CN114371249A - Method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder - Google Patents
Method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder Download PDFInfo
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Abstract
The invention provides a method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder, belonging to the technical field of chemical analysis, and the method comprises the following steps of (1) sample preparation: a resin powder sample; (2) sample treatment: a sample solution; (3) preparing a standard test solution: a fluorine standard solution, a chlorine-bromine mixed standard solution and a fluorine-chlorine-bromine mixed standard series solution; (4) and (4) measuring the amount of fluorine, chlorine and bromine. The method realizes the determination of the contents of fluorine, chlorine and bromine by physically separating the waste circuit boards into the resin powder samples, so that the method can be applied to different waste circuit boards and has wide applicability; a sample is reasonably selected and combusted in an oxygen bomb bottle through oxygenation, the sample is absorbed in an alkali liquid medium, and the content of fluorine, chlorine and bromine in the waste circuit board stripping resin powder is continuously measured by ion chromatography, so that the problem that the result is low due to incomplete absorption caused by insufficient combustion in the combustion process is solved, the content of fluorine, chlorine and bromine is not influenced while the loss of halogen is avoided.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder.
Background
The circuit board is a core component of various electronic products. China has become the largest world-wide country for generating electronic wastes, wherein waste circuit boards belong to the core components of waste electrical and electronic products, are rich in valuable metals such as copper, gold, silver, platinum, palladium, nickel, tin and the like, and harmful elements such as fluorine, chlorine, bromine and the like, and are often used as flame retardants to be added into various circuit boards.
However, the lack of the relevant analysis method standard of the waste circuit board in the domestic market at present leads to the fact that the transaction price is often achieved through the agreement between the buyer and the seller, which not only reflects the market value of the waste circuit board, but also seriously affects the recovery, utilization and sustainable development of the waste circuit board.
With the rapid development of the electronic information industry, the number of waste circuit boards (WPCB) is also rapidly increased, the types of the waste circuit boards are various, and the distribution of various contents is greatly changed, so that the accurate determination of the contents of harmful elements such as fluorine, chlorine, bromine and the like in the waste circuit boards is very important for understanding the recovery value of the waste circuit boards and determining the recovery processing method.
At present, the method for simultaneously measuring harmful elements such as fluorine, chlorine, bromine and the like in waste circuit board samples is less explored. Therefore, it is necessary to develop a fast and accurate method capable of satisfying the analysis and test requirements of the waste circuit board sample.
Disclosure of Invention
Based on this, the present invention aims to provide a method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder, so as to solve the above-mentioned deficiencies in the related art.
The invention provides a method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder, which comprises the following steps:
(1) sample preparation:
extracting a waste circuit board sample according to a sampling proportion, crushing and stripping the waste circuit board sample to obtain a resin powder sample, weighing a predetermined amount of the numerical value powder sample, and placing the numerical value powder sample in a sample crucible;
(2) sample treatment:
weighing a predetermined amount of absorption liquid, pouring the absorption liquid into an absorption cup, placing the absorption cup in an oxygen bomb bottle, contacting a combustion filament with the resin powder sample in the sample crucible, placing the combustion filament above the liquid level of the absorption liquid, sealing the oxygen bomb bottle, carrying out circulating oxygenation, and controlling the oxygen pressure of the oxygen bomb bottle within a preset range;
putting the oxygen bomb bottle subjected to the circulating oxygenation into a cooling barrel containing cooling water for ignition, taking out the oxygen bomb bottle at intervals of first preset time, shaking, deflating and opening the oxygen bomb bottle after second preset time, collecting absorption liquid in the oxygen bomb bottle, transferring the absorption liquid to a volumetric flask, adding water to dilute the absorption liquid to a volumetric flask constant volume scale, and uniformly mixing to obtain a sample solution;
(3) preparing a standard test solution:
weighing predetermined amounts of fluorine standard stock solution, chlorine standard stock solution and bromine standard stock solution in sequence, mixing the chlorine standard stock solution and the bromine standard stock solution to form chlorine-bromine mixed solution, respectively placing the chlorine-bromine mixed solution and the fluorine standard stock solution into two volumetric flasks, adding water to dilute the chlorine-bromine mixed solution and the fluorine standard stock solution until the volumetric flasks have constant volume scales, and uniformly mixing to obtain fluorine standard solution and chlorine-bromine mixed standard solution;
weighing a plurality of fluorine standard solutions with different preset amounts respectively, transferring a plurality of chlorine and bromine mixed standard solutions with different preset amounts respectively, sequentially and correspondingly placing the solutions into seven volumetric flasks, adding water to dilute the solutions until the volumetric scales of the volumetric flasks are constant, and uniformly mixing the solutions to obtain a fluorine-chlorine-bromine mixed standard series solution;
(4) and (3) measuring the amount of fluorine, chlorine and bromine:
and (3) measuring the contents of fluorine, chlorine and bromine of the sample solution obtained in the step (2) by an ion chromatograph according to the corresponding fluorine-chlorine-bromine mixed standard series solution.
In some of the examples, in the step of preparing the sample, the predetermined amount of the resin powder sample is 0.15 to 0.20g by weight, and the resin powder sample is weighed by a standard of 0.0001 g.
In some embodiments, in the step of sample processing, the step of circularly oxygenating is to oxygenate in the sealed oxygen bomb, deflate and oxygenate again after oxygenation is finished, and circularly do three times, and the oxygen pressure of the oxygen bomb is controlled to be 1.0-1.5 Mpa.
In some embodiments, the predetermined amount of the absorption liquid is 20mL, the concentration of the absorption liquid is controlled to be 0.045-0.050 mol/L, the first preset time is 5min, and the second preset time is 30 min.
In some of these embodiments, the standard solution preparing step comprises preparing a predetermined amount of a fluorine standard stock solution of 5mL, wherein each 1mL of the fluorine standard solution contains 50 μ g of fluorine, preparing a predetermined amount of a chlorine standard stock solution of 5mL, preparing a predetermined amount of a bromine standard stock solution of 10mL, and mixing the chlorine and the bromine to obtain a standard solution of 50 μ g of chlorine and 100 μ g of bromine per 1 mL.
In some embodiments, the step of preparing the standard test solution further comprises the steps of:
preparing a fluorine standard stock solution:
weighing a predetermined amount of sodium fluoride serving as a reference substance dried to constant weight within a preset temperature range, placing the sodium fluoride in a volumetric flask, adding water to dilute the sodium fluoride until the volume of the volumetric flask is constant, and uniformly mixing the sodium fluoride and the volumetric flask to obtain a fluorine standard stock solution;
preparing a chlorine standard stock solution:
weighing a predetermined amount of a reference substance sodium chloride burnt to constant weight within a preset temperature range, placing the reference substance sodium chloride into a volumetric flask, adding water to dilute the reference substance sodium chloride until the volumetric flask has constant volume scales, and uniformly mixing the reference substance sodium chloride and the water to obtain a chlorine standard stock solution;
preparing a bromine standard stock solution:
weighing a predetermined amount of potassium bromide serving as a reference substance dried to constant weight within a preset temperature range, placing the potassium bromide in a volumetric flask, adding water to dilute the potassium bromide until the volume of the volumetric flask is constant, and uniformly mixing the potassium bromide and the volumetric flask to obtain a bromine standard stock solution.
In some embodiments, the predetermined temperature range is 100-105 ℃, the predetermined amount of sodium fluoride weighs 2.2110g, and the fluorine standard stock solution contains 1000 μ g fluorine per 1 mL.
In some embodiments, the chlorine standard stock solution is prepared at a preset temperature range of 500-600 ℃ and the predetermined amount of sodium chloride weighs 1.6485g, and the chlorine standard stock solution contains 1000 μ g of chlorine per 1 mL.
In some embodiments, the bromine standard stock solution is prepared at a preset temperature range of 100-105 ℃ and a predetermined amount of 1.4900g of sodium chloride, and the bromine standard stock solution contains 1000 μ g of bromine per 1 mL.
In some of these embodiments, the volume fraction of fluorine, chlorine, and bromine in the sample solution is calculated by the formula:
in the formula: omega(B)-represents the percentage of fluorine, chlorine, bromine content, respectively, in units;
rho is the mass concentration of fluorine, chlorine and bromine in the solution to be detected, unit u g/mL;
ρ0-mass concentration of fluorine, chlorine, bromine in the blank solution, unit u g/mL;
V0-total volume of solution tested, in mL;
V1-dividing the volume of the test solution in mL;
V2-volume of the liquid to be tested, in mL;
m is the mass of the sample in g.
Compared with the prior art, the invention has the beneficial effects that: the method has the advantages that the resin powder samples are physically separated from the waste circuit boards, so that the fluorine, chlorine and bromine contents can be measured, the method can be applied to different waste circuit boards, and the applicability is wide; in addition, a sample is reasonably selected and combusted in an oxygen bomb bottle through oxygenation, the sample is absorbed in an alkali liquor medium, the contents of fluorine, chlorine and bromine in the waste circuit board stripping resin powder are continuously measured through ion chromatography, the problem that the content of fluorine, chlorine and bromine is low due to incomplete absorption caused by insufficient combustion in the combustion process is solved, the measurement of the contents of fluorine, chlorine and bromine is not influenced while the halogen loss is avoided, the method is convenient, simple and rapid, the sensitivity for continuously measuring the contents of fluorine, chlorine and bromine in the waste circuit board stripping resin powder through ion chromatography is high, and the daily measurement of the contents of fluorine, chlorine and bromine in the waste circuit board stripping resin powder can be effectively met.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used in the description herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The invention will be further illustrated with reference to specific embodiments:
a method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder comprises the following steps:
(1) sample preparation:
extracting a waste circuit board sample according to a sampling proportion, crushing and stripping the waste circuit board sample to obtain a resin powder sample, weighing a predetermined amount of the numerical value powder sample, and placing the numerical value powder sample in a sample crucible;
(2) sample treatment:
weighing a predetermined amount of absorption liquid, pouring the absorption liquid into an absorption cup, placing the absorption cup in an oxygen bomb bottle, contacting a combustion filament with the resin powder sample in the sample crucible, placing the combustion filament above the liquid level of the absorption liquid, sealing the oxygen bomb bottle, carrying out circulating oxygenation, and controlling the oxygen pressure of the oxygen bomb bottle within a preset range;
putting the oxygen bomb bottle subjected to the circulating oxygenation into a cooling barrel containing cooling water for ignition, taking out the oxygen bomb bottle at intervals of first preset time, shaking, deflating and opening the oxygen bomb bottle after second preset time, collecting absorption liquid in the oxygen bomb bottle, transferring the absorption liquid to a volumetric flask, adding water to dilute the absorption liquid to a volumetric flask constant volume scale, and uniformly mixing to obtain a sample solution;
(3) preparing a standard test solution:
weighing predetermined amounts of fluorine standard stock solution, chlorine standard stock solution and bromine standard stock solution in sequence, mixing the chlorine standard stock solution and the bromine standard stock solution to form chlorine-bromine mixed solution, respectively placing the chlorine-bromine mixed solution and the fluorine standard stock solution into two volumetric flasks, adding water to dilute the chlorine-bromine mixed solution and the fluorine standard stock solution until the volumetric flasks have constant volume scales, and uniformly mixing to obtain fluorine standard solution and chlorine-bromine mixed standard solution;
respectively weighing 0.00mL, 0.10mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL and 10.00mL of fluorine standard solution, respectively transferring 0.00mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL, 20.00mL of chlorine and bromine mixed standard solution, sequentially and correspondingly placing the mixed standard solution in seven volumetric flasks, adding water for diluting until the volumetric capacity of the volumetric flask is scaled and uniformly mixing to obtain a fluorine-chlorine-bromine mixed standard series solution;
(4) and (3) measuring the amount of fluorine, chlorine and bromine:
and (3) measuring the contents of fluorine, chlorine and bromine of the sample solution obtained in the step (2) by an ion chromatograph according to the corresponding fluorine-chlorine-bromine mixed standard series solution.
Before the method is implemented, firstly, implementation conditions need to be determined:
(1) selection of conditions for instrument parameters
The chromatographic profile image displayed on the screen was observed by scanning each single-element standard solution, mixed standard solution and sample solution in order at the analysis line of each selected element. And (3) comparing the sensitivity of each spectrogram of the detected element and the interference condition of the chromatogram, and finally determining the conditions of small interference, low background and high signal-to-noise ratio as instrument parameter conditions (see table 1).
TABLE 1 working conditions of the apparatus
(2) Detection limit and lower measurement limit of the method
Under the selected working conditions of the instrument, the fluorine, chlorine and bromine are mixed with the standard series solution to establish a calibration curve, 11 times of reagent blank solutions are continuously measured, the detection limit is calculated by a 3-time standard deviation calculation method, the measurement lower limit is calculated by a 10-time standard deviation calculation method, and the results are shown in table 2.
TABLE 2 detection limits and lower limits of measurement
| Item | Fluorine | Chlorine | Bromine compound |
| Detection Limit/. mu.g/mL | 0.010 | 0.028 | 0.020 |
| Lower limit of measurement/(μ g/mL) | 0.034 | 0.092 | 0.066 |
(3) Selection of assay conditions
TABLE 3 influence of the weighing on the determination
As is clear from Table 3, the measurement results of fluorine, chlorine and bromine were more favorable when the sample amounts were 0.15g and 0.20 g. When the sample weighing amount is increased, the oxygen in the oxygen bomb system is not sufficiently combusted due to insufficient oxygen, so that the measurement results of fluorine, chlorine and bromine are reduced, and the sample weighing amount is selected to be 0.15 g-0.20 g comprehensively.
TABLE 4 influence of absorption liquid volume on the determination
As is clear from Table 4, the measurement results of fluorine, chlorine and bromine were better when the volume of the absorbing solution was 20mL, and the absorbing solution volume was selected to be 20mL in the present application.
TABLE 5 Effect of oxygenation pressure on measurements
As is clear from Table 5, when the oxygen charging pressure is 1.0 to 1.5MPa, the measured values of fluorine, chlorine and bromine increase as the oxygen charging pressure increases. When the oxygenation pressure is higher than 1.5Mpa, the oxygenation pressure is increased, the measured values of fluorine, chlorine and bromine are basically consistent, and the oxygenation pressure is selected to be 1.5Mpa according to the application, considering the possibility that the sample in the sample crucible is blown away due to insufficient combustion caused by too low oxygenation pressure and too high oxygenation pressure.
TABLE 6 influence of reaction time on the assay
As can be seen from Table 6, when the reaction time is longer than 30min, the measurement results of fluorine, chlorine and bromine are basically unchanged, and the reaction time selected in the present application is 30 min.
TABLE 7 Effect of absorption liquid concentration on the measurement
As can be seen from Table 7, the concentration of the absorbing solution is 45mmol/L to 50mmol/L, the measurement results of fluorine, chlorine and bromine tend to be stable, and the absorbing solution concentration is selected to be 45mmol/L in the present application in consideration of the above.
(4) Interference test of solution cations
TABLE 8 influence of the cation of the solution on the measurement
As can be seen from Table 8, the presence of a small amount of cations in the test solution had little effect on the results of fluorine, chlorine and bromine measurements due to the low content of these cations.
According to the above experiments, specific embodiments of the present invention are as follows:
1. sample preparation:
firstly, according to a waste circuit board of a specific inventory condition, extracting a waste circuit board sample according to a sampling proportion, crushing and stripping the waste circuit board sample to obtain a resin powder sample, weighing 0.15-0.20 g of the numerical value powder sample through a 0.0001g standard, and placing the numerical value powder sample in a sample crucible;
2. sample treatment:
preparation of absorption liquid (0.045 mol/L): weighing 2.970g of high-grade pure potassium hydroxide in a beaker, dissolving the high-grade pure potassium hydroxide with water, transferring the high-grade pure potassium hydroxide into a 1000mL volumetric flask, diluting the solution to a scale, shaking up the solution, and placing the solution in a reagent bottle;
dissolution of resin powder sample: 20mL of an absorbent solution (C) was poured into the absorption cup(KOH)0.045mol/L), placing in an oxygen bomb, and mixing the burning wire with the sampleAnd (3) contacting the sample in the crucible, placing the sample above the liquid level of the absorption liquid, covering an oxygen bomb bottle, and screwing the oxygen bomb bottle to oxygenate. After the oxygenation is finished, the operation is repeated for 3 times by discharging and refilling oxygen, and finally the oxygen pressure is controlled to be 1.5 Mpa. And putting the oxygen bomb into a cooling barrel filled with cooling water for ignition, and taking out the oxygen bomb bottle and slightly shaking the oxygen bomb bottle every 5min or so after the ignition is successful so as to fully absorb the halogen-containing gas after the oxygen bomb bottle is combusted. After 30min, the gas absorption is completed. Opening the oxygen bomb after air leakage, collecting absorption liquid, washing the sample crucible and the absorption cup with water, transferring to a 100mL volumetric flask, diluting with water to a scale, and mixing uniformly;
3. preparing a standard test solution:
preparing a fluorine standard stock solution: 2.2110g of reference substance sodium fluoride dried at 100-105 ℃ to constant weight is accurately weighed and dissolved in a proper amount of water. All transferred to a 1000mL volumetric flask, diluted to the mark with deionized water and shaken up. The mixture was transferred to a dry plastic bottle for storage. 1mL of this solution contained 1000. mu.g of fluorine. Commercially available certified standard materials can also be purchased;
preparing a chlorine standard stock solution: 1.6485g of reference substance sodium chloride which is burned to constant weight at 500-600 ℃ is accurately weighed and dissolved in a proper amount of water. All transferred to a 1000mL volumetric flask, diluted to the mark with deionized water and shaken up. The mixture was transferred to a dry plastic bottle for storage. 1mL of this solution contained 1000. mu.g of chlorine. Commercially available certified standard materials can also be purchased;
preparing a bromine standard stock solution: 1.4900g of standard substance potassium bromide which is dried at 100-105 ℃ to constant weight is accurately weighed and dissolved in a proper amount of water. All transferred to a 1000mL volumetric flask, diluted to the mark with deionized water and shaken up. The mixture was transferred to a dry brown bottle for storage. 1mL of this solution contained 1000. mu.g of bromine. Commercially available certified standard materials can also be purchased;
preparing a fluorine standard solution: accurately transferring 5mL of fluorine standard stock solution into a 100mL volumetric flask, diluting the stock solution to a scale with deionized water, and uniformly mixing. 1mL of this solution contained 50. mu.g of fluorine;
preparing a chlorine and bromine mixed standard solution: accurately transferring 5mL of chlorine standard stock solution and 10mL of bromine standard stock solution into a 100mL volumetric flask, diluting the solution to a scale with deionized water, and uniformly mixing. 1mL of this solution contained 50. mu.g of chlorine and 100. mu.g of bromine, respectively;
preparing a fluorine-chlorine-bromine mixed standard series solution: transferring 0.00mL, 0.10mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL and 10.00mL of fluorine standard solution and transferring 0.00mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL and 20.00mL of chlorine and bromine mixed standard solution into the same group of 100mL volumetric flasks in sequence, diluting the solution to a scale with deionized water, uniformly mixing and fixing the volume;
drawing a standard curve: respectively analyzing the fluorine-chlorine-bromine mixed standard determination solution in the 7 volumetric flasks according to the working conditions of the instrument, and automatically drawing a working curve by the instrument;
4. determination and calculation of the fluorine, chlorine and bromine content: putting the dissolved sample solution into a volumetric flask, shaking up to constant volume to obtain a measurement solution of the waste circuit board stripping resin powder sample, and standing for more than 30 min; analyzing the measuring solution of the waste circuit board stripping resin powder sample in the volumetric flask according to the working conditions of the instrument to obtain the concentration rho of the measuring solution of the waste circuit board stripping resin powder sample;
calculating the content of fluorine, chlorine and bromine in the waste circuit board stripping resin powder sample according to the following formula:
wherein: omega(B)-represents the percentage of fluorine, chlorine, bromine content, respectively, in units;
rho is the mass concentration of fluorine, chlorine and bromine in the solution to be detected, unit u g/mL;
ρ0-mass concentration of fluorine, chlorine, bromine in the blank solution, unit u g/mL;
V0-total volume of solution tested, in mL;
V1-dividing the volume of the test solution in mL;
V2-volume of the liquid to be tested, in mL;
m is the mass of the sample in g;
it should be noted that the result calculated by the formula is expressed to the second decimal place, and if the result is less than 0.1%, the result is expressed to the third decimal place.
The instrument is characterized in that: the Aquion-1200 ion chromatograph (Saimer Feishell science and technology Co., Ltd.) has the instrument working conditions shown in Table 1;
5. precision and accuracy test
The precision and accuracy of the above test samples were tested according to the analytical procedures, and the results are shown in Table 9.
Table 9: test results of measuring precision and accuracy
6. Recovery test
2 test samples were selected, treated according to the method specified, and subjected to a standard recovery test, the analytical results of which are shown in Table 10.
Table 10: recovery rate of added standard
Note: the precision normalized recovery is an index used to characterize the reproducibility and accuracy of the method, respectively.
Precision is expressed in RSD (relative standard deviation); for instrumental analysis results, the RSD should be less than 10%.
The accuracy can be verified by a recovery rate experiment, and as can be seen from table 10, the recovery rates of fluorine, chlorine and bromine in the waste circuit board measured by the method are between 90% and 110%.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for measuring fluorine, chlorine and bromine in waste circuit board stripping material resin powder is characterized by comprising the following steps:
(1) sample preparation:
extracting a waste circuit board sample according to a sampling proportion, crushing and stripping the waste circuit board sample to obtain a resin powder sample, weighing a predetermined amount of the numerical value powder sample, and placing the numerical value powder sample in a sample crucible;
(2) sample treatment:
weighing a predetermined amount of absorption liquid, pouring the absorption liquid into an absorption cup, placing the absorption cup in an oxygen bomb bottle, contacting a combustion filament with the resin powder sample in the sample crucible, placing the combustion filament above the liquid level of the absorption liquid, sealing the oxygen bomb bottle, carrying out circulating oxygenation, and controlling the oxygen pressure of the oxygen bomb bottle within a preset range;
putting the oxygen bomb bottle subjected to the circulating oxygenation into a cooling barrel containing cooling water for ignition, taking out the oxygen bomb bottle at intervals of first preset time, shaking, deflating and opening the oxygen bomb bottle after second preset time, collecting absorption liquid in the oxygen bomb bottle, transferring the absorption liquid to a volumetric flask, adding water to dilute the absorption liquid to a volumetric flask constant volume scale, and uniformly mixing to obtain a sample solution;
(3) preparing a standard test solution:
weighing predetermined amounts of fluorine standard stock solution, chlorine standard stock solution and bromine standard stock solution in sequence, mixing the chlorine standard stock solution and the bromine standard stock solution to form chlorine-bromine mixed solution, respectively placing the chlorine-bromine mixed solution and the fluorine standard stock solution into two volumetric flasks, adding water to dilute the chlorine-bromine mixed solution and the fluorine standard stock solution until the volumetric flasks have constant volume scales, and uniformly mixing to obtain fluorine standard solution and chlorine-bromine mixed standard solution;
weighing a plurality of fluorine standard solutions with different preset amounts respectively, transferring a plurality of chlorine and bromine mixed standard solutions with different preset amounts respectively, sequentially and correspondingly placing the solutions into seven volumetric flasks, adding water to dilute the solutions until the volumetric scales of the volumetric flasks are constant, and uniformly mixing the solutions to obtain a fluorine-chlorine-bromine mixed standard series solution;
(4) and (3) measuring the amount of fluorine, chlorine and bromine:
and (3) measuring the contents of fluorine, chlorine and bromine of the sample solution obtained in the step (2) by an ion chromatograph according to the corresponding fluorine-chlorine-bromine mixed standard series solution.
2. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 1, wherein in the step of sample preparation, the weight of a predetermined amount of resin powder sample is 0.15-0.20 g, and the resin powder sample is weighed by 0.0001g standard.
3. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 1, wherein in the step of sample processing, the step of circularly oxygenating is to oxygenate in the sealed oxygen bomb, deflate and oxygenate again after oxygenation is finished, and the step of circularly oxygenating is carried out three times, and the oxygen pressure of the oxygen bomb is controlled to be 1.0-1.5 Mpa.
4. The method for measuring fluorine, chlorine and bromine in the waste circuit board stripping resin powder according to claim 3, characterized in that the predetermined amount of absorption liquid is 20mL, the concentration of the absorption liquid is controlled to be 0.045-0.050 mol/L, the first preset time is 5min, and the second preset time is 30 min.
5. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 1, wherein in the step of preparing the standard test solution, a predetermined amount of fluorine standard stock solution is 5mL, wherein each 1mL of the fluorine standard solution contains 50 μ g of fluorine, a predetermined amount of chlorine standard stock solution is 5mL, a predetermined amount of bromine standard stock solution is 10mL, and wherein each 1mL of the chlorine-bromine mixed standard solution contains 50 μ g of chlorine and 100 μ g of bromine.
6. The method for measuring fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 1, wherein the step of preparing the standard test solution further comprises the steps of:
preparing a fluorine standard stock solution:
weighing a predetermined amount of sodium fluoride serving as a reference substance dried to constant weight within a preset temperature range, placing the sodium fluoride in a volumetric flask, adding water to dilute the sodium fluoride until the volume of the volumetric flask is constant, and uniformly mixing the sodium fluoride and the volumetric flask to obtain a fluorine standard stock solution;
preparing a chlorine standard stock solution:
weighing a predetermined amount of a reference substance sodium chloride burnt to constant weight within a preset temperature range, placing the reference substance sodium chloride into a volumetric flask, adding water to dilute the reference substance sodium chloride until the volumetric flask has constant volume scales, and uniformly mixing the reference substance sodium chloride and the water to obtain a chlorine standard stock solution;
preparing a bromine standard stock solution:
weighing a predetermined amount of potassium bromide serving as a reference substance dried to constant weight within a preset temperature range, placing the potassium bromide in a volumetric flask, adding water to dilute the potassium bromide until the volume of the volumetric flask is constant, and uniformly mixing the potassium bromide and the volumetric flask to obtain a bromine standard stock solution.
7. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 6, wherein in the step of preparing the fluorine standard stock solution, the preset temperature range is 100-105 ℃, the weight of the predetermined amount of sodium fluoride is 2.2110g, and the fluorine standard stock solution contains 1000 μ g of fluorine per 1 mL.
8. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 6, wherein the step of preparing the chlorine standard stock solution comprises the steps of preparing the chlorine standard stock solution at a preset temperature range of 500-600 ℃, wherein the preset amount of sodium chloride weighs 1.6485g, and the chlorine standard stock solution contains 1000 μ g of chlorine per 1 mL.
9. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 6, wherein in the step of preparing the bromine standard stock solution, the preset temperature range is 100-105 ℃, the weight of the preset amount of sodium chloride is 1.4900g, and the bromine standard stock solution contains 1000 μ g bromine per 1 mL.
10. The method for determining fluorine, chlorine and bromine in waste circuit board stripping resin powder according to claim 1, wherein the volume fraction of fluorine, chlorine and bromine in the sample solution is calculated by the formula:
in the formula: omega(B)-represents the percentage of fluorine, chlorine, bromine content, respectively, in units;
rho is the mass concentration of fluorine, chlorine and bromine in the solution to be detected, unit u g/mL;
ρ0-mass concentration of fluorine, chlorine, bromine in the blank solution, unit u g/mL;
V0-total volume of solution tested, in mL;
V1-dividing the volume of the test solution in mL;
V2-volume of the liquid to be tested, in mL;
m is the mass of the sample in g.
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