CN103852463A - Method for detecting content of eight heavy metals in plastic - Google Patents
Method for detecting content of eight heavy metals in plastic Download PDFInfo
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- CN103852463A CN103852463A CN201410115256.7A CN201410115256A CN103852463A CN 103852463 A CN103852463 A CN 103852463A CN 201410115256 A CN201410115256 A CN 201410115256A CN 103852463 A CN103852463 A CN 103852463A
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Abstract
The invention discloses a method for detecting the contents of cadmium, lead, mercury and chromium in plastic. The detection method comprises the following steps of (a) processing a sample into particles, wherein the weight of each particle is not greater than 0.2g; (b) adding nitric acid, hydrochloric acid and hydrogen peroxide in the sample after processing in the step (a) and carrying out microwave digestion, wherein the ratio of the sample to the nitric acid is 1 to 30-50g/ml, the ratio of the sample to the hydrochloric acid is 1 to 10-20g/ml, and the ratio of the sample to the hydrogen peroxide is 1 to 5-10g/ml; and (c) after finishing the digestion, taking out a digestion solution, filtering and carrying out ICP-OES (Inductively Coupled Plasma Optical Emission Spectrometer) analysis on the digestion solution. The detection method provided by the invention has the advantages that the analytical method is rapid, the accuracy is high, and the repeatability and reproducibility are good.
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 the eight heavy metal species content such as cadmium, lead, mercury, chromium in a kind of plastics.
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.
Regenerated resources are Strategic Measures that make up china natural resources shortage, the recycling of waste or used plastics as one economize on resources, the measure of protection of the environment more and more comes into one's own.Because plastics source is complicated, be inevitably mixed with various snotteres or poisonous and harmful substance.Waste or used plastics can produce waste water, waste gas and solid waste in recycling process, need adopt an effective measure and administer.In order to control and to reduce environmental risk, before plastics recovery, content of beary metal in plastics is detected to determine that it is necessary how carrying out technics of reclaim of plastic waste.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 plastics.
Summary of the invention
The object of the present invention is to provide the detection method of cadmium in a kind of plastics, lead, mercury, chromium, arsenic, selenium, antimony, barium eight heavy metal species content.Method of the present invention is by the microwave digestion disposal route of sample, can obtain fast and accurately in plastics the content of the heavy metal element of eight kinds.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 plastics, a detection method for cadmium, lead, mercury, chromium content, 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) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:30-50g/ml, be for example 1:3g/ml, 1:36g/ml, 1:41g/ml, 1:47g/ml etc., be for example, the ratio of sample and hydrochloric acid is 1:10-20g/ml, be for example 1:13g/ml, 1:16g/ml, 1:19g/ml etc., the ratio of sample and hydrogen peroxide is 1:5-10g/ml, for example, be 1:7g/ml, 1:9g/ml etc.;
(c) after having cleared up, take out digestion solution, after filtration, carry out 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.
The present invention by a large amount of determined use microwave abstracting then carry out that ICP-OES analyzes can be accurate, obtain reliably the content of heavy metal in plastics, wherein choosing of the solvent of microwave abstracting and proportioning thereof has important impact to the extraction completely of heavy metal element, can better heavy metal element be extracted from product.
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, the process of described microwave abstracting is as follows: sample is put into Teflon microwave tube, then add nitric acid, hydrochloric acid and hydrogen peroxide, the parameter of microwave abstracting is set to: sample solution temperature is 200-220 ℃, rate of pressure rise is 0.5-1.0bar/s, rising to stage by stage power is that 750-850kw keeps 10-30min, then in 3min, be down to 0kw and keep 10-20min, after cooling 1min is above, sample is taken out and naturally cools to room temperature, when rising, power should make rate of pressure rise also meet the lifting range of 0.5-1.0bar/s.
Preferably, the parameter of described microwave abstracting is set to: sample solution temperature is 210 ℃, and rate of pressure rise is 0.7bar/s, and it is that 800kw keeps 20min that point 5 stages rise to power, then in 1min, is down to 0kw and keeps 15min, cooling 3min.
As optimal technical scheme, detection method of the present invention, the ratio of described sample and nitric acid is 1:40g/ml, and the ratio of sample and hydrochloric acid is 1:17g/ml, and the ratio of sample and hydrogen peroxide is 1:6-7g/ml.
As optimal technical scheme, detection method of the present invention, constant volume after described digestion solution filters.
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 0.2g;
(b) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:30-50g/ml, and the ratio of sample and hydrochloric acid is 1:10-20g/ml, and the ratio of sample and hydrogen peroxide is 1:5-10g/ml; The process of described microwave abstracting is as follows: sample is put into Teflon microwave tube, then add nitric acid, hydrochloric acid and hydrogen peroxide, the parameter of microwave abstracting is set to: sample solution temperature is 200-220 ℃, rate of pressure rise is 0.5-1.0bar/s, rising to stage by stage power is that 750-850kw keeps 10-30min, then in 3min, be down to 0kw and keep 10-20min, after cooling 1min is above, sample is taken out and naturally cools to room temperature;
(c) after having cleared up, take out digestion solution, after filtration, carry out ICP-OES analysis.
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) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:40g/ml, and the ratio of sample and hydrochloric acid is 1:17g/ml, and the ratio of sample and hydrogen peroxide is 1:6-7g/ml; The parameter of described microwave abstracting is set to: sample solution temperature is 210 ℃, and rate of pressure rise is 0.7bar/s, and it is that 800kw keeps 20min that point 5 stages rise to power, then in 1min, is down to 0kw and keeps 15min, cooling 3min;
(c) after having cleared up, take out digestion solution, after filtration, constant volume, carry out 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:
25ml volumetric flask (A level), filter paper: aperture 0.45 μ m, electronic balance: can smart scale to 0.01mg, microwave digestion device, analyzes 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), analyzes pure hydrogen peroxide (H
2o
2), proportion 1.10g/L, 30% (m/m);
Standard items: plumbous (Pb), cadmium (Cd), mercury (Hg), chromium (Cr), arsenic (As), selenium (Se), antimony (Sb), barium (Ba) titer 1000ppm.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 plastic sample 0.15 ± 0.001g and be cut into the particle that is not more than 0.2g size, put into the Teflon pipe of microwave digestion device;
(b) in Teflon pipe, add 6ml to analyze pure nitron, 2ml analyzes pure hydrochloric acid reagent, and 1ml analyzes pure hydrogen peroxide reagent, builds explosion-proof head, puts into rotor in microwave device; Open microwave device and start setup parameter by F1-Library, use lower right and left key system of selection, to set; If will, in the time of binding method, please select " Make New Sample ", F4and F5 is key position up and down;
Microwave abstracting parameters R eagent is set to:
(1)HNO
3---6ml,HCl---2ml
(2)Power---800,Ramp---10,Hold---25,Fan---1
(3)Power---0,Ramp---0,Hold---20,Fan---3
(4)IR:210℃，Rate:0.7bar/s
(c) after microwave abstracting completes, be cooled to room temperature, pressure release is taken out, and with a small amount of deionized water rinsing,, and transfers in 25ml volumetric flask solution filter with 0.45 μ m filter paper, is finally settled to 25ml groove with deionized water; Constant volume liquid is carried out to 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 96-103%, 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 (8)
1. a detection method for cadmium, lead, mercury, chromium content in plastics, comprises the steps:
(a) sample preparation is become to every particle that is not more than 0.2g;
(b) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:30-50g/ml, and the ratio of sample and hydrochloric acid is 1:10-20g/ml, and the ratio of sample and hydrogen peroxide is 1:5-10g/ml;
(c) after having cleared up, take out digestion solution, after filtration, carry out 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, it is characterized in that, the process of described microwave abstracting is as follows: sample is put into Teflon microwave tube, then add nitric acid, hydrochloric acid and hydrogen peroxide, the parameter of microwave abstracting is set to: sample solution temperature is 200-220 ℃, and rate of pressure rise is 0.5-1.0bar/s, and rising to stage by stage power is that 750-850kw keeps 10-30min, then in 3min, be down to 0kw and keep 10-20min, after cooling 1min is above, sample is taken out and naturally cools to room temperature.
4. detection method as claimed in claim 3, is characterized in that, the parameter of described microwave abstracting is set to: sample solution temperature is 210 ℃, rate of pressure rise is 0.7bar/s, dividing for 5 stages rose to power is that 800kw keeps 20min, then in 1min, is down to 0kw and keeps 15min, cooling 3min.
5. detection method as claimed in claim 1, is characterized in that, the ratio of described sample and nitric acid is 1:40g/ml, and the ratio of sample and hydrochloric acid is 1:17g/ml, and the ratio of sample and hydrogen peroxide is 1:6-7g/ml.
6. detection method as claimed in claim 1, is characterized in that, constant volume after described digestion solution filters.
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 0.2g;
(b) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:30-50g/ml, and the ratio of sample and hydrochloric acid is 1:10-20g/ml, and the ratio of sample and hydrogen peroxide is 1:5-10g/ml; The process of described microwave abstracting is as follows: sample is put into Teflon microwave tube, then add nitric acid, hydrochloric acid and hydrogen peroxide, the parameter of microwave abstracting is set to: sample solution temperature is 200-220 ℃, rate of pressure rise is 0.5-1.0bar/s, rising to stage by stage power is that 750-850kw keeps 10-30min, then in 3min, be down to 0kw and keep 10-20min, after cooling 1min is above, sample is taken out and naturally cools to room temperature;
(c) after having cleared up, take out digestion solution, after filtration, carry out ICP-OES analysis.
8. 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) in step (a) sample after treatment, add nitric acid, hydrochloric acid and hydrogen peroxide to carry out micro-wave digestion; The ratio of sample and nitric acid is 1:40g/ml, and the ratio of sample and hydrochloric acid is 1:17g/ml, and the ratio of sample and hydrogen peroxide is 1:6-7g/ml; The parameter of described microwave abstracting is set to: sample solution temperature is 210 ℃, and rate of pressure rise is 0.7bar/s, and it is that 800kw keeps 20min that point 5 stages rise to power, then in 1min, is down to 0kw and keeps 15min, cooling 3min;
(c) after having cleared up, take out digestion solution, after filtration, constant volume, carry out ICP-OES analysis.
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| CN104122253A (en) * | 2014-07-31 | 2014-10-29 | 深圳出入境检验检疫局玩具检测技术中心 | Method for detecting heavy metals in plastics |
| CN104122218A (en) * | 2014-07-31 | 2014-10-29 | 深圳出入境检验检疫局玩具检测技术中心 | Method for detecting heavy metals in plastics |
| CN104713871A (en) * | 2015-02-09 | 2015-06-17 | 南京市产品质量监督检验院 | Detection method of heavy metals Pb, Cd, Cr and Hg in solid surfacing material |
| CN106908438A (en) * | 2017-03-08 | 2017-06-30 | 江门出入境检验检疫局检验检疫技术中心 | It is a kind of while detecting that each heavy metal species in tableware polytetrafluorethylecoatings coatings distinguish the micro-wave digestion ICP OES methods of content |
| CN107101995A (en) * | 2017-06-05 | 2017-08-29 | 苏州市信测标准技术服务有限公司 | The assay method of micro gold content in a kind of ion exchange resin |
| CN110470656A (en) * | 2019-09-09 | 2019-11-19 | 华东师范大学 | The detection method of heavy metal in a kind of vinyon |
| CN113607510A (en) * | 2021-06-22 | 2021-11-05 | 广东华声电器实业有限公司 | Microwave pretreatment method of plastic material special for electronics |
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| CN107101995A (en) * | 2017-06-05 | 2017-08-29 | 苏州市信测标准技术服务有限公司 | The assay method of micro gold content in a kind of ion exchange resin |
| CN110470656A (en) * | 2019-09-09 | 2019-11-19 | 华东师范大学 | The detection method of heavy metal in a kind of vinyon |
| CN113607510A (en) * | 2021-06-22 | 2021-11-05 | 广东华声电器实业有限公司 | Microwave pretreatment method of plastic material special for electronics |
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Application publication date: 20140611 |