CN105929129A - Detection method for hydrogen content of titanium alloy bolt or screw - Google Patents
Detection method for hydrogen content of titanium alloy bolt or screw Download PDFInfo
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- CN105929129A CN105929129A CN201610253290.XA CN201610253290A CN105929129A CN 105929129 A CN105929129 A CN 105929129A CN 201610253290 A CN201610253290 A CN 201610253290A CN 105929129 A CN105929129 A CN 105929129A
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Abstract
The invention provides a detection method for a hydrogen content of titanium alloy bolt or screw. The detection method comprises the following steps: preparation of a sample; determination of a blank sample; determination of a standard sample; drafting of a standard curve; and determination of the sample. The special method for detecting the hydrogen content of the titanium alloy bolt or screw is established in the invention and overcomes the disadvantage that a sample has poor representativeness since a surface layer of a titanium alloy bolt or screw has to be removed during sampling in ASTM 1447-09 technology detecting hydrogen content by using an inert gas fusion and thermal conductance detection method and an infrared detection method. The standard sample used in the method provided by the invention is identical to the sampling weight of the titanium alloy bolt or screw, so a detection range is controlled, determination conditions are consistent, measurement errors are reduced, and high detection accuracy is obtained. The method provided by the invention provides accurate hydrogen content data of the titanium alloy bolt or screw for production control and scientific research and ensures product quality of the titanium alloy bolt or screw used for spaceflight and aviation.
Description
Technical field
The present invention relates to the detection method of hydrogen content in a kind of titanium alloy bolt or screw.
Background technology
The detection method of hydrogen content in titanium alloy bolt or screw in prior art, uses inert gas fusion Thermal Conductivity methods and infrared detecting method to survey hydrogen content, ASTM 1447-09 technology more.
There is following point in it:
1. a kind of method having not seen detection being specifically designed to titanium alloy bolt or screw hydrogen content.
2. inert gas fusion Thermal Conductivity method and infrared detecting method survey hydrogen content, ASTM
1447-09 technology pilot sample is prepared requirement and is made suitable dimension weight 0.15g-0.30g, and space flight, air standard, such as HB6568, Q/4A1-286, Q/2AJ652-2009 etc., sampling requirement to titanium alloy bolt or screw is at bolt or screw head transition circle Subsampling, because of titanium alloy bolt or the processed rear hydrogen of screw, to be gathered in transition circle part top layer more, there is the sample difficulty of suitable dimension as made weight 0.15g-0.30g by ASTM 1447-09 standard sample, and sample representativeness is the strongest.
3. ordinary test requires nothing more than hydrogen content in standard specimen and is not less than sample hydrogen content, but do not make scope and limit.
Summary of the invention
The invention aims to overcome deficiency of the prior art, thus the detection method of hydrogen content in a kind of titanium alloy bolt or screw is provided.
The detection method of hydrogen content in a kind of titanium alloy bolt or screw, comprises the following steps:
Step one, the preparation of sample: cut away under titanium alloy bolt or head of screw, at transition circle position sample, the depth of cut controls at 0.1mm～0.2mm, and lathe rotating speed is not more than 250r/min；Consider length to be worth doing the bar sample shear following sample of growth 5mm；Sampling total amount is 0.30g；After cleaning with acetone, air-dry 20min, during use, each test portion loads pure nickel capsule φ 5mm × 10mm, seals so that it is weight is in the range of 0.04g～0.06g in 0.36g；
Step 2, the mensuration of sample blank: take a new graphite crucible, on hydrogen determinator, it is placed on bottom electrode, close electrode furnace, measures hydrogen content；Being repeated three times, if blank value is more than 0.0000% ± 0.0001%, or the standard deviation of three serial numbers has exceeded 0.0001%, finds out reason and does respective handling, then redeterminating；
Step 3, the mensuration of standard sample: weigh standard sample 0.05g ± 0.01g, load pure nickel capsule φ 5mm × 10mm, 0.36g seals, takes a new graphite crucible, on hydrogen determinator, be placed on bottom electrode, close electrode furnace, measures hydrogen content；It is repeated three times, if measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating；
Step 4, the drafting of standard curve: select 3 passages, be about 0.0050% by hydrogen content value, 3 standard sample of 0.0100%, 0.0150% are made to make 3 criterion of acceptability curves by hydrogen determinator description, are respectively used to measure hydrogen content 0.0010%～0.0050%;＞ 0.0050%～0.0100%;The sample of ＞ 0.010%～0.0150% scope；
Step 5, the mensuration of sample:
1) analysis condition is determined: degassing power 5500W, degassing time, 50S；Analyze power 5200W, analysis time, 35S；
2) according to sample hydrogen content approximate range, standard curve passage is selected；
3) input titanium alloy bolt or screw sample number into spectrum, inputs sample weighting amount；The titanium alloy bolt or screw sample that wrap sealing with nickel capsule being placed in sample block, be placed on bottom electrode by new crucible, close electrode furnace, and instrument is automatically performed mensuration video data；Each sample METHOD FOR CONTINUOUS DETERMINATION 3 times, averages, if measurement result and the deviation of meansigma methods are less than 10% every time, then meansigma methods is quoted as sample analysis result；If measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating.
Technique scheme is used to provide the benefit that:
1. a kind of method that the present invention sets up detection being specifically designed to titanium alloy bolt or screw hydrogen content.
2. instant invention overcomes and survey in hydrogen content ASTM 1447-09 technology with inert gas fusion Thermal Conductivity method and infrared detecting method, sample is prepared requirement and is made suitable dimension weight 0.15g～0.30g, on titanium alloy bolt or screw, sampling need to remove top layer, makes the unfavorable factor of sample representativeness difference.
3. the present invention uses standard sample consistent with titanium alloy bolt or screw sampling weight, controls measurement scope, makes condition determination consistent, reduces measurement error.
4. the present invention measures the mass fraction of titanium alloy bolt or screw hydrogen content in the range of 0.0010%～0.0150%.The RSD of measurement result is respectively less than 5%, and precision is preferable.Accuracy in detection is high.For producing control, scientific research provides titanium alloy bolt or screw hydrogen content data accurately.Guarantee space flight, Titanium Alloys for Aviation bolt or screw product quality.
Detailed description of the invention
Below the present invention is described in further detail:
The detection method of hydrogen content in a kind of titanium alloy bolt or screw, comprises the following steps:
Step one, the preparation of sample: cut away under titanium alloy bolt or head of screw, at transition circle position sample, the depth of cut controls at 0.1mm～0.2mm, and lathe rotating speed is not more than 250r/min；In turning process, inaccurate employing liquid cooling, consider length to be worth doing the bar sample shear following sample of growth 5mm；Sampling total amount is 0.30g；After cleaning with acetone, air-dry 20min, during use, each test portion loads pure nickel capsule φ 5mm × 10mm, seals so that it is weight is in the range of 0.04g～0.06g in 0.36g；
Step 2, the mensuration of sample blank: take a new graphite crucible, on hydrogen determinator, it is placed on bottom electrode, close electrode furnace, measures hydrogen content；Being repeated three times, if blank value is more than 0.0000% ± 0.0001%, or the standard deviation of three serial numbers has exceeded 0.0001%, finds out reason and does respective handling, then redeterminating；
Step 3, the mensuration of standard sample: weigh standard sample 0.05g ± 0.01g, load pure nickel capsule φ 5mm × 10mm, 0.36g seals, takes a new graphite crucible, on hydrogen determinator, be placed on bottom electrode, close electrode furnace, measures hydrogen content；It is repeated three times, if measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating；
Step 4, the drafting of standard curve: select 3 passages, be about 0.0050% by hydrogen content value, 3 standard sample of 0.0100%, 0.0150% are made to make 3 criterion of acceptability curves by hydrogen determinator description, are respectively used to measure hydrogen content 0.0010%～0.0050%;＞ 0.0050%～0.0100%;The sample of ＞ 0.010%～0.0150% scope；
Step 5, the mensuration of sample:
1) analysis condition is determined: degassing power 5500W, degassing time, 50S；Analyze power 5200W, analysis time, 35S；
2) according to sample hydrogen content approximate range, standard curve passage is selected；
3) input titanium alloy bolt or screw sample number into spectrum, inputs sample weighting amount；The titanium alloy bolt or screw sample that wrap sealing with nickel capsule being placed in sample block, be placed on bottom electrode by new crucible, close electrode furnace, and instrument is automatically performed mensuration video data；Each sample METHOD FOR CONTINUOUS DETERMINATION 3 times, averages, if measurement result and the deviation of meansigma methods are less than 10% every time, then meansigma methods is quoted as sample analysis result；If measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating.
The principle of the present invention is: the nickel capsule parcel sample being included in a graphite crucible small-sized, disposable melts in carrier gas (argon) atmosphere of a flowing.The hydrogen occurred in sample enters in the air-flow of flowing with the form of hydrogen molecule.Hydrogen is separated from the gas that other decomposes, and finally records its content in thermal conductivity cell detector.
Claims (1)
1. the detection method of hydrogen content in a titanium alloy bolt or screw, it is characterised in that: it comprises the following steps:
Step one, the preparation of sample: cut away under titanium alloy bolt or head of screw, at transition circle position sample, the depth of cut controls at 0.1mm～0.2mm, and lathe rotating speed is not more than 250r/min；Consider length to be worth doing the bar sample shear following sample of growth 5mm；Sampling total amount is 0.30g；After cleaning with acetone, air-dry 20min, during use, each test portion loads pure nickel capsule φ 5mm × 10mm, seals so that it is weight is in the range of 0.04g～0.06g in 0.36g；
Step 2, the mensuration of sample blank: take a new graphite crucible, on hydrogen determinator, it is placed on bottom electrode, close electrode furnace, measures hydrogen content；Being repeated three times, if blank value is more than 0.0000% ± 0.0001%, or the standard deviation of three serial numbers has exceeded 0.0001%, finds out reason and does respective handling, then redeterminating；
Step 3, the mensuration of standard sample: weigh standard sample 0.05g ± 0.01g,
Loading pure nickel capsule φ 5mm × 10mm, seal, take a new graphite crucible, on hydrogen determinator, be placed on bottom electrode in 0.36g, close electrode furnace, measures hydrogen content；It is repeated three times, if measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating；
Step 4, the drafting of standard curve: select 3 passages, be about 0.0050% by hydrogen content value, 3 standard sample of 0.0100%, 0.0150% are made to make 3 criterion of acceptability curves by hydrogen determinator description, are respectively used to measure hydrogen content 0.0010%～0.0050%;＞ 0.0050%～0.0100%;The sample of ＞ 0.010%～0.0150% scope；
Step 5, the mensuration of sample:
1) analysis condition is determined: degassing power 5500W, degassing time, 50S；Analyze power 5200W, analysis time, 35S；
2) according to sample hydrogen content approximate range, standard curve passage is selected；
3) input titanium alloy bolt or screw sample number into spectrum, inputs sample weighting amount；The titanium alloy bolt or screw sample that wrap sealing with nickel capsule being placed in sample block, be placed on bottom electrode by new crucible, close electrode furnace, and instrument is automatically performed mensuration video data；Each sample METHOD FOR CONTINUOUS DETERMINATION 3 times, averages, if measurement result and the deviation of meansigma methods are less than 10% every time, then meansigma methods is quoted as sample analysis result；If measurement result and the deviation of meansigma methods are more than 10% every time, reason should be analyzed and do respective handling, then redeterminating.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107192733A (en) * | 2016-10-27 | 2017-09-22 | 上海景瑞阳实业有限公司 | Hydrogen analyzer is spread in a kind of intelligent quick high accuracy analysis metal |
| CN112415049A (en) * | 2020-11-09 | 2021-02-26 | 辽宁红银金属有限公司 | Method for measuring oxygen content in metal rhenium |
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| CN107192733A (en) * | 2016-10-27 | 2017-09-22 | 上海景瑞阳实业有限公司 | Hydrogen analyzer is spread in a kind of intelligent quick high accuracy analysis metal |
| CN112415049A (en) * | 2020-11-09 | 2021-02-26 | 辽宁红银金属有限公司 | Method for measuring oxygen content in metal rhenium |
| CN112415049B (en) * | 2020-11-09 | 2024-03-29 | 辽宁红银金属有限公司 | Method for measuring oxygen content in metal rhenium |
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