CN103698351B - The check processing liquid that leather heavy metal fluorescence chromatogram is analyzed and detection method - Google Patents
The check processing liquid that leather heavy metal fluorescence chromatogram is analyzed and detection method Download PDFInfo
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- CN103698351B CN103698351B CN201410006760.3A CN201410006760A CN103698351B CN 103698351 B CN103698351 B CN 103698351B CN 201410006760 A CN201410006760 A CN 201410006760A CN 103698351 B CN103698351 B CN 103698351B
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Abstract
The present invention relates to the method for heavy metal in a kind of Fast Measurement leather, particularly a kind of is check processing liquid and the detection method of with XRF Method of Energy Spectrum Analysis, heavy metal in leather being carried out to Fast Measurement.Check processing formula of liquid: 75% glycerine 20 ~ 30mL, 1% AEO 0.5 ~ 2.0mL, 85% phosphatase 24 ~ 8mL, 1% nitric acid 60 ~ 70mL, deionized water are finally settled to 1000mL.Detecting step: (1) pulverizes that leather becomes sample powder, (2) to being pressed into that diameter is 25 mm disks after sample powder adds the mixing of check processing liquid, (3) powder and treating fluid, (4) become content of beary metal with heavy metal line strength of XRF energy spectrum analysis detection disk, (5) line strength data reduction.
Description
Technical field
The present invention relates to the method for heavy metal in a kind of Fast Measurement leather, particularly a kind of is carry out heavy metal detection method in the check processing liquid of Fast Measurement and leather with XRF Method of Energy Spectrum Analysis to heavy metal in leather.
Background technology
At present, require strict both at home and abroad to the content of beary metal in leather, GB/T 22930-2008 clear stipulaties leather needs the metallic element measured: lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury, totally nine kinds.
These the nine kinds methods detecting heavy metal mainly contain at present: atomic absorption method, atomic fluorescence method, plasma emission spectrometry, chemical measure etc.Adopt atomic absorption method, content of beary metal in Atomic Fluorescence Spectrometry leather, accuracy is high, but sample preparation is loaded down with trivial details, can not multiple element in Simultaneously test sample, therefore operates and wastes time and energy.Plasma emission spectrometry, sample preparation is loaded down with trivial details, multiple element in energy Simultaneously test sample, but instrument price is expensive, and testing cost costly.Portable X-Ray Fluorescence energy spectrometer method is by heavy metal in XRF energy spectrum analysis leather, because spectral line is simple, after adopting leather to pulverize, the method for direct powder compression, extract, but error is difficult to use in more greatly accurate detection without the need to chemical method pre-treatment to metallic element.
Summary of the invention
The invention provides when detecting by XRF energy spectrum analysis leather heavy metal, for carrying out detecting heavy metal detection method in the check processing liquid of pre-treatment and leather to detected leather sample.
Leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment, and each raw material is as follows by volume:
Mass concentration be 75% glycerine 20.0mL ~ 30.0mL,
Mass concentration be 1% AEO 0.5mL ~ 2.0mL,
Mass concentration be 85% pure strong phosphoric acid 4.0mL ~ 8.0mL,
Mass concentration be 1% nitric acid 60.0mL ~ 70.0mL,
Finally 1000mL is dissolved to deionized water.
Check processing liquid outfit method: filling in the deionized 1000mL glass beaker of about 500mL, first add mass concentration be 1% nitric acid add to total amount 60.0mL ~ 70.0mL mixing, then add mass concentration be 85% pure strong phosphoric acid 4.0mL ~ 8.0mL mixing, more then add mass concentration be 75% glycerine 20.0mL ~ 30.0mL mix, finally adding mass concentration is that 1% AEO 0.5mL ~ 2.0mL mixes, after being cooled to room temperature, move in 1000mL volumetric flask, be dissolved to 1000mL with deionized water.
The effect of glycerine: the fat in glycerine energy rapid solution leather sample powder, make the heavy metal in fat can thereupon evenly be dispersed in leather sample powder, improve the degree of accuracy that XRF energy depressive spectroscopy measures nine heavy metal species line strength values.So add glycerine in leather sample check processing liquid to be measured.
The effect of AEO: due in line strength value of formulation nine heavy metal species and the regression equation process of the test of this heavy metal species content, add AEO, and XRF energy spectrum analysis line strength value of leather sample is converted into nine heavy metal species content in leather sample with these nine regression equations.For eliminating systematic error, so add AEO in leather sample check processing liquid to be measured.
The effect of strong phosphoric acid: due in line strength value of formulation nine heavy metal species and the regression equation process of the test of this heavy metal species content, add strong phosphoric acid, and XRF energy spectrum analysis line strength value of leather sample is converted into nine heavy metal species content in leather sample with these nine regression equations.For eliminating systematic error, so add strong phosphoric acid in leather sample check processing liquid to be measured.
The effect of nitric acid: due in line strength value of formulation nine heavy metal species and the regression equation process of the test of this heavy metal species content, add nitric acid, and XRF energy spectrum analysis line strength value of leather sample is converted into nine heavy metal species content in leather sample with these nine regression equations.For eliminating systematic error, so add nitric acid in leather sample check processing liquid to be measured.
XRF energy spectrum analysis leather heavy metal detection method:
As follows to the step of lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury nine heavy metal species detection method in leather with XRF energy depressive spectroscopy:
1. pulverize leather: shredded by leather, size is no more than 5mm × 5mm, puts into micronizer and is crushed to below 200 orders, obtain leather sample powder.
2, add check processing liquid: diameter is in the compacting tool set cylinder of 25 mm, puts into 5g leather sample powder, and add the check processing liquid that 5mL leather sample carries out detecting pre-treatment, be mixed into leather mud.
Described leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment:
Mass concentration be 75% glycerine 20.0mL ~ 30.0mL,
Mass concentration be 1% AEO 0.5mL ~ 2.0mL,
Mass concentration be 85% pure strong phosphoric acid 4.0mL ~ 8.0mL,
Mass concentration be 1% nitric acid 60.0mL ~ 70.0mL,
Finally 1000mL is dissolved to deionized water.
3, compressing tablet: with 25,000 newton's pressure, the leather mud in mould cylinder being pressed into diameter is 25 mm, thickness is the leather disk to be measured of 2 mm, takes out leather disk to be measured for subsequent use.
4, detect: diameter is 25 mm, and thickness is that the leather disk to be measured of 2 mm puts into XRF energy depressive spectroscopy, detect line strength data that lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury nine heavy metal species are different respectively.
5, data reduction: converse the content of this heavy metal species in leather disk with every heavy metal species XRF energy spectrum analysis line strength value of nine heavy metal species and the regression equation of this heavy metal species content.
Table 1, line strength value of nine heavy metal species and the regression equation table of this heavy metal species content
In table 1, XRF energy spectrum analysis line strength value is " X ", and the content of beary metal in leather disk is " Y ".
Advantage of the present invention: before carrying out nine heavy metal species content detection with XRF energy depressive spectroscopy to leather sample of the present invention, carries out process leather sample with detection pretreatment liquid both check processing liquid, makes detection more accurate.What detect nine heavy metal species due to XRF energy depressive spectroscopy is line strength, line strength to be converted into content of beary metal, need the regression equation of line strength and content of beary metal, and obtain in the code test of regression equation, add strong phosphoric acid and nitric acid processes leather, systematic error is eliminated with leather line strength in the code test of acquisition regression equation in order to make XRF energy spectrum analysis line strength of leather sample, so, process with check processing liquid before leather sample carries out content of beary metal detection, and containing the principal ingredient strong phosphoric acid in leather cleanup standard liquid when obtaining the code test of regression equation and nitric acid in leather sample check processing liquid.
Leather sample of the present invention carries out in the check processing liquid before content of beary metal detection also containing glycerine, fat in glycerine energy rapid solution leather sample powder, make the heavy metal in fat can thereupon evenly be dispersed in leather sample powder, improve the degree of accuracy that XRF energy depressive spectroscopy measures nine heavy metal species line strength values.
Due in line strength value of formulation nine heavy metal species and the regression equation process of the test of this heavy metal species content, add AEO, phosphoric acid, nitric acid, and XRF energy spectrum analysis line strength value of leather sample is converted into nine heavy metal species content in leather sample with these nine regression equations.For eliminating systematic error, so add AEO, phosphoric acid, nitric acid in leather sample check processing liquid to be measured.Energy elimination regression equation is converted into line strength the systematic error of content of beary metal.
Embodiment
Embodiment 1, ox leather sample carries out the check processing liquid detecting pre-treatment
Ox leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment:
Mass concentration be 75% glycerine 30.0mL,
Mass concentration be 1% AEO 1.0mL,
Mass concentration be 85% pure strong phosphoric acid 8.0mL,
Mass concentration be 1% nitric acid 70.0mL,
Finally 1000mL is dissolved to deionized water.
Check processing liquid outfit method: filling in the deionized 1000mL glass beaker of about 500mL, first add mass concentration be 1% nitric acid 70.0mL mix, then add mass concentration be 85% pure strong phosphoric acid 8.0mL mixing, more then add mass concentration be 75% glycerine 30.0mL mix, finally adding mass concentration is that 1% AEO 1.0mL mixes, after being cooled to room temperature, move in 1000mL volumetric flask, be dissolved to 1000mL with deionized water.
Embodiment 2, pig leather sample carries out the check processing liquid detecting pre-treatment
Pig leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment:
Mass concentration be 75% glycerine 20.0mL,
Mass concentration be 1% AEO 0.5mL,
Mass concentration be 85% pure strong phosphoric acid 5.0mL,
Mass concentration be 1% nitric acid 60.0mL,
1000 mL are finally dissolved to deionized water.
Check processing liquid outfit method: filling in the deionized 1000mL glass beaker of about 500mL, first add mass concentration be 1% nitric acid 60.0mL mix, then add mass concentration be 85% pure strong phosphoric acid 5.0mL mixing, more then add mass concentration be 75% glycerine 20.0mL mix, finally adding mass concentration is that 1% AEO 0.5mL mixes, after being cooled to room temperature, move in 1000mL volumetric flask, be dissolved to 1000mL with deionized water.
Embodiment 3, XRF energy spectrum analysis leather heavy metal detection method
As follows to the step of lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury nine heavy metal species detection method in leather with XRF energy depressive spectroscopy:
1. pulverize leather: shredded by leather, size is no more than 5mm × 5mm, puts into micronizer and is crushed to below 200 orders, obtain leather sample powder.
2, check processing liquid is added: diameter is in the compacting tool set cylinder of 25 mm, puts into 5g leather sample powder, and adds 5mL check processing liquid, is mixed into leather mud.
Described leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment:
Mass concentration be 75% glycerine 20.0mL ~ 30.0mL,
Mass concentration be 1% AEO 0.5mL ~ 2.0mL,
Mass concentration be 85% pure strong phosphoric acid 4.0mL ~ 8.0mL,
Mass concentration be 1% nitric acid 60.0mL ~ 70.0mL,
Finally 1000mL is dissolved to deionized water.
Check processing liquid outfit method: filling in the deionized 1000mL glass beaker of about 500mL, first the nitric acid mixing that mass concentration is 1% is added, then add mass concentration be 85% the mixing of pure strong phosphoric acid, then add the glycerine mixing that mass concentration is 75% again, finally adding mass concentration is 1% AEO mixing, after being cooled to room temperature, move in 1000mL volumetric flask, be dissolved to 1000mL with deionized water.
3, compressing tablet: with 25,000 newton's pressure, the leather mud in mould cylinder being pressed into diameter is 25 mm, thickness is the leather disk to be measured of 2 mm, takes out leather disk to be measured for subsequent use.
4, detect: diameter is 25 mm, and thickness is that the leather disk to be measured of 2 mm puts into XRF energy depressive spectroscopy, detect line strength data that lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury nine heavy metal species are different respectively.
5, data reduction: converse the content of this heavy metal species in leather disk with every heavy metal species XRF energy spectrum analysis line strength value of nine heavy metal species and the regression equation of this heavy metal species content.Line strength value of nine heavy metal species and the regression equation of this heavy metal species content are in table 1.
Table 1, line strength value of nine heavy metal species and the regression equation table of this heavy metal species content
In table 1, XRF energy spectrum analysis line strength value is " X ", and the content of beary metal in leather disk is " Y ".
Claims (2)
1. leather sample carries out the check processing liquid detecting pre-treatment, and the formula rate that various raw material by volume calculates is as follows:
Mass concentration be 75% glycerine 20.0mL ~ 30.0mL,
Mass concentration be 1% AEO 0.5mL ~ 2.0mL,
Mass concentration be 85% top grade pure strong phosphoric acid 4.0mL ~ 8.0mL,
Mass concentration be 1% nitric acid 60.0mL ~ 70.0mL,
Finally 1000mL is settled to deionized water.
2.X ray fluorescence energy spectrum analysis leather heavy metal detection method, comprises the following steps:
(1) leather is pulverized: shredded by leather, size is no more than 5mm × 5mm, puts into micronizer and is crushed to below 200 orders, obtain leather sample powder;
(2) add check processing liquid: diameter is in the compacting tool set cylinder of 25 mm, puts into 5g leather sample powder, and add the check processing liquid that 5mL leather sample carries out detecting pre-treatment, be mixed into leather mud;
Described leather sample carries out each composition of raw materials detected in the check processing liquid l000mL of pre-treatment:
Mass concentration be 75% glycerine 20.0mL ~ 30.0mL,
Mass concentration be 1% AEO 0.5mL ~ 2.0mL,
Mass concentration be 85% top grade pure strong phosphoric acid 4.0mL ~ 8.0mL,
Mass concentration be 1% nitric acid 60.0mL ~ 70.0mL,
Finally 1000mL is settled to deionized water;
(3) compressing tablet: with 25,000 newton's pressure, the leather mud in mould cylinder being pressed into diameter is 25 mm, thickness is the leather disk to be measured of 2 mm, takes out leather disk to be measured for subsequent use;
(4) detect: diameter is 25 mm, and thickness is that the leather disk to be measured of 2 mm puts into XRF energy depressive spectroscopy, detect line strength data that lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury nine heavy metal species are different respectively;
(5) data reduction: converse the content of this heavy metal species in leather disk with every heavy metal species XRF energy spectrum analysis line strength value of nine heavy metal species and the regression equation of this heavy metal species content.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865797A (en) * | 2010-06-29 | 2010-10-20 | 中国皮革和制鞋工业研究院 | Leather proficiency testing sample containing heavy metals and preparation method thereof |
| CN103389317A (en) * | 2013-07-28 | 2013-11-13 | 浙江出入境检验检疫局检验检疫技术中心 | Analysis method of heavy metals in textiles |
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| US20020097833A1 (en) * | 2001-01-19 | 2002-07-25 | Bruce Kaiser | Methods for identification and verification |
| US20030194052A1 (en) * | 2002-04-12 | 2003-10-16 | Price L. Stephen | Methods for identification and verification |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865797A (en) * | 2010-06-29 | 2010-10-20 | 中国皮革和制鞋工业研究院 | Leather proficiency testing sample containing heavy metals and preparation method thereof |
| CN103389317A (en) * | 2013-07-28 | 2013-11-13 | 浙江出入境检验检疫局检验检疫技术中心 | Analysis method of heavy metals in textiles |
Non-Patent Citations (4)
| Title |
|---|
| Okoh, S. et al..Determination of Some Trace Elements in Leather.《International Journal of Applied Science and Technology》.2013,第3卷(第1期), * |
| Tetsuya Sano et al..Basic forensic identification of artificial leather for hit-and-run cases.《Forensic Science International》.2009,第192卷 * |
| 张海娟等.ICP-AES 测定皮革及其制品中的可溶性重金属含量.《西部皮革》.2012,第34卷(第12期), * |
| 蒋瑾华等.石墨炉原子吸收光谱法测定皮革制品中铅、镉和铬.《光谱实验室》.2002,第19卷(第5期), * |
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