CN106680066A - Method for analyzing metal elements in electronic waste - Google Patents
Method for analyzing metal elements in electronic waste Download PDFInfo
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- CN106680066A CN106680066A CN201611180506.0A CN201611180506A CN106680066A CN 106680066 A CN106680066 A CN 106680066A CN 201611180506 A CN201611180506 A CN 201611180506A CN 106680066 A CN106680066 A CN 106680066A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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Abstract
The invention provides a method for analyzing metal elements in electronic waste. The method comprises the following steps: performing aerobic roasting on pre-treated electronic waste to obtain a waste sample; taking the waste sample and dissolving the waste sample with acid, performing heating digestion with a first kind mixed acid, and performing cooling, filtration and constant volume setting to obtain a first kind metal ionic mixed solution; taking the waste sample and dissolving the waste sample with acid, carrying out a reaction with a second kind mixed acid, performing heating for evaporation, dissolving the residue with acid, and performing cooling, filtration and constant volume setting to obtain a second kind metal ionic mixed solution; taking the pre-treated electronic waste and dissolving the pre-treated electronic waste with acid, performing heating digestion with a third kind mixed acid, and performing cooling, filtration and constant volume setting to obtain a third kind metal ionic mixed solution; and measuring the content of metal elements in each metal ionic mixed solution. Through adoption of aerobic high-temperature treatment combining with heating digestion, to-be-measured metal elements are dissolved from the electronic waste, so that the content of metal ions in the electronic waste is accurately measured.
Description
Technical field
The invention belongs to analyze testing field, it is related to a kind of analysis method of metallic element, more particularly to a kind of electronics to give up
The analysis method of metallic element in gurry.
Background technology
Discarded circuit board is a class rich in metal and the considerably complicated exemplary electronic of the Nomenclature Composition and Structure of Complexes is useless in electron wastes
, because its contained metal species is more, easily there is spectral line disturbed condition in gurry, and also containing substantial amounts of Non-metallic components,
Accurate Determining on metal element content can produce influence, so such as being difficult to reach by single analysis process or single analysis method
The purpose of accurate analysis.
CN 104178629A reclaim the side of valuable metal in disclosing a kind of many metal dusts from waste electronic wiring board
Method, comprises the following steps：(1) leach：With many metal dusts of waste electronic wiring board as raw material, and it is solvent to original to use nitric acid
Material is leached, and infusion solution and tin mud are obtained through solid-liquor separation after Leach reaction；(2) except lead：Dilute sulphur is added to infusion solution
Acid carries out, except lead, after being separated by filtration, obtaining copper nitrate solution and lead sulfate precipitation；(3) it is electrolysed：Copper nitrate solution is electrolysed
Obtain metallic copper.
The method that CN 103981366A disclose the metal on a kind of recovery train plate, it is first to provide wiring board, wherein
Copper Foil is formed on wiring board, and goldleaf is formed on Copper Foil.Then, wiring board is placed in dissolve Copper Foil in acid solution,
So that goldleaf comes off from wiring board, and obtain copper ions solution.Afterwards, copper ions solution is filtered, to obtain goldleaf.
The above method has focused largely on recovery process flow to wherein precious metal etc. for the research of electron wastes
Aspect, lacks explicitly for metal in electron wastes and the qualitative and quantitative assay method of nonmetallic substance.Existing method
Mostly relatively simple acid Wet, it is not thorough to nonmetallic dissolving, remain more；Meanwhile, sample epoxy resin etc.
Organic principle has larger absorption to metal, ultimately results in the unreliable of analysis result.
The metal ingredient analysis of electron wastes is always the problem of electron wastes synthesis regeneration.Chen Hao et al.
(" analysis method of content of beary metal in printed circuit board (PCB) ", Tongji University's journal, the 12nd phase of volume 40, December in 2012) carries
Metal, the method for then carrying out metal analysis test in one kind micro-wave digestion dissolving waste printed circuit board are gone out.But, due to useless
Abandon the presence of cured epoxy resin in circuit board, its under the action of an acid can activity recovery, adsorbing metal ions, cause detection tie
It is really relatively low.
As can be seen here, metal ingredient has important meaning to the metal for reclaiming electron wastes in accurate analysis electron wastes
Justice, by metal ingredient in accurate analysis electron wastes, can bring directive significance for subsequent recovery process.
The content of the invention
For present in the assay method qualitative with nonmetallic substance and quantitative of metal in existing electron wastes to non-
Dissolving metal is not thorough, remains more, and each element is interfered, and the organic principle such as epoxy resin analysis result is caused compared with
The problems such as influenceing the analysis result that causes inaccurate greatly, the invention provides a kind of analysis side of metallic element in electron wastes
Method.The present invention can effectively by the metal to be measured in electron wastes by way of aerobic high-temperature process combined heat is cleared up
Element is dissolved out, and then the accurate metal ion content measured in electron wastes.
It is that, up to this purpose, the present invention uses following technical scheme：
The invention provides a kind of analysis method of metallic element in electron wastes, the described method comprises the following steps：
(1) electron wastes are carried out into aerobic roasting, obtains electron wastes sample；
(2) after taking the electron wastes sample acid dissolving that step (1) is obtained, add first kind nitration mixture to carry out heating and disappear
Solution, is filtered and constant volume after cooling, obtains first kind metal ion mixed liquor；
(3) after taking the electron wastes sample acid dissolving that step (1) is obtained, Equations of The Second Kind nitration mixture is added to be reacted, instead
Heating evaporation after should terminating, the residue for obtaining is obtained Equations of The Second Kind metal ion and is mixed with being cooled down after acid dissolving, being filtered and constant volume
Close liquid；
(4) after taking the pretreated electron wastes acid dissolving of step (1), add the 3rd class nitration mixture to carry out heating and disappear
Solution, is filtered and constant volume after cooling, obtains the 3rd metalloid Ar ion mixing liquid；
(5) detection first kind metal ion mixed liquor, Equations of The Second Kind metal ion mixed liquor and the 3rd metalloid Ar ion mixing
Metal element content in liquid.
Wherein, the state for having oxygen atmosphere to keep sufficient is ensured in step (1) the aerobic roasting, so that epoxy resin etc.
Organic principle is fully oxidized ashing.
The present invention is different for the property of different metal element, is leached using different acid, then using differing needles pair
The mixed acid of property is cleared up, and while the metallic element in ensuring electron wastes is leached completely, can make different gold
Category element enters in different metal ion mixed liquor, it is to avoid the analysis result that the test interference between various metals is caused is not
The phenomenon of stabilization, to ensure the accuracy of test result.
It is following as currently preferred technical scheme, but not as the present invention provide technical scheme limitation, pass through
Following technical scheme, can preferably reach and realize technical purpose of the invention and beneficial effect.
Used as currently preferred technical scheme, step (1) described electron wastes are discarded circuit board, and it can be computer
Mainboard, TV SKD or cell phone mainboard etc., it is not limited to the mainboard.
Preferably, step (1) described electron wastes are the electron wastes by pre-processing；
Preferably, the pretreatment is broken and screening.
Preferably, the powder size of step (1) electron wastes after pretreatment is 80 mesh~200 mesh, for example
80 mesh, 100 mesh, 120 mesh, 140 mesh, 160 mesh, 180 mesh or 200 mesh etc., it is not limited to cited numerical value, the numerical value model
Other unrequited numerical value are equally applicable in enclosing.
In the present invention, electron wastes are pre-processed to certain powder size, it is therefore intended that ensure the equal of sample
Even property, so that metal can sufficiently dissolution in end processing sequences.
Preferably, step (1) the aerobic roasting is carried out in Muffle furnace.
Preferably, the temperature of step (1) the aerobic roasting be 450 DEG C~850 DEG C, such as 450 DEG C, 470 DEG C, 500 DEG C,
530℃、550℃、570℃、600℃、630℃、650℃、670℃、700℃、730℃、750℃、770℃、800℃、830℃
Or 850 DEG C etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range, preferably
It is 600 DEG C~800 DEG C.
In the present invention, it is to destroy the organic principles such as epoxy resin that electron wastes are carried out with aerobic roasting purpose, makes electricity
The organic principles such as the epoxy resin in sub- discarded object can carry out sufficient aerobic ashing, with prevent incomplete combustion it is organic into
Divide and descend adsorbing metal ions under the action of an acid, the test result of metal ion in influence leachate.The roasting of the aerobic roasting
Burn temperature also has considerable influence to test result, if temperature is too low (400 DEG C of ＜), epoxy resin can be made to be converted into substantial amounts of carbon,
The metal ion of Ore Leaching is adsorbed, causes testing result relatively low；If temperature is too high (850 DEG C of ＞), can make part metals lose to
In flue gas, cause testing result relatively low.
Preferably, the time of step (1) the aerobic roasting is 1h~6h, such as 1h, 2h, 3h, 4h, 5h or 6h etc., but
It is not limited in other unrequited numerical value in cited numerical value, the number range equally applicable.
Used as currently preferred technical scheme, it with concentration is 15wt%~65wt% that step (2) the acid dissolving is
Nitric acid is dissolved, wherein the concentration of nitric acid can for 15wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt%,
45wt%, 50wt%, 55wt%, 60wt% or 65wt% etc., it is not limited to cited numerical value, in the number range its
His unrequited numerical value is equally applicable.
Preferably, the consumption of the nitric acid is：0.5g~10g electron wastes samples use 2mL~20mL concentration for
The nitric acid of 15wt%~65wt% is dissolved, and preferably uses 10mL concentration to be carried out for the nitric acid of 25wt%~40wt% molten
Solution.Wherein, the sampling amount of electron wastes sample can be for 0.5g, 1g, 2g, 3g, 4g, 5g, 6g, 7g, 8g, 9g or 10g etc., but simultaneously
It is not limited only to other unrequited numerical value in cited numerical value, the number range equally applicable；The addition of nitric acid can be
2mL, 4mL, 6mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL or 20mL etc., it is not limited to cited numerical value, should
Other unrequited numerical value are equally applicable in number range.
Preferably, step (2) the sour dissolution time is 0.5h~12h, such as 0.5h, 2h, 4h, 6h, 8h, 10h or 12h
Deng it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range.
Preferably, step (2) described acid is carried out in being dissolved in counteracting tank.
Preferably, the counteracting tank is polytetrafluoroethylene (PTFE) counteracting tank.
Used as currently preferred technical scheme, step (2) first kind nitration mixture includes：Concentration be 15wt%~
The chloroazotic acid of 35wt%, concentration are that the hydrofluoric acid and concentration of 25wt%~45wt% are the hydrogen peroxide of 15wt%~30wt%.
Wherein, the concentration of chloroazotic acid can for 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt%, 30wt%,
33wt% or 35wt% etc., it is not limited to other unrequited numerical value are equally fitted in cited numerical value, the number range
With；The concentration of hydrofluoric acid can for 25wt%, 27wt%, 30wt%, 33wt%, 35wt%, 37wt%, 40wt%, 43wt% or
45wt% etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；Hydrogen peroxide
Concentration can be for 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt% or 30wt% etc., it is not limited to institute
Other unrequited numerical value are equally applicable in the numerical value enumerated, the number range.
In the present invention, electron wastes sample is cleared up using first kind nitration mixture, it is therefore intended that by electron wastes
In metallic element Cu ions, Au ions, Pd ions, Ni ions, Fe ions and Zn ions leach.
Preferably, the volume ratio of nitric acid and hydrochloric acid is 1 in the chloroazotic acid:3.
Preferably, the consumption of the chloroazotic acid is：0.5g~10g electron wastes sample add 2mL~10mL concentration be
The chloroazotic acid of 15wt%~35wt%, wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 2g, 3g, 4g, 5g, 6g,
7g, 8g, 9g or 10g etc., it is not limited to other unrequited numerical value are equally fitted in cited numerical value, the number range
With；The addition of chloroazotic acid can be 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., it is not limited to cited
Numerical value, other unrequited numerical value are equally applicable in the number range.
Preferably, the consumption of the hydrofluoric acid is：0.5g~10g electron wastes sample add 0.5mL~5mL concentration be
The hydrofluoric acid of 25wt%~48wt%, wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 2g, 3g, 4g, 5g, 6g,
7g, 8g, 9g or 10g etc., it is not limited to other unrequited numerical value are equally fitted in cited numerical value, the number range
With；The addition of hydrofluoric acid can be 0.5mL, 1mL, 2mL, 3mL, 4mL or 5mL etc., it is not limited to cited numerical value, is somebody's turn to do
Other unrequited numerical value are equally applicable in number range.
Preferably, the consumption of the hydrogen peroxide is：0.5g~10g electron wastes sample adds 0.5mL~10mL concentration
Be the hydrogen peroxide of 15wt%~30wt%, wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 2g, 3g, 4g, 5g,
6g, 7g, 8g, 9g or 10g etc., it is not limited to other unrequited numerical value are same in cited numerical value, the number range
It is applicable；The addition of hydrogen peroxide can be for 0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., but simultaneously
It is not limited only to other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, the mode of addition first kind nitration mixture is in step (2)：It is 15wt%~35wt%'s to sequentially add concentration
Chloroazotic acid, concentration are the hydrogen peroxide of 15wt%~30wt% for the hydrofluoric acid and concentration of 25wt%~48wt%.
Used as currently preferred technical scheme, step (2) heating is cleared up and is carried out in an oven.
Preferably, step (2) temperature cleared up of heating is 80 DEG C~200 DEG C, such as 80 DEG C, 100 DEG C, 120 DEG C,
140 DEG C, 160 DEG C, 180 DEG C or 200 DEG C etc., it is not limited to other are unrequited in cited numerical value, the number range
Numerical value is equally applicable, preferably 100 DEG C~150 DEG C.
In the present invention, the temperature cleared up of heating is too low (80 DEG C of ＜), and leaching can be made insufficient, in making electron wastes
The original leaching of part metals thoroughly, does not influence the accuracy of late detection；The temperature that heating is cleared up is too high (200 DEG C of ＞), can make
Solution boiling is violent, and solution evaporation is too fast, and Partial Elements may volatilize with steam, the accuracy of same influence late detection.
Preferably, step (2) is described heats time for clearing up for 2h~6h, such as 2h, 3h, 4h, 5h or 6h etc., but not
It is only limitted to other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, step (2) constant volume carries out constant volume with the chloroazotic acid that concentration is 5wt%~35wt%, wherein chloroazotic acid
Concentration can for 5wt%, 7wt%, 10wt%, 13wt%, 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt%,
30wt%, 33wt% or 35wt% etc., it is not limited to other unrequited numerical value in cited numerical value, the number range
It is equally applicable.
Preferably, in step (2) first kind metal ion mixed liquor comprising Cu ions, Au ions, Pd ions, Ni from
Son, Fe ions and Zn ions.
Used as currently preferred technical scheme, it with concentration is 15wt%~65wt% that acid dissolving described in step (3) is
Nitric acid dissolved, wherein the concentration of nitric acid can for 15wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt%,
45wt%, 50wt%, 55wt%, 60wt% or 65wt% etc., it is not limited to cited numerical value, in the number range its
His unrequited numerical value is equally applicable.
Preferably, the consumption of the nitric acid is：0.5g~20g electron wastes samples use 3mL~10mL concentration for
The nitric acid of 15wt%~65wt% is dissolved, it is preferred to use 5mL concentration is dissolved for the nitric acid of 30wt%~45wt%.Its
In, the sampling amount of electron wastes sample can be 1g, 3g, 5g, 7g, 10g, 13g, 15g, 17g or 20g etc., it is not limited to
Other unrequited numerical value are equally applicable in cited numerical value, the number range；The consumption of the nitric acid can for 3mL, 4mL,
5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., it is not limited to other are unrequited in cited numerical value, the number range
Numerical value is equally applicable.
Preferably, step (3) it is described acid dissolving time be 0.5h~2h, such as 0.5h, 0.7h, 1h, 1.3h, 1.5h,
1.7h or 2h etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range.
Preferably, step (3) described acid is carried out in being dissolved in beaker.
Preferably, the beaker is polytetrafluoroethylene beaker.
Used as currently preferred technical scheme, step (3) the Equations of The Second Kind nitration mixture includes：Concentration be 15wt%~
The nitric acid of 65wt%, concentration are the sulfuric acid of 50wt%~98wt%, concentration for the hydrofluoric acid and concentration of 15wt%~30wt% are
The concentration of the perchloric acid of 36wt%~72wt%, wherein nitric acid can for 15wt%, 20wt%, 25wt%, 30wt%, 35wt%,
40wt%, 45wt%, 50wt%, 55wt%, 60wt% or 65wt% etc., it is not limited to cited numerical value, the numerical value
In the range of other unrequited numerical value it is equally applicable；The concentration of sulfuric acid can for 50wt%, 55wt%, 60wt%, 65wt%,
70wt%, 75wt%, 80wt%, 85wt%, 90wt%, 95wt% or 98wt% etc., it is not limited to cited numerical value,
Other unrequited numerical value are equally applicable in the number range；The concentration of hydrofluoric acid can for 15wt%, 17wt%, 20wt%,
23wt%, 25wt%, 27wt% or 30wt% etc., it is not limited to other are not arranged in cited numerical value, the number range
The numerical value of act is equally applicable；The concentration of perchloric acid can for 36wt%, 40wt%, 44wt%, 46wt%, 50wt%, 54wt%,
56wt%, 60wt%, 64wt%, 66wt%, 70wt% or 72wt% etc., it is not limited to cited numerical value, the numerical value
In the range of other unrequited numerical value it is equally applicable.
In the present invention, electron wastes sample is cleared up using Equations of The Second Kind nitration mixture, it is therefore intended that by electron wastes
In metallic element Cu ions, Au ions, Ag ions, Pd ions, Ni ions, Fe ions and Zn ions leach.
Preferably, the consumption of described nitric acid is：0.5g~20g electron wastes sample add 5mL~20mL concentration be
The nitric acid of 15wt%~65wt%.Wherein, the sampling amount of electron wastes sample can for 1g, 3g, 5g, 7g, 10g, 13g, 15g,
17g or 20g etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；It is described
The addition of nitric acid can for 5mL, 7mL, 10mL, 13mL, 15mL, 17mL or 20mL etc., it is not limited to cited numerical value,
Other unrequited numerical value are equally applicable in the number range.
Preferably, the consumption of the sulfuric acid is：0.5g~20g electron wastes sample add 0.5mL~10mL concentration be
The sulfuric acid of 50wt%~98wt%.Wherein, the sampling amount of electron wastes sample can for 1g, 3g, 5g, 7g, 10g, 13g, 15g,
17g or 20g etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；Sulfuric acid
Addition can be for 0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., it is not limited to institute
Other unrequited numerical value are equally applicable in the numerical value enumerated, the number range.
Preferably, the consumption of the hydrofluoric acid is：0.5g~20g electron wastes sample adds 0.5mL~20mL concentration
It is the hydrofluoric acid of 15wt%~30wt%；Wherein, the sampling amount of electron wastes sample can for 1g, 3g, 5g, 7g, 10g, 13g,
15g, 17g or 20g etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；
The addition of hydrofluoric acid can for 0.5mL, 2mL, 4mL, 6mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL or 20mL etc., but
It is not limited in other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, the consumption of the perchloric acid is：0.5g~20g electron wastes sample adds 0.5mL~10mL concentration
It is the perchloric acid of 36wt%~72wt%；Wherein, the sampling amount of electron wastes sample can for 1g, 3g, 5g, 7g, 10g, 13g,
15g, 17g or 20g etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；
The addition of perchloric acid can be for 0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., but simultaneously not only
It is limited to other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, the mode of addition Equations of The Second Kind nitration mixture is in step (3)：Concentration is sequentially added in solution after being dissolved to acid
Nitric acid, the hydrogen fluorine that the sulfuric acid and concentration that concentration is 50wt%~98wt% are 25wt%~45wt% for 15wt%~65wt%
Acid carries out first set reaction, and addition concentration is 36wt%~72wt%'s after first set reaction terminates rear heating evaporation to wet salt shape
Perchloric acid carries out the second secondary response.
In the present invention, the perchloric acid added in step (3) can provide high oxidative and highly acid for reaction system
Environment, accelerates the dissolving of insoluble metal, the particularly dissolving of noble metal.
Preferably, it is 80 DEG C that the heating evaporation temperature in heating evaporation to wet salt shape is carried out after the first set reaction terminates
~150 DEG C, such as 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C etc., it is not limited to listed
Other unrequited numerical value are equally applicable in the numerical value of act, the number range.
Preferably, it is 80 DEG C~150 DEG C that step (3) reaction carries out the temperature of heating evaporation after terminating, such as 80 DEG C,
90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C etc., it is not limited to cited numerical value, the numerical value model
Other unrequited numerical value are equally applicable in enclosing.Now heating evaporation is to the closely dry state of solution.
Preferably, acid used in step (3) the residue acid dissolving is the nitric acid that concentration is 20wt%~30wt%,
Its concentration can be 20wt%, 22wt%, 24wt%, 26wt%, 28wt% or 30wt% etc., it is not limited to cited number
Other unrequited numerical value are equally applicable in value, the number range, and preferably concentration is the nitric acid of 30wt%.
Preferably, step (3) described constant volume is with the nitric acid constant volume that concentration is 5wt%~35wt%, wherein concentration of nitric acid
Can for 5wt%, 7wt%, 10wt%, 13wt%, 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt%,
30wt%, 33wt% or 35wt% etc., it is not limited to other unrequited numerical value in cited numerical value, the number range
It is equally applicable.
Preferably, in step (3) the Equations of The Second Kind metal ion mixed liquor comprising Cu ions, Au ions, Ag ions, Pd from
Son, Ni ions, Fe ions and Zn ions.
Used as currently preferred technical scheme, it with concentration is 10wt%~30wt% that acid dissolving described in step (4) is
Hydrochloric acid dissolved, the concentration of the hydrochloric acid can for 10wt%, 13wt%, 15wt%, 17wt%, 20wt%, 23wt%,
25wt%, 27wt% or 30wt% etc., it is not limited to other unrequited numerical value in cited numerical value, the number range
It is equally applicable.
Preferably, the consumption of the hydrochloric acid is：0.5g~20g electron wastes samples use 2mL~20mL concentration for
The hydrochloric acid of 10wt%~30wt% is dissolved, it is preferred to use 10mL concentration is dissolved for the hydrochloric acid of 10wt%~30wt%.
Wherein, the sampling amount of electron wastes sample can be for 0.5g, 1g, 3g, 5g, 7g, 10g, 13g, 15g, 17g or 20g etc., but not
It is only limitted to other unrequited numerical value in cited numerical value, the number range equally applicable；The addition of hydrochloric acid can for 2mL,
4mL, 6mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL or 20mL etc., it is not limited to cited numerical value, the numerical value
In the range of other unrequited numerical value it is equally applicable.
Preferably, the time of step (4) the acid dissolving is 2h~12h, such as 2h, 4h, 6h, 8h, 10h or 12h etc., but
It is not limited in other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, step (4) described acid is carried out in being dissolved in counteracting tank.
Preferably, the counteracting tank is polytetrafluoroethylene (PTFE) counteracting tank.
Used as currently preferred technical scheme, step (4) the 3rd class nitration mixture includes：Concentration be 15wt%~
The hydrofluoric acid of 30wt%, concentration are the hydrogen peroxide that the hydrochloric acid and concentration of 10wt%~30wt% are 15wt%~30wt%, wherein
The concentration of the hydrofluoric acid can be for 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt% or 30wt% etc., but simultaneously
It is not limited only to other unrequited numerical value in cited numerical value, the number range equally applicable；The concentration of hydrochloric acid can be
10wt%, 13wt%, 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt% or 30wt% etc., but simultaneously not only limit
It is equally applicable in other unrequited numerical value in cited numerical value, the number range；The concentration of hydrogen peroxide can for 15wt%,
17wt%, 20wt%, 23wt%, 25wt%, 27wt% or 30wt% etc., it is not limited to cited numerical value, the numerical value
In the range of other unrequited numerical value it is equally applicable.
In the present invention, electron wastes sample is cleared up using the 3rd class nitration mixture, it is therefore intended that by electron wastes
In metallic element Cu ions, Pb ions, Sn ions, Ni ions, Fe ions and Zn ions leach.
Preferably, the consumption of the hydrofluoric acid is：0.5g~20g electron wastes sample adds 0.5mL~10mL concentration
It is the hydrofluoric acid of 15wt%~30wt%.Wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 3g, 5g, 7g, 10g,
13g, 15g, 17g or 20g etc., it is not limited to other unrequited numerical value are same in cited numerical value, the number range
It is applicable；The addition of hydrofluoric acid can be for 0.5mL, 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., but simultaneously
It is not limited only to other unrequited numerical value in cited numerical value, the number range equally applicable.
Preferably, the consumption of the hydrochloric acid is：0.5g~20g electron wastes sample add 2mL~20mL concentration be
The hydrochloric acid of 10wt%~30wt%.Wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 3g, 5g, 7g, 10g, 13g,
15g, 17g or 20g etc., it is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range；
The addition of hydrochloric acid can for 2mL, 4mL, 6mL, 8mL, 10mL, 12mL, 14mL, 16mL, 18mL or 20mL etc., it is not limited to
Other unrequited numerical value are equally applicable in cited numerical value, the number range.
Preferably, the consumption of the hydrogen peroxide is：0.5g~20g electron wastes sample add 1mL~10mL concentration be
The hydrogen peroxide of 15wt%~30wt%；Wherein, the sampling amount of electron wastes sample can for 0.5g, 1g, 3g, 5g, 7g, 10g,
13g, 15g, 17g or 20g etc., it is not limited to other unrequited numerical value are same in cited numerical value, the number range
It is applicable；The addition of hydrogen peroxide can be 1mL, 2mL, 3mL, 4mL, 5mL, 6mL, 7mL, 8mL, 9mL or 10mL etc., but simultaneously not only limit
It is equally applicable in other unrequited numerical value in cited numerical value, the number range.
Preferably, the mode of the 3rd class nitration mixture of step (4) addition is：Concentration is sequentially added for 15wt%~30wt%
Hydrofluoric acid, concentration for 10wt%~30wt% hydrochloric acid and concentration for 15wt%~30wt% hydrogen peroxide.
Preferably, reaction is cleared up in step (4) heating is carried out in an oven.
Preferably, step (4) is described heats that to clear up the reaction temperature of reaction be 80 DEG C~200 DEG C, such as 80 DEG C, 100 DEG C,
120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C or 200 DEG C etc., it is not limited to cited numerical value, in the number range, other are not
The numerical value enumerated is equally applicable, preferably 100 DEG C~150 DEG C.
In the present invention, the temperature cleared up of heating is too low (80 DEG C of ＜), and leaching can be made insufficient, in making electron wastes
The original leaching of part metals thoroughly, does not influence the accuracy of late detection；The temperature that heating is cleared up is too high (200 DEG C of ＞), can make
Solution boiling is violent, and solution evaporation is too fast, and Partial Elements may volatilize with steam, the accuracy of same influence late detection.
Preferably, the described heating of step (4) clears up reaction time of reaction for 2h~5h, such as 2h, 3h, 4h or 5h etc.,
It is not limited to other unrequited numerical value are equally applicable in cited numerical value, the number range.
Preferably, step (4) described constant volume is with the hydrochloric acid constant volume that concentration is 5wt%~35wt%, wherein concentration of hydrochloric acid
Can for 5wt%, 7wt%, 10wt%, 13wt%, 15wt%, 17wt%, 20wt%, 23wt%, 25wt%, 27wt%,
30wt%, 33wt% or 35wt% etc., it is not limited to other unrequited numerical value in cited numerical value, the number range
It is equally applicable.
Preferably, in step (4) the 3rd metalloid Ar ion mixing liquid comprising Cu ions, Pb ions, Sn ions, Ni from
Son, Fe ions and Zn ions.
Preferably, the mode of step (5) the detection metal element content is ICP-OES detections.
Used as currently preferred technical scheme, methods described is further comprised the following steps：
(1) electron wastes that powder size after pretreatment is 80 mesh~200 mesh are entered at 600 DEG C~800 DEG C
The aerobic roasting 1h~6h of row, obtains electron wastes sample；
(2) it is 25wt%~40wt%'s to take the electron wastes sample 5mL concentration that 0.5g~10g steps (1) obtain
After nitric acid dissolving 0.5h~12h, to add 2mL~10mL concentration successively be the chloroazotic acid of 15wt%~35wt%, 0.5mL~5mL is dense
Spend the hydrofluoric acid and 0.5mL~10mL concentration for 25wt%~48wt% for 15wt%~30wt% hydrogen peroxide in 120 DEG C~
150 DEG C carry out heating and clear up 2h~6h, are filtered after cooling and with the chloroazotic acid constant volume that concentration is 5wt%~35wt%, obtained
First kind metal ion mixed liquor comprising Cu ions, Au ions, Pd ions, Ni ions, Fe ions and Zn ions；
(3) nitre that the electron wastes sample 5mL concentration that 1g~20g steps (1) obtain is 30wt%~45wt% is taken
After acid dissolving 0.5h~2h, nitric acid, 0.5mL~10mL concentration that 5mL~20mL concentration is 15wt%~65wt% are sequentially added
For the sulfuric acid and 0.5mL~20mL concentration of 50wt%~98wt% are anti-for the hydrofluoric acid of 25wt%~30wt% carries out first time
Should, it is 36wt% that first set reaction terminates after 0.5mL~10mL concentration is added after 80 DEG C~150 DEG C heating evaporation to wet salt shapes
The perchloric acid of~72wt% carries out the second secondary response, and reaction terminates after 80 DEG C~150 DEG C heating evaporations, and the residue for obtaining is with dense
Spend after the nitric acid dissolving for 30wt% and cooled down, filtered and with the nitric acid constant volume that concentration is 5wt%~35wt%, comprising
The Equations of The Second Kind metal ion mixed liquor of Cu ions, Au ions, Ag ions, Pd ions, Ni ions, Fe ions and Zn ions；
(4) it is 10wt%~30wt%'s to take the pretreated electron wastes 10mL concentration of 0.5g~20g steps (1)
After dissolving with hydrochloric acid 2h~2h, it is the hydrofluoric acid of 25wt%~45wt%, 2mL~20mL dense to sequentially add 0.5mL~10mL concentration
It is the hydrogen peroxide of 15wt%~30wt% in 100 DEG C~150 DEG C to spend the hydrochloric acid and 1mL~10mL concentration for 10wt%~30wt%
Carry out heating and clear up 2h~5h, filtered after cooling and with the hydrochloric acid constant volume that concentration is 5wt%~35wt%, obtained comprising Cu
3rd metalloid Ar ion mixing liquid of ion, Pb ions, Sn ions, Ni ions, Fe ions and Zn ions；
(5) using ICP-OES detection first kind metal ions mixed liquor, Equations of The Second Kind metal ion mixed liquor and the 3rd eka-gold
Metal element content in category Ar ion mixing liquid.
Compared with prior art, the invention has the advantages that：
The present invention breaks the organic principles such as the epoxy resin in words electron wastes by aerobic high-temperature process, and for difference
Metallic element processed using different targetedly mixed acid, can be effectively first by the metal to be measured in electron wastes
Element is dissolved out, and then the accurate content for measuring metallic element in electron wastes, the present invention for common metal such as Cu, Ni,
The relative error of the testing result of Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is respectively less than ± 1%, and result has preferably reproduction
Property.
Brief description of the drawings
Fig. 1 is the process chart of the analysis method of metallic element in electron wastes of the present invention.
Specific embodiment
For the present invention is better described, technical scheme is readily appreciated, below to the present invention further specifically
It is bright.But following embodiments is only simple example of the invention, the scope of the present invention is not represented or limits, this
Invention protection domain is defined by claims.
As indicated with 1, specific embodiment of the invention part provides a kind of analysis method of metallic element in electron wastes,
The described method comprises the following steps：
(1) electron wastes are carried out into aerobic roasting, obtains electron wastes sample；
(2) after taking the electron wastes sample acid dissolving that step (1) is obtained, add first kind nitration mixture to carry out heating and disappear
Solution, is filtered and constant volume after cooling, obtains first kind metal ion mixed liquor；
(3) after taking the electron wastes sample acid dissolving that step (1) is obtained, Equations of The Second Kind nitration mixture is added to be reacted, instead
Heating evaporation after should terminating, the residue for obtaining is obtained Equations of The Second Kind metal ion and is mixed with being cooled down after acid dissolving, being filtered and constant volume
Close liquid；
(4) after taking the pretreated electron wastes acid dissolving of step (1), add the 3rd class nitration mixture to carry out heating and disappear
Solution, is filtered and constant volume after cooling, obtains the 3rd metalloid Ar ion mixing liquid；
(5) detection first kind metal ion mixed liquor, Equations of The Second Kind metal ion mixed liquor and the 3rd metalloid Ar ion mixing
Metal element content in liquid.
It is below present invention typical case but non-limiting example：
Embodiment 1：
A kind of analysis method of metallic element in computer main board is present embodiments provided, be the described method comprises the following steps：
(1) by computer main board through Mechanical Crushing and screening after, its powder size is maintained between 80 mesh；
(2) step (1) is placed in high temperature Muffle furnace through the computer main board after Mechanical Crushing and screening, is being passed through abundant oxygen
650 DEG C of temperature in Muffle furnace is kept under atmosphere, 6h is incubated, computer main board sample is obtained；
(3) the computer main board sample in 10g steps (2) is chosen, adds concentration to be 65wt% in polytetrafluoroethylene (PTFE) counteracting tank
Concentrated nitric acid 20mL stand 2h, sequentially add HNO3It is 1 with HCl volume ratios:3 concentration for 35wt% dense chloroazotic acid 10mL,
Concentration is the hydrogen peroxide 10mL of 30wt% for the hydrofluoric acid 5mL and concentration of 45wt%, in an oven after 2h is cleared up in 80 DEG C of heating,
Cooling is stood after Specimen eliminating is complete；Dilute chloroazotic acid that rear solution example concentration is 5wt% is cleared up to filter and be settled to capacity
In bottle, 1. metalloid Ar ion mixing liquid is marked；
(4) the computer main board sample chosen in 0.5g steps (2) is placed in polytetrafluoroethylene beaker, plus 10mL concentration is
The concentrated nitric acid dissolving 2h of 65wt%, the concentrated nitric acid 5mL that concentration is 65wt% is sequentially added according to sequencing, and concentration is 98wt%
Sulfuric acid 1mL, concentration is the hydrofluoric acid 1mL of 30wt%, after after vigorous reaction stopping, being steamed to wet salt shape in 120 DEG C of heating, is continued
It is the HClO of 72wt% to add 5mL concentration4Acid, continue to steam after 80 DEG C of heating vigorous reactions to it is near it is dry and cold but after, add concentration
The salpeter solution dissolved residue of 35wt%, stands cooling, clears up the dust technology that rear solution example concentration is 5wt% and filters and determine
Hold into volumetric flask, mark 2. metalloid Ar ion mixing liquid；
(5) take through the computer main board after Mechanical Crushing and screening in 20g steps (1), in polytetrafluoroethylene (PTFE) counteracting tank plus
Concentration stands 6h for the concentrated hydrochloric acid 20mL of 30wt%, then it is the hydrofluoric acid 5mL of 30wt% that successively order adds concentration, and concentration is
The concentrated hydrochloric acid 5mL and concentration of 30wt% are the hydrogen peroxide 10mL of 30wt%, are placed in baking oven at a temperature of 80 DEG C, and heating 2h is carried out
Clear up, cooling is stood after Specimen eliminating is complete.It is that 5wt% watery hydrochloric acid is filtered and is settled to appearance to clear up rear solution example concentration
In measuring bottle, 3. metalloid Ar ion mixing liquid is marked；
(6) will 1. 2. 3. metalloid Ar ion mixing liquid be detected wherein using ICP-OES in the range of specific spectral line, respectively
Different metal constituent content.
Wherein, the relative error of the testing result of common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is small
In ± 1%, and result has preferable reappearance.
Embodiment 2：
A kind of analysis method of metallic element in TV SKD is present embodiments provided, methods described includes following step
Suddenly：
(1) by TV SKD through Mechanical Crushing and screening after, its powder size is maintained between 120 mesh；
(2) step (1) is placed in high temperature Muffle furnace through the TV SKD after Mechanical Crushing and screening, is being passed through fully
Under oxygen atmosphere, 450 DEG C of temperature in Muffle furnace is kept, be incubated 1h, obtain TV SKD sample；
(3) the TV SKD sample in 0.5g steps (2) is chosen, in polytetrafluoroethylene (PTFE) counteracting tank plus concentration is
The concentrated nitric acid 5mL of 65wt% stands 0.5h, sequentially adds HNO3It is 1 with HCl volume ratios:3 concentration are the dense chloroazotic acid of 30wt%
5mL, concentration is the hydrogen peroxide 5mL of 30wt% for the hydrofluoric acid 0.5mL and concentration of 45wt%, and 150 DEG C of heating in an oven are cleared up
After 6h, cooling is stood after Specimen eliminating is complete；Dilute chloroazotic acid that rear solution example concentration is 5wt% is cleared up to filter and be settled to appearance
In measuring bottle, 1. metalloid Ar ion mixing liquid is marked.
(4) the TV SKD sample chosen in 10g steps (2) is placed in polytetrafluoroethylene beaker, plus 5mL concentration is
The concentrated nitric acid dissolving 2h of 65wt%, it is that the concentrated nitric acid 10mL of 65wt%, concentration are to sequentially add concentration according still further to sequencing
The sulfuric acid 5mL and concentration of 98wt% are the hydrofluoric acid 20mL of 30wt%, after after vigorous reaction stopping, being steamed to wet in 150 DEG C of heating
Salt shape, continuously adds the HClO that 10mL concentration is 72wt%4, continue to steam after 100 DEG C of heating vigorous reactions to it is near it is dry and cold but after, plus
Enter the salpeter solution dissolved residue of concentration 35wt%, stand cooling, clear up the dust technology mistake that rear solution example concentration is 5wt%
Filter, be settled in volumetric flask, mark 2. metalloid Ar ion mixing liquid；
(5) through the TV SKD after Mechanical Crushing and screening in taking in 0.5g steps (1), in polytetrafluoroethylene (PTFE) counteracting tank
In plus concentration for 30wt% concentrated hydrochloric acid 10mL stand 12h, then successively order add concentration for 30wt% hydrofluoric acid 2mL,
Concentration is the hydrogen peroxide 5mL of 30wt% for the concentrated hydrochloric acid 2mL and concentration of 30wt%, is placed in baking oven at a temperature of 150 DEG C, is heated
5h is cleared up, and cooling is stood after Specimen eliminating is complete, is cleared up the watery hydrochloric acid that rear solution example concentration is 5wt% and is filtered simultaneously
It is settled in volumetric flask, marks 3. metalloid Ar ion mixing liquid.
(6) will 1. 2. 3. metalloid Ar ion mixing liquid be detected wherein using ICP-OES in the range of specific spectral line, respectively
Different metal constituent content.
Wherein, the relative error of the testing result of common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is small
In ± 1%, and result has preferable reappearance.
Embodiment 3：
A kind of analysis method of metallic element in cell phone mainboard is present embodiments provided, be the described method comprises the following steps：
(1) by cell phone mainboard through Mechanical Crushing and screening after, its powder size is maintained between 200 mesh；
(2) step (1) is placed in high temperature Muffle furnace through the cell phone mainboard after Mechanical Crushing and screening, is being passed through abundant oxygen
Under atmosphere, 850 DEG C of temperature in Muffle furnace is kept, be incubated 3h, obtain cell phone mainboard sample；
(3) the cell phone mainboard sample in 5g steps (2) is chosen, adds concentration to be 65wt%'s in polytetrafluoroethylene (PTFE) counteracting tank
Concentrated nitric acid 10mL stands 12h, sequentially adds HNO3It is 1 with HCl volume ratios:3 concentration is the dense chloroazotic acid 2mL, dense of 30wt%
Spend for the hydrofluoric acid 0.5mL and concentration of 45wt% are the hydrogen peroxide 5mL of 30wt%, after 4h is cleared up in 200 DEG C of heating in an oven, treat
Specimen eliminating stands cooling afterwards completely, clears up dilute chloroazotic acid that rear solution example concentration is 35wt% and filters, is settled to volumetric flask
In, mark 1. metalloid Ar ion mixing liquid；
(4) the cell phone mainboard sample chosen in 20g steps (2) is placed in polytetrafluoroethylene beaker, plus 5mL concentration is
The concentrated nitric acid dissolving 0.5h of 65wt%, it is that the concentrated nitric acid 20mL of 65wt%, concentration are to sequentially add concentration according still further to sequencing
The sulfuric acid 10mL and concentration of 98wt% are the hydrofluoric acid 10mL of 45wt%, after after vigorous reaction stopping, being steamed to wet in 150 DEG C of heating
Salt shape, continuously adds the HClO that 10mL concentration is 72wt%4, continue to steam after 80 DEG C of heating vigorous reactions to it is near it is dry and cold but after, plus
Enter the salpeter solution dissolved residue that concentration is 35wt%, stand cooling, clear up the dust technology that rear solution example concentration is 5wt%
Filter, be settled in volumetric flask, mark 2. metalloid Ar ion mixing liquid；
(5) take in 5g steps (1) through the cell phone mainboard after Mechanical Crushing and screening, the enriching in polytetrafluoroethylene (PTFE) counteracting tank
Spend for the concentrated hydrochloric acid 2mL of 30wt% stands 2h, then successively order adds the concentration to be for the hydrofluoric acid 0.5mL of 30wt%, concentration
The concentrated hydrochloric acid 8mL and concentration of 30wt% are the hydrogen peroxide 2mL of 30wt%, are placed in baking oven at a temperature of 200 DEG C, and heating 5h is carried out
Clear up, cooling is stood after Specimen eliminating is complete, clear up the watery hydrochloric acid that rear solution example concentration is 5wt% and filter, be settled to
In volumetric flask, 3. metalloid Ar ion mixing liquid is marked.
(6) will 1. 2. 3. metalloid Ar ion mixing liquid be detected wherein using ICP-OES in the range of specific spectral line, respectively
Different metal constituent content.
Wherein, the relative error of the testing result of common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is small
In ± 1%, and result has preferable reappearance.
Embodiment 4：
A kind of analysis method of metallic element in computer main board is present embodiments provided, be the described method comprises the following steps：
(1) it is identical with step (1) in embodiment 1；
(2) it is identical with step (2) in embodiment 1；
(3) except adding concentration to stand 6h for the concentrated nitric acid 2mL of 65wt% in polytetrafluoroethylene (PTFE) counteracting tank, sequentially add
HNO3It is 1 with HCl volume ratios:Dense chloroazotic acid 10mL, hydrofluoric acid 3mL and concentration that concentration be 45wt% of 3 concentration for 30wt%
Outside for the hydrogen peroxide 0.5mL of 30wt%, other processes are identical with step (3) in embodiment 1；
(4) the computer main board sample chosen in 0.5g steps (2) is placed in polytetrafluoroethylene beaker, plus 3mL concentration is
The concentrated nitric acid dissolving 1h of 65wt%, the concentrated nitric acid 5mL that concentration is 65wt% is sequentially added according to sequencing, and concentration is 98wt%
Sulfuric acid 0.5mL, concentration for 30wt% hydrofluoric acid 0.5mL, after vigorous reaction stopping after, in 80 DEG C heating steam to wet salt shape,
Continuously add the HClO that 0.5mL concentration is 72wt%4Acid, continue to steam after 150 DEG C of heating vigorous reactions to it is near it is dry and cold but after, add
The salpeter solution dissolved residue of concentration 20wt%, stands cooling, clears up the dust technology mistake that rear solution example concentration is 25wt%
Filter and be settled in volumetric flask, mark 2. metalloid Ar ion mixing liquid；
(5) it is the hydrofluoric acid 10mL of 72wt% except successively order adds concentration, concentration is the concentrated hydrochloric acid of 30wt%
20mL and concentration are the hydrogen peroxide 1mL of 30wt%, are filtered with the watery hydrochloric acid that concentration is 35wt% and are settled to volumetric flask at home and abroad, its
His process is identical with step (5) in embodiment 1；
(6) it is identical with step (6) in embodiment 1；
Wherein, the relative error of the testing result of common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is small
In ± 1%, and result has preferable reappearance.
Comparative example 1：
This comparative example provides a kind of analysis method of metallic element in computer main board, and methods described is not except carrying out step
(2) (aerobic roasting is not carried out), unclassified stores consumption is in the same manner as in Example 1 with preparation process outward.
Will 1. 2. 3. metalloid Ar ion mixing liquid be detected wherein not using ICP-OES in the range of specific spectral line, respectively
The relative error of the testing result of same metal element content, common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc. is
± 1%.
The 1. 2. 3. metal ion in metalloid Ar ion mixing liquid for obtaining is leached in testing example 1 and comparative example 1 respectively
Leaching rate, its result is as shown in table 1-3.
Table 1：1. metalloid Ar ion mixing immersion extracting rate result
| Element | Cu | Ni | Fe | Zn | Au | Pd |
| Embodiment 1 | 100% | 99.9% | 99.9% | 100% | 99.8% | 80.0% |
| Comparative example 1 | 99.5% | 99.1% | 99.3% | 100% | 97.0% | 98.0% |
As it can be seen from table 1 higher by most 1. metalloid ion leaching rate after high-temperature roasting, test result compared with
Accurately, but except Pd elements, it is primarily due to be oxidized to PdO by Pd after high-temperature roasting, the oxide of palladium is molten in acid
Solution is difficult, leaches not thoroughly, therefore the method is not suitable for the test of palladium in 1. metalloid ion.
Table 2：2. metalloid Ar ion mixing immersion extracting rate result
From table 2 it can be seen that higher by most 2. metalloid ion leaching rate after high-temperature roasting, test result compared with
Accurately, but except Ag elements, it is primarily due to form halogenation by the halogen in part Ag after high-temperature roasting and wiring board
Silver-colored (AgX, X=F, Cl, Br, I), the halide of silver dissolves difficulty in acid, leaches not thoroughly, therefore the method is not suitable for 2. class
The test of palladium in metal ion.
Table 3：3. metalloid Ar ion mixing immersion extracting rate result
| Element | Cu | Ni | Fe | Zn | Pb | Sn |
| Embodiment 1 | 100% | 99.9% | 98.9% | 99.8% | 76.8% | 83.2% |
| Comparative example 1 | 99.3% | 99.2% | 98.4% | 100% | 99.6% | 99.7% |
From table 3 it can be seen that higher by most 3. metalloid ion leaching rate after high-temperature roasting, test result compared with
Accurately, but except Pb and Sn elements, the high-temperature calcination process volatile loss of Pb and Sn is primarily due to, causes element loss,
Therefore the method is not suitable for the test of Pb and Sn in 3. metalloid ion.
The result of integrated embodiment 1-4 and comparative example 1 can be seen that the present invention and be given up by aerobic high-temperature process destruction electronics
The organic principles such as the epoxy resin in gurry, and used at different targetedly mixed acid for different metallic elements
, effectively can be dissolved out for the metallic element to be measured in electron wastes by reason, and then accurately measure gold in electron wastes
Belong to the content of element, the phase of testing result of the present invention for common metal such as Cu, Ni, Fe, Zn, Au, Pd, Pb, Sn and Ag etc.
± 1% is respectively less than to error, and result has preferable reappearance.
Applicant states that the present invention illustrates method detailed of the invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. in a kind of electron wastes metallic element analysis method, it is characterised in that the described method comprises the following steps：
(1) electron wastes are carried out into aerobic roasting, obtains electron wastes sample；
(2) after taking the electron wastes sample acid dissolving that step (1) is obtained, add first kind nitration mixture to carry out heating and clear up, it is cold
But filtered afterwards and constant volume, obtained first kind metal ion mixed liquor；
(3) after taking the electron wastes sample acid dissolving that step (1) is obtained, Equations of The Second Kind nitration mixture is added to be reacted, reaction knot
Heating evaporation after beam, the residue for obtaining obtains the mixing of Equations of The Second Kind metal ion with being cooled down after acid dissolving, being filtered and constant volume
Liquid；
(4) after taking the pretreated electron wastes acid dissolving of step (1), add the 3rd class nitration mixture to carry out heating and clear up, it is cold
But filtered afterwards and constant volume, obtained the 3rd metalloid Ar ion mixing liquid；
(5) in detection first kind metal ion mixed liquor, Equations of The Second Kind metal ion mixed liquor and the 3rd metalloid Ar ion mixing liquid
Metal element content.
2. analysis method according to claim 1, it is characterised in that step (1) described electron wastes are discarded circuit
Plate；
Preferably, step (1) described electron wastes are the electron wastes by pre-processing；
Preferably, the pretreatment is broken and screening；
Preferably, the powder size of step (1) electron wastes after pretreatment is 80 mesh~200 mesh；
Preferably, step (1) the aerobic roasting is carried out in Muffle furnace；
Preferably, the temperature of step (1) the aerobic roasting is 450 DEG C~850 DEG C, preferably 600 DEG C~800 DEG C；Preferably,
The time of step (1) the aerobic roasting is 1h~6h.
3. analysis method according to claim 1 and 2, it is characterised in that step (2) the acid dissolving is to be with concentration
The nitric acid of 15%~65wt% is dissolved；
Preferably, the consumption of the nitric acid is：It is 15wt% that 0.5g~10g electron wastes samples use 2mL~20mL concentration
The nitric acid of~65wt% is dissolved, and preferably uses 5mL concentration to be dissolved for the nitric acid of 25wt%~40wt%；
Preferably, step (2) the sour dissolution time is 0.5h~12h；
Preferably, step (2) described acid is carried out in being dissolved in counteracting tank；
Preferably, the counteracting tank is polytetrafluoroethylene (PTFE) counteracting tank.
4. the analysis method according to claim any one of 1-3, it is characterised in that step (2) first kind nitration mixture bag
Include：Concentration is the chloroazotic acid of 15wt%~35wt%, concentration for the hydrofluoric acid and concentration of 25wt%~48wt% be 15wt%~
The hydrogen peroxide of 30wt%；
Preferably, the volume ratio of nitric acid and hydrochloric acid is 1 in the chloroazotic acid:3；
Preferably, the consumption of the chloroazotic acid is：It is 15wt% that 0.5g~10g electron wastes sample adds 2mL~10mL concentration
The chloroazotic acid of~35wt%；
Preferably, the consumption of the hydrofluoric acid is：0.5g~10g electron wastes sample add 0.5mL~5mL concentration be
The hydrofluoric acid of 25wt%~48wt%；
Preferably, the consumption of the hydrogen peroxide is：It is 15wt%~30wt% that 0.5g~10g electron wastes sample adds concentration
0.5mL~10mL hydrogen peroxide；
Preferably, the mode of addition first kind nitration mixture is in step (2)：Sequentially add the king that concentration is 15wt%~35wt%
Water, concentration are the hydrogen peroxide of 15wt%~30wt% for the hydrofluoric acid and concentration of 25wt%~48wt%.
5. the analysis method according to claim any one of 1-4, it is characterised in that step (2) heating is cleared up and dried
Carried out in case；
Preferably, step (2) temperature cleared up that heats is 80 DEG C~200 DEG C, preferably 120 DEG C~150 DEG C；
Preferably, the time that step (2) heating is cleared up is 2h~6h；
Preferably, step (2) constant volume carries out constant volume with the chloroazotic acid that concentration is 5wt%~35wt%；
Preferably, in step (2) first kind metal ion mixed liquor comprising Cu ions, Au ions, Pd ions, Ni ions,
Fe ions and Zn ions.
6. the analysis method according to claim any one of 1-5, it is characterised in that acid dissolving described in step (3) is to use
Concentration is dissolved for the nitric acid of 15wt%~65wt%；
Preferably, the consumption of the nitric acid is：It is 15wt% that 0.5g~20g electron wastes samples use 3mL~10mL concentration
The nitric acid of~65wt% is dissolved, it is preferred to use 5mL concentration is dissolved for the nitric acid of 30wt%~45wt%；
Preferably, the time of step (3) the acid dissolving is 0.5h~2h；
Preferably, step (3) described acid is carried out in being dissolved in beaker；
Preferably, the beaker is polytetrafluoroethylene beaker.
7. the analysis method according to claim any one of 1-6, it is characterised in that step (3) the Equations of The Second Kind nitration mixture bag
Include：Concentration is the nitric acid of 15wt%~65wt%, concentration is the sulfuric acid of 50wt%~98wt%, concentration is 15wt%~30wt%
Hydrofluoric acid and concentration for 36wt%~72wt% perchloric acid；
Preferably, the consumption of the nitric acid is：It is 15wt% that 0.5g~20g electron wastes sample adds 5mL~20mL concentration
The nitric acid of~65wt%；
Preferably, the consumption of the sulfuric acid is：0.5g~20g electron wastes sample add 0.5mL~10mL concentration be
The sulfuric acid of 50wt%~98wt%；
Preferably, the consumption of the hydrofluoric acid is：0.5g~20g electron wastes sample add 0.5mL~20mL concentration be
The hydrofluoric acid of 15wt%~30wt%；
Preferably, the consumption of the perchloric acid is：0.5g~20g electron wastes sample add 0.5mL~10mL concentration be
The perchloric acid of 36wt%~72wt%；
Preferably, the mode of addition Equations of The Second Kind nitration mixture is in step (3)：It is to concentration is sequentially added in the solution after acid dissolving
The nitric acid of 15wt%~65wt%, concentration are that the sulfuric acid and concentration of 50wt%~98wt% are the hydrofluoric acid of 15wt%~30wt%
First set reaction is carried out, first set reaction adds the height that concentration is 36wt%~72wt% after terminating rear heating evaporation to wet salt shape
Chloric acid carries out the second secondary response；
Preferably, carried out after the first set reaction terminates heating evaporation temperature in heating evaporation to wet salt shape for 80 DEG C~
150℃；
Preferably, it is 80 DEG C~150 DEG C that step (3) reaction heats the temperature being evaporated after terminating；
Preferably, acid used in step (3) the residue acid dissolving is the nitric acid that concentration is 20wt%~35wt%, preferably
For concentration is the nitric acid of 30wt%；
Preferably, step (3) described constant volume is with the nitric acid constant volume that concentration is 5wt%~35wt%；
Preferably, in step (3) the Equations of The Second Kind metal ion mixed liquor comprising Cu ions, Au ions, Ag ions, Pd ions,
Ni ions, Fe ions and Zn ions.
8. the analysis method according to claim any one of 1-7, it is characterised in that acid dissolving described in step (4) is to use
Concentration is dissolved for the hydrochloric acid of 10wt%~30wt%；
Preferably, the consumption of the hydrochloric acid is：It is 10wt% that 0.5g~20g electron wastes samples use 2mL~20mL concentration
The hydrochloric acid of~30wt% is dissolved, it is preferred to use 10mL concentration is dissolved for the hydrochloric acid of 10wt%~30wt%；
Preferably, the time of step (4) the acid dissolving is 2h~12h；
Preferably, step (4) described acid is carried out in being dissolved in counteracting tank；
Preferably, the counteracting tank is polytetrafluoroethylene (PTFE) counteracting tank.
9. the analysis method according to claim any one of 1-8, it is characterised in that step (4) the 3rd class nitration mixture bag
Include：Concentration is the hydrofluoric acid of 15wt%~30wt%, concentration for the hydrochloric acid and concentration of 10wt%~30wt% be 15wt%~
The hydrogen peroxide of 30wt%；
Preferably, the consumption of the hydrofluoric acid is：0.5g~20g electron wastes sample add 0.5mL~10mL concentration be
The hydrofluoric acid of 15wt%~30wt%；
Preferably, the consumption of the hydrochloric acid is：It is 10wt% that 0.5g~20g electron wastes sample adds 2mL~20mL concentration
The hydrochloric acid of~30wt%；
Preferably, the consumption of the hydrogen peroxide is：0.5g~20g electron wastes sample add 1mL~10mL concentration be
The hydrogen peroxide of 15wt%~30wt%；
Preferably, the mode of the 3rd class nitration mixture of step (4) addition is：Sequentially add the hydrogen that concentration is 15wt%~30wt%
Fluoric acid, concentration are the hydrogen peroxide of 15wt%~30wt% for the hydrochloric acid and concentration of 10wt%~30wt%；
Preferably, reaction is cleared up in step (4) heating is carried out in an oven；
Preferably, the reaction temperature that reaction is cleared up in step (4) heating is 80 DEG C~200 DEG C, preferably 100 DEG C~150 DEG C；
Preferably, the reaction time that reaction is cleared up in step (4) heating is 2h~5h；
Preferably, step (4) described constant volume is with the hydrochloric acid constant volume that concentration is 5wt%~35wt%；
Preferably, in step (4) the 3rd metalloid Ar ion mixing liquid comprising Cu ions, Pb ions, Sn ions, Ni ions,
Fe ions and Zn ions；
Preferably, the mode of step (5) the detection metal element content is ICP-OES detections.
10. the analysis method according to claim any one of 1-9, it is characterised in that the described method comprises the following steps：
(1) electron wastes that powder size after pretreatment is 80 mesh~200 mesh are had at 600 DEG C~800 DEG C
Oxygen is calcined 1h~6h, obtains electron wastes sample；
(2) nitric acid that the electron wastes sample 5mL concentration that 0.5g~10g steps (1) obtain is 25wt%~40wt% is taken
After dissolving 0.5h~12h, it is that the chloroazotic acid of 15wt%~35wt%, 0.5mL~5mL concentration are to sequentially add 2mL~10mL concentration
The hydrofluoric acid and 0.5mL~10mL concentration of 25wt%~48wt% are the hydrogen peroxide of 15wt%~30wt% in 120 DEG C~150 DEG C
Carry out heating and clear up 2h~6h, filtered after cooling and with the chloroazotic acid constant volume that concentration is 5wt%~35wt%, obtained comprising Cu
The first kind metal ion mixed liquor of ion, Au ions, Pd ions, Ni ions, Fe ions and Zn ions；
(3) nitric acid that the electron wastes sample 5mL concentration that 0.5g~20g steps (1) obtain is 30wt%~45wt% is taken
After dissolving 0.5h~2h, it is that the nitric acid of 15wt%~65wt%, 0.5mL~10mL concentration are to sequentially add 5mL~20mL concentration
The sulfuric acid and 0.5mL~20mL concentration of 50wt%~98wt% carry out first set reaction for the hydrofluoric acid of 25wt%~30wt%,
First set reaction terminate after added after 80 DEG C~150 DEG C heating evaporation to wet salt shapes 0.5mL~10mL concentration be 36wt%~
The perchloric acid of 72wt% carries out the second secondary response, and reaction terminates after 80 DEG C~150 DEG C heating evaporations, the residue concentration for obtaining
To be cooled down, being filtered and with the nitric acid constant volume that concentration is 5wt%~35wt%, being obtained comprising Cu after the nitric acid dissolving of 30wt%
The Equations of The Second Kind metal ion mixed liquor of ion, Au ions, Ag ions, Pd ions, Ni ions, Fe ions and Zn ions；
(4) hydrochloric acid that the pretreated electron wastes 10mL concentration of 0.5g~20g steps (1) is 10wt%~30wt% is taken
After dissolving 2h~2h, it is that the hydrofluoric acid of 25wt%~45wt%, 2mL~20mL concentration are to sequentially add 0.5mL~10mL concentration
The hydrochloric acid and 1mL~10mL concentration of 10wt%~30wt% are carried out for the hydrogen peroxide of 15wt%~30wt% in 100 DEG C~150 DEG C
2h~5h is cleared up in heating, is filtered after cooling and with the hydrochloric acid constant volume that concentration is 5wt%~35wt%, obtain comprising Cu from
3rd metalloid Ar ion mixing liquid of son, Pb ions, Sn ions, Ni ions, Fe ions and Zn ions；
(5) using ICP-OES detections first kind metal ion mixed liquor, Equations of The Second Kind metal ion mixed liquor and the 3rd metalloid from
Metal element content in sub- mixed liquor.
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| CN107036988A (en) * | 2017-05-18 | 2017-08-11 | 山东玉皇新能源科技有限公司 | It is a kind of to detect the method that graphene Gold Samples belong to constituent content |
| CN108816065A (en) * | 2018-04-24 | 2018-11-16 | 中国科学技术大学 | A method of being completely dissolved barite |
| CN109813835A (en) * | 2017-11-22 | 2019-05-28 | 中国瑞林工程技术股份有限公司 | The method for measuring gold and silver content in useless circuit board |
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| JP2005030663A (en) * | 2003-07-11 | 2005-02-03 | Ebara Corp | Waste treatment device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107036988A (en) * | 2017-05-18 | 2017-08-11 | 山东玉皇新能源科技有限公司 | It is a kind of to detect the method that graphene Gold Samples belong to constituent content |
| CN109813835A (en) * | 2017-11-22 | 2019-05-28 | 中国瑞林工程技术股份有限公司 | The method for measuring gold and silver content in useless circuit board |
| CN109813835B (en) * | 2017-11-22 | 2021-10-26 | 中国瑞林工程技术股份有限公司 | Method for measuring gold and silver content in waste circuit board |
| CN108816065A (en) * | 2018-04-24 | 2018-11-16 | 中国科学技术大学 | A method of being completely dissolved barite |
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