CN110220887A - A method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal - Google Patents
A method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal Download PDFInfo
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Abstract
The present invention relates to a kind of measurement useless circuit boards to remove lead in material resin-oatmeal, zinc, the method of tin and nickel, broken and selection by winnowing is carried out using by useless circuit board sample, collect metal and nonmetallic (toner) two kinds of materials, for stanniferous higher in the resin-oatmeal sample of useless circuit board, processing to sample, measure medium, the influence and working curve of matrix and coexistence elements to measurement are linear etc. to be tested, it explores with hydrochloric acid, nitric acid, tartaric acid, nitric-sulfuric acid and hydrogen peroxide dissolved samples, tartaric acid is added in diluted hydrochloric acid medium and tin forms complex, to prevent the hydrolysis of tin, with lead in inductively coupled plasma emission spectrography METHOD FOR CONTINUOUS DETERMINATION useless circuit board toner sample in same solution, zinc, tin and nickel amount.The present invention can efficiently and accurately analysis ingredient complexity useless circuit board removing material resin-oatmeal in lead, zinc, tin and nickel content, it is easy to operate, quick, accurate to have many advantages, such as.
Description
Technical field
The present invention relates to the measurement analysis methods that a kind of useless circuit board removes metallic element in material resin-oatmeal.
Background technique
With the development of information technology, the update of electronic product is maked rapid progress, and the various functions of new product make people
Constantly update household electrical appliance and portable device, people enjoy various new digital electronic goods brings it is convenient while,
Discarded electronic product has also manufactured a large amount of electronic waste rubbish.Simultaneously as useless circuit board is the core of each electronic product
Center portion part, wherein contain a large amount of valuable metal element, especially valuable elements such as the lead containing high-content, zinc, tin and nickel can be with
It takes suitable method to be recycled, is greatly improved the utilization rate of secondary resource in this way, be the important set developed a circular economy
At part.Currently, there is no the analysis method and standard about useless circuit board sample measurement lead, zinc, tin and nickel element both at home and abroad.Cause
This, lead, zinc, nickel and tin metal constituent content in Accurate Determining useless circuit board establish correlation analysis method, to the valuable gold of recycling
Belong to and resource circulation utilization has important practical significance and directive significance.The property of useless circuit board determines answering for its composition
Polygamy and composition differ greatly, and think Accurate Determining its lead, zinc, tin and nickel content using traditional sampling, sample preparation and analysis method
Certainly exist many difficulties.
Summary of the invention
The method for expecting lead, zinc, tin and nickel in resin-oatmeal is removed the purpose of the present invention is to provide a kind of measurement useless circuit board,
Overcome traditional sampling, sample preparation and analysis method can not Accurate Determining its lead, zinc, tin and the shortcomings that nickel content.
A method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal, which is characterized in that including following
Step:
(1) sample be all crushed to full dose and pass through standard screen with pulverizer；
(2) resin-oatmeal sample is accurately weighed in 250mL conical beaker, is accurate to 0.0001g；
(3) add water wetting in Xiang Suoshu resin-oatmeal sample, concentrated hydrochloric acid, concentrated nitric acid and tartaric acid solution dissolution examination is then added
Sample removes cold filtration, filtrate and filter residue is obtained by filtration after being placed in electric hot plate low-temperature heat reaction；
(4) filtrate is moved in 250mL volumetric flask, is diluted with water to scale, stand or do filtering；
(5) the filtered filter residue is moved in former conical flask together with filter paper, addition concentrated nitric acid, tartaric acid solution,
Cap upper surface ware is placed in electric hot plate heating reaction；
(6) nitric-sulfuric acid is added into solution after the reaction, heats and be evaporated to and emits sulfuric acid cigarette filter paper is made to be carbonized, such as exist
There is black particle object when smoldering in beaker, indicates that filter paper carbonization is not complete, add nitric-sulfuric acid, and evaporate and emit white cigarette to wet salt
Shape removes cooling；
(7) hydrochloric acid is added to solution after the cooling, hydrogen peroxide is placed in electric hot plate heating, evaporation dissolved salts, is added
Hydrochloric acid, heating, which is boiled, removes cooling, and solution is moved into 100mL volumetric flask, scale is diluted with water to, and mixes, stands or did
Filter；
(8) lead, zinc, tin and nickel in the filtrate, filter residue are contained respectively using inductively coupled plasma emission spectrography
The analysis of amount measures.
Further, in step (1), the full dose passes through 0.2nm standard screen, it is ensured that the uniformity of sample；Step
(2) in, the dosage for accurately weighing resin-oatmeal is 0.5g, it is ensured that sample is representative, improves lead, zinc, nickel and tin
Analyze the accuracy of result.
Further, in step (3), the concentrated hydrochloric acid and concentrated nitric acid dosage are respectively 10mL, and tartaric acid solution concentration is
100g/L, tartaric acid solution dosage are 3mL, sample can be made sufficiently to dissolve；In step (5), the concentrated nitric acid dosage is 10mL,
Tartaric acid solution dosage is 3mL.
Further, in step (6), the nitric-sulfuric acid volume ratio is 7:3, and nitric-sulfuric acid dosage is 2mL, can be made
Sample sufficiently dissolves, and obtains higher preci-sion and accuracy.
Further, in step (7), the hydrochloric acid dosage is 10mL, and hydrogen peroxide use 2mL can be such that salt fills
Divide dissolution, obtains higher preci-sion and accuracy.
The present invention is for stanniferous higher in the resin-oatmeal sample of useless circuit board, to the processing of sample, measurement medium, matrix and altogether
It deposits that influence and working curve of the element to measurement are linear etc. to be tested, explores with hydrochloric acid, nitric acid, tartaric acid, nitric-sulfuric acid
With hydrogen peroxide dissolved samples, tartaric acid is added in diluted hydrochloric acid medium and tin forms complex, to prevent the hydrolysis of tin, same
With lead, zinc, tin and nickel amount in ICP-AES METHOD FOR CONTINUOUS DETERMINATION useless circuit board toner sample in one solution.The present invention can efficiently and
Accurately the content of lead, zinc, tin and nickel in resin-oatmeal is expected in the useless circuit board removing of analysis ingredient complexity, is had easy to operate, fast
The advantages that fast, accurate.
Specific embodiment
The invention will be further described With reference to embodiment:
A method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal, comprising the following steps:
(1) sample is carried out all being crushed to full dose with pulverizer through standard screen, the preferred 0.2nm of standard screen, thus, it is possible to
Guarantee the uniformity of sample；
(2) resin-oatmeal sample is accurately weighed in 250mL conical beaker, is accurate to 0.0001g；The sample weighting amount of resin-oatmeal selects
0.5g is selected, thus, it is possible to improve the accuracy and precision of data；
(3) add water wetting in Xiang Suoshu resin-oatmeal sample, concentrated hydrochloric acid, concentrated nitric acid and tartaric acid solution dissolution examination is then added
Sample removes cold filtration, filtrate and filter residue is obtained by filtration after being placed in electric hot plate low-temperature heat reaction；Concentrated hydrochloric acid and concentrated nitric acid are used
Preferred 10mL is measured, tartaric acid solution concentration selects 100g/L, and tartaric acid solution dosage selects 3mL.Thus, it is possible to keep sample abundant
Dissolution；
(4) filtrate is moved in 250mL volumetric flask, is diluted with water to scale, stand or do filtering；
(5) the filtered filter residue is moved in former conical flask together with filter paper, addition concentrated nitric acid, tartaric acid solution,
Cap upper surface ware is placed in electric hot plate heating reaction；The preferred 10mL of concentrated nitric acid dosage, tartaric acid solution dosage select excellent 3mL；
(6) nitric-sulfuric acid is added into solution after the reaction, heats and be evaporated to and emits sulfuric acid cigarette filter paper is made to be carbonized, such as exist
There is black particle object when smoldering in beaker, indicates that filter paper carbonization is not complete, add nitric-sulfuric acid, and evaporate and emit white cigarette to wet salt
Shape removes cooling；Nitric-sulfuric acid volume ratio is preferably 7:3, and nitric-sulfuric acid dosage selects 2mL, thus, it is possible to keep sample abundant
Dissolution, obtains higher preci-sion and accuracy；
(7) hydrochloric acid is added to solution after the cooling, hydrogen peroxide is placed in electric hot plate and dissolves by heating salt, is evaporated to 5mL
Hydrochloric acid is added in left and right, and heating, which is boiled, removes cooling, and solution is moved into 100mL volumetric flask, scale is diluted with water to, and mixes, quiet
Set or do filtering；The preferred 10mL of hydrochloric acid dosage, hydrogen peroxide use selection 2mL are obtained thus, it is possible to dissolve salt sufficiently
Higher preci-sion and accuracy；
(8) lead, zinc, tin and nickel in the filtrate, filter residue are contained respectively using inductively coupled plasma emission spectrography
The analysis of amount measures.
Specific embodiment and verifying analysis:
1, prepared by sample
Useless circuit board sample carries out broken and selection by winnowing, collects metal and nonmetallic (toner) two kinds of materials, nonmetallic
Material (toner) carries out whole full doses that are crushed to pulverizer and passes through 0.2nm standard screen.
2, the preparation of test solution is analyzed
0.5g toner sample is accurately weighed in 250mL conical beaker, is accurate to 0.0001g.As on sample sub-sieve,
Under sieve, sample is weighed by the quality composition and division in a proportion after its screening.Add a small amount of water to soak, 10mL hydrochloric acid, 10mL nitric acid, 3mL is then added
(100g/L) tartaric acid solution removes cold filtration after being placed in electric hot plate low-temperature heat 5min.Filtrate moves into 250mL volumetric flask
In, it is diluted with water to scale, stands or do filtering.Filter residue is moved in former conical beaker together with filter paper, addition 10mL nitric acid,
3mL tartaric acid solution, cap upper surface ware are placed in electric hot plate heating 10min.2mL nitric-sulfuric acid (nitric-sulfuric acid volume ratio is added
7:3), it heats and is evaporated to and emit sulfuric acid cigarette filter paper is made to be carbonized.(such as there is black particle object in beaker when smoldering, indicate filter paper carbon
Change is not complete, adds a small amount of nitric-sulfuric acid, and evaporate and emit white cigarette to wet salt, removes cooling.) 10mL hydrochloric acid, 2mL peroxide is added
Change hydrogen, be placed in electric hot plate and dissolve by heating salt, be evaporated to 5mL or so, 10mL hydrochloric acid is added, heating, which is boiled, removes cooling, will be molten
Liquid moves into 100mL volumetric flask, is diluted with water to scale, mixes, and stands or do filtering.
3, the preparation of Working Standard Solution
Lead, zinc, tin and nickel each unit element standard solution (A): lead standard solution ρ (Pb)=2000 μ g/mL；Zinc standard solution
ρ (Zn)=2000 μ g/mL；Nickel standard solution ρ (Ni)=1000 μ g/mL；Tin standard solution ρ (Sn)=2000 μ g/mL；
Lead, zinc, tin and nickel mixed standard solution (B): Pb, Zn, Sn are configured to above-mentioned concentration each unit element standard solution
Mass concentration is respectively 200 μ g/mL；Ni mass concentration is the mixed standard solution of 100 μ g/mL；
Hybrid standard serial solution (C): take respectively above-mentioned lead, zinc, tin and nickel mixed standard solution 0ml, 2.5mL, 5mL,
In one group of 100ml volumetric flask, addition 10mL hydrochloric acid, 3mL tartaric acid (100g/L) are diluted to scale by 10mL, 20mL and 25mL,
It mixes.
4, it measures
Test solution and standard serial solution (C) will be analyzed and carry out plasma spectrometry simultaneously under selected instrument operating condition
Method lead, zinc, tin and nickel-silicon nitride.
5, influence of the different factors to measurement result is investigated
The selection of 5.1 analysis spectral lines
From spectrometer spectral line library, the spectral line interference and the intensity of spectral line information of the analytical line, element of each element to be measured are checked,
Select three stronger spectral lines of intensity.With each unit element standard solution, mixed standard solution and sample solution, in selected each element
Analytical line at successively scan, the spectral profile image shown on viewing screen.Compare each spectral line of tested element sensitivity and
Spectra1 interfer- situation, the final spectral line for determining that interference is small, background is low, signal-to-noise ratio is high is analysis spectral line (being shown in Table 1).
1 element analysis spectrum line of table
| Project | Lead | Zinc | Tin | Nickel |
| Analytical line/nm | 220.353 | 206.200 | 189.927 | 231.604 |
The detection limit of 5.2 methods is tested
Under selected analysis spectral line and instrument operating condition, established with lead, zinc, nickel, tin hybrid standard serial solution (C)
Calibration curve, 10 blank reagent solutions of METHOD FOR CONTINUOUS DETERMINATION, with the method detection limit of 3 times of standard deviation calculations, as a result such as following table institute
Show:
2 lead of table, zinc, nickel and tin detection limit (mg/L)
| Project | Lead | Zinc | Nickel | Tin |
| Detection limit | 0.10 | 0.024 | 0.021 | 0.19 |
The selection of 5.3 measurement media
Influence of the 3 chloroazotic acid dosage of table to measurement
Influence of 4 hydrochloric acid dosage of table to measurement
According to the method for the present invention, change the dosage of chloroazotic acid and hydrochloric acid respectively, is established and corrected with hybrid standard serial solution (C)
Curve, measures lead, zinc, nickel and tin amount in respective media solution respectively, and measurement result is shown in Table 3, table 4.The result shows that hydrochloric acid system
With chloroazotic acid (hydrochloric acid+nitric acid=3+1v/v) system, measurement result is almost the same, and selecting hydrochloric acid herein is measurement system；Hydrochloric acid
Concentration (volume fraction) has no significant effect measurement result between 5%~10%, and the measurement result of each element does not become substantially
Change, when concentration of hydrochloric acid is more than 10%, each element result reduces with the increase of concentration of hydrochloric acid.Sn element hydrolyzes in order to prevent,
Therefore, selecting concentration of hydrochloric acid (volume fraction) is 10%, and the salt acidacidity of solution and standard solution to be measured should be consistent as far as possible.
5.4, the selection of tartaric acid dosage
According to the method for the present invention, establish calibration curve with hybrid standard serial solution (C), measure respectively lead in each solution,
Zinc, nickel and tin amount, measurement result are as shown in the table:
The influence of 5 tartaric acid dosage of table is tested
Test result discovery: tartaric acid concentration is in 1-3mg/L range, and as concentration increases, measurement result is close to really
Value, when concentration is more than 3mg/L, measurement result is integrally relatively low.Therefore select concentration for 3mg/L.
The selection of 5.5 sample dissolving methods
5.00mL lead, zinc, tin, nickel mixed standard solution (B) are pipetted in conical beaker, according to following 2 kinds of mixed acid systems
Molten sample test is carried out, as a result see the table below shown.
1) hydrochloric acid+nitric acid+perchloric acid+hydrochloric acid+tartaric acid+hydrogen peroxide
2) hydrochloric acid+nitric acid+nitric-sulfuric acid+hydrochloric acid+tartaric acid+hydrogen peroxide
6 method choice of table tests (mg/L)
The result shows that, it is affected using method 1 to tin result by table, tin loss is larger, method 2 and standard value basic one
It causes, the result influence of two methods of lead, zinc and nickel is almost consistent, influences less.Therefore 2 dissolved samples of selecting method.
6, the reliability and feasibility of verification method
6.1 sample precision
2 samples of 058-D# and 103-D# are subjected to precision test by experimental method, test result is shown in Table shown.
7 sample precision test of table
6.2 method accuracy tests
Mark-on reclaims test is carried out by experimental method to 058-D# sample, sample mark-on reclaims test result is shown in Table.
The test of 8 mark-on reclaims of table
As seen from the results in Table 8, lead, zinc, tin, nickel show that this method accuracy is higher between 97.5%~103.2%.
The present invention is for stanniferous higher in the resin-oatmeal sample of useless circuit board, to the processing of sample, measurement medium, matrix and altogether
It deposits that influence and working curve of the element to measurement are linear etc. to be tested, explores with hydrochloric acid, nitric acid, tartaric acid, nitric-sulfuric acid
With hydrogen peroxide dissolved samples, tartaric acid is added in diluted hydrochloric acid medium and tin forms complex, to prevent the hydrolysis of tin, same
Lead, zinc, tin and nickel amount in ICP-AES METHOD FOR CONTINUOUS DETERMINATION useless circuit board toner sample are used in one solution, and under this determination condition
Method precision, accuracy test are carried out.In the present specification, the schematic representation of term need not be directed to identical
Embodiment or example.Moreover, particular features, structures, materials, or characteristics described can in any one or more embodiments or
It can be combined in any suitable manner in example.In addition, without conflicting with each other, those skilled in the art can illustrate this
The feature of different embodiments or examples and different embodiments or examples described in book is combined.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Several equivalent substitute or obvious modifications are made under the premise of not departing from present inventive concept, and performance or use is identical, then should
It is considered as belonging to the protection scope that claims that the present invention is submitted determine.
Claims (5)
1. a kind of method of lead, zinc, tin and nickel in measurement useless circuit board removing material resin-oatmeal, which is characterized in that including following step
It is rapid:
(1) sample be all crushed to full dose and pass through standard screen with pulverizer；
(2) resin-oatmeal sample is accurately weighed in 250mL conical beaker, is accurate to 0.0001g；
(3) add water wetting in Xiang Suoshu resin-oatmeal sample, concentrated hydrochloric acid, concentrated nitric acid and tartaric acid solution dissolved samples be then added,
After being placed in electric hot plate low-temperature heat reaction, cold filtration is removed, filtrate and filter residue is obtained by filtration；
(4) filtrate is moved in 250 mL volumetric flasks, is diluted with water to scale, stand or do filtering；
(5) the filtered filter residue is moved in former conical flask together with filter paper, concentrated nitric acid is added, tartaric acid solution covers
Surface plate is placed in electric hot plate heating reaction；
(6) nitric-sulfuric acid is added into solution after the reaction, heats and be evaporated to and emits sulfuric acid cigarette filter paper is made to be carbonized, such as smoldering
When beaker in have a black particle object, indicate that filter paper carbonization is not complete, add nitric-sulfuric acid, and evaporate and emit white cigarette to wet salt, take
Lower cooling；
(7) hydrochloric acid is added to solution after the cooling, hydrogen peroxide is placed in electric hot plate heating, evaporation dissolved salts, salt is added
Acid, heating, which is boiled, removes cooling, and solution is moved into 100mL volumetric flask, scale is diluted with water to, and mixes, and stands or do filtering；
(8) using inductively coupled plasma emission spectrography respectively to lead in the filtrate, filter residue, zinc, tin and nickel content
Analysis measurement.
2. the method for lead, zinc, tin and nickel, feature in measurement useless circuit board removing material resin-oatmeal according to claim 1
Be: in step (1), the full dose passes through 0.2nm standard screen, it is ensured that the uniformity of sample；In step (2), the standard
The dosage for really weighing resin-oatmeal is 0.5g, it is ensured that sample is representative, improves the standard of lead, zinc, nickel and tin analysis result
Exactness.
3. the method for lead, zinc, tin and nickel, feature in measurement useless circuit board removing material resin-oatmeal according to claim 2
Be: in step (3), the concentrated hydrochloric acid and concentrated nitric acid dosage are respectively 10mL, and tartaric acid solution concentration is 100g/L, and tartaric acid is molten
Liquid dosage is 3 mL, sample can be made sufficiently to dissolve；In step (5), the concentrated nitric acid dosage is 10 mL, and tartaric acid solution is used
Amount is 3 mL.
4. the method for lead, zinc, tin and nickel, feature in measurement useless circuit board removing material resin-oatmeal according to claim 3
Be: in step (6), the nitric-sulfuric acid volume ratio is 7:3, and nitric-sulfuric acid dosage is 2 mL, and sample can be made sufficiently molten
Solution, obtains higher preci-sion and accuracy.
5. the method for lead, zinc, tin and nickel, special in measurement useless circuit board removing material resin-oatmeal according to claim 1 or 4
Sign is: in step (7), the hydrochloric acid dosage is 10 mL, and hydrogen peroxide use is 2 mL, salt can be made sufficiently to dissolve, obtained
To higher preci-sion and accuracy.
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| CN113358735B (en) * | 2021-06-02 | 2022-10-28 | 河北省地质实验测试中心(国土资源部保定矿产资源监督检测中心、河北省金银宝玉饰品质量监督检验站) | Method for decomposing cassiterite-containing mineral suitable for measuring tin content and application thereof |
| CN113984476A (en) * | 2021-10-29 | 2022-01-28 | 北京星航机电装备有限公司 | Digestion solution and method for determining multi-element content in tin-lead solder |
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| Publication number | Publication date |
|---|---|
| CN110220887B (en) | 2021-09-24 |
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