CN103389317B - A kind of Analysis of Heavy Metal method in textile - Google Patents
A kind of Analysis of Heavy Metal method in textile Download PDFInfo
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- CN103389317B CN103389317B CN201310319308.8A CN201310319308A CN103389317B CN 103389317 B CN103389317 B CN 103389317B CN 201310319308 A CN201310319308 A CN 201310319308A CN 103389317 B CN103389317 B CN 103389317B
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Abstract
The invention discloses a kind of Analysis of Heavy Metal method in textile, the method is first by cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate mix and the some mark product making different quality concentration after milling stock thing, the fragment again mark product being stocked thing and polyester standard stickers lining is mixed and made into some standard items of different quality concentration, then the fluorescence intensity of each element in standard items is recorded, take concentration as X-axis, fluorescence intensity is that Y-axis makes scatter diagram, obtain each elemental standards curve and calculate the equation of linear regression of each typical curve, finally measure cadmium in textile sample to be measured, nickel, plumbous x-ray fluorescence intensity, corresponding concentration is checked in from typical curve, or calculate cadmium in institute's test sample product by equation of linear regression, nickel, plumbous concentration.The present invention directly former state test can need not destroy sample, and detection speed is fast, can save the strong acid and strong oxidizer of clearing up use, reduce the harm to environment and tester.
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 extensive concern is caused as heavy metal pollution in the textile garment of daily necessities.America and Europe distributed many instructions about textile heavy metal limit and regulation, must not more than 100mg/kg every total amount in textile product as final in 91/338/EEC directives prescribe, in United States consumes product improvements in security bill regulation juvenile product, lead content must not more than 100mg/kg.Method of testing corresponding to above textile heavy metal limit regulation generally uses atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, these instrument compare are expensive, and require that sample carries out clearing up process in advance, finally make solution could detect, therefore costly, take time and effort, efficiency is low.In addition clear up strong acid and strong oxidizer both contaminated environment of use, be also unfavorable for the safety of testing staff.
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) cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate is taken, mix and make mark product after milling and stock thing A, mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400mg/kg and 31250mg/kg, mark product are stocked thing A lithium borate and dilute 10 times, mix and make mark product after milling and stock thing B, mark product are stocked in thing B, and the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040mg/kg and 3125mg/kg; Mark product are stocked thing B lithium borate and dilute 10 times, mix and make mark product after milling and stock thing C, mark product are stocked in thing C, and the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404mg/kg and 312mg/kg;
(2) polyester standard stickers lining is cut into the fragment D that area is less than 2 square millimeters; The mark product got in 0.1g step 1 are stocked thing C and are mixed with 0.9g fragment D and mill evenly, and be pressed into No. 1 standard items with sheeter, in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40mg/kg and 31mg/kg; The mark product got in 0.02g step 1 are stocked thing B and are mixed with 0.98g fragment D and mill evenly, and be pressed into No. 2 standard items with sheeter, in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81mg/kg and 62mg/kg; The mark product got in 0.03g step 1 are stocked thing B and are mixed with 0.97g fragment D and mill evenly, and be pressed into No. 3 standard items with sheeter, 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 got in 0.04g step 1 are stocked thing B and are mixed with 0.96g fragment D and mill evenly, and be pressed into No. 4 standard items with sheeter, in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162mg/kg and 125mg/kg; The mark product got in 0.08g step 1 are stocked thing B and are mixed with 0.92g fragment D and mill evenly, and be pressed into No. 5 standard items with sheeter, in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323mg/kg and 250mg/kg; The mark product got in 0.016g step 1 are stocked thing A and are mixed with 0.984g fragment D and mill evenly, and be pressed into No. 6 standard items with sheeter, in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646mg/kg and 500mg/kg;
(3) by the condition of work of XRF spectrometer listed by table l, distinguish the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure 2, take concentration as X-axis, fluorescence intensity is that Y-axis makes scatter diagram, adopt trend prediction/linear regression method in Excell software, make 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 |
| 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 | Non rotating | Non rotating | Non rotating |
The equation of linear regression of cadmium element is obtained by cadmium element typical curve:
, wherein,
for the fluorescence intensity of cadmium element,
for the concentration (mg/kg) of cadmium element; The equation of linear regression of nickel element is obtained by nickel element typical curve:
, wherein,
for the fluorescence intensity of nickel element,
for the concentration (mg/kg) of nickel element; The equation of linear regression of lead element is obtained by lead element typical curve:
, wherein,
for the fluorescence intensity of lead element,
for the concentration (mg/kg) of lead element;
(4) textile to be measured is directly put into XRF spectrometer, by the condition of work of instrument listed by table 1, cadmium, nickel, plumbous x-ray fluorescence intensity in working sample respectively, corresponding concentration is checked in from typical curve, or respectively cadmium, nickel, plumbous fluorescence intensity are substituted into their respective equations of linear regression, calculate cadmium in institute's test sample product, nickel, plumbous concentration.
The invention has the beneficial effects as follows,
1, for atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, sample does not need to clear up pre-treatment, directly former state test can need not destroy sample;
2, detection speed is fast, only needs 1-2 minute;
3, the strong acid clearing up use and strong oxidizer can be saved, reduce the harm to environment and tester;
4, fluorescent X-ray spectral line is simple, and interference is few, and accurately qualitative, quantitative accuracy meets relevant criterion requirement.
Accompanying drawing explanation
Fig. 1 is method flow diagram of the present invention;
Fig. 2 is cadmium element canonical plotting;
Fig. 3 is nickel element canonical plotting;
Fig. 4 is lead element canonical plotting.
Embodiment
Applying X-ray fluorometry of the present invention analyzes 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 a room is produced on atomic orbital, outer field electronic transition is on this track, and to fill up this room, unnecessary energy is released 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 launched also is certain, and can this be qualitative.After measuring fluorescence intensity, check in corresponding concentration from typical curve or adopt the equation of linear regression of typical curve, calculating the content of heavy metal element to be measured in sample.
Describe the present invention in detail below in conjunction with accompanying drawing, object of the present invention and effect will become more obvious.
In textile of the present invention, Analysis of Heavy Metal method comprises the following steps:
Step 1: take cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate, mix and make mark product after milling and stock thing A, mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400mg/kg and 31250mg/kg, mark product are stocked thing A lithium borate and dilute 10 times, mix and make mark product after milling and stock thing B, mark product are stocked in thing B, and the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040mg/kg and 3125mg/kg.Mark product are stocked thing B lithium borate and dilute 10 times, mix and make mark product after milling and stock thing C, mark product are stocked in thing C, and the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404mg/kg and 312mg/kg.
Step 2: polyester standard stickers lining (GB/T7568.4-2002) is cut into the fragment D that area is less than 2 square millimeters.The mark product got in 0.1g step 1 are stocked thing C and are mixed with 0.9g fragment D and mill evenly, and be pressed into No. 1 standard items with sheeter, in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40mg/kg and 31mg/kg.The mark product got in 0.02g step 1 are stocked thing B and are mixed with 0.98g fragment D and mill evenly, and be pressed into No. 2 standard items with sheeter, in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81mg/kg and 62mg/kg.The mark product got in 0.03g step 1 are stocked thing B and are mixed with 0.97g fragment D and mill evenly, and be pressed into No. 3 standard items with sheeter, 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 got in 0.04g step 1 are stocked thing B and are mixed with 0.96g fragment D and mill evenly, and be pressed into No. 4 standard items with sheeter, in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162mg/kg and 125mg/kg.The mark product got in 0.08g step 1 are stocked thing B and are mixed with 0.92g fragment D and mill evenly, and be pressed into No. 5 standard items with sheeter, in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323mg/kg and 250mg/kg.The mark product got in 0.016g step 1 are stocked thing A and are mixed with 0.984g fragment D and mill evenly, and be pressed into No. 6 standard items with sheeter, in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646mg/kg and 500mg/kg.
Step 3: by the condition of work of XRF spectrometer listed by table l, distinguish the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure 2, take concentration as X-axis, fluorescence intensity is that Y-axis makes scatter diagram, adopt trend prediction/linear regression method in Excell software, make 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 |
| 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 | Non rotating | Non rotating | Non rotating |
Figure 2 shows that cadmium element canonical plotting, obtained the equation of linear regression of cadmium element by cadmium element typical curve:
, wherein,
for the fluorescence intensity of cadmium element,
for the concentration (mg/kg) of cadmium element.
Figure 3 shows that nickel element canonical plotting, obtained the equation of linear regression of nickel element by nickel element typical curve:
, wherein,
for the fluorescence intensity of nickel element,
for the concentration (mg/kg) of nickel element.
Figure 4 shows that lead element canonical plotting, obtained the equation of linear regression of lead element by lead element typical curve:
, wherein,
for the fluorescence intensity of lead element,
for the concentration (mg/kg) of lead element.
Step 4: textile to be measured is directly put into XRF spectrometer, by the condition of work of instrument listed by table 1, cadmium, nickel, plumbous x-ray fluorescence intensity in working sample respectively, check in corresponding concentration from typical curve or adopt the equation of linear regression of typical curve, respectively cadmium, nickel, plumbous fluorescence intensity are substituted into their respective equations of linear regression, calculate cadmium in institute's test sample product, nickel, plumbous concentration.
From above method, for atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography, sample of the present invention does not need to clear up pre-treatment, directly former state test can need not destroy sample, speed is fast, only need 1-2 minute, the strong acid and strong oxidizer of clearing up use can be saved, reduce the harm to environment and tester.Secondly fluorescent X-ray spectral line is simple, and interference is few, and accurately qualitative, quantitative accuracy meets relevant criterion requirement.
Claims (1)
1. an Analysis of Heavy Metal method in textile, it is characterized in that, the method comprises the following steps:
(1) cadmium nitrate, nickel nitrate, plumbi nitras and lithium borate is taken, mix and make mark product after milling and stock thing A, mark product are stocked in thing A, the mass concentration of cadmium, nickel and lead element is respectively 36400mg/kg, 40400mg/kg and 31250mg/kg, mark product are stocked thing A lithium borate and dilute 10 times, mix and make mark product after milling and stock thing B, mark product are stocked in thing B, and the concentration of cadmium, nickel and lead element is respectively 3640mg/kg, 4040mg/kg and 3125mg/kg; Mark product are stocked thing B lithium borate and dilute 10 times, mix and make mark product after milling and stock thing C, mark product are stocked in thing C, and the concentration of cadmium, nickel and lead element is respectively 364mg/kg, 404mg/kg and 312mg/kg;
(2) polyester standard stickers lining is cut into the fragment D that area is less than 2 square millimeters; The mark product got in 0.1g step (1) are stocked thing C and are mixed with 0.9g fragment D and mill evenly, and be pressed into No. 1 standard items with sheeter, in No. 1 standard items, the concentration of cadmium, nickel and lead element is respectively 36mg/kg, 40mg/kg and 31mg/kg; The mark product got in 0.02g step (1) are stocked thing B and are mixed with 0.98g fragment D and mill evenly, and be pressed into No. 2 standard items with sheeter, in No. 2 standard items, the concentration of cadmium, nickel and lead element is respectively 73mg/kg, 81mg/kg and 62mg/kg; The mark product got in 0.03g step (1) are stocked thing B and are mixed with 0.97g fragment D and mill evenly, and be pressed into No. 3 standard items with sheeter, 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 got in 0.04g step (1) are stocked thing B and are mixed with 0.96g fragment D and mill evenly, and be pressed into No. 4 standard items with sheeter, in No. 4 standard items, the concentration of cadmium, nickel and lead element is respectively 146mg/kg, 162mg/kg and 125mg/kg; The mark product got in 0.08g step (1) are stocked thing B and are mixed with 0.92g fragment D and mill evenly, and be pressed into No. 5 standard items with sheeter, in No. 5 standard items, the concentration of cadmium, nickel and lead element is respectively 291mg/kg, 323mg/kg and 250mg/kg; The mark product got in 0.016g step (1) are stocked thing A and are mixed with 0.984g fragment D and mill evenly, and be pressed into No. 6 standard items with sheeter, in No. 6 standard items, the concentration of cadmium, nickel and lead element is respectively 582mg/kg, 646mg/kg and 500mg/kg;
(3) by the condition of work of XRF spectrometer listed by table l, distinguish the fluorescence intensity of each element in No. 1 to No. 6 standard items in testing procedure (2), take concentration as X-axis, fluorescence intensity is that Y-axis makes scatter diagram, adopt trend prediction/linear regression method in Excel software, make linear fit straight line, calculate the equation of linear regression of each typical curve;
Table 1: condition of work
The equation of linear regression of cadmium element is obtained: y by cadmium element typical curve
1=0.0085x
1+ 0.002, wherein, y
1for the fluorescence intensity of cadmium element; x
1for the concentration of cadmium element, unit is mg/kg; The equation of linear regression of nickel element is obtained: y by nickel element typical curve
2=0.0025x
2+ 0.0211, wherein, y
2for the fluorescence intensity of nickel element; x
2for the concentration of nickel element, unit is mg/kg; The equation of linear regression of lead element is obtained: y by lead element typical curve
3=0.0020x
3+ 0.0464, wherein, y
3for the fluorescence intensity of lead element; x
3for the concentration of lead element, unit is mg/kg;
(4) textile to be measured is directly put into XRF spectrometer, by the condition of work of instrument listed by table 1, cadmium, nickel, plumbous x-ray fluorescence intensity in working sample respectively, corresponding concentration is checked in from typical curve, or respectively cadmium, nickel, plumbous fluorescence intensity are substituted into their respective equations of linear regression, calculate cadmium in institute's test sample product, nickel, plumbous concentration.
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| 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 |
| CN103698352B (en) * | 2014-01-08 | 2016-01-20 | 四川出入境检验检疫局检验检疫技术中心 | The standard solution mother liquor of leather heavy metal stratographic analysis and typical curve preparation 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 |
| JP2016017823A (en) * | 2014-07-08 | 2016-02-01 | 株式会社日立ハイテクサイエンス | Sample plate for x-ray analysis and fluorescent x-ray 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 |
| CN108120625B (en) * | 2017-09-30 | 2020-06-30 | 广东华科检测技术服务有限公司 | Standard sample of total lead and total cadmium in textile and preparation method thereof |
| 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 |
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