CN102169091B - Method for analyzing and measuring typical metal in circuit board of discarded electrical equipment - Google Patents
Method for analyzing and measuring typical metal in circuit board of discarded electrical equipment Download PDFInfo
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Abstract
The invention relates to a method for analyzing and measuring typical metal in a circuit board of discarded electrical equipment and relates to the technology for pre-treating the circuit board of discarded electrical equipment and detecting and analyzing the content of the typical metal element. The method comprises the following steps: collecting a sample of the circuit board part of discarded electrical equipment and then performing the operations of surface dressing, cleaning, and rough and fine grinding on the sample; adding a proper amount of digestion reagent into the prepared sample, digesting the prepared sample by using a microwave digestion device and then extracting metal matter from the discarded circuit board; and using an inductively coupled plasma emission spectrometer to analyze the nature and quantity of the digested sample. According to the method, the operations of sample grinding and digesting are simple, the reagent consumption is less, the analysis result is accurate and reliable, the detection concentration range is wide, the technical problem of difficultly pre-treating the circuit board sample is solved, and the method is suitable for quickly identifying and accurately measuring the typical metal elements in the circuit boards of various discarded electrical products (such as televisions, refrigerators, washing machines, computers, printers, and the like) and the typical metal elements in the corner wastes generated in the circuit board production process.
Description
Technical field
The present invention relates to the analysis determining method of typical metal in a kind of discarded appliance circuit plate.
Background technology
Along with the raising of productive life level and the acceleration of electric equipment update have caused the discarded of a large amount of circuit boards.Waste printed circuit board mainly contains two and originates greatly: the one, and discarded electrical equipment; The 2nd, the leftover bits that produce in the board production process.Owing to need good electrical conductivity, the content of metallic element and kind are very abundant in the circuit board.Wherein tenor such as copper, nickel accounts for 5 ~ 30% of circuit board gross mass, has higher recovery value; Constituent content such as chromium, arsenic is relatively low in the circuit board, and recovery value is low, and these elements get into environment can cause the long-term hazards that is difficult to repair.If lack strict supervision, recovery or Disposal Measures, waste printed circuit board maintenance, recycle with discarded process in, metallic element will be released in the environment and to the ecosystem and human health and cause harmful effect.Along with people's is to the concern of metallic pollution at agricultural, ecology and health effect, and the pollution problem that electron wastes causes obtains more concern and attention gradually.Therefore, detect kind, content and the distribution characteristics of discarding typical metal in the electrical equipment and become the problem that the environmentalist presses for solution.
Circuit board mainly is made up of the baseplate material of insulation and the circuit of conduction, and composition is numerous and diverse, material is special and homogeneity is inconsistent.Metallics accounts for 5～30% of circuit board general assembly (TW) in the circuit board, and containing element is of a great variety, content difference is big, has brought difficulty to analyzing and testing.The circuit board substrate material is formed complicacy and is different from common environment solid samples such as soil, rubbish, flying dust.Common appliance circuit base board material has: paper substrate plate, glass cloth substrate, epoxy resin substrate and polyesters substrate etc.In discarded electrical equipment, the circuit board substrate material is main with paper substrate plate and glass cloth substrate at present.In the preprocessing process of circuit board, the paper substrate plate can well be dissolved in and clearing up in the reagent, and the dissolving of glass cloth substrate is difficulty comparatively.Discarded electrical equipment baseplate material has characteristics such as high heat-resisting, high tenacity, high flame retardant, strong corrosion resistant property, so the preparation of circuit board sample and pre-service difficulty are very big.The method that does not have standard at present both at home and abroad for the pre-service of metallics in the testing circuit plate, so the preprocessing process of circuit board is one of innovative point of the present invention.
In the circuit board sample analysis determining method of metal generally comprise sample pulverizing, Specimen eliminating, clear up the back digestion solution catch up with acid, sample constant volume and five processes of assay determination.Aspect the sample pulverizing, main at present employing liquid nitrogen comminutor is directly pulverized, but the liquid nitrogen comminutor costs an arm and a leg, and crushing effect is bad, influences the follow-up reappearance of clearing up effect and analysis result.Aspect the clearing up of sample, adopt traditional dry type resolution method, wet type resolution method and develop Microwave Digestion rapidly at present for clearing up of solid sample more.Wherein, when the dry type resolution method was cleared up sample, there was loss in metal and follows the release of a large amount of toxic gases; Common wet type resolution method digestion time is long, and the reagent use amount is big, produces toxic gas simultaneously; Though micro-wave digestion can effectively be avoided the problems referred to above, the concrete grammar and the effect of at present relevant microwave digestion technology treatment circuit plate sample still do not have report.Therefore when utilizing micro-wave digestion treatment circuit plate sample, selecting which kind of clears up reagent, difference is cleared up the amount ratio of reagent and how the condition of clearing up is set all is to adopt the technical matters of the required solution of Microwave Digestion.The instrument analysis technology aspect of metallic element, main both at home and abroad employing atomic absorption spectrum (AAS), inductively coupled plasma emission/spectrum (ICP-AES) and inductively coupled plasma/mass spectrum instruments such as (ICP-MS) come the typical metal in the working sample.Because it is complicated that circuit board is cleared up back testing sample matrix; The metallic element kind is many; The concentration difference span is big between the difference elements, so select suitable analytical instrument optimization spectrum condition, minimizing matrix to disturb, guarantee that precision of analysis also is one of key content of such sample analysis detection.
Summary of the invention
The object of the present invention is to provide a kind of easy to operate, result accurately, the analyzing detecting method of typical metal in the discarded appliance circuit plate of favorable reproducibility, with realize to the quick identification of typical metal element in the circuit board of multiple discarded electric equipment products (televisor, refrigerator, washing machine, computer, printer etc.) and the circuit board processing leftover pieces with accurately measure.Through the repeated examinations of actual sample,
The analyzing detecting method of typical metal in the discarded appliance circuit plate that the present invention proposes, concrete steps are following:
(1) analytic sample preparation
Meal is broken into coarse grain or the sheet that diameter is 1～2cm size after the waste printed circuit board of gathering being extractd electron devices such as electric capacity, resistance; Further coarse grain or sheet are ground into 50～100 purpose particulates again; Particulate is carried out inquartation repeatedly, obtain the circuit board testing sample;
(2) the circuit board sample clears up processing
A. circuit board Specimen eliminating pre-treatment: take by weighing the circuit board testing sample 0.2～0.5g that handles well through the first step; Put into the special-purpose counteracting tank of microwave; Add 10～20mL subsequently and clear up reagent; Mix to avoid the circuit board testing sample to be bonded at and clear up on the tank skin,, cover and clear up lid adding the circuit board testing sample and clearing up counteracting tank behind the reagent and be placed in the fuming cupboard room temperature reaction 9-12 minute;
B. micro-wave digestion circuit board sample: step (A) is made the counteracting tank that contains the circuit board testing sample put into microwave dissolver, the power of setting micro-wave digestion is 700～1000W; Digestion time is controlled at 30～40min; Clear up finish to treat that the counteracting tank temperature is reduced to room temperature after, take out counteracting tank;
(3) catch up with acid, constant volume to clearing up the back sample liquid
It is on 125-135 ℃ the electric hot plate that the counteracting tank that contains digestion solution that step (2) is obtained places preset temperature; Add several perchloric acid; Heating 4～8h obtains the small size digestion solution; It is that 2～5% nitric acid is settled to 25～50mL that the small size digestion solution that obtains is used volume fraction, and the digestion solution behind the constant volume is filtered through 0.45 μ m water pin type filter, and the digestion solution after the filtration is final testing sample solution;
(4) inductively coupled plasma emission spectrography is measured the typical metal in the testing sample
The testing sample solution that step (3) is obtained adopts inductive coupling plasma emission spectrograph to carry out the qualitative and quantitative analysis of metal target, and the main analytical parameters of instrument is set: plasma power is 1200～1500W; Carrier gas is that pure argon (Ar) flow is 0.70～0.9L/min; The plasma flow amount is 15～18L/min; The secondary air amount is 0.2～0.3 L/min; The sample pulling speed is 1.5mL/min; Through analysis, confirm the metallic element of 10 kinds of metallic elements such as copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and tin as key monitoring in the circuit board sample to dissimilar circuit boards in the discarded electric equipment products of kind surplus 10.According to the spectroscopic data between 180～800nm, analyze the accurate concentration that the photon intensity of above-mentioned multiple element under characteristic spectral line can obtain each element in the digestion solution.According to sampling amount in the digestion process, calculate the accurate content of typical metal element in the circuit board again.
Among the present invention, the said reagent of clearing up is one to multiple kind in the mixed liquors such as nitric acid, oxydol, hydrofluorite or fluoboric acid.
Among the present invention, the volume ratio of hydrofluorite, nitric acid and three kinds of reagent of oxydol is 4:7:2.
Among the present invention, said microwave dissolver model is Mile Stone ETHOS 1.
Advantage of the present invention is following:
1, the present invention has contrasted and multiplely commonly used has cleared up reagent, has finally confirmed by the polynary system of clearing up that hydrofluorite, nitric acid and oxydol are formed the circuit board sample to be cleared up.Wherein oxydol has strong oxidizing property, nitric acid has strong acid and strong oxidizing property, and hydrofluorite helps the decomposition of circuit board basic material.This acid mixture combination is compared with the solvent of clearing up that system and other combinations are cleared up in the unit, more helps the stripping of metallic element in the waste printed circuit board sample, has solved the required choice of Solvent difficult problems of indissoluble Specimen eliminating such as circuit board.The present invention also offsets in the enzymatic hydrolysis system consumption proportion of all ingredients and optimizes.When sample volume was about 0.2 ~ 0.5g, the ratio of hydrofluorite, nitric acid and three kinds of reagent of oxydol was: 4:7:2.
2, the present invention optimizes the heating schedule of micro-wave digestion.Clearing up initial temperature is room temperature, and 10～15min rises to 165 ℃ in order to avoid the safety problem that rapid intensification possibly cause; Heating rate with 3～8 ℃/min keeps a period of time with temperature from 165 ℃ to 200 ℃ and at 200 ℃.Whole digestion process can make sample matrices thoroughly decompose, and metallic element fully is dissolved in the reagent.The optimization of heating schedule had both guaranteed to help the safety cleared up digestion process again and carry out quickly and efficiently, had shortened digestion time, improved widely commonly do, metal is prone to loss and a large amount of toxic gas is discharged into the medium problem of environment during wet clearing up.
3, the present invention analytic sample prepare process adopt coarse crushing-fine powder broken-three step of inquartation treatment scheme repeatedly, improved the homogeneity of circuit board sample; Simultaneously common beater grinder ventilating opening is wrapped up with mouth mask, reduce the eliminating of dust.The invention solves circuit board sample sampling and be difficult for evenly being prone to cause the problem of reproducibility of analysis results difference, reduced Dust Capacity, reduced in the specimen preparation process experiment operator the suction of dust.A kind of safety, simple analysis sample preparation technology.
4, the present invention adopt that inductive coupling plasma emission spectrograph is qualitative, typical metal element in the discarded appliance circuit plate member of quantitative measurement.Avoided because the detection problem that the sample matrices complicacy possibly brought, the present invention has added internal standard element when utilizing inductively-coupled plasma spectrometer to detect, adopt internal standard method to eliminate the interference of matrix, makes the analysis result more reliable.The present invention has set up the analysis determining method fast and accurately of typical metal in a kind of discarded appliance circuit plate member.Realized the accurate assay determination of typical metal in the discarded appliance circuit plate sample.
5, the present invention is applicable to the circuit board of multiple discarded electric equipment products (televisor, refrigerator, washing machine, computer, printer etc.) and the quick identification and accurate mensuration that typical metal element in the leftover pieces is discarded in circuit board processing.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Fig. 2 is the heating schedule of the present invention when micro-wave digestion.
Embodiment
Embodiment 1
With the present invention the leftover pieces that domestic certain brand computer board production process produces are analyzed, measured the wherein kind and the content of typical metal.
The collecting circuit board leftover pieces are as sample.With scissors the sample meal is broken into diameter 2cm size, adopts beater grinder that the further fine powder of coarse crushing sample is broken, the homogeneity of sample was collected the testing sample particulate at last when the broken sample afterwards of fine powder was repeated 3 inquartations with the assurance sampling.
Took by weighing circuit board leftover pieces sample 0.2012g that a last step handles as in the counteracting tank with electronic balance; Measure 7mL nitric acid, 2mL oxydol and 4mL hydrofluorite (it is pure that the agents useful for same purity grade is top grade) and sample mix and vibration with liquid-transfering gun, avoid sample attached to clearing up on the tank skin.
Counteracting tank is installed on Mile Stone ETHOS 1 microwave dissolver, and the counteract appearance power setting is 1000W; Heating schedule is as shown in Figure 2; To clear up the digestion solution that obtains behind the 45min, to be placed on preset temperature be on 130 ℃ the heating plate; And add 3～5 perchloric acid digestion solution is caught up with acid; Catch up with about 6 hours of the time of acid, obtain small size leftover pieces circuit board extract, extract is settled to 25mL with 5% nitric acid.Digestion solution behind the constant volume is filtered through 0.45 μ m water pin type filter, obtain testing sample.
Testing sample is carried out qualitative and quantitative detection through PerkinElmer Optima 2100DV inductively coupled plasma emission spectrometer.Parameter setting is during mensuration: plasma power is 1300W; Carrier gas flux is 0.75L/min; The plasma flow amount is 15L/min; The secondary air amount is 0.2 L/min; The sample pulling speed is 1.5mL/min; Condensate temperature remains on 20 ℃; The dilution of 4% salpeter solution is as standard reserving solution; Make typical curve (0.5mg/L, 1mg/L and 10mg/L) with the standard model of variable concentrations gradient; Wavelength and intensity according to the characteristic spectral line of element to be measured are carried out qualitative and quantitative analysis to the metallic element in the sample.Because copper, tin and aluminium content are higher, need analyzing with instrument again behind the diluted sample.Analysis obtains the content of heavy metal in these circuit board processing leftover pieces and sees table 1.
Table 1
| Element term | Cd | As | Mn | Cr | Ni | Zn | Al | Pb | Sn | Cu |
| Content (mg/kg) | Do not detect | 65 | 59 | 35 | 92 | 288 | 27,140 | Do not detect | 65,147 | 282,243 |
Embodiment 2
To certain brand TV set circuit plate analysis of Japan, measure the wherein kind and the content of typical metal with the present invention.
Gather the TV set circuit plate as sample.Utilize heat gun to take off with covering the electric capacity, the resistance that contain on the circuit board; The circuit board that does not contain electric capacity, resistance is broken into diameter 2cm size with the scissors meal; With beater grinder that the further fine powder of coarse crushing sample is broken; The homogeneity of sample was collected the testing sample particulate at last when the broken sample afterwards of fine powder was repeated 3 inquartations with the assurance sampling.
Took by weighing TV set circuit plate sample 0.2020g that a last step handles as in the counteracting tank with electronic balance; Measure 7mL nitric acid, 2mL oxydol and 4mL hydrofluorite (it is pure that the agents useful for same purity grade is top grade) and sample mix and vibration with liquid-transfering gun, avoid sample attached to clearing up on the tank skin.
Counteracting tank is installed on Mile Stone ETHOS 1 microwave dissolver, and the counteract appearance power setting is 1000W; Heating schedule is as shown in Figure 2; To clear up the digestion solution that obtains behind the 45min, to be placed on preset temperature be on 130 ℃ the heating plate; And add 3～5 perchloric acid digestion solution is caught up with acid; Catch up with about 6 hours of the time of acid, obtain small size TV set circuit plate extract, with extract with 5% nitric acid constant volume to 25mL.Digestion solution behind the constant volume is filtered through 0.45 μ m water pin type filter, obtain testing sample.
Testing sample is carried out qualitative and quantitative detection through PerkinElmer Optima 2100DV inductively coupled plasma emission spectrometer.Parameter setting is during mensuration: plasma power is 1300W; Carrier gas flux is 0.75L/min; The plasma flow amount is 15L/min; The secondary air amount is 0.2 L/min; The sample pulling speed is 1.5mL/min; Condensate temperature remains on 20 ℃; With 4% salpeter solution dilution standard storing solution; Do typical curve (0.5mg/L, 1mg/L and 10mg/L) with the standard model of variable concentrations gradient; Wavelength and intensity according to the characteristic spectral line of element to be measured are carried out qualitative and quantitative analysis to the metallic element in the sample.Because copper, tin, aluminium and lead content are higher, need analyzing with instrument again behind the diluted sample.Analysis obtains the content results of typical metal in this circuit board and sees table 2.
Table 2
| Element term | Cd | As | Mn | Cr | Ni | Zn | Al | Pb | Sn | Cu |
| Content (mg/kg) | Do not detect | 35 | 16 | 174 | 367 | 202 | 25,219 | 12,751 | 108,819 | 46,156 |
Claims (3)
1. the analysis determining method of copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and tin in the discarded appliance circuit plate is characterized in that concrete steps are following:
(1) analytic sample preparation
Meal behind the waste printed circuit board excision electric capacity of gathering, the resistance electron device is broken into coarse grain or the sheet that diameter is 1～2cm size; Further coarse grain or sheet fine powder are broken into 50～100 purpose particulates again; Particulate is carried out inquartation repeatedly, obtain the circuit board testing sample;
(2) the circuit board sample clears up processing
A. circuit board Specimen eliminating pre-treatment: take by weighing the circuit board testing sample 0.2～0.5g that handles well through step (1); Put into the special-purpose counteracting tank of microwave dissolver; Add 10～20mL subsequently and clear up reagent; Mix to avoid the circuit board testing sample to be bonded at and clear up on the tank skin,, clear up lid on the bonnet adding the circuit board testing sample and clearing up counteracting tank behind the reagent and be placed in the fuming cupboard room temperature reaction 9-12 minute;
B. micro-wave digestion circuit board sample: the counteracting tank that contains the circuit board testing sample that step (A) makes is put into microwave dissolver, and the power of setting micro-wave digestion is 700～1000W; Digestion time is controlled at 30～40min; Clear up finish to treat that the counteracting tank temperature is reduced to room temperature after, take out counteracting tank;
(3) catch up with acid, constant volume to clearing up the back sample liquid
It is on 125-135 ℃ the electric hot plate that the counteracting tank that contains digestion solution that step (2) is obtained places preset temperature; Add several perchloric acid; Heating 4～8h obtains the small size digestion solution; It is that 2～5% nitric acid is settled to 25～50mL that the small size digestion solution that obtains is used volume fraction, and the digestion solution behind the constant volume is filtered through 0.45 μ m water pin type filter, and the digestion solution after the filtration is final testing sample solution;
(4) inductively coupled plasma emission spectrography is measured copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and the tin in the testing sample
The testing sample solution that step (3) is obtained adopts inductive coupling plasma emission spectrograph to carry out the qualitative and quantitative analysis of metal target, and the main analytical parameters that instrument is set is: plasma power is 1200～1500W; Carrier gas is a pure argon, and flow is 0.70～0.9L/min; The plasma flow amount is 15～18L/min; The secondary air amount is 0.2～0.3 L/min; The sample pulling speed is 1.5mL/min; Through analysis, confirm copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and 10 kinds of metallic elements of tin metallic element as key monitoring in the circuit board sample to dissimilar circuit boards in the discarded electric equipment products; According to the spectroscopic data between 180～800nm, analyze the accurate concentration that the spectral intensity of above-mentioned multiple element under characteristic spectral line obtains each element in the digestion solution; According to sampling amount in the digestion process, calculate the accurate content of copper in the circuit board, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and tin element again.
2. the analysis determining method of copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and tin in the discarded appliance circuit plate according to claim 1 is characterized in that the said reagent of clearing up is one to multiple kind in nitric acid, oxydol, hydrofluorite or the fluoboric acid.
3. the analysis determining method of copper, lead, nickel, cadmium, chromium, zinc, manganese, aluminium, arsenic and tin in the discarded appliance circuit plate according to claim 2; It is characterized in that the volume ratio of hydrofluorite, nitric acid and three kinds of reagent of oxydol is 4:7:2 when clearing up reagent employing hydrofluorite, nitric acid and oxydol.
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