CN103698352B - The standard solution mother liquor of leather heavy metal stratographic analysis and typical curve preparation method - Google Patents
The standard solution mother liquor of leather heavy metal stratographic analysis and typical curve preparation method Download PDFInfo
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Abstract
The present invention relates to the technology of heavy metal in a kind of Fast Measurement leather, special preparation XRF Method of Energy Spectrum Analysis carries out Fast Measurement to heavy metal in leather and uses typical curve, and the standard solution mother liquor that preparation standard curve will use.The national standard solution preparation of standard solution mother liquor leather bleeding agent, phosphoric acid, nitric acid and nine heavy metal species forms.Preparation standard curve method is rapid: (1) preparing standard solution mother liquor, (2) prepare many gradients standard solution, the preparation of (3) leather heavy metal series standard sample, (4) prepare leather standard sample disk to be measured, the stratographic analysis of (5) use XRF detects, (6) drawing standard curve.Advantage: the present invention makes the precision that in leather, nine heavy metal species objectionable impuritiess detect can bring up to national standard requirement, thus just make this advanced technology of XRF stratographic analysis can be applied to nine heavy metal species objectionable impuritiess detections in leather.
Description
Technical field
The present invention relates to the technology of heavy metal in a kind of Fast Measurement leather, special preparation XRF Method of Energy Spectrum Analysis carries out Fast Measurement to heavy metal in leather and uses typical curve, and the standard solution mother liquor that preparation standard curve will use.
Background technology
At present, require strict both at home and abroad to the content of beary metal in leather, GB/T22930-2008 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 and can improve XRF energy spectrum analysis leather lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury, the standard solution mother liquor of totally nine heavy metal species accuracy of detection, and with this standard solution mother liquor, this nine heavy metal species in leather is accurately detected to the method obtaining typical curve or claim regression equation.
The standard solution mother liquor of XRF energy spectrum analysis leather nine heavy metal species, each raw material volume ratio formula is as follows:
National standard solution 100mL(both lead solutions of content 1g/L lead),
National standard solution 100mL(both cadmium solutions of content 1g/L cadmium),
National standard solution 100mL(both nickel solutions of content 1g/L nickel),
National standard solution 100mL(both cobalt liquors of content 1g/L chromium),
National standard solution 100mL(both copper solutions of content 1g/L cobalt),
National standard solution 100mL(both copper solutions of content 1g/L copper),
National standard solution 100mL(both lead solutions of content 1g/L antimony),
National standard solution 100mL(both arsenic solutions of content 1g/L arsenic),
National standard solution 10mL(both arsenic solutions of content 1g/L mercury),
Mass concentration be 1% leather bleeding agent AEO 8mL ~ 10mL,
Mass concentration be 85% pure strong phosphoric acid 4mL ~ 8mL,
Mass concentration be 1% nitric acid add to total amount 1000mL.
The compound method of standard solution mother liquor: the national standard solution that mass concentration is respectively the lead of 1g/L, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic and mercury nine heavy metal species is purchased from State center for standard matter.Draw the lead of 100mL, cadmium, nickel, chromium, cobalt, copper, antimony and arsenic eight national standard solution of heavy metal species national standard solution and 10mL mercury respectively, these nine kinds of national standard solution are moved into after in same 1000mL volumetric flask respectively, adding 4mL ~ 8mL mass concentration is the pure strong phosphoric acid of 85% top grade, with the leather bleeding agent AEO that 8mL ~ 10mL mass concentration is 1%, be finally the salpeter solution of 1% by mass concentration
be settled tovolumetric flask scale 1000mL, puts the even standard solution mother liquor (oneself is lower is called for short: standard solution mother liquor) being namely mixed with leather heavy metal XRF chromatogram analysis method production standard model curve.
The typical curve preparation method of content of beary metal XRF stratographic analysis in leather, comprises the steps:
(1) preparing standard solution mother liquor
Drawing 100mL mass concentration is respectively the lead of 1g/L, cadmium, nickel, chromium, cobalt, copper, antimony and arsenic eight heavy metal species national standard solution and 10mL mass concentration are the national standard solution of 1g/L mercury, these nine kinds of national standard solution are moved into after in same 1000mL volumetric flask respectively, adding 4mL ~ 8mL mass concentration is the pure strong phosphoric acid of 85% top grade, with the leather bleeding agent AEO that 8mL ~ 10mL mass concentration is 1%, finally be settled to volumetric flask scale 1000mL with the salpeter solution that mass concentration is 1%, be mixed the standard solution mother liquor (oneself is lower is called for short: standard solution mother liquor) being namely mixed with leather heavy metal XRF chromatogram analysis method production standard model curve.Mass concentration is respectively the plumbous national standard solution of 1g/L, cadmium national standard solution, nickel national standard solution, chromium national standard solution, cobalt national standard solution, copper national standard solution, antimony national standard solution, arsenic national standard solution and mercury national standard solution, and the national standard solution of this nine heavy metal species adopts the standard solution provided of State center for standard matter.
The formula of standard solution mother liquor is as follows:
National standard solution 100mL(both lead solutions of content 1g/L lead),
National standard solution 100mL(both cadmium solutions of content 1g/L cadmium),
National standard solution 100mL(both nickel solutions of content 1g/L nickel),
National standard solution 100mL(both cobalt liquors of content 1g/L chromium),
National standard solution 100mL(both copper solutions of content 1g/L cobalt),
National standard solution 100mL(both copper solutions of content 1g/L copper),
National standard solution 100mL(both lead solutions of content 1g/L antimony),
National standard solution 100mL(both arsenic solutions of content 1g/L arsenic),
National standard solution 10mL(both arsenic solutions of content 1g/L mercury),
Mass concentration be 1% leather bleeding agent AEO 8mL ~ 10mL,
Mass concentration be 85% pure strong phosphoric acid 4mL ~ 8mL,
Mass concentration be 1% nitric acid add to total amount 1000mL.
The effect of phosphoric acid: the effect adding strong phosphoric acid in standard solution mother liquor effectively can ensure that each heavy metal mixed dissolution is in standard solution mother liquor, avoid occurring to produce complexing phenomenon between different heavy metal in solution, improve XRF chromatograph to the mensuration accuracy of heavy metal amount each in standard solution mother liquor.
The effect of nitric acid: the effect adding nitric acid in standard solution mother liquor effectively can ensure that each heavy metal mixed dissolution is in standard solution mother liquor, gets rid of carbonate (CO in solution
3 2-), bicarbonate radical (HCO
3 -), sulfate radical (SO
4 2-) etc. the deliquescent impact of negative ion heavy metal, improve XRF chromatograph to the mensuration accuracy of heavy metal amount each in standard solution mother liquor.
The effect of AEO: add leather bleeding agent AEO in standard solution mother liquor, effect be make each heavy metal species added in standard solution mother liquor can simulate leather produce in each heavy metal species in the effect of leather bleeding agent, the state that each heavy metal species exists in actual leather, with reach be added to without each heavy metal species by additional known each heavy metal species amount leather sample in after, the amount of each heavy metal species in the leather sample measured with XRF chromatograph, closer to measured quantity in actual leather.Measure the difference between the content of beary metal in the leather made of standard solution mother liquor in content of beary metal and standard solution mother liquor like this, error correction can be carried out.So in the XRF stratographic analysis typical curve preparation method of leather heavy metal content, it is very important for adding leather bleeding agent AEO in standard solution mother liquor.
(2) the multiple gradient standard solution of various criterion solution mother liquor content is prepared
Many gradients standard solution forms with the dilution of standard solution mother liquor, and dilution is diluted nine heavy metal species content in standard solution mother liquor with phosphoric acid, AEO, nitric acid three kinds of liquid.Make the typical curve of nine heavy metal species content in leather, both XRF stratographic analysis line strength of nine heavy metal species content and the regression equation of nine heavy metal species content, needed the multiple Graded amounts of this nine heavy metal species.Many gradients standard solution is just to provide the liquid of many Graded amounts of this nine heavy metal species.
As follows by the step of a certain gradient standard solution of standard solution mother liquor dilution preparation:
Get the standard solution mother liquor of a certain volume in 1mL ~ 100mL scope, move in 100mL volumetric flask, add the pure strong phosphoric acid of top grade that 0.4mL ~ 0.8mL mass concentration is 85%, add leather bleeding agent AEO 0.5mL ~ 2.0mL that mass concentration is 1% again, finally be settled to volumetric flask scale 100mL with the nitric acid that mass concentration is 1%, just preparation become preparation standard detection curve and, containing nine heavy metal species, for carrying out the gradient standard solution of leather XRF stratographic analysis; Repeatedly repeat abovementioned steps, obtain the standard solution of multiple different gradient.As the standard solution formula table that table 1 is seven kinds of different gradients.
Table 1: the standard solution formula table of seven kinds of different gradients
(3) preparation of leather heavy metal series standard sample
For overcoming this locality interference of leather sample in determining heavy metals process, get not leaded, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic and mercury nine the leather sample of heavy metal species or above nine heavy metal species content very low (its content of beary metal is negligible) be ground into leather sample powder.Get leather sample powder 5g, the standard solution 10mL of a certain gradient prepared in (2) step is added in leather sample powder, at room temperature 35 DEG C ~ 38 DEG C condition mixing 10min, after drying, i.e. the leather standard powder mud sample (hereinafter referred to as standard powder mud sample) of obtained known nine heavy metal species content; Repeat to prepare the leather standard powder mud sample series of at least five kinds of different known nine heavy metal species content.
(4) leather standard sample disk to be measured is prepared
Make standard round plate shape to the standard powder mud sample of above-mentioned steps (3), pending XRF stratographic analysis detects; Its method making standard round plate shape is, fills a certain 5 grams, standard powder mud sample in the mould to pressing mold diameter being 25mm, and with the pressure of 20,000 newton ~ 40,000 newton, being pressed into diameter is 25mm, and thickness is the leather standard sample disk to be measured of 2mm; Repeat to prepare the leather standard sample disk to be measured of at least five kinds of different known nine heavy metal species content.
(5) detect with XRF stratographic analysis
The leather standard sample disk to be measured of different known nine heavy metal species content is put into XRF stratographic analysis respectively and carries out nine heavy metal species line strength detections, each standard sample disk obtains one group of nine heavy metal species and divides other different line strength measured value.
(6) drawing standard curve
By the nine heavy metal species content value added actual in the multiple different gradient standard solution of step (2), carry out computing from different line strength measured values of step (5) and set up regression equation, obtain nine heavy metal species and divide other regression equation, the curve drawn with these regression equations is typical curve, both line strength measured value having obtained the stratographic analysis of leather nine heavy metal species XRF imitates positive typical curve with the error of nine corresponding heavy metal species content value, is called for short typical curve.This typical curve is just being used for the error effect of other leather nine heavy metal species content of XRF stratographic analysis sampling Detection.
During actual drawing standard curve, XRF stratographic analysis parameter line strength that nine kinds of metals are different represents every heavy metal species respectively, and line strength ordinate Y represents, the heavy metals added in seven kinds of groupings are horizontal ordinate X, drawing standard curve.
Advantage of the present invention: add among sample leather by strong phosphoric acid, avoids occurring to produce complexing phenomenon between different heavy metal in solution, improves XRF chromatograph to the mensuration accuracy of heavy metal amount each in standard solution mother liquor.
Add among sample leather with nitric acid, carbonate (CO in solution can be got rid of
3 2-), bicarbonate radical (HCO
3 -), sulfate radical (SO
4 2-) etc. the deliquescent impact of negative ion heavy metal, improve XRF chromatograph to the mensuration accuracy of heavy metal amount each in standard solution mother liquor.
Add among sample leather with leather bleeding agent AEO, make each heavy metal species added in standard solution mother liquor can simulate the state that in leather production, each heavy metal species exists in actual leather, with reach be added to without each heavy metal species by additional known each heavy metal species amount leather sample in after, in the leather sample measured with XRF chromatograph, the amount of each heavy metal species just can carry out error effect, makes the content of beary metal of drafting bent more accurate to reality sampling leather heavy metal assay.
Because the present invention can to metrical error effect just, it can meet national examination criteria by the error that drawing standard curve of the present invention detects for leather sample of sampling, its XRF stratographic analysis is made to can be used in lead, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic, mercury in leather, the detection of totally nine heavy metal species objectionable impuritiess.Because XRF stratographic analysis avoids miscellaneous (consuming time more than 2 hours) of chemical analysis method test and the consumption of a large amount of reagent; The time measuring a sample is no more than 0.5 hour, without the need to the process of chemical reagent, make the detection of nine heavy metal species objectionable impuritiess in leather more more convenient than existing chemical analysis method, both the present invention made the detection of nine heavy metal species objectionable impuritiess in leather can select this advanced technology of XRF stratographic analysis.
In a word, the present invention makes the precision that in leather, nine heavy metal species objectionable impuritiess detect can bring up to national standard requirement, thus just makes this advanced technology of XRF stratographic analysis can be applied to nine heavy metal species objectionable impuritiess detections in leather.
Embodiment
Embodiment 1, the standard solution mother liquor nine heavy metal species in ox-hide leather detected with XRF energy depressive spectroscopy
The standard solution mother liquor of nine heavy metal species in XRF energy spectrum analysis ox-hide leather, each composition of raw materials is as follows:
National standard solution 100mL(both lead solutions of content 1g/L lead),
National standard solution 100mL(both cadmium solutions of content 1g/L cadmium),
National standard solution 100mL(both nickel solutions of content 1g/L nickel),
National standard solution 100mL(both cobalt liquors of content 1g/L chromium),
National standard solution 100mL(both copper solutions of content 1g/L cobalt),
National standard solution 100mL(both copper solutions of content 1g/L copper),
National standard solution 100mL(both lead solutions of content 1g/L antimony),
National standard solution 100mL(both arsenic solutions of content 1g/L arsenic),
National standard solution 10mL(both arsenic solutions of content 1g/L mercury),
Mass concentration be 1% leather bleeding agent AEO 10mL,
Mass concentration be 85% pure strong phosphoric acid 8mL,
Mass concentration be 1% nitric acid add to total amount 1000mL.
The compound method of above-mentioned standard solution mother liquor: draw lead, cadmium, nickel, chromium, cobalt, copper, antimony and arsenic eight national standard solution of heavy metal species national standard solution and mercury respectively, these nine kinds of national standard solution are moved into after in same 1000mL volumetric flask respectively, adding mass concentration is the pure strong phosphoric acid of 85% top grade, finally be settled to volumetric flask scale 1000mL with the salpeter solution that mass concentration is 1%, put the even standard solution mother liquor being namely mixed with leather heavy metal XRF chromatogram analysis method production standard model curve.The national standard solution that mass concentration is respectively the lead of 1g/L, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic and mercury nine heavy metal species is purchased from State center for standard matter.
Embodiment 2, the standard solution mother liquor nine heavy metal species in pig leather detected with XRF energy depressive spectroscopy
The standard solution mother liquor of nine heavy metal species in XRF energy spectrum analysis pig leather, each composition of raw materials is as follows:
National standard solution 100mL(both lead solutions of content 1g/L lead),
National standard solution 100mL(both cadmium solutions of content 1g/L cadmium),
National standard solution 100mL(both nickel solutions of content 1g/L nickel),
National standard solution 100mL(both cobalt liquors of content 1g/L chromium),
National standard solution 100mL(both copper solutions of content 1g/L cobalt),
National standard solution 100mL(both copper solutions of content 1g/L copper),
National standard solution 100mL(both lead solutions of content 1g/L antimony),
National standard solution 100mL(both arsenic solutions of content 1g/L arsenic),
National standard solution 10mL(both arsenic solutions of content 1g/L mercury),
Mass concentration be 1% leather bleeding agent AEO 8mL,
Mass concentration be 85% pure strong phosphoric acid 4mL,
Mass concentration be 1% nitric acid add to total amount 1000mL.
The compound method of above-mentioned standard solution mother liquor: be same as embodiment 1.
The typical curve preparation method of content of beary metal XRF stratographic analysis in embodiment 3, leather
The typical curve preparation method of content of beary metal XRF stratographic analysis in leather, comprises the steps:
(1) preparing standard solution mother liquor
Draw the national standard solution that lead, cadmium, nickel, chromium, cobalt, copper, antimony and arsenic eight heavy metal species national standard solution that 100mL mass concentration is 1g/L and 10mL mass concentration are 1g/L mercury respectively, these nine kinds of national standard solution are moved into after in same 1000mL volumetric flask respectively, adding 4mL ~ 8mL mass concentration is the pure strong phosphoric acid of 85% top grade, with the leather bleeding agent AEO that 8mL ~ 10mL mass concentration is 1%, be finally the salpeter solution of 1% by mass concentration
be settled tovolumetric flask scale 1000mL, is mixed and is namely mixed with the standard solution mother liquor of leather heavy metal XRF chromatogram analysis method production standard model curve.Above-mentioned mass concentration is respectively the plumbous national standard solution of 1g/L, cadmium national standard solution, nickel national standard solution, chromium national standard solution, cobalt national standard solution, copper national standard solution, antimony national standard solution, arsenic national standard solution and mercury national standard solution, and the national standard solution of this nine heavy metal species adopts the standard solution provided of State center for standard matter.
The formula of standard solution mother liquor is as follows:
National standard solution 100mL(both lead solutions of content 1g/L lead),
National standard solution 100mL(both cadmium solutions of content 1g/L cadmium),
National standard solution 100mL(both nickel solutions of content 1g/L nickel),
National standard solution 100mL(both cobalt liquors of content 1g/L chromium),
National standard solution 100mL(both copper solutions of content 1g/L cobalt),
National standard solution 100mL(both copper solutions of content 1g/L copper),
National standard solution 100mL(both lead solutions of content 1g/L antimony),
National standard solution 100mL(both arsenic solutions of content 1g/L arsenic),
National standard solution 10mL(both arsenic solutions of content 1g/L mercury),
Mass concentration be 1% leather bleeding agent AEO 8mL ~ 10mL,
Mass concentration be 85% pure strong phosphoric acid 4mL ~ 8mL,
Mass concentration be 1% nitric acid add to total amount 1000mL.
(2) many gradients standard solution of various criterion solution mother liquor content is prepared
Many gradients standard solution forms with the dilution of standard solution mother liquor.Make the typical curve of nine heavy metal species content in leather, both XRF stratographic analysis line strength of nine heavy metal species content and the regression equation of nine heavy metal species content, needed many Graded amounts of this nine heavy metal species.Many gradients standard solution is just to provide many Graded amounts liquid of this nine heavy metal species.
As follows by the step of a certain gradient standard solution of standard solution mother liquor dilution preparation:
Get the standard solution mother liquor of a certain volume in 1mL ~ 100mL scope, move in 100mL volumetric flask, add the pure strong phosphoric acid of top grade that 0.4mL ~ 0.8mL mass concentration is 85%, add leather bleeding agent AEO 0.5mL ~ 2.0mL that mass concentration is 1% again, finally be settled to volumetric flask scale 100mL with the nitric acid that mass concentration is 1%, just preparation become preparation standard detection curve and, containing nine heavy metal species, for carrying out the gradient standard solution of leather XRF stratographic analysis; Repeat abovementioned steps 7 times, obtain the standard solution of seven kinds of different gradients.As the standard solution formula table that table 1 is seven kinds of different gradients.
Table 1: the standard solution formula table of seven kinds of different gradients
(3) preparation of leather heavy metal series standard sample
For overcoming this locality interference of leather sample in determining heavy metals process, get not leaded, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic and mercury nine the leather sample of heavy metal species or content very low (its content of beary metal is negligible) be ground into leather sample powder.Get leather sample powder 5g, the standard solution 10mL of a certain gradient prepared in (2) step is added in leather sample powder, at room temperature 35 DEG C ~ 38 DEG C condition mixing 10min, after drying, i.e. the leather standard powder mud sample (hereinafter referred to as standard powder mud sample) of obtained known nine heavy metal species content; Repeat the leather standard powder mud sample series of the known nine heavy metal species content of seven kinds of differences that preparation table 1 provides.
(4) leather standard sample disk to be measured is prepared
Make standard round plate shape to the standard powder mud sample of above-mentioned steps (3), pending XRF stratographic analysis detects; Its method making standard round plate shape is, fills a certain 5 grams, standard powder mud sample in the mould to pressing mold diameter being 25mm, and with the pressure of 20,000 newton ~ 40,000 newton, being pressed into diameter is 25mm, and thickness is the leather standard sample disk to be measured of 2mm; The leather standard sample disk to be measured of the different known nine heavy metal species content of preparation table 1 seven kinds of providing is provided.
(5) detect with XRF stratographic analysis
The leather standard sample disk to be measured of seven kinds of different known nine heavy metal species content is put into XRF stratographic analysis respectively carry out nine heavy metal species line strength and detect, each standard sample disk obtains one group of nine heavy metal species and divides other different line strength measured value.
(6) drawing standard curve
By the nine heavy metal species content value added actual in the multiple different gradient standard solution of step (2), carry out computing from different line strength measured values of step (5) and set up regression equation, obtain nine heavy metal species and divide other regression equation, the curve drawn with these regression equations is typical curve, both line strength measured value having obtained the stratographic analysis of leather nine heavy metal species XRF imitates positive typical curve with the error of nine corresponding heavy metal species content value, is called for short typical curve.This typical curve is just being used for the error effect of other leather nine heavy metal species content of XRF stratographic analysis sampling Detection.
During actual drawing standard curve, XRF stratographic analysis parameter line strength that nine heavy metal species are different represents every heavy metal species respectively, and line strength ordinate Y represents, the heavy metal added in seven kinds of groupings is horizontal ordinate X, drawing standard curve.
Claims (2)
1., with the standard solution mother liquor of XRF energy spectrum analysis leather heavy metal, its each composition of raw materials is as follows:
The national standard solution 100mL of content 1g/L lead,
The national standard solution 100mL of content 1g/L cadmium,
The national standard solution 100mL of content 1g/L nickel,
The national standard solution 100mL of content 1g/L chromium,
The national standard solution 100mL of content 1g/L cobalt,
The national standard solution 100mL of content 1g/L copper,
The national standard solution 100mL of content 1g/L antimony,
The national standard solution 100mL of content 1g/L arsenic,
The national standard solution 10mL of content 1g/L mercury,
Mass concentration be 1% leather bleeding agent AEO 8mL ~ 10mL,
Mass concentration be 85% top grade pure strong phosphoric acid 4mL ~ 8mL.
Mass concentration be 1% nitric acid add to total amount 1000mL.
2. the typical curve preparation method of content of beary metal XRF stratographic analysis in leather, comprises the steps:
(1) preparing standard solution mother liquor
Draw the mercury national standard solution of the plumbous national standard solution of 100mL content 1g/L, the cadmium national standard solution of 100mL content 1g/L, the nickel national standard solution of 100mL content 1g/L, the chromium national standard solution of 100mL content 1g/L, the cobalt national standard solution of 100mL content 1g/L, the copper national standard solution of 100mL content 1g/L, the antimony national standard solution of 100mL content 1g/L, the arsenic national standard solution of 100mL content 1g/L and 10mL content 1g/L respectively; These nine kinds of national standard solution are moved into after in same 1000mL volumetric flask respectively, adding 4mL ~ 8mL mass concentration is the pure strong phosphoric acid of 85% top grade, with the leather bleeding agent AEO that 8mL ~ 10mL mass concentration is 1%, finally be settled to volumetric flask scale 1000mL with the salpeter solution that mass concentration is 1%, put the even standard solution mother liquor (hereinafter referred to as standard solution mother liquor) being namely mixed with leather heavy metal XRF chromatogram analysis method production standard model curve;
The formula of standard solution mother liquor is as follows:
The national standard solution 100mL of content 1g/L lead,
The national standard solution 100mL of content 1g/L cadmium,
The national standard solution 100mL of content 1g/L nickel,
The national standard solution 100mL of content 1g/L chromium,
The national standard solution 100mL of content 1g/L cobalt,
The national standard solution 100mL of content 1g/L copper,
The national standard solution 100mL of content 1g/L antimony,
The national standard solution 100mL of content 1g/L arsenic,
The national standard solution 10mL of content 1g/L mercury,
Mass concentration be 1% leather bleeding agent AEO 8mL ~ 10mL,
Mass concentration be 85% top grade pure strong phosphoric acid 4mL ~ 8mL,
Mass concentration be 1% nitric acid add to total amount 1000mL;
(2) many gradients standard solution is prepared
As follows by the step of a certain gradient standard solution of standard solution mother liquor dilution preparation:
Get the standard solution mother liquor of a certain volume in 1mL ~ 100mL scope, move in 100mL volumetric flask, add the pure strong phosphoric acid of top grade that 0.4mL ~ 0.8mL mass concentration is 85%, add leather bleeding agent AEO 0.5mL ~ 2.0mL that mass concentration is 1% again, finally be settled to volumetric flask scale 100mL with the nitric acid that mass concentration is 1%, be just mixed with a certain
gradientstandard solution; Repeatedly repeat abovementioned steps, obtain the standard solution of multiple different gradient;
(3) preparation of leather heavy metal series standard sample
The leather of not leaded, cadmium, nickel, chromium, cobalt, copper, antimony, arsenic and mercury nine heavy metal species is ground into leather sample powder, sample thief powder 5g, the standard solution 10mL of a certain gradient of preparation in step (2) is added in leather sample powder, at room temperature 35 DEG C ~ 38 DEG C condition mixing 10min, after drying, i.e. the leather standard powder mud sample (hereinafter referred to as standard powder mud sample) of obtained known nine heavy metal species content; Repeat to prepare the leather standard powder mud sample series of at least five kinds of different known nine heavy metal species content;
(4) leather standard sample disk to be measured is prepared
Be a certain 5 grams, the standard powder mud sample loading step (3) in the mould of 25mm at pressing mold diameter, with the pressure of 20,000 newton ~ 40,000 newton, being pressed into diameter is 25mm, and thickness is the leather standard sample disk to be measured of 2mm; Repeat to prepare the leather standard sample disk to be measured of at least five kinds of different known nine heavy metal species content;
(5) detect with XRF stratographic analysis
The leather standard sample disk to be measured of different known nine heavy metal species content is put into XRF stratographic analysis respectively and carries out nine heavy metal species line strength detections, each standard sample disk obtains one group of nine heavy metal species and divides other different line strength measured value;
(6) drawing standard curve
By the nine heavy metal species content value added actual in the multiple different gradient standard solution of step (2), carry out computing from different line strength measured values of step (5) and set up regression equation, obtain nine heavy metal species and divide other regression equation, the curve drawn with these regression equations is typical curve, both obtain line strength measured value of leather nine heavy metal species XRF stratographic analysis and the error correction typical curve of nine corresponding heavy metal species content value, be called for short typical curve.
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| 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 |
| CN106226340A (en) * | 2016-08-31 | 2016-12-14 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate |
| CN106290435A (en) * | 2016-08-31 | 2017-01-04 | 安徽紫山农业科技有限公司 | Heavy metal component method for quick in a kind of starch food |
| CN106370686A (en) * | 2016-08-31 | 2017-02-01 | 广西出入境检验检疫局危险品检测技术中心 | Method for determining copper content in basic copper carbonate for fireworks and firecrackers |
| CN108593692B (en) * | 2018-05-04 | 2021-04-27 | 蒋小良 | Leather standard sample for quantitative screening of high-concern substances of European Union REACH regulation by X fluorescence spectrometry and preparation method thereof |
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| 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 |
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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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2014
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| 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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| Basic forensic identification of artificial leather for hit-and-run cases;Tetsuya Sano et al.;《Forensic Science International》;20090917;第192卷;第e27-e32页 * |
| Determination of Some Trace Elements in Leather;Okoh, S. et al.;《International Journal of Applied Science and Technology》;20130131;第3卷(第1期);第101-105页 * |
| ICP-AES 测定皮革及其制品中的可溶性重金属含量;张海娟等;《西部皮革》;20120630;第34卷(第12期);第27-30页 * |
| 石墨炉原子吸收光谱法测定皮革制品中铅、镉和铬;蒋瑾华等;《光谱实验室》;20020930;第19卷(第5期);第702-702页 * |
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