CN103901019A - Method for detecting content of heavy metal elements in metal or alloy material - Google Patents
Method for detecting content of heavy metal elements in metal or alloy material Download PDFInfo
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- CN103901019A CN103901019A CN201410115185.0A CN201410115185A CN103901019A CN 103901019 A CN103901019 A CN 103901019A CN 201410115185 A CN201410115185 A CN 201410115185A CN 103901019 A CN103901019 A CN 103901019A
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Abstract
The invention discloses a method for detecting content of heavy metal elements in metal or an alloy material. The method comprises the following steps: (a) processing a sample into grains which are not heavier than 0.2g; (b) adding the sample processed in the step (a) into a mixture solution of analysis pure nitric acid and analysis pure hydrochloric acid to completely dissolve the sample, wherein the ratio of the sample to the mixture solution is 1:(15-25g/ml), and the volume ratio of the analysis pure nitric acid to the analysis pure hydrochloric acid in the mixture solution is (1-5):1; (c) putting the completely filtered dissolved solution into a volumetric flask, and achieving a constant volume, wherein the ratio of the quantified volume to the sample mass is (150-250):1ml/g; and (d) performing inductively coupled plasma-optical emission spectroscopy (ICP-OES) analysis on the solution obtained in the step (c). The analysis method provided in the invention is rapid, and high in repeatability and reproducibility.
Description
Technical field
The present invention relates to a kind of detection method of contents of heavy metal elements, relate in particular to the detection method of contents of heavy metal elements in a kind of metal or alloy material.
Background technology
Heavy metal element, generally refers to that under status of criterion simple substance density is greater than the metallic element of 4500kg/ cubic meter, is different from light metal element (as aluminium, magnesium).Common heavy metal element has cadmium (Cd), mercury (Hg), arsenic (As), Cr (chromium) copper (Cu), barium (Ba), plumbous (Pb) etc.The ion of heavy metal element is generally poisonous, and such as copper simple substance is nontoxic, but copper ion makes protein denaturation, poisonous.
Along with getting more and more that metal or alloy uses in commercial production, the increasing rubbish of generation, has brought tremendous influence to global ecologic environment.Wherein, heavy metal element is also more and more serious to the pollution of environment.Therefore, develop the detection method of the content of beary metal efficient, convenient, accuracy is high, thereby effectively control content of beary metal is wherein significant for contents of heavy metal elements in detection metal or alloy.
Summary of the invention
The object of the present invention is to provide the detection method of contents of heavy metal elements in a kind of metal or alloy material.Method of the present invention is by suitable sample treatment, can obtain fast and accurately the heavy metal element (plumbous (Pb) in metal or alloy material, cadmium (Cd), mercury (Hg), chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), barium (Ba)) content.And show through large quantity research, method accuracy of the present invention is high, repeatability and repeatability excellence.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
In metal or alloy material, a detection method for contents of heavy metal elements, comprises the steps:
(a) becoming every to be not more than 0.2g sample preparation, for example, is the particle of 0.05g, 0.12g, 0.14g, 0.18g etc.;
(b) step (a) sample after treatment is added the mixed solution of analyzing pure nitric acid and analyzing pure hydrochloric acid sample is dissolved completely; The ratio of sample and mixed solution is 1:15-25g/ml, for example, be 1:17g/mL, 1:21g/mL, 1:24g/mL etc., and the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 1-5:1, for example, be 2:1,4:1 etc.;
(c) filter solution after dissolving completely to volumetric flask, constant volume, the volume after constant volume and sample quality are than being 150-250:1ml/g;
(d) step (c) gained solution is carried out to ICP-OES analysis.
The present invention, by selecting suitable pre-treatment and suitable digestion solution, can complete the testing of heavy metal element in sample fast and accurately.
As optimal technical scheme, detection method of the present invention, described sample preparation becomes every particle that is not more than 0.1g.
As optimal technical scheme, detection method of the present invention, at 90-110 ℃, for example, is more than the lower heating 3min such as 93 ℃, 97 ℃, 103 ℃, 108 ℃ in described sample dissolution process, for example, be 6min, 9min, 12min etc.
Preferably, in described sample dissolution process, at 100 ℃, heat 5-10min.
As optimal technical scheme, detection method of the present invention, the ratio of described sample and solvent is 1:20g/mL, the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 3:1.
As optimal technical scheme, detection method of the present invention, the volume after described constant volume is 200:1ml/g with sample quality ratio.
As optimal technical scheme, detection method of the present invention, comprises the steps:
(a) sample preparation is become to every particle that is not more than 0.1g;
(b) step (a) sample after treatment is added the mixed solution of analyzing pure nitric acid and analyzing pure hydrochloric acid sample is dissolved completely, in course of dissolution, for more than sample being dissolved completely can heat 3min at 90-110 ℃, preferably heat 5-10min at 100 ℃; The ratio of sample and mixed solution is 1:20g/ml, and the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 3:1;
(c) filter solution after dissolving completely to volumetric flask, constant volume, the volume after constant volume and sample quality are than being 200:1ml/g;
(d) step (c) gained solution is carried out to ICP-OES analysis.
Detection method of the present invention is easy, quick, and accuracy is high, repeatability and repeatability good.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows.
Instrument equipment in embodiment:
100ml beaker, 100ml volumetric flask (A level), filter paper, aperture 0.45 μ m, electronic balance: can smart scale to 0.01mg, analyze quantitative instrument (ICP-OES);
Agents useful for same in embodiment:
Analyze pure nitric acid (HNO
3), proportion 1.40g/L, 65% (m/m); Analyze pure hydrochloric acid (HCl), proportion 1.18g/L, 37% (m/m);
Standard items: 1000ppm lead (Pb), cadmium (Cd), mercury (Hg), chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), barium (Ba) titer.Prepare the solution of the series concentration of drawing standard curve with 1000ppm titer.
10ppm titer: get the each titer of 1ml1000ppm and 2ml analyze pure for nitron volumetric flask (A level) add deionized water and be diluted to 100ml and get final product;
1ppm titer: get 10ml10ppm each for titer volumetric flask (A level) add deionized water and be diluted to 100ml and get final product, regulate the pH value making after dilution to mate with sample with nitric acid around here;
0.5ppm titer: get 5ml10ppm each for titer volumetric flask (A level) add deionized water and be diluted to 100ml and get final product, regulate the pH value making after dilution to mate with sample with nitric acid around here;
0.1ppm titer: get 1ml10ppm each for titer volumetric flask (A level) add deionized water and be diluted to 100ml and get final product, regulate the pH value making after dilution to mate with sample with nitric acid around here;
Blank solution: be mixed with the solution mating with sample pH value value as blank solution with deionized water with analyzing pure nitron.
Embodiment 1
(a), with electronics capacity of balance sample wire strip diode plastic components and be cut into the particle that is not more than 0.2g size, put into 100ml beaker;
(b) will include the pure nitric acid of analysis that adds 10ml in the beaker of sample: analyze pure hydrochloric acid=3:1(volume ratio) solution, whether observe sample dissolves completely, if completely do not dissolve and add again a small amount of above solution until sample dissolves completely, if when sample can not dissolve completely, can on the heating plate of 100 ℃, heat 5-10min, until metal sample all dissolves; The beaker of pre-treatment use is with a small amount of deionized water rinsing, with 0.45 μ m filter paper by solution filter, and quantitatively to 100ml in volumetric flask, finally with deionized water quantitatively to volumetric flask groove;
(c) ICP-OES quantitative test.
Same laboratory records the content (unit is mg/kg) of heavy metal element in sample and repeatability thereof in table 1.
Table 1
The method is carried out to the repeatability test between different experiments chamber, the results are shown in Table 2.
Table 2
Can find out from table 1 and 2, repeatability of the present invention and repeatability are very good.Meanwhile, the recovery of the recovery of standard addition test all elements carrying out, between 95-103%, illustrates that the inventive method has higher accuracy.
Applicant's statement, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thereby the new numerical range producing, also be one of record scope of the present invention, the application, for making instructions simple and clear, is no longer enumerated these numerical ranges.
Applicant's statement, the present invention illustrates manufacture craft of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned making step, does not mean that the present invention must rely on above-mentioned making step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out combination in any between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (7)
1. a detection method for contents of heavy metal elements in metal or alloy material, comprises the steps:
(a) sample preparation is become to every particle that is not more than 0.2g;
(b) step (a) sample after treatment is added the mixed solution of analyzing pure nitric acid and analyzing pure hydrochloric acid sample is dissolved completely; The ratio of sample and mixed solution is 1:15-25g/ml, and the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 1-5:1;
(c) filter solution after dissolving completely to volumetric flask, constant volume, the volume after constant volume and sample quality are than being 150-250:1ml/g;
(d) step (c) gained solution is carried out to ICP-OES analysis.
2. detection method as claimed in claim 1, is characterized in that, described sample preparation becomes every particle that is not more than 0.1g.
3. detection method as claimed in claim 1, is characterized in that, more than heating 3min in described sample dissolution process at 90-110 ℃.
4. detection method as claimed in claim 3, is characterized in that, in described sample dissolution process, at 100 ℃, heats 5-10min.
5. detection method as claimed in claim 1, is characterized in that, the ratio of described sample and solvent is 1:20g/mL, and the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 3:1.
6. detection method as claimed in claim 1, is characterized in that, the volume after described constant volume is 200:1ml/g with sample quality ratio.
7. detection method as claimed in claim 1, is characterized in that, comprises the steps:
(a) sample preparation is become to every particle that is not more than 0.1g;
(b) step (a) sample after treatment is added the mixed solution of analyzing pure nitric acid and analyzing pure hydrochloric acid sample is dissolved completely, in course of dissolution, for more than sample being dissolved completely can heat 3min at 90-110 ℃, preferably heat 5-10min at 100 ℃; The ratio of sample and mixed solution is 1:20g/ml, and the volume ratio of analyzing pure nitric acid and analysis pure hydrochloric acid in mixed solution is 3:1;
(c) filter solution after dissolving completely to volumetric flask, constant volume, the volume after constant volume and sample quality are than being 200:1ml/g;
(d) step (c) gained solution is carried out to ICP-OES analysis.
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Cited By (6)
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| CN104089948A (en) * | 2014-07-08 | 2014-10-08 | 第一拖拉机股份有限公司 | Method for measuring content of lead in paint coating of mechanical product |
| CN104655611A (en) * | 2015-01-20 | 2015-05-27 | 北方工业大学 | Method for continuously testing element distribution in aluminum alloy plate |
| CN105866102A (en) * | 2016-03-28 | 2016-08-17 | 超威电源有限公司 | Method for determining content of lanthanum element in lead or lead alloy through plasma emission spectroscopy |
| CN106706605A (en) * | 2016-12-27 | 2017-05-24 | 武汉泛洲中越合金有限公司 | Method for detecting content of chromium in copper alloy |
| CN107782605A (en) * | 2017-09-28 | 2018-03-09 | 中国航发动力股份有限公司 | A kind of dissolving method of graininess indissoluble alloy |
| CN114749042A (en) * | 2022-04-12 | 2022-07-15 | 宁波江丰电子材料股份有限公司 | Dissolving method of AgCuTi alloy |
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| CN106706605A (en) * | 2016-12-27 | 2017-05-24 | 武汉泛洲中越合金有限公司 | Method for detecting content of chromium in copper alloy |
| CN107782605A (en) * | 2017-09-28 | 2018-03-09 | 中国航发动力股份有限公司 | A kind of dissolving method of graininess indissoluble alloy |
| CN114749042A (en) * | 2022-04-12 | 2022-07-15 | 宁波江丰电子材料股份有限公司 | Dissolving method of AgCuTi alloy |
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Application publication date: 20140702 |