CN1064941A - Oxygen in Oxygen-Free Copper standard substance and preparation method - Google Patents
Oxygen in Oxygen-Free Copper standard substance and preparation method Download PDFInfo
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- CN1064941A CN1064941A CN 92106078 CN92106078A CN1064941A CN 1064941 A CN1064941 A CN 1064941A CN 92106078 CN92106078 CN 92106078 CN 92106078 A CN92106078 A CN 92106078A CN 1064941 A CN1064941 A CN 1064941A
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Abstract
A kind of standard substance of Oxygen in Oxygen-Free Copper and manufacture method, its principal character are that the definite value of oxygen content in this standard substance is not more than 10ppm, and the definite value of embodiment is 3.0 ± 0.7ppm.The technology for preparing this standard substance by strict selection from oxygen-free copper bar, is repeatedly drawn and is rolled, and uniformity cuts into sample, and steps such as machine barking and chemical polishing are formed.Through with various analytical approachs and Instrument measuring, prove that its oxygen content is even, value data is reliable, standard deviation is little, and sample surfaces is bright and clean, and sampling is convenient and cheap, the single analyses cost is 1/13 of an external like product only, uses when being suitable for oxygen-free copper manufacturer and user's testing product.
Description
The present invention relates to a kind of standard substance and preparation technology who is used for measuring the copper oxygen content, belong to physical and chemical testing and standard matter preparing technology field, when oxygen-free copper manufacturer and user's product detects, use.
As everyone knows, the content of Oxygen in Oxygen-Free Copper has appreciable impact to its conductivity and mechanical property, be accurately to determine in time the content in the product, promptly need advanced pick-up unit, also need definite value accurately and reliably in the copper standard substance of oxygen as correcting sample.In recent years, domestic many users have introduced advanced apparatus for determination of oxygen, but in real work because the domestic standard substance that does not prepare oxygen in the copper as yet, and can only replace as correcting sample with the mark steel, because the standard substance of oxygen is different with the standard substance of oxygen in the copper in the copper, especially Oxygen in Oxygen-Free Copper content is very low, the affinity of copper and carbon a little less than, after the sample melted carburizing ability a little less than, and the extraction curve of oxygen in steel is different with the extraction curve in copper, the people is thrown doubt upon to the accuracy and the reliability of measurement result, for guaranteeing product quality, the standard substance of seeking Oxygen in Oxygen-Free Copper is the task of top priority of domestic production producer as correcting sample, abroad can production of copper in the producer of standard substance of oxygen also very few, not only its preparation technology maintains secrecy, cost an arm and a leg, specification is unreasonable, and can not guarantee the timely supply of material, therefore, domestic production producer can't adopt the standard substance of oxygen in the external copper for preparing in routine analysis work.
The objective of the invention is to overcome the above-mentioned deficiency of prior art, develop a kind of standard substance, thereby solve the matter of great urgency of domestic production producer with Oxygen in Oxygen-Free Copper of good accuracy and degree of accuracy.
The standard substance of the Oxygen in Oxygen-Free Copper that the present invention develops, the anaerobic copper material that has drawn from homemade, as diameter is the oxygen-free copper bar of 8mm, the definite value that it is characterized by oxygen content in this standard substance is not more than 10PPm, to satisfy the needs that domestic Tul trade mark oxygen-free copper bar and electron level oxygen-free copper are produced, consider the needs of domestic main manufacturer international sale, to contain best definite value be 3.0 ± 0.7PPm to oxygen in the standard substance that the present invention provides.
For realizing goal of the invention, the process of the standard substance that preparation the present invention provides mainly may further comprise the steps:
A, strictness are selected materials.In view of the content of homemade Oxygen in Oxygen-Free Copper should not surpass 10PPm, therefore can directly select the raw material of anaerobic copper material for use as the development standard substance.Certainly cathode copper of GB is dropped into smelting furnace and melt in protective atmosphere, the raw material of making the development standard substance certainly is good.
B, under free of contamination environment, adopt at least that secondary draws the type of rolling into.
C, with the oxygen-free copper bar branch section of being cut into of moulding, carry out the uniformity of oxygen content.
D, will measure qualified oxygen-free copper bar and shear sample preparation, and after machine barking and chemical polishing, be packaged into standard substance and sell.
For finishing goal of the invention better, guarantee that the standard substance preparation work of Oxygen in Oxygen-Free Copper is smooth, oxygen-free copper bar being drawn when rolling into type, for avoiding polluting the oxygen-free copper bar surface, can adopt hospital gauze repeatedly wiping copper bar one end draw the way of wire drawing; When carrying out the uniformity of oxygen content, adopted U.S. LecoRO-416DR type apparatus for determination of oxygen, to every group of sample replication 3 times, reliable to guarantee measurement result; For making the standard substance any surface finish, reduce the oxidation and the pollution of its superficial layer to greatest extent, behind machine barking, immerse anhydrous spilling again and soaked at least in the essence 2 minutes.Carefully dry and be encapsulated into bag.
The standard substance of the Oxygen in Oxygen-Free Copper that the present invention provides compares with external like product, has oxygen level and is evenly distributed, and standard deviation is little, sample surfaces is smooth, advantages such as sampling is convenient and cheap, and can develop series of products, as bar-shaped, spherical, wire and granular.The preparation technology of this standard substance is simple possible also, and operation is reasonable, is convenient to tissue and produces in batches.
At last, be the embodiment of the standard substance of 3.0PPm in conjunction with the definite value for preparing oxygen content, sketch preparation technology's method that the present invention provides once more.
At first from being the diameter 8mm oxygen-free copper bar of 3～5PPm, actual oxygen level selects the raw material that is fit to do the development standard substance, divide the oxygen-free copper bar that is drawn into any surface finish of diameter 5mm for three times with wire drawing machine then, roll in the type process drawing, for avoiding polluting the oxygen-free copper bar surface, adopt hospital gauze wiping copper bar one end to draw the method for rolling, the chemical constitution of this oxygen-free copper bar sees Table one:
With the oxygen-free copper bar branch section of being cut into of diameter 5mm, every section long for 2m, gets 15 groups altogether.Carry out uniformity, accurate for guaranteeing measurement result, adopt U.S. LecoRO-416DR type apparatus for determination of oxygen to measure, every group of sample counterpoise repetition measurement decided 3 times, degassing electric current 1100A with pulse infrared method, analyze electric current 1050A, minimum analysis time 25 seconds, the homogeneity initial survey population mean that obtains is 0.19PPm for the 2.9PPm standard deviation, and homogeneity calibrating data are calculated with the F method of inspection, the result proves that its uniformity coefficient is good, can process packing.
The oxygen-free copper bar that uniformity inspection is qualified is sheared sample preparation, and specification is the bar-shaped of ∮ 5 * 75mm, for guaranteeing that sample surfaces is bright and clean, reduce the oxidation and the pollution of superficial layer, sample embathes 3 times through distilled water behind machine barking, puts into anhydrous alcohol and soaks 2 minutes, dries after the taking-up and is encapsulated into bag.Per two is a cover, heavily about 27 grams, and price is 1/10th of an external like product, the single analyses cost only is 1/13rd.
The standard substance of the Oxygen in Oxygen-Free Copper after the packing, by " national metering technology normalized JJG1006-86 " regulation, grab sample is rechecked it and is contained the oxygen uniformity coefficient, it rechecks population mean is 2.9PPm, standard deviation is 0.35PPm, calculate with the F method of inspection rechecking data, it is good to prove that once more this standard substance contains the oxygen uniformity coefficient.Through the standard substance that the present invention provides being measured with different analytical approachs and instrument, its definite value is 3.0 ± 0.7PPm, instrument and the method used during mensuration have: LecoTc-136, LecoRo-316, pulsed infrared apparatus for determination of oxygen and the coulometric titration of LecoRo-416 and LecoRo-416DR, and with oxygen standard substance verification in the U.S. LecoPartNO502-031 copper, the standard substance of the Oxygen in Oxygen-Free Copper that proof the present invention provides, oxygen content is even, value data is reliable, reach the level of the similar standard substance of external advanced country, can at home and abroad sell on the market as the correcting sample of routine analysis work.
Claims (5)
1, a kind of standard substance that is used for measuring the copper oxygen content is characterized in that the definite value of oxygen content in this standard substance is not more than 10PPm.
2, standard substance according to claim 1, the definite value that it is characterized in that oxygen content in this standard substance is 3.0 ± 0.7PPm.
3, a kind of process for preparing the described standard substance of claim 1 is characterized in that mainly may further comprise the steps:
A, select for use oxygen level to be not more than the anaerobic copper material of 10PPm;
B, under free of contamination environment, adopt at least that secondary draws the type of rolling into;
C, with the anaerobic copper material branch section of being cut into of moulding, carry out uniformity;
D, will measure qualified anaerobic copper material and shear sample preparation, through being packaged into bag after machine barking and the chemical polishing.
4, process according to claim 3 is characterized in that the b step draws the anaerobic copper material when rolling into type, adopted hospital gauze repeatedly wiping draw the anti-pollution measure that rolls.
5, process according to claim 3 is characterized in that the chemically polishing method that the d step adopts is: the anaerobic copper material that will cut into sample is immersed in the anhydrous alcohol at least 2 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106078 CN1064941A (en) | 1992-03-06 | 1992-03-06 | Oxygen in Oxygen-Free Copper standard substance and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106078 CN1064941A (en) | 1992-03-06 | 1992-03-06 | Oxygen in Oxygen-Free Copper standard substance and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1064941A true CN1064941A (en) | 1992-09-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92106078 Pending CN1064941A (en) | 1992-03-06 | 1992-03-06 | Oxygen in Oxygen-Free Copper standard substance and preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100337288C (en) * | 2005-06-27 | 2007-09-12 | 江阴市电工合金有限公司 | Oxygen-free copper generatrix and its preparing method |
| CN108287227A (en) * | 2017-12-25 | 2018-07-17 | 新兴铸管（浙江）铜业有限公司 | A kind of diameter 8mm continuous casting and rolling low oxygens copper bar high oxygen content accuracy checking method |
| CN109781482A (en) * | 2018-12-24 | 2019-05-21 | 新兴铸管（浙江）铜业有限公司 | Continuous casting and rolling produces the copper bar method of production measurement of oxygen content sample |
-
1992
- 1992-03-06 CN CN 92106078 patent/CN1064941A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100337288C (en) * | 2005-06-27 | 2007-09-12 | 江阴市电工合金有限公司 | Oxygen-free copper generatrix and its preparing method |
| CN108287227A (en) * | 2017-12-25 | 2018-07-17 | 新兴铸管（浙江）铜业有限公司 | A kind of diameter 8mm continuous casting and rolling low oxygens copper bar high oxygen content accuracy checking method |
| CN108287227B (en) * | 2017-12-25 | 2020-10-13 | 新兴铸管（浙江）铜业有限公司 | High-precision detection method for oxygen content of 8 mm-diameter continuous casting and rolling low-oxygen copper rod |
| CN109781482A (en) * | 2018-12-24 | 2019-05-21 | 新兴铸管（浙江）铜业有限公司 | Continuous casting and rolling produces the copper bar method of production measurement of oxygen content sample |
| CN109781482B (en) * | 2018-12-24 | 2021-08-13 | 新兴铸管（浙江）铜业有限公司 | Method for manufacturing oxygen content detection sample for copper rod production by continuous casting and rolling |
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