CN101968416B - Method for detecting weight of fingerprint resistant film of fingerprint-resistant electro-galvanized sheet - Google Patents
Method for detecting weight of fingerprint resistant film of fingerprint-resistant electro-galvanized sheet Download PDFInfo
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- CN101968416B CN101968416B CN 200910055491 CN200910055491A CN101968416B CN 101968416 B CN101968416 B CN 101968416B CN 200910055491 CN200910055491 CN 200910055491 CN 200910055491 A CN200910055491 A CN 200910055491A CN 101968416 B CN101968416 B CN 101968416B
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Abstract
The invention relates to a fingerprint resistant film, in particular to a method for detecting the weight of the fingerprint resistant film. The method for detecting the weight of the fingerprint resistant film of a fingerprint-resistant electro-galvanized sheet comprises the following steps of: preparing dezincing solution and zinc standard solution; sampling; sample processing; detecting the total weight of a galvanized coating; detecting galvanized amount; and working out the weight of the fingerprint resistant film. By the method, the weight of the fingerprint resistant film can be directly, correctly and quickly detected, and the detection is not influenced by the change of fingerprint resistant raw material components and a production process.
Description
Technical field
The present invention relates to the film of anti-the fingerprint, relate in particular to a kind of detection method of the film of anti-fingerprint weight.
Background technology
The film of anti-the fingerprint is a kind of organic coating, can effectively improve its corrosion stability and anti-contamination ability at electrolytic galvanized sheet coating one deck film of anti-the fingerprint.Because the film of anti-the fingerprint is as too thin, then the product corrosion stability is relatively poor; And if too thick, then the processability of product and electric conductivity are relatively poor, can not satisfy requirement of client, and cost of idleness, so the amount of filming need detect, with control within the specific limits.At present, the open report that does not also have the film of anti-fingerprint weight detecting.It is reported, fluorescence method is adopted in the detection of the domestic and international film of anti-fingerprint weight usually, its measuring principle is: the content that the luminoscope that contains in the working sample film of anti-the fingerprint can be measured is the fluorescence intensity of fixing element comparatively, try to achieve the film of anti-fingerprint weight of sample then by the calibration curve of prior making, the on-gauge plate of anti-fingerprint that the making calibration curve is used is produced by the paint supply merchant and is provided.
Owing to being produced by the paint supply merchant with the used on-gauge plate of anti-fingerprint of the fluorescence spectrometry film of anti-fingerprint weight and its accuracy invalidated being provided.In addition, the mensuration accuracy of fluorescence method is that the composition that is based upon fingerprint-resistant coating is stablized on the constant basis, and the film component of anti-fingerprint of sample must be identical with standard specimen.But the different batches composition has fluctuation during owing to the fingerprint-resistant coating actual production; In addition, unit is when producing fingerprint-proof plate, and production run can be influential to paint ingredient, so there is certain problem in the mensuration accuracy of fluorescence method.
Direct and the most reliable detection method of the film of anti-fingerprint weight is gravimetric method, namely adopt certain reagent only the film of anti-the fingerprint to be removed and do not corrode the zinc layer that contacts with it, remove weight difference and the area of front and back sample according to the film of anti-the fingerprint, thereby try to achieve the film of anti-fingerprint weight of unit area.But because the good solvent resistance of the film of anti-the fingerprint, be difficult to find and only remove the film of anti-the fingerprint and the reagent of corrosion zinc layer not.
Summary of the invention
The present invention is intended to address the aforementioned drawbacks, and a kind of assay method of the film of anti-fingerprint weight is provided.The present invention can directly measure the film of anti-fingerprint weight accurately, comparatively rapidly, is not subjected to the influence of the material composition of anti-fingerprint change and production technology.
The present invention is achieved in that
A kind of detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, it comprises:
The preparation steps of dezincification liquid and zinc standard solution;
Sampling procedure: cut or dash and get a sample from the electrolytic galvanized sheet of anti-the fingerprint, area is A (m
2);
Sample treatment step: dip in detersive wiping specimen surface with soft paper handkerchief or absorbent cotton, remove oil stain and dirt, dry up with hair-dryer then;
The determination step of zinc coat general assembly (TW):
The sample weight W1 (g) that handles well with analytical balance weighing place places container with sample then earlier, makes coat side to be measured upwards;
At room temperature slowly add 50mL dezincification liquid by its vigorous reaction to stopping, being about to sample takes out, water washes and washing fluid is washed in the described container, then with this towards the thin liquid constant volume to 250mL, take out sample and dry up specimen surface with hair-dryer, re-use with the identical analytical balance of a preceding weighing and carry out weighing W2 (g);
The determination step of zinc-plated amount: adopt the ICP-AES method, try to achieve the zinc-plated amount W3 (g) of sample according to calibration curve;
The film of anti-fingerprint weight film of anti-fingerprint weight=(W1-W2-W3)/A then
Unit: g/m
2
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, the preparation steps of described dezincification liquid comprises: the 500mL concentrated hydrochloric acid is joined in the beaker that contains 500mL water and 3.5g hexamethylenetetramine, shake up.
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, the concentration of described zinc standard solution are 10g/L, and it is to be dissolved in the 100ml concentrated hydrochloric acid and to be diluted to 1000ml with water by the 10g high-purity Zn forming.
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, as be that single face is measured, described sample treatment step also comprises: sample is not needed the face closure measured with closed material.
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, described closed material are acid proof paint or acidproof adhesive tape.
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, the method for making of the calibration curve in the described zinc-plated quantitative determination step is: preparation one cover comprises the zinc-plated amount concentration of sample in interior zinc standard solution series, and this serial constant volume is 250ml; The ICP point fight stable after, measure calibration solution zinc element in the intensity of one or more spectral line of 328.2nm, 330.2nm, 334.5,472.2nm, 481.0nm, corresponding zinc content is made calibration curve, and the calibration curve linearly dependent coefficient satisfies r 〉=0.9999.
The detection method of the described electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight, when the mensuration spectral line had many, zinc-plated amount W3 was the mean value of many spectral line measurement results.
The present invention can be comparatively fast, the accurate quantitative measurement film of anti-fingerprint weight, do not use toxic reagent in the mensuration process.Compare with fluorescence method, solved the problem that fluorescence method must prepare the film of anti-fingerprint weight standard plate, also solved the fluctuation of the raw material of anti-fingerprint paint ingredient and fingerprint-proof plate production to the influence of film component.
Embodiment
The specific embodiment of the present invention is as follows:
1 reagent and material
Annotate: in analytic process, the preparation test solution should adopt analytical reagent, and institute's water should adopt distilled water or deionized water.
1.1 concentrated hydrochloric acid, ρ ≈ 1.18g/mL.
1.2 hexamethylenetetramine, C
6H
12N
4, corrosion inhibiter, the corrosion of protection base steel acid and alkali when being used for dissolving coating.
1.3 dezincification liquid joins 500mL hydrochloric acid (1.1) in the beaker that contains 500mL water and 3.5g hexamethylenetetramine (1.2), shakes up.
1.4 closed material, acid proof paint or acidproof adhesive tape.
1.5 the zinc standard solution, 10g/L accurately takes by weighing 10g high purity zinc (purity is not less than 99.99%), is accurate to 0.001g, is dissolved in the 100mL hydrochloric acid (1.1), after the cooling solution is changed in the 1000mL volumetric flask, is diluted with water to scale and shakes up.
1.6 detersive, acetone or anhydrous alcohol.
2 instrument and equipments
2.1 analytical balance, sensibility reciprocal are 0.1mg
2.2 vernier caliper, minimum calibration 0.02mm
2.3 inductively coupled plasma atomic emission spectrometer (ICP)
2.3.1 use ICP to use after with the instrument optimization according to operation instruction.
2.3.2 short-term stability: 10 sample solutions of continuous coverage, the relative standard deviation of measurement result should not surpass 0.5%.
2.3.3 zinc elements are contained spectral line:.
2.4 sampling instrument is as plate shearing machine or punch press
2.5 glass wares, volumetric flask, transfer pipet, beaker etc.
3 determination steps
3.1 sampling: dashing mode such as get with cutting implement clip or punch press, to get area be sample about 0.01 square metre, and sampling process should avoid destroying the film of anti-fingerprint that needs measurement.
3.2 sample is handled: dip in detersive (1.6) wiping specimen surface with soft paper handkerchief or absorbent cotton, remove oil stain and dirt, dry up with hair-dryer then.As be that single face is measured, must sample not needed the face closure measured with closed material (1.4).If use adhesive tape as closed material, adhesive tape should be pressed in specimen surface, remove bubble or fold, and cut the unnecessary part of adhesive tape.The marginal portion of sample is also sealed with closed material.
3.3 the mensuration of coated layer general assembly (TW): use the size of vernier caliper measurement sample, be accurate to 0.05mm, calculate sample area A (m
2) be accurate to 0.1mm
2The sample weight W1 (g) that uses the analytical balance weighing to prepare is accurate to 0.1mg, notes as the original weight of sample.Sample is placed proper container, make coat side to be measured upwards.At room temperature slowly add 50mL dezincification liquid (1.3), when vigorous reaction stops, immediately sample being taken out.Water flushing also washes washing fluid in the same container, then with this solution constant volume to 250mL, be used for the zinc-plated amount of mensuration.The sample that takes out dries up specimen surface with hair-dryer, re-uses with the identical analytical balance of a preceding weighing and carries out weighing W2 (g), is accurate to 0.1mg.
3.4 the mensuration of zinc-plated amount
3.4.1 make the ICP calibration curve
Preparation one cover comprises the zinc-plated amount concentration of sample in interior zinc standard solution series, and table 1 has been enumerated a kind of method of preparing standard series, and this calibrates serial constant volume is 250mL.
Table 1 calibration series
| Calibration solution | The volume (mL) that adds standard solution (1.5) | The quality of Zn (g) in the 250mL standard solution | The volume (mL) that adds membrane removal liquid (1.3) |
| 1 | 0 | 0 | 50 |
| 2 | 10 | 0.1 | 50 |
| 3 | 20 | 0.2 | 50 |
| 4 | 30 | 0.3 | 50 |
| 5 | 40 | 0.4 | 50 |
| 6 | 50 | 0.5 | 50 |
The ICP point fight stable after, measure the intensity of one or more spectral line among calibration solution zinc element 328.2nm, 330.2nm, 334.5, the 472.2nm, 481.0, corresponding zinc content is made calibration curve, and the calibration curve linearly dependent coefficient should satisfy r 〉=0.9999.
3.4.2 measure the zinc-plated amount of sample
Adopt the condition identical with making calibration curve to measure sample solution zinc element, try to achieve the zinc-plated amount W3 (g) of sample according to calibration curve.As adopting many spectral lines to measure, W3 is the mean value of many spectral line measurement results.
4 results calculate
The film of anti-fingerprint weight=(W1-W2-W3)/A
Unit: g/m2
Adopt method of the present invention that the fingerprint-proof plate that certain steel plant produces is measured with fluorescence method and the inventive method respectively, the result is as follows:
The gravimetric determination result: sample original weight W1:90.2269g,
Sample is removed the weight W 2:90.0337g behind zinc layer and the film of anti-the fingerprint;
Zinc layer weight (ICP-AES method): calibration curve linearity, measurement result, each spectral line are measured repeatability for 10 times and be the results are shown in Table 2;
Table 2ICP-AES method measurement result
| Spectral line | Zn328.2 | Zn330.2 | Zn334.5 | Zn472.2 | Zn481.0 |
| The calibration curve linearly dependent coefficient | 0.99996 | 0.99997 | 0.99999 | 0.99996 | 0.99998 |
| Mean value (g) | 0.1792 | 0.1769 | 0.1773 | 0.1778 | 0.1787 |
| Standard deviation (g) | 0.0006 | 0.0010 | 0.0006 | 0.0008 | 0.0007 |
| Relative standard deviation (%) | 0.33 | 0.57 | 0.32 | 0.48 | 0.36 |
Because 10 measurement result relative standard deviations of Zn3302 spectral line are greater than 0.5%, this result casts out, and other spectral line measurement result is averaged, and getting the zinc amount is 0.1782g;
The area of materialsing is 0.0098175m
2So the film of anti-fingerprint weight per unit area is: (90.2269-90.0337-0.1782)/0.0098175=1.5g/m
2
This sample is 1.3g/m with the fluorescence spectrometry film of anti-fingerprint result before this
2
Claims (7)
1. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-a fingerprint weight is characterized in that, it comprises:
The preparation steps of dezincification liquid and zinc standard solution;
Sampling procedure: cut or dash and get a sample from the electrolytic galvanized sheet of anti-the fingerprint, area is A m
2
Sample treatment step: dip in detersive wiping specimen surface with soft paper handkerchief or absorbent cotton, remove oil stain and dirt, dry up with hair-dryer then;
The determination step of coated layer general assembly (TW):
The sample weight W1g that handles well with the analytical balance weighing places container with sample then earlier, makes coat side to be measured upwards;
At room temperature slowly add 50mL dezincification liquid by its vigorous reaction to stopping, being about to sample takes out, water washes and washing fluid is washed in the described container, then with the solution constant volume in this container to 250mL, take out sample and dry up specimen surface with hair-dryer, re-use with the identical analytical balance of a preceding weighing and carry out weighing W2g;
The determination step of zinc-plated amount: adopt the ICP-AES method, try to achieve the zinc-plated amount W3g of sample according to calibration curve;
The film of anti-fingerprint weight film of anti-fingerprint weight=(W1-W2-W3)/A then
Unit: g/m
2
2. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 1 is characterized in that, the preparation steps of described dezincification liquid comprises: the 500mL concentrated hydrochloric acid is joined in the beaker that contains 500mL water and 3.5g hexamethylenetetramine, shake up.
3. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 1 is characterized in that, the concentration of described zinc standard solution is 10g/L, and it is to be dissolved in the 100ml concentrated hydrochloric acid and to be diluted to 1000ml with water by the 10g high-purity Zn forming.
4. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 1 is characterized in that, as is that single face is measured, and described sample treatment step also comprises: sample is not needed the face closure measured with closed material.
5. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 4 is characterized in that, described closed material is acid proof paint or acidproof adhesive tape.
6. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 1, it is characterized in that, the method for making of the calibration curve in the described zinc-plated quantitative determination step is: preparation one cover comprises the zinc-plated amount concentration of sample in interior zinc standard solution series, and this serial constant volume is 250ml; The ICP point fight stable after, measure calibration solution zinc element in the intensity of one or more spectral line of 328.2nm, 330.2nm, 334.5nm, 472.2nm, 481.0nm, corresponding zinc content is made calibration curve, and the calibration curve linearly dependent coefficient satisfies r 〉=0.9999.
7. the detection method of the electrolytic galvanized sheet of anti-fingerprint film of anti-fingerprint weight according to claim 6 is characterized in that, when the mensuration spectral line had many, zinc-plated amount W3 was the mean value of many spectral line measurement results.
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| CN 200910055491 CN101968416B (en) | 2009-07-28 | 2009-07-28 | Method for detecting weight of fingerprint resistant film of fingerprint-resistant electro-galvanized sheet |
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| CN106770188A (en) * | 2015-11-24 | 2017-05-31 | 上海梅山钢铁股份有限公司 | A kind of detection method of tin plate chromium-free passivating film film weight |
| CN105466909A (en) * | 2015-12-23 | 2016-04-06 | 重庆长安工业(集团)有限责任公司 | Method for fast quantitative analysis for six-element content in powder metallurgy |
| CN106814126A (en) * | 2017-03-27 | 2017-06-09 | 山东钢铁集团日照有限公司 | A kind of method of testing of galvanizing layer weight and wherein trace element distribution |
| CN108469243A (en) * | 2018-03-26 | 2018-08-31 | 常德金德新材料科技股份有限公司 | A kind of measurement method of the transfer dry Tu amount of membrane coat |
| CN109540726A (en) * | 2019-01-09 | 2019-03-29 | 江苏鸿凌达科技有限公司 | A kind of high-efficiency artificial graphene film discrimination method |
| CN111504840A (en) * | 2020-01-15 | 2020-08-07 | 马鞍山马钢废钢有限责任公司 | Method for detecting zinc content of galvanized waste steel |
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| CN101000262A (en) * | 2007-01-17 | 2007-07-18 | 西南铝业（集团）有限责任公司 | Method for measuring weigh of two-sided coated plate film |
| JP2007229652A (en) * | 2006-03-02 | 2007-09-13 | Toppan Printing Co Ltd | Calculation method for coating quantity in dry lamination step |
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| JP2007229652A (en) * | 2006-03-02 | 2007-09-13 | Toppan Printing Co Ltd | Calculation method for coating quantity in dry lamination step |
| CN101082483A (en) * | 2006-06-01 | 2007-12-05 | 鞍钢股份有限公司 | Online detection method for thickness of coating film of color-coated strip steel |
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