CN103389317A - Analysis method of heavy metals in textiles - Google Patents
Analysis method of heavy metals in textiles Download PDFInfo
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- CN103389317A CN103389317A CN2013103193088A CN201310319308A CN103389317A CN 103389317 A CN103389317 A CN 103389317A CN 2013103193088 A CN2013103193088 A CN 2013103193088A CN 201310319308 A CN201310319308 A CN 201310319308A CN 103389317 A CN103389317 A CN 103389317A
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Abstract
The invention discloses an analysis method of heavy metals in textiles. The method comprises the following steps: firstly, uniformly mixing cadmium nitrate, nickel nitrate, lead nitrate and lithium borate, and grinding to prepare a plurality of standard reserve substances in different mass concentrations; secondly, mixing the standard reverse substances with standard polyester-accompanied fragments to prepare a plurality of standard products in different mass concentrations; thirdly, measuring the fluorescence intensity of each element in the standard products, drawing a scatter diagram by taking the concentration as an X axis and the fluorescence intensity of the element as a Y axis to obtain a standard curve of each element and calculating a linear regression equation of each standard curve; and finally, measuring the X ray fluorescence intensities of cadmium, nickel and lead in a textile sample to be detected, checking the corresponding concentrations on the standard curve, or calculating the concentrations of the cadmium, the nickel and the lead in the sample to be detected according to the linear regression equations. The analysis method disclosed by the invention can be used for directly testing an original sample without damaging the sample and high in detection speed; the dosages of strong acid and a strong oxidant for digestion are reduced, and the damages to environments and testers are reduced.
Description
Technical field
The present invention relates to the qualitative and quantitative analysis method of heavy metal in a kind of textile.
Background technology
In recent years, along with the enhancing of people's ecological, environmental protective consciousness, the safety of textile garment and environmental issue are subject to showing great attention to of people gradually.Also cause extensive concern as heavy metal pollution in the textile garment of daily necessities.America and Europe distributed many instructions about the textile heavy metal limit and rules, as surpassing 100 mg/kg every total amount in the final textile product of 91/338/EEC instruction regulation, in U.S.'s consumer goods improvements in security bill regulation juvenile product, lead content must not surpass 100 mg/kg.Method of testing corresponding to above textile heavy metal limit rules generally used atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, these instruments are more expensive, and require sample to clear up in advance processing, making finally solution could detect, therefore expense is high, take time and effort, efficiency is low.Clear up in addition both contaminated environment of the strong acid of use and strong oxidizer, also be unfavorable for testing staff's safety.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of Analysis of Heavy Metal method in textile is provided.
The technical scheme that technical solution problem of the present invention adopts: a kind of Analysis of Heavy Metal method in textile, the method comprises the following steps:
(1) take cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate, mix and mill after make the mark product and stock thing A, the mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400 mg/kg and 31250mg/kg, the mark product are stocked thing A with lithium borate, dilute 10 times, mix and mill after make the mark product and stock thing B, the mark product are stocked in thing B, the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040 mg/kg and 3125mg/kg; The mark product are stocked thing B with 10 times of lithium borate dilutions, mix and mill after make the mark product and stock thing C, the mark product are stocked in thing C, the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404 mg/kg and 312mg/kg;
(2) polyester standard is pasted lining and be cut into area less than the fragment D of 2 square millimeters; The mark product in 0.1g step 1 got are stocked thing C and are mixed with 0.9g fragment D and mill evenly, with sheeter, are pressed into standard items No. 1, and in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40 mg/kg and 31mg/kg; The mark product in 0.02g step 1 got are stocked thing B and are mixed with 0.98g fragment D and mill evenly, with sheeter, are pressed into standard items No. 2, and in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81 mg/kg and 62mg/kg; The mark product in 0.03g step 1 got are stocked thing B and are mixed with 0.97g fragment D and mill evenly, with sheeter, are pressed into standard items No. 3, and in No. 3 standard items, the concentration of cadmium, nickel and lead element is respectively 109mg/kg, 121mg/kg and 94mg/kg; The mark product in 0.04g step 1 got are stocked thing B and are mixed with 0.96g fragment D and mill evenly, with sheeter, are pressed into standard items No. 4, and in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162 mg/kg and 125mg/kg; The mark product in 0.08g step 1 got are stocked thing B and are mixed with 0.92g fragment D and mill evenly, with sheeter, are pressed into standard items No. 5, and in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323 mg/kg and 250mg/kg; The mark product in 0.016g step 1 got are stocked thing A and are mixed with 0.984g fragment D and mill evenly, with sheeter, are pressed into standard items No. 6, and in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646 mg/kg and 500mg/kg;
(3) by the condition of work of showing the listed XRF spectrometer of l, the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure 2 respectively, take concentration as X-axis, fluorescence intensity is that Y-axis is made scatter diagram, adopt trend prediction/linear regression method in Excell software, make the linear fit straight line, calculate the equation of linear regression of each typical curve;
Table 1: test condition
| Element | Cd | Pb | Ni |
| Spectral line | CdKa | PbLb1 | NiKa |
| The X-ray tube target | Rh | Rh | Rh |
| Voltage | 50kV | 50kV | 50kV |
| Electric current | 100μA | 100μA | 100μA |
| Optical filter | Mo | Ni | Nothing |
| Integral time | 100s | 100s | 100s |
| Diaphragm | 10mm | 10mm | 10mm |
| Atmosphere | Air | Air | Air |
| Rotation mode | Do not rotate | Do not rotate | Do not rotate |
Obtained the equation of linear regression of cadmium element by the cadmium element typical curve:
, wherein,
For the fluorescence intensity of cadmium element,
Concentration (mg/kg) for cadmium element; Obtained the equation of linear regression of nickel element by the nickel element typical curve:
, wherein,
For the fluorescence intensity of nickel element,
Concentration (mg/kg) for nickel element; Obtained the equation of linear regression of lead element by the lead element typical curve:
, wherein,
For the fluorescence intensity of lead element,
Concentration (mg/kg) for lead element;
(4) textile to be measured is directly put into the XRF spectrometer, press the condition of work of the listed instrument of table 1, the X ray fluorescence intensity of cadmium, nickel, lead in the difference working sample, check in corresponding concentration from typical curve, perhaps, respectively with their equations of linear regression separately of fluorescence intensity substitution of cadmium, nickel, lead, calculate the concentration of cadmium in institute's test sample product, nickel, lead.
The invention has the beneficial effects as follows,
1, for atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, sample need not cleared up pre-treatment, and directly the former state test needn't destroy sample;
2, detection speed is fast, only needs 1-2 minute;
3, can save strong acid and the strong oxidizer of clearing up use, reduce the harm to environment and tester;
4, the fluorescent X-ray spectral line is simple, disturbs less, and qualitative accurate, quantitative accuracy meets the relevant criterion requirement.
Description of drawings
Fig. 1 is method flow diagram of the present invention;
Fig. 2 is the cadmium element canonical plotting;
Fig. 3 is the nickel element canonical plotting;
Fig. 4 is the lead element canonical plotting.
Embodiment
Applying X-ray fluorometry of the present invention is analyzed content of beary metal in textile, its principle is: sample is after suitable x-ray bombardment, electronics in heavy metal atom is expelled out of, and produce a room on atomic orbital, outer field electronic transition is to this track, and to fill up this room, unnecessary energy is emitted with the form of XRF, in spectrum, can be considered a spectral line.The energy of XRF depends on the interorbital energy difference of transition, and the energy of each atom is certain, so the characteristic spectral line of launching is also certain, and can this be qualitative.After measuring fluorescence intensity, check in the equation of linear regression of corresponding concentration or employing typical curve from typical curve, calculate the content of heavy metal element to be measured in sample.
Describe the present invention in detail below in conjunction with accompanying drawing, it is more obvious that purpose of the present invention and effect will become.
In textile of the present invention, the Analysis of Heavy Metal method comprises the following steps:
Step 1: take cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate, mix and mill after make the mark product and stock thing A, the mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400 mg/kg and 31250mg/kg, the mark product are stocked thing A with lithium borate, dilute 10 times, mix and mill after make the mark product and stock thing B, the mark product are stocked in thing B, the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040 mg/kg and 3125mg/kg.The mark product are stocked thing B with 10 times of lithium borate dilutions, mix and mill after make the mark product and stock thing C, the mark product are stocked in thing C, the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404 mg/kg and 312mg/kg.
Step 2: polyester standard is pasted lining (GB/T 7568.4-2002) be cut into area less than the fragment D of 2 square millimeters.The mark product in 0.1g step 1 got are stocked thing C and are mixed with 0.9g fragment D and mill evenly, with sheeter, are pressed into standard items No. 1, and in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40 mg/kg and 31mg/kg.The mark product in 0.02g step 1 got are stocked thing B and are mixed with 0.98g fragment D and mill evenly, with sheeter, are pressed into standard items No. 2, and in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81 mg/kg and 62mg/kg.The mark product in 0.03g step 1 got are stocked thing B and are mixed with 0.97g fragment D and mill evenly, with sheeter, are pressed into standard items No. 3, and in No. 3 standard items, the concentration of cadmium, nickel and lead element is respectively 109mg/kg, 121mg/kg and 94mg/kg.The mark product in 0.04g step 1 got are stocked thing B and are mixed with 0.96g fragment D and mill evenly, with sheeter, are pressed into standard items No. 4, and in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162 mg/kg and 125mg/kg.The mark product in 0.08g step 1 got are stocked thing B and are mixed with 0.92g fragment D and mill evenly, with sheeter, are pressed into standard items No. 5, and in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323 mg/kg and 250mg/kg.The mark product in 0.016g step 1 got are stocked thing A and are mixed with 0.984g fragment D and mill evenly, with sheeter, are pressed into standard items No. 6, and in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646 mg/kg and 500mg/kg.
Step 3: by the condition of work of the listed XRF spectrometer of table l, the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure 2 respectively, take concentration as X-axis, fluorescence intensity is that Y-axis is made scatter diagram, adopt trend prediction/linear regression method in Excell software, make the linear fit straight line, calculate the equation of linear regression of each typical curve.
Table 1: test condition
| Element | Cd | Pb | Ni |
| Spectral line | CdKa | PbLb1 | NiKa |
| The X-ray tube target | Rh | Rh | Rh |
| Voltage | 50kV | 50kV | 50kV |
| Electric current | 100μA | 100μA | 100μA |
| Optical filter | Mo | Ni | Nothing |
| Integral time | 100s | 100s | 100s |
| Diaphragm | 10mm | 10mm | 10mm |
| Atmosphere | Air | Air | Air |
| Rotation mode | Do not rotate | Do not rotate | Do not rotate |
Figure 2 shows that the cadmium element canonical plotting, obtained the equation of linear regression of cadmium element by the cadmium element typical curve:
, wherein,
For the fluorescence intensity of cadmium element,
Concentration (mg/kg) for cadmium element.
Figure 3 shows that the nickel element canonical plotting, obtained the equation of linear regression of nickel element by the nickel element typical curve:
, wherein,
For the fluorescence intensity of nickel element,
Concentration (mg/kg) for nickel element.
Figure 4 shows that the lead element canonical plotting, obtained the equation of linear regression of lead element by the lead element typical curve:
, wherein,
For the fluorescence intensity of lead element,
Concentration (mg/kg) for lead element.
Step 4: textile to be measured is directly put into the XRF spectrometer, press the condition of work of the listed instrument of table 1, the X ray fluorescence intensity of cadmium, nickel, lead in the difference working sample, check in the equation of linear regression of corresponding concentration or employing typical curve from typical curve,, with their equations of linear regression separately of fluorescence intensity substitution of cadmium, nickel, lead, calculate the concentration of cadmium in institute's test sample product, nickel, lead respectively.
By above method as seen, for atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, sample of the present invention need not cleared up pre-treatment, directly the former state test needn't destroy sample, speed is fast, only need 1-2 minute, can save strong acid and the strong oxidizer of clearing up use, reduce the harm to environment and tester.Secondly the fluorescent X-ray spectral line is simple, disturbs less, and qualitative accurate, quantitative accuracy meets the relevant criterion requirement.
Claims (1)
1. Analysis of Heavy Metal method in a textile, is characterized in that, the method comprises the following steps:
(1) take cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate, mix and mill after make the mark product and stock thing A, the mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400 mg/kg and 31250mg/kg, the mark product are stocked thing A with lithium borate, dilute 10 times, mix and mill after make the mark product and stock thing B, the mark product are stocked in thing B, the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040 mg/kg and 3125mg/kg; The mark product are stocked thing B with 10 times of lithium borate dilutions, mix and mill after make the mark product and stock thing C, the mark product are stocked in thing C, the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404 mg/kg and 312mg/kg;
(2) polyester standard is pasted lining and be cut into area less than the fragment D of 2 square millimeters; The mark product in 0.1g step 1 got are stocked thing C and are mixed with 0.9g fragment D and mill evenly, with sheeter, are pressed into standard items No. 1, and in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40 mg/kg and 31mg/kg; The mark product in 0.02g step 1 got are stocked thing B and are mixed with 0.98g fragment D and mill evenly, with sheeter, are pressed into standard items No. 2, and in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81 mg/kg and 62mg/kg; The mark product in 0.03g step 1 got are stocked thing B and are mixed with 0.97g fragment D and mill evenly, with sheeter, are pressed into standard items No. 3, and in No. 3 standard items, the concentration of cadmium, nickel and lead element is respectively 109mg/kg, 121mg/kg and 94mg/kg; The mark product in 0.04g step 1 got are stocked thing B and are mixed with 0.96g fragment D and mill evenly, with sheeter, are pressed into standard items No. 4, and in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162 mg/kg and 125mg/kg; The mark product in 0.08g step 1 got are stocked thing B and are mixed with 0.92g fragment D and mill evenly, with sheeter, are pressed into standard items No. 5, and in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323 mg/kg and 250mg/kg; The mark product in 0.016g step 1 got are stocked thing A and are mixed with 0.984g fragment D and mill evenly, with sheeter, are pressed into standard items No. 6, and in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646 mg/kg and 500mg/kg;
(3) by the condition of work of showing the listed XRF spectrometer of l, the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure 2 respectively, take concentration as X-axis, fluorescence intensity is that Y-axis is made scatter diagram, adopt trend prediction/linear regression method in Excell software, make the linear fit straight line, calculate the equation of linear regression of each typical curve;
Table 1: test condition
Obtained the equation of linear regression of cadmium element by the cadmium element typical curve:
, wherein,
For the fluorescence intensity of cadmium element,
Concentration (mg/kg) for cadmium element; Obtained the equation of linear regression of nickel element by the nickel element typical curve:
, wherein,
For the fluorescence intensity of nickel element,
Concentration (mg/kg) for nickel element; Obtained the equation of linear regression of lead element by the lead element typical curve:
, wherein,
For the fluorescence intensity of lead element,
Concentration (mg/kg) for lead element;
(4) textile to be measured is directly put into the XRF spectrometer, press the condition of work of the listed instrument of table 1, the X ray fluorescence intensity of cadmium, nickel, lead in the difference working sample, check in corresponding concentration from typical curve, perhaps, respectively with their equations of linear regression separately of fluorescence intensity substitution of cadmium, nickel, lead, calculate the concentration of cadmium in institute's test sample product, nickel, lead.
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Cited By (9)
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| CN103698351A (en) * | 2014-01-08 | 2014-04-02 | 四川出入境检验检疫局检验检疫技术中心 | Detection treatment solution for leather heavy metal fluorescence chromatography and detection method |
| CN103698352A (en) * | 2014-01-08 | 2014-04-02 | 四川出入境检验检疫局检验检疫技术中心 | Mother solution of standard solution for chromatography of heavy metals in leather and preparation method of standard curve |
| CN103822935A (en) * | 2014-03-07 | 2014-05-28 | 钢研纳克检测技术有限公司 | Fast analyzer for nondestructive measuring heavy metal cadmium in foods and analyzing method |
| CN104181183A (en) * | 2014-09-12 | 2014-12-03 | 江苏天瑞仪器股份有限公司 | Method for rapidly measuring lead element in grain by X fluorescent spectrometry |
| CN104483336A (en) * | 2014-12-23 | 2015-04-01 | 陕西迪泰克新材料有限公司 | Method, device and system for detecting heavy metals in soil |
| CN105259196A (en) * | 2014-07-08 | 2016-01-20 | 日本株式会社日立高新技术科学 | Sample Plate for X-Ray Analysis and X-Ray Fluorescent Analyzer |
| CN108120625A (en) * | 2017-09-30 | 2018-06-05 | 广东华科检测技术服务有限公司 | Total lead and total cadmium standard sample and preparation method thereof in textile |
| CN109030527A (en) * | 2018-06-22 | 2018-12-18 | 广东产品质量监督检验研究院 | Rapid detection method based on content of beary metal in XRF technique in children textile and shoe parts |
| CN110261419A (en) * | 2019-05-28 | 2019-09-20 | 广东产品质量监督检验研究院 | Device and method, the textile production equipment of automatic on-line detection heavy metal |
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| CN103698352A (en) * | 2014-01-08 | 2014-04-02 | 四川出入境检验检疫局检验检疫技术中心 | Mother solution of standard solution for chromatography of heavy metals in leather and preparation method of standard curve |
| CN103698351A (en) * | 2014-01-08 | 2014-04-02 | 四川出入境检验检疫局检验检疫技术中心 | Detection treatment solution for leather heavy metal fluorescence chromatography and detection method |
| CN103698351B (en) * | 2014-01-08 | 2015-09-16 | 四川出入境检验检疫局检验检疫技术中心 | The check processing liquid that leather heavy metal fluorescence chromatogram is analyzed and detection method |
| CN103822935A (en) * | 2014-03-07 | 2014-05-28 | 钢研纳克检测技术有限公司 | Fast analyzer for nondestructive measuring heavy metal cadmium in foods and analyzing method |
| CN103822935B (en) * | 2014-03-07 | 2015-11-25 | 钢研纳克检测技术有限公司 | The quick analytic instrument of heavy metal cadmium and analytical approach in a kind of non-destructive determination food |
| CN105259196A (en) * | 2014-07-08 | 2016-01-20 | 日本株式会社日立高新技术科学 | Sample Plate for X-Ray Analysis and X-Ray Fluorescent Analyzer |
| CN104181183A (en) * | 2014-09-12 | 2014-12-03 | 江苏天瑞仪器股份有限公司 | Method for rapidly measuring lead element in grain by X fluorescent spectrometry |
| CN104483336A (en) * | 2014-12-23 | 2015-04-01 | 陕西迪泰克新材料有限公司 | Method, device and system for detecting heavy metals in soil |
| CN108120625A (en) * | 2017-09-30 | 2018-06-05 | 广东华科检测技术服务有限公司 | Total lead and total cadmium standard sample and preparation method thereof in textile |
| CN109030527A (en) * | 2018-06-22 | 2018-12-18 | 广东产品质量监督检验研究院 | Rapid detection method based on content of beary metal in XRF technique in children textile and shoe parts |
| CN110261419A (en) * | 2019-05-28 | 2019-09-20 | 广东产品质量监督检验研究院 | Device and method, the textile production equipment of automatic on-line detection heavy metal |
| CN110261419B (en) * | 2019-05-28 | 2024-05-17 | 广东产品质量监督检验研究院 | Automatic on-line heavy metal detection equipment and method and textile production equipment |
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