CN112268883B - Method for determining mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry - Google Patents
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Abstract
The invention discloses a method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry, which comprises the following steps: s1: mixing a coal sample, nitric acid and sulfuric acid to obtain a mixed sample; s2: carrying out microwave digestion on the mixed sample, taking out and cooling; s3: adding hydrogen peroxide, and performing microwave digestion again to obtain a digestion solution; s4: adding water into the digestion solution, shaking up, adding water to dilute at a ratio of more than 5 times, filtering, and fixing the volume to obtain the digestion solution after the first dilution; s5: taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid, adding water for the second dilution with the dilution ratio of more than 2 times, and shaking up to obtain the digestion solution after the second dilution; s6: drawing a standard curve of mercury and arsenic, taking the rest digestion solution after the first dilution and the digestion solution after the second dilution, and measuring the mercury and arsenic content in the digested coal sample by adopting an atomic fluorescence spectrophotometer. The invention has the advantages of simple operation method, high test efficiency, accurate test result and the like.
Description
Technical Field
The invention mainly relates to the technical field of measuring the content of elements such as mercury and arsenic in combustible substances, in particular to a method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry.
Background
Mercury and arsenic are common toxic trace elements in coal, can enter a human body through modes of breathing, skin adsorption or food intake and the like, cause damage to the central nerve and various organs of the human body, are accumulative elements, and can cause cancer after long-term chronic poisoning, so that accurate determination of the content of mercury and arsenic in coal has very important significance for environmental protection and human health.
At present, a plurality of methods for detecting mercury and arsenic in coal are available, for example, the national standard GB/T16659-2008 method for measuring mercury in coal adopts a chemical digestion and atomic absorption spectroscopy technology, the pretreatment steps for quantitative detection of mercury are complicated, a target substance and a reagent need to be mixed and digested at high temperature, and a target element needs to be converted into a substance to be detected through a series of redox reactions. The low-pressure high-temperature digestion and reduction processes of the target substance can cause the volatilization loss of elements; meanwhile, a quantitative analysis instrument cold atomic absorption spectrometry and a cold atomic absorption spectrophotometry are adopted, the detection limit of the instrument is large, the detection accuracy of trace elements cannot be enough, the equipment debugging is complicated, the testing time by using the detection method is long, the measurement of one sample usually needs hours or even one day, and the efficiency is low.
A hydride generation-atomic absorption method introduced in the American society for testing materials (ASTM D4606-03) and the national standard GB/T3058 & ltmethod for measuring arsenic in coal & gt 2008 & ltmethod for measuring arsenic in coal & gt is characterized in that a coal sample is mixed with an aldrin and burned, the burned product is dissolved by hydrochloric acid, pentavalent arsenic is reduced to trivalent by potassium iodide, trivalent arsenic is reduced to arsenic hydride by sodium borohydride, the arsenic hydride is introduced into a quartz tube atomizer by taking nitrogen as a carrier gas, and the measurement is carried out by an atomic absorption method. The hydride generation-atomic absorption method uses less reagents and has high precision, and is widely used in the detection of arsenic element at present. However, the pretreatment time of the method is long, the combustion of the aldrin is at least more than five hours, and the whole experimental period is at least two days due to the subsequent sample treatment, transfer and reduction.
The national standard GB/T3058-2008 determination method for arsenic in coal comprises an arsenic-molybdenum blue spectrophotometry, which is an arbitration method. Mixing a coal sample and an Eschka reagent, burning, dissolving a burning substance by hydrochloric acid, adding a reducing agent to reduce pentavalent arsenic into trivalent arsenic, adding zinc particles, releasing hydrogen to release arsenic to form hydrogenated arsenic gas, then absorbing the arsenic gas by an iodine solution and oxidizing the arsenic gas into arsenic acid, adding an ammonium molybdate-hydrazine sulfate solution to generate arsenic-molybdenum blue, and then measuring by a spectrophotometer. The arsenic molybdenum blue spectrophotometry is a classic method for detecting arsenic in coal, and the method is an arbitration method. However, the method has long detection time, more reagents and complicated steps.
The method comprises the steps of simultaneously measuring the content of mercury and arsenic in coal by using an SN/T3521-2013 imported coal and simultaneously measuring hydride generation-atomic fluorescence spectrometry, carrying out microwave digestion on a sample, pre-reducing pentavalent arsenic into trivalent arsenic by using thiourea-ascorbic acid in a dilute nitric acid medium, then using potassium borohydride as a reducing agent to reduce the arsenic and the mercury in the sample into arsenic hydride gas and mercury vapor, introducing argon gas into an atomizer as a carrier gas, simultaneously measuring the fluorescence intensity of arsenic and mercury atoms on a double-channel atomic fluorescence spectrometer, and analyzing the content of the arsenic and the mercury in the coal. However, the method for testing acid removal has low efficiency, the mercury content test result is large in deviation when the standard coal is tested, the arsenic is not removed completely, the test result is obviously low, and the recovery rate is low.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry, which is simple in operation method, short in test time, high in efficiency and more accurate in test result.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry is characterized by comprising the following steps:
step S1: mixing a coal sample, nitric acid and sulfuric acid to obtain a mixed sample;
step S2: carrying out microwave digestion on the mixed sample, taking out and cooling;
step S3: adding hydrogen peroxide, and performing microwave digestion again to obtain a digestion solution;
step S4: adding water into the digestion solution, shaking up, adding water to dilute at a ratio of more than 5 times, filtering, and fixing the volume to obtain the digestion solution after the first dilution;
step S5: taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid and a diluent for second dilution, wherein the dilution ratio is more than 2 times, and shaking up to obtain the digestion solution after the second dilution;
step S6: drawing a standard curve of mercury and arsenic, taking the rest digestion solution after the first dilution and the digestion solution after the second dilution, and measuring the mercury content and the arsenic content in the digested coal sample by adopting an atomic fluorescence spectrophotometer.
As a further improvement of the above technical solution: the coal sample weighed in the step S1 is 50 mg-100 mg, the nitric acid is 5 mL-10 mL, and the sulfuric acid is 2 mL-4 mL.
As a further improvement of the above technical solution: the step S2 specifically includes: and (3) carrying out microwave digestion on the mixed sample, wherein the microwave digestion temperature and time are respectively 95 ℃, 5min, 120 ℃, 10min, 160 ℃ and 5min, and taking out and cooling.
As a further improvement of the above technical solution: the step S3 specifically includes: adding 2-4 mL of hydrogen peroxide, and performing microwave digestion again at 100 ℃ for 5 min.
As a further improvement of the above technical solution: the step S4 specifically includes: and filtering the digestion solution, diluting for the first time, and fixing the volume to 100ml to obtain the digestion solution after the first dilution.
As a further improvement of the above technical solution: the step S5 specifically includes: and (3) taking part of the digestion solution after the first dilution, adding 20mL of thiourea-ascorbic acid, adding water for second dilution, wherein the dilution ratio is more than 2 times, and shaking up to obtain the digestion solution after the second dilution.
As a further improvement of the above technical solution: step S6 specifically includes:
step S6.1: drawing a mercury standard curve, taking the rest digestion solution after the first dilution, and measuring the mercury content in the digestion coal sample by adopting an atomic fluorescence spectrophotometer;
step S6.2: drawing an arsenic standard curve, taking the digestion solution after the second dilution, and measuring the content of arsenic in the digested coal sample by using an atomic fluorescence spectrophotometer.
Compared with the prior art, the invention has the advantages that:
according to the method for determining mercury and arsenic in coal by using the microwave digestion atomic fluorescence spectrometry, the coal sample is subjected to early treatment by using the microwave digestion method, so that element volatilization caused by high-temperature ignition of the treatment method can be avoided, and the loss of elements to be detected can be effectively reduced; the method comprises the steps of diluting twice, cooling after microwave digestion is completed, filtering and diluting the digestion solution by more than 5 times, taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid and water for second dilution by more than 2 times, shaking up, drawing mercury and arsenic standard curves, and testing by adopting an atomic fluorescence spectrometry. According to the invention, the determination of mercury and arsenic can be realized only by sample treatment once, part of the digestion solution after the first dilution is used for arsenic content test after the second dilution, and the rest of the digestion solution after the first dilution is used for mercury content test, so that the test sample can be avoided from being wasted, the test time can be effectively saved, acid removing operation is not required in the test process, the consumption of acid removing time is greatly reduced, and the whole determination method is simple in operation, high in test efficiency and higher in accuracy of the test result.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
Detailed Description
The invention will be described in further detail below with reference to the drawings and specific examples.
Example 1
As shown in figure 1, the method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry comprises the following steps:
step S1: weighing a coal sample, and mixing nitric acid and sulfuric acid to obtain a mixed sample;
step S2: carrying out microwave digestion on the mixed sample, taking out and cooling;
step S3: adding hydrogen peroxide, and performing microwave digestion again to obtain a digestion solution;
step S4: adding water into the digestion solution, shaking up, adding water to dilute at a ratio of more than 5 times, filtering, and fixing the volume to obtain the digestion solution after the first dilution;
step S5: taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid, adding water for the second dilution with the dilution ratio of more than 2 times, and shaking up to obtain the digestion solution after the second dilution;
step S6: drawing a standard curve of mercury and arsenic, taking the rest digestion solution after the first dilution and the digestion solution after the second dilution, and measuring the mercury content and the arsenic content in the digested coal sample by adopting an atomic fluorescence spectrophotometer.
According to the method for determining mercury and arsenic in coal by using the microwave digestion atomic fluorescence spectrometry, the coal sample is subjected to early treatment by using the microwave digestion method, so that element volatilization caused by high-temperature ignition of the treatment method can be avoided, and the loss of elements to be detected can be effectively reduced; the method comprises the steps of diluting twice, cooling after microwave digestion is completed, filtering and diluting the digestion solution by more than 5 times, taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid, adding water for the second dilution, diluting by more than 2 times, shaking up, drawing mercury and arsenic standard curves, and testing by adopting an atomic fluorescence spectrometry. According to the invention, the determination of mercury and arsenic can be realized only by sample treatment once, part of the digestion solution after the first dilution is used for arsenic content test after the second dilution, and the rest digestion solution after the first dilution is used for mercury content test, so that the waste of test samples is avoided, the test time is effectively saved, the acid removing operation is not required in the test process, the consumption of the acid removing time is greatly reduced, the whole determination method is simple to operate, the test efficiency is high, and the test result is higher in accuracy.
In this embodiment, the coal sample weighed in step S1 is 50mg to 100mg, the nitric acid amount is 5mL to 10mL, and the sulfuric acid amount is 2mL to 4 mL.
In this embodiment, step S2 specifically includes: performing microwave digestion on the sample, wherein the microwave digestion temperature and time are respectively 95 ℃, 5min, 120 ℃, 10min, 160 ℃ and 5min, taking out the sample and cooling, preferably, the cooling temperature is 60 ℃. The mercury and arsenic in the sample can be effectively dissolved out through microwave digestion, and the digestion time can be effectively shortened.
In this embodiment, step S3 specifically includes: adding 2-4 mL of hydrogen peroxide, and performing microwave digestion again at 100 ℃ for 5 min.
In this embodiment, step S4 specifically includes: and filtering the digestion solution, diluting for the first time, diluting and fixing the volume to 100ml to obtain the digestion solution after the first dilution, wherein the dilution of the digestion solution is more than 5 times.
In this embodiment, step S5 specifically includes: and (3) taking 20mL of digestion solution after the first dilution, adding 20mL of thiourea-ascorbic acid, adding water for the second dilution, and fixing the volume to 100 mL.
According to the method, the concentration of nitrogen oxides and nitrite is greatly reduced through two times of dilution, acid removing operation is not needed, the testing accuracy is improved, the acid removing time is shortened, and the testing efficiency is greatly improved.
In this embodiment, step S6 specifically includes: step S6.1: drawing a mercury standard curve, taking the rest digestion solution after the first dilution, and measuring the mercury content in the digestion coal sample by adopting an atomic fluorescence spectrophotometer;
step S6.2: drawing an arsenic standard curve, taking the digestion solution after the second dilution, and measuring the content of arsenic in the digestion coal sample by adopting an atomic fluorescence spectrophotometer. The test results of digesting arsenic and mercury in the coal sample are shown in the table 1 and the table 2:
TABLE 1
| Sample name | Arsenic test value (ppm) | Marking value | Degree of uncertainty | Deviation of | Recovery (%) |
| W1-161-01 | 15.550 | 16 | 2 | -0.450 | 97.18 |
| W1-161-02 | 14.850 | 16 | 2 | -1.150 | 92.81 |
| W1-162-01 | 11.008 | 13 | 2 | -1.992 | 84.68 |
| W1-162-02 | 11.170 | 13 | 2 | -1.830 | 85.92 |
TABLE 2
| Sample name | Mercury test value (ppm) | Marking value | Degree of uncertainty | Deviation of | Recovery (%) |
| W1-161-01 | 0.567 | 0.576 | 0.054 | -0.009 | 98.438 |
| W1-161-02 | 0.552 | 0.576 | 0.054 | -0.024 | 95.833 |
| W1-162-01 | 0.789 | 0.794 | 0.058 | -0.005 | 99.370 |
| W1-162-02 | 0.761 | 0.794 | 0.058 | -0.033 | 95.844 |
Example 2
A method for determining mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry is basically the same as that in embodiment 1 in steps S1-S4, and is different in that 50mL of digestion solution after first dilution is taken, 20mL of thiourea-ascorbic acid and dilution solution are added for second dilution and volume is determined to be 100mL, the digestion solution is diluted by 2 times, a standard curve of mercury and arsenic is drawn, the remaining digestion solution after first dilution and the digestion solution after second dilution are taken, and mercury content and arsenic content in a digestion coal sample are determined by an atomic fluorescence spectrophotometer. The test results of digesting arsenic and mercury in the coal sample are shown in tables 3 and 4:
TABLE 3
TABLE 4
According to the test result, the digestion solution is subjected to microwave digestion and diluted twice by adopting the method to obtain the digestion solution after the first dilution and the digestion solution after the second dilution, the mercury and arsenic contents in the coal sample are measured by adopting an atomic fluorescence spectrophotometer, the deviation range of the arsenic contents is within +/-2, the deviation range of the mercury contents is within +/-0.06, the recovery rate is high, the test result is superior to that of the method in the existing standard, and the method is simple to operate, short in test time and high in test efficiency.
Comparative example:
in the comparison example, the experiment is carried out by adopting a method of simultaneously measuring the content of arsenic and mercury in SN/T3521-2013 imported coal and hydrogen generation-atomic fluorescence spectrometry, and the method comprises the following specific steps:
s01, digestion step: weighing 0.1g of standard coal, putting the standard coal into a digestion tube, adding 3mL of nitric acid, heating the mixture for 15min at 60 ℃ by using an electric heating plate, cooling the mixture, adding 3mL of nitric acid, 1mL of hydrogen peroxide and 0.5mL of hydrofluoric acid, filling the mixture into an outer tank after the reaction is eased, screwing and sealing the mixture, and putting the mixture into a microwave digestion instrument for microwave digestion (the temperature and the time of the microwave digestion are 135 ℃, 5min, 165 ℃, 5min, 190 ℃, 20 min); the solution is transparent orange yellow after the digestion is completed.
S02, acid removal: cooling the digestion solution, washing the inner wall of the digestion tank with water, and heating the digestion tank on an electric heating plate at 100 ℃ for 1 h;
s03, transferring to fix the volume: and completely transferring the residual solution into a 100mL volumetric flask by using water, adding 5mL of saturated boric acid solution before constant volume, diluting to 60mL by using water, cooling, adding 20mL of thiourea ascorbic acid solution, diluting to a scale by using water, shaking up, and standing for 0.5h for detection.
S04: drawing an arsenic and mercury standard curve, and measuring the content of mercury and arsenic in the digested coal sample by using an atomic fluorescence spectrometer. The test results of the arsenic and mercury digestion in the coal sample are shown in the following table:
TABLE 5
TABLE 6
The test results show that the method of simultaneously measuring the arsenic and mercury contents in SN/T3521-2013 imported coal and hydride generation-atomic fluorescence spectrometry is adopted to measure the mercury and arsenic contents in the coal sample, two standard coals are respectively measured twice, the arsenic content test results of 4 measured samples are low, and the recovery rate is very low; the mercury content of 4 test samples has 3 result deviation ranges exceeding the uncertainty of standard coal.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (6)
1. A method for measuring mercury and arsenic in coal by microwave digestion atomic fluorescence spectrometry is characterized by comprising the following steps:
step S1: mixing a coal sample, nitric acid and sulfuric acid to obtain a mixed sample;
step S2: carrying out microwave digestion on the mixed sample, taking out and cooling;
step S3: adding hydrogen peroxide, and performing microwave digestion again to obtain a digestion solution;
step S4: adding water into the digestion solution, shaking up, adding water to dilute at a ratio of more than 5 times, filtering, and fixing the volume to obtain the digestion solution after the first dilution;
step S5: taking part of the digestion solution after the first dilution, adding thiourea-ascorbic acid, adding water for the second dilution with the dilution ratio of more than 2 times, and shaking up to obtain the digestion solution after the second dilution;
step S6: drawing a standard curve of mercury and arsenic, taking the rest digestion solution after the first dilution and the digestion solution after the second dilution, and measuring the mercury content and the arsenic content in the digested coal sample by adopting an atomic fluorescence spectrophotometer; the method specifically comprises the following steps: step S6.1: drawing a mercury standard curve, taking the rest digestion solution after the first dilution, and measuring the mercury content in the digestion coal sample by adopting an atomic fluorescence spectrophotometer;
step S6.2: drawing an arsenic standard curve, taking the digestion solution after the second dilution, and measuring the content of arsenic in the digested coal sample by using an atomic fluorescence spectrophotometer.
2. The method for determining mercury and arsenic in coal by microwave-assisted atomic fluorescence spectrometry according to claim 1, wherein the coal sample weighed in step S1 is 50mg to 100mg, the nitric acid amount is 5mL to 10mL, and the sulfuric acid amount is 2mL to 4 mL.
3. The method for determining mercury and arsenic in coal by microwave-assisted atomic fluorescence spectrometry according to claim 2, wherein the step S2 specifically comprises: and (3) carrying out microwave digestion on the mixed sample, wherein the microwave digestion temperature and time are respectively 95 ℃, 5min, 120 ℃, 10min, 160 ℃ and 5min, and taking out and cooling.
4. The method for determining mercury and arsenic in coal by microwave-assisted atomic fluorescence spectrometry according to claim 3, wherein the step S3 specifically comprises: adding 2-4 mL of hydrogen peroxide, and performing microwave digestion again at 100 ℃ for 5 min.
5. The method for determining mercury and arsenic in coal by microwave-assisted atomic fluorescence spectrometry according to claim 4, wherein the step S4 specifically comprises: and filtering the digestion solution, diluting for the first time, and fixing the volume to 100ml to obtain the digestion solution after the first dilution.
6. The method for determining mercury and arsenic in coal by microwave-assisted atomic fluorescence spectrometry according to claim 5, wherein the step S5 specifically comprises: and (3) taking part of the digestion solution after the first dilution, adding 20mL of thiourea-ascorbic acid and a diluent for second dilution, wherein the dilution ratio is more than 2 times, and shaking up to obtain the digestion solution after the second dilution.
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