, hydrogen blank averages are input in system；The hydrogen content measured value of empty high-temperature crucibles is less than
0.00004%；
Step 4：Hydrogen analyzer is calibrated
Step by step 4.1：Calibrated using hydrogen content standard substance in steel
Hydrogen content standard substance in steel is put into into hydrogen analyzer, by the working condition that hydrogen analyzer is selected
Hydrogen content standard substance in steel is measured, 3 standard substances are at least analyzed, hydrogen content mark is obtained
The average measurement of quasi- material, if the average measurement is consistent with the standard value of standard substance, in card
In the range of the tolerance that book is provided, then step by step 4.2 are carried out, otherwise, according to hydrogen in known steel
The standard value of content standard material is calibrated to hydrogen analyzer so as to which deviation is in permitting that certificate is given
Perhaps in deviation range；
Step by step 4.2：Determine hydrogen content standard substance in steel and determine calibration
Hydrogen content standard substance in steel is put into into hydrogen analyzer, by the working condition that hydrogen analyzer is selected
Hydrogen content standard substance in steel is measured, the measured value of hydrogen content standard substance is obtained, the survey
Definite value should be in the range of the tolerance that certificate is given, now, and hydrogen analyzer calibration is completed；
Step 5：Determine the hydrogen content in sample
The sample of 0.500g～1.000g steps 2 is weighed, 0.0001g is accurate to, sample is put into
Hydrogen analyzer, the working condition selected by hydrogen analyzer is measured to hydrogen content, the measure for obtaining
Value is directly displayed in the results window of screen.
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Cited By (6)
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| CN108318306A (en) * | 2018-03-22 | 2018-07-24 | 中航金属材料理化检测科技有限公司 | A kind of method of protium content in measurement titanium or titanium alloy |
| CN108663497A (en) * | 2018-03-30 | 2018-10-16 | 中航金属材料理化检测科技有限公司 | A method of measuring Dissolved H in Liquid Al-Si Alloy content |
| CN108872004A (en) * | 2018-06-04 | 2018-11-23 | 中钢集团新型材料（浙江）有限公司 | A kind of measuring method for ultra-pure graphite ash content |
| CN111781088A (en) * | 2020-07-14 | 2020-10-16 | 广东省特种设备检测研究院珠海检测院 | Method for detecting hydrogen content in solid metal |
| CN112986524A (en) * | 2021-03-12 | 2021-06-18 | 北京北冶功能材料有限公司 | Method for accurately measuring oxygen content in manganese-based alloy |
| CN114184692A (en) * | 2021-08-16 | 2022-03-15 | 人本股份有限公司 | Method for detecting hydrogen content in steel |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108318306A (en) * | 2018-03-22 | 2018-07-24 | 中航金属材料理化检测科技有限公司 | A kind of method of protium content in measurement titanium or titanium alloy |
| CN108663497A (en) * | 2018-03-30 | 2018-10-16 | 中航金属材料理化检测科技有限公司 | A method of measuring Dissolved H in Liquid Al-Si Alloy content |
| CN108872004A (en) * | 2018-06-04 | 2018-11-23 | 中钢集团新型材料（浙江）有限公司 | A kind of measuring method for ultra-pure graphite ash content |
| CN111781088A (en) * | 2020-07-14 | 2020-10-16 | 广东省特种设备检测研究院珠海检测院 | Method for detecting hydrogen content in solid metal |
| CN111781088B (en) * | 2020-07-14 | 2023-05-12 | 广东省特种设备检测研究院珠海检测院 | Method for detecting hydrogen content in solid metal |
| CN112986524A (en) * | 2021-03-12 | 2021-06-18 | 北京北冶功能材料有限公司 | Method for accurately measuring oxygen content in manganese-based alloy |
| CN114184692A (en) * | 2021-08-16 | 2022-03-15 | 人本股份有限公司 | Method for detecting hydrogen content in steel |
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