CN107356519A - A kind of method for the corrosion weight loss for determining copper - Google Patents
A kind of method for the corrosion weight loss for determining copper Download PDFInfo
- Publication number
- CN107356519A CN107356519A CN201710589688.5A CN201710589688A CN107356519A CN 107356519 A CN107356519 A CN 107356519A CN 201710589688 A CN201710589688 A CN 201710589688A CN 107356519 A CN107356519 A CN 107356519A
- Authority
- CN
- China
- Prior art keywords
- corrosion
- copper
- sample
- weight loss
- ammoniacal liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention belongs to inorganic chemical analysis technical field, in particular it relates to a kind of method for the corrosion weight loss for determining copper.The quality of testing sample is weighed first, then under anaerobic, detected sample is placed in the ammoniacal liquor for removing oxygen, ultrasonic oscillation, after corrosion product is all dissolved in ammoniacal liquor, sample is cleaned, dry, finally weigh the quality of the sample after removing corrosion product.The quality that the quality of testing sample subtracts the sample after removing corrosion product is the corrosion weight loss of corrosion copper sheet.
Description
Technical field
The invention belongs to inorganic chemical analysis technical field, in particular it relates to which a kind of corrosion for determining copper is lost
The method of weight.
Background technology
Because copper has excellent ductility and conductive, thermal conductivity, good metallic luster, it is widely used in electric
The fields such as industry, building industry, machinery manufacturing industry, light industry and national defense industry.Although the corrosion resistance of copper is stronger,
When humidity is higher or in Korrosionsmedium, more serious corrosion can occur for copper, cause huge economic loss.Therefore, grind
Study carefully the corrosion behavior of copper, tool has very important significance.And the corrosion behavior of copper is studied, it can typically be represented by corrosion weight loss method
The corrosion rate of copper.Thus it is possible to the corrosion weight loss of Accurate Determining copper is to the corrosion rate of qualitative assessment copper and the corruption of research copper
Erosion behavior has very important significance.
At present, the method for determining the corrosion weight loss of copper has：Dissolving with hydrochloric acid method, sulfamic acid dissolution method etc..Both approaches
Relatively good the corrosion product of copper can be dissolved down, but sulfamic acid dissolution method dissolve copper corrosion product when, shape
Into univalent copper ion disproportionated reaction can occur, the metallic copper of generation is attached to copper sheet surface so that remove corrosion product after
The quality of copper sheet is bigger than actual mass, ultimately results in the corrosion weight loss Lower result of the copper measured.And dissolving with hydrochloric acid method is that having
Carried out under the conditions of oxygen, can somewhat damage Copper substrate, metallic copper is dissolved down, cause the corrosion weight loss result of copper that measures inclined
It is high.
And then be badly in need of it is a kind of can the more corrosion weight loss of Accurate Determining copper method, to represent the corrosion rate of copper.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of method for the corrosion weight loss for determining copper.
To achieve the above object, the present invention takes following technical scheme：
A kind of method for the corrosion weight loss for determining copper, under anaerobic, pending sample is placed in the ammonia for removing oxygen
In water, ultrasonic oscillation so that the corrosion product on detected sample is dissolved to ammoniacal liquor, then by sample clean, drying, will shake
Swing the of poor quality of front and rear detected sample, the as corrosion weight loss of testing sample.
The ammonia concn (with water volume ratio) is 1:10-1:3.
Further：
1) (time does not limit, but itself and corruption during under anaerobic, testing sample is immersed in the ammoniacal liquor for removing oxygen
The amount for losing product is relevant), the corrosion product of pending copper sheet sample surfaces is rapidly dissolved in ammoniacal liquor through shaking；
2) detected sample under anaerobic, cleaned with deionized water after removing corrosion product, front and rear treat is shaken
Detect the of poor quality of sample, the as corrosion weight loss of testing sample.
The dry detected sample for removing corrosion product, is carried out with filter paper suck dry moisture or with alcohol or acetone
After flushing, it is dried with natural wind.
The oxygen free condition is to be continually fed into high pure nitrogen (99.99%) to system, flow 10-200mL/min, is passed through
The nitrogen time does not limit, but it is relevant with the time of dissolved corrosion product.
Further：
1) quality of testing sample is weighed with assay balance；
2) under anaerobic, by (time does not limit, but its amount with corrosion product in pending sample immersion ammoniacal liquor
It is relevant), the corrosion product of pending sample surfaces is rapidly dissolved in ammoniacal liquor through shaking；
3) the copper sheet sample under anaerobic, cleaned with deionized water after removing corrosion product；
4) copper sheet after blotting moisture on copper sheet with filter paper or being cleaned with ethanol or acetone rinsing, is carried out with natural wind
Dry；
5) dried copper sheet is weighed with assay balance.
Advantage for present invention：The various corrosion products of copper can be completely dissolved by the inventive method, neither
Disproportionated reaction generation metallic copper can occur and be attached to copper sheet surface, also do not damage Copper substrate, therefore more accurately copper can be obtained
Corrosion weight loss data.
Brief description of the drawings
Fig. 1 is the experiment flow figure for the dissolving testing sample corrosion product that the embodiment of the present invention 1 provides.
Fig. 2 is the SEM figures of the good pure copper sheet of the grinding and polishing of the offer of the embodiment of the present invention 1.
Fig. 3 is the XRD of the good pure copper sheet of the grinding and polishing of the offer of the embodiment of the present invention 1.
Fig. 4 be the embodiment of the present invention 1 provide by step 1) 2) after, the XRD of testing sample.
Fig. 5 is the XRD of the testing sample for the preparation that the embodiment of the present invention 2 provides.
Fig. 6 be the embodiment of the present invention 2 provide by step 1) 2) after, removal corrosion product after copper sheet XRD.
Embodiment
Below in conjunction with the accompanying drawings, the present invention, but do not limit the invention in any way are further described by example.
Embodiment 1
It is another to take the pure copper sheet that size is 25mm × 10mm × 1mm, it is polishing to 3000 mesh with SiC rubbing down paper, then adopted
It is polished to 1 μm (referring to Fig. 2, Fig. 3) with diamond grinding polishing agent.Weigh pure copper sheet quality be：1.894340g.
According to flow shown in Fig. 1：
1) dissolving of copper：Deoxygenation 1h is carried out using high pure nitrogen (99.99%), flow 100mL/min, then persistently led to
Enter high pure nitrogen to keep the anaerobic state of system, be 1 by concentration:The ammoniacal liquor of 5 (with water volume ratio) is added to equipped with copper sheet
In bottle, ultrasonic oscillation, solution is colourless, illustrates that ammoniacal liquor does not react generation divalence copper ammonia complexation ion with copper.
2) cleaning of copper sheet:Under anaerobic, the copper sheet after step 1) is pulled to more than ammoniacal liquor liquid level with rope,
Then clean copper sheet with deionized water (referring to Fig. 4).
3) drying of copper sheet：After filter paper suck dry moisture, natural wind is dried.
Weigh cleaning, the quality of dried copper sheet is：1.894328g.
Solution after above-mentioned cleaning copper sheet is placed under aerobic environment, the change of solution colour：Solution is exposed to air
In, rock, solution illustrate that ammoniacal liquor does not generate monovalence copper ammonia complexation ion with copper reaction still to be colourless, in addition 1) in solution
Color solution is colourless, illustrates that ammoniacal liquor does not react generation divalence copper ammonia complexation ion with copper, both combine, it was demonstrated that are entirely surveying
Copper is not dissolved in ammoniacal liquor during examination, and Copper substrate does not have mass loss.
And as seen from Figure 3, there was only copper on the copper sheet after having cleaned, exist without other corrosion products, it was demonstrated that ammoniacal liquor does not have
It is attached to copper-based precursor reactant generation solid matter on copper sheet.
The quality of copper sheet before and after measuring is weighed, it is found that copper sheet quality has almost no change.
In summary, Copper substrate is not participating in reaction, and the corrosion product on removing copper sheet surface is cleaned with ammoniacal liquor
When, Copper substrate is not influenceed, copper-based weight will not change.
Embodiment 2
It is quick to prepare corrosion copper sheet sample：By size be 25mm × 10mm × 1mm pure copper sheet with SiC rubbing downs paper by slightly to
3000 mesh are finely ground to, are then polished to 1 μm using diamond grinding polishing agent.The good copper sheet of rubbing down is put into 0.1molL-1Sulfuric acid
Soaked 12 days in copper solution, forming surface on copper sheet surface has cuprous oxide and basic copper sulfate (Cu4(OH)6SO4) corrosion copper
Piece (referring to Fig. 5).The quality for weighing corrosion copper sheet is 1.751662g.
According to flow shown in Fig. 1：
1) dissolving of corrosion copper sheet surface corrosion product：Deoxygenation 1h is carried out using high pure nitrogen (99.99%), flow is
100mL/min, high pure nitrogen is then continually fed into keep the anaerobic state of system, be 1 by concentration:The ammoniacal liquor of 5 (volume ratios)
It is added in the bottle equipped with corrosion copper sheet, ultrasonic oscillation, the corrosion product on corrosion copper sheet surface is dissolved down, corrosion product
In copper ion and ammonia form copper ammonia complexation ion.
2) after removing corrosion product, the cleaning of copper sheet：Under anaerobic, by the copper sheet rope after removing corrosion product
It is pulled to more than ammoniacal liquor liquid level, the copper sheet then cleaned with deionized water after removing corrosion product (referring to Fig. 6).
3) drying of copper sheet：After filter paper suck dry moisture, natural wind is dried.
As seen from Figure 6, remove the copper sheet surface after corrosion product and there was only copper, illustrate that corrosion product is dissolved almost completely down
Come.
Weighing the quality of copper sheet after removing corrosion product is：1.746891g.
The quality of copper sheet after the quality of corrosion weight loss=testing sample of copper-removing corrosion product
=1.751662g -1.746891g
=4.771 × 10-3g。
Claims (5)
- A kind of 1. method for the corrosion weight loss for determining copper, it is characterised in that：Under anaerobic, pending sample is placed in removing In the ammoniacal liquor of oxygen, ultrasonic oscillation so that the corrosion product on detected sample is dissolved to ammoniacal liquor, then by sample clean, Dry, the of poor quality of front and rear detected sample, the as corrosion weight loss of testing sample will be shaken.
- 2. the method for the corrosion weight loss of the measure copper as described in claim 1, it is characterised in that：The ammonia concn is (with water body Product ratio) it is 1:10-1:3.
- 3. the weightless method of corrosion copper corrosion is tested as described in claim 1, it is characterised in that：1) during under anaerobic, testing sample is immersed in the ammoniacal liquor for removing oxygen, through shaking pending copper sheet sample table The corrosion product in face is rapidly dissolved in ammoniacal liquor；2) detected sample under anaerobic, cleaned with deionized water after removing corrosion product, it is to be detected before and after shaking Of poor quality, the as corrosion weight loss of testing sample of sample.
- 4. by the method that the test corrosion copper corrosion of claim 1 or 3 is weightless, it is characterised in that：Dry and remove corrosion production The detected sample of thing, it is after being rinsed with filter paper suck dry moisture or with alcohol or acetone, to be dried with natural wind.
- 5. the method for the test corrosion copper corrosion weightlessness as described in claim 1 or 2, it is characterised in that：The oxygen free condition To be continually fed into high pure nitrogen (99.99%), flow 10-200mL/min to system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710589688.5A CN107356519A (en) | 2017-07-19 | 2017-07-19 | A kind of method for the corrosion weight loss for determining copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710589688.5A CN107356519A (en) | 2017-07-19 | 2017-07-19 | A kind of method for the corrosion weight loss for determining copper |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107356519A true CN107356519A (en) | 2017-11-17 |
Family
ID=60284429
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710589688.5A Pending CN107356519A (en) | 2017-07-19 | 2017-07-19 | A kind of method for the corrosion weight loss for determining copper |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107356519A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106894025A (en) * | 2017-04-14 | 2017-06-27 | 中国科学院海洋研究所 | The pickle of zero-g aircraft detection metallic material corrosion thing and application |
-
2017
- 2017-07-19 CN CN201710589688.5A patent/CN107356519A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106894025A (en) * | 2017-04-14 | 2017-06-27 | 中国科学院海洋研究所 | The pickle of zero-g aircraft detection metallic material corrosion thing and application |
Non-Patent Citations (1)
| Title |
|---|
| 刘静宜 等: ""含铜铁矿中氧化亚铜的测定"", 《中国科学院1955年分析化学研究工作报告会会刊》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107742662B (en) | A kind of black silicon suede structure of honeycomb wet process and preparation method thereof and black silion cell and preparation method thereof | |
| CN101256134B (en) | Method for measurement of printed circuit gold-plating layer porosity | |
| CN102764897A (en) | Method for preparing submicron silver powder for electro-conductive paste | |
| JP4737278B2 (en) | Method for analyzing precipitates and / or inclusions in metal materials | |
| CN104357827B (en) | A kind of preparation method of super-hydrophobic corrosion-resistant copper-based surfaces | |
| CN101793855A (en) | Gas sensor with silicon micro-nano structure and manufacturing method thereof | |
| CN106783655A (en) | A kind of method for preparing semiconductor device metal cross section sample | |
| Ikechukwu et al. | Studies on corrosion characteristics of carbon steel exposed to Na2CO3, Na2SO4 and NaCl solutions of different concentrations | |
| CN105177577A (en) | Corrosion method for small-specification red copper rod | |
| CN101314851A (en) | Fine aluminium sheet material corrosive agent | |
| TW201843361A (en) | Method for manufacturing polycrystalline silicon fragment and method for managing surface metal concentration of polycrystalline silicon fragment | |
| CN106404502A (en) | Corrosive agent for displaying grain boundaries of high-damping manganese-based copper alloys and corrosion method thereof | |
| CN111487308B (en) | Microelectrode glucose sensor and preparation method and application thereof | |
| CN103364390A (en) | Surface-enhanced Raman substrate, preparation method and application thereof | |
| CN107356519A (en) | A kind of method for the corrosion weight loss for determining copper | |
| CN112067490B (en) | Novel gravimetric method for determining gold content in aqua regia | |
| CN104593774B (en) | A kind of magnesium alloy metallographic structure observational technique | |
| CN106894025B (en) | Zero-g aircraft detects pickling solution and the application of metallic material corrosion object | |
| CN109713086B (en) | Non-metal black silicon texturing liquid and texturing method using same | |
| CN101493395B (en) | Method for measuring rhodium content in plating liquid | |
| CN109518186B (en) | Alpha and beta biphase brass metallographic corrosive agent and display method of metallographic structure thereof | |
| CN104975294A (en) | Metallographic phase corrosive agent suitable for silver-palladium copper alloy, and preparation method and use method thereof | |
| CN106693727A (en) | Preparation method of super-hydrophobic polyvinylidene fluoride microporous membrane | |
| CN107315064A (en) | A kind of method of cuprous oxide content in golden corrosion product for quantitative determining copper | |
| Srivastava | Mild steel corrosion inhibition, in 4 N sulphuric acid, by a green inhibitor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171117 |