CN109781497A - A kind of quantitative detecting method of electrolytic copper foil surface chromium content - Google Patents
A kind of quantitative detecting method of electrolytic copper foil surface chromium content Download PDFInfo
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- CN109781497A CN109781497A CN201811620162.XA CN201811620162A CN109781497A CN 109781497 A CN109781497 A CN 109781497A CN 201811620162 A CN201811620162 A CN 201811620162A CN 109781497 A CN109781497 A CN 109781497A
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- copper foil
- detection method
- standard curve
- chromium
- hydrochloric acid
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Abstract
The invention discloses a kind of quantitative detecting methods of electrolytic copper foil surface chromium content, comprising the following steps: 1) weighs after copper foil sample shreds and be put into container, hydrochloric acid solution is added, is heated to boiling, filtrate is obtained by filtration；2) heating filtrate concentration, after cooling, constant volume；3) chromium standard curve is made with Atomic Absorption Spectrometer, according to standard curve determination chromium content.Beneficial effects of the present invention: testing background interference is small, and signal-to-noise ratio is high, and test error is low, and sample treatment is simple, and test speed is fast.
Description
Technical field
The present invention relates to analysis and testing technology fields, it particularly relates to which a kind of electrolytic copper foil surface chromium content quantifies
Detection method.
Background technique
In electrolytic copper foil production, it is a critically important content that copper foil surface, which handles passivation technology, and used is one
Kind liquid containing chromium passivating.For copper foil in the passivating solution of energization, surface forms the film of dense structure, and it is anti-oxidant can to greatly improve its
Property.Copper foil surface chromium content is too low to will affect its inoxidizability, and too high levels not only influence copper foil electric conductivity, can also make to human body
At injury, larger pollution is caused to environment.Copper foil surface chromium content detection method is not yet established at present.
For the problems in the relevant technologies, currently no effective solution has been proposed.
Summary of the invention
For above-mentioned technical problem in the related technology, the present invention proposes a kind of quantitative inspection of electrolytic copper foil surface chromium content
Survey method, testing background interference is small, and signal-to-noise ratio is high, and test error is low, and sample treatment is simple, and test speed is fast.
To realize the above-mentioned technical purpose, the technical scheme of the present invention is realized as follows:
A kind of quantitative detecting method of electrolytic copper foil surface chromium content, comprising the following steps:
1) it weighs after copper foil sample shreds and is put into container, hydrochloric acid solution is added, is heated to boiling, filtrate is obtained by filtration；
2) heating filtrate concentration, after cooling, constant volume；
3) chromium standard curve is made with Atomic Absorption Spectrometer, according to standard curve determination chromium content.
Further, the step 1) sample size is 20cm*20cm, with a thickness of 6-9mm.
Further, the step 1) hydrochloric acid solution mass percent concentration is 15-21%, and hydrochloric acid additional amount is 80-
160mL。
Further, the step 1) concentration of hydrochloric acid is 18%, additional amount 100-140mL.
Further, it is 5-15min that the step 1), which begins to warm up boiling time,.
Further, it is 10min that the step 1), which begins to warm up boiling time,.
Further, constant volume 250ml volumetric flask constant volume in the step 2.
Further, chromium standard solution used in the step 3) chromium standard curve is 0ppm, 1ppm, 2ppm, 3ppm.
Further, the correction coefficient of determination of the step 3) standard curve needs >=0.99.
Beneficial effects of the present invention: testing background interference is small, and signal-to-noise ratio is high, and test error is low, and sample treatment is simple, test
Speed is fast.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only some implementations of the invention
Example, for those of ordinary skill in the art, without creative efforts, can also obtain according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the canonical plotting of according to embodiments of the present invention 1 chromium standard solution；
Fig. 2 is the canonical plotting of according to embodiments of the present invention 2 chromium standard solutions；
Fig. 3 is the canonical plotting of according to embodiments of the present invention 3 chromium standard solutions.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art's every other embodiment obtained belong to what the present invention protected
Range.
Embodiment 1
Gauze gloves are put on, extract 20cm*20cm with a thickness of 8 microns of copper foil sample, weighing quality is 2.876g, and sample is rubbed
Accordion is helped, cuts and fritter is made, fritter sample is put into 250mL beaker, the hydrochloric acid that addition 120mL concentration is 18% to sample
Product are totally submerged, and are placed the beaker and are boiled after heating 10min on electric furnace, filter after boiling, and filtrate is poured into 500mL beaker, are remained
Remaining copper foil twice with pure water, all pour into beaker and merge twice by filtrate, and filtrate continues to boil, after concentration volume to 200mL
It is cooled to room temperature, with 250mL volumetric flask constant volume, shakes up stand-by.
4 small beakers pour into 0ppm, 1ppm, 2ppm, 3ppm chromium standard solution respectively, make chromium with Atomic Absorption Spectrometer
Standard curve.Curvature correction coefficient of determination is 0.9972, and linear relationship is fine, and the canonical plotting of acquisition is as shown in Figure 1, explanation
Standard curve is qualified.
According to standard curve test sample, measuring result is 0.877ppm.
Unit mass chromium content=cv/m=(0.877*0.25/2.876) * 1000=76.3ppm.
Embodiment 2:
Gauze gloves are put on, extract 20cm*20cm with a thickness of 9 microns of copper foil sample, weighing quality is 3.501g, and sample is rubbed
Accordion is helped, cuts and fritter is made, fritter sample is put into 250mL beaker, the hydrochloric acid that addition 140mL concentration is 18% to sample
Product are totally submerged, and are placed the beaker and are boiled after heating 10min on electric furnace, filter after boiling, and filtrate is poured into 500mL beaker, are remained
Remaining copper foil twice with pure water, all pour into beaker and merge twice by filtrate, and filtrate continues to boil, after concentration volume to 200mL
It is cooled to room temperature, with 250mL volumetric flask constant volume, shakes up stand-by.
4 small beakers pour into 0ppm, 1ppm, 2ppm, 3ppm chromium standard solution respectively, make chromium with Atomic Absorption Spectrometer
Standard curve, curvature correction coefficient of determination are 0.9992, and linear relationship is fine, and canonical plotting is as shown in Fig. 2, description standard is bent
Line is qualified.
According to standard curve test sample, measuring result is 0.875ppm.
Unit mass chromium content=cv/m=(0.875*0.25/2.876) * 1000=62.5ppm.
Embodiment 3:
Gauze gloves are put on, extract 20cm*20cm with a thickness of 6 microns of copper foil sample, weighing quality is 2.097g, and sample is rubbed
Accordion is helped, cuts and fritter is made, fritter sample is put into 250mL beaker, the hydrochloric acid that addition 100mL concentration is 18% to sample
Product are totally submerged, and are placed the beaker and are boiled after heating 10min on electric furnace, filter after boiling, and filtrate is poured into 500mL beaker, are remained
Remaining copper foil twice with pure water, all pour into beaker and merge twice by filtrate, and filtrate continues to boil, after concentration volume to 200mL
It is cooled to room temperature, with 250mL volumetric flask constant volume, shakes up stand-by.
4 small beakers pour into 0ppm, 1ppm, 2ppm, 3ppm chromium standard solution respectively, make chromium with Atomic Absorption Spectrometer
Standard curve, curvature correction coefficient of determination are 0.9995, and linear relationship is fine, and canonical plotting is as shown in figure 3, description standard is bent
Line is qualified.
According to standard curve test sample, measuring result is 1.336ppm.
Unit mass chromium content=cv/m=(1.336*0.25/2.876) * 1000=159.3ppm.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of quantitative detecting method of electrolytic copper foil surface chromium content, which comprises the following steps:
1) it weighs after copper foil sample shreds and is put into container, hydrochloric acid solution is added, is heated to boiling, filtrate is obtained by filtration；
2) heating filtrate concentration, after cooling, constant volume；
3) chromium standard curve is made with Atomic Absorption Spectrometer, according to standard curve determination chromium content.
2. detection method according to claim 1, which is characterized in that the step 1) sample size is 20cm*20cm, thick
Degree is 6-9mm.
3. detection method according to claim 1, which is characterized in that the step 1) hydrochloric acid solution mass percent concentration
For 15-21%, hydrochloric acid additional amount is 80-160mL.
4. detection method according to claim 1, which is characterized in that the step 1) concentration of hydrochloric acid is 18%, and additional amount is
100-140mL。
5. detection method according to claim 1, which is characterized in that it is 5- that the step 1), which begins to warm up boiling time,
15min。
6. detection method according to claim 1, which is characterized in that the step 1) begins to warm up boiling time and is
10min。
7. detection method according to claim 1, which is characterized in that constant volume is fixed with 250ml volumetric flask in the step 2
Hold.
8. detection method according to claim 1, which is characterized in that chromium standard used in the step 3) chromium standard curve
Solution is 0ppm, 1ppm, 2ppm, 3ppm.
9. detection method according to claim 1, which is characterized in that the correction coefficient of determination of the step 3) standard curve
Need >=0.99.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811620162.XA CN109781497A (en) | 2018-12-28 | 2018-12-28 | A kind of quantitative detecting method of electrolytic copper foil surface chromium content |
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| CN201811620162.XA CN109781497A (en) | 2018-12-28 | 2018-12-28 | A kind of quantitative detecting method of electrolytic copper foil surface chromium content |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610181A (en) * | 2020-06-05 | 2020-09-01 | 多氟多新能源科技有限公司 | Quantitative detection method for chromium content of copper foil |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103852434A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Quantitative analysis method for content of hexavalent chromium in polymer and electronic components |
-
2018
- 2018-12-28 CN CN201811620162.XA patent/CN109781497A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103852434A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Quantitative analysis method for content of hexavalent chromium in polymer and electronic components |
Non-Patent Citations (1)
| Title |
|---|
| 孟广政 等: "镀锡薄钢板钝化膜中铬的原子吸收光谱分析", 《原子光谱分析》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111610181A (en) * | 2020-06-05 | 2020-09-01 | 多氟多新能源科技有限公司 | Quantitative detection method for chromium content of copper foil |
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Application publication date: 20190521 |