CN110987564A - Method for extracting black carbon from peat soil - Google Patents

Method for extracting black carbon from peat soil Download PDF

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CN110987564A
CN110987564A CN201911354456.7A CN201911354456A CN110987564A CN 110987564 A CN110987564 A CN 110987564A CN 201911354456 A CN201911354456 A CN 201911354456A CN 110987564 A CN110987564 A CN 110987564A
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black carbon
peat soil
centrifuging
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高传宇
丛金鑫
王国平
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Northeast Institute of Geography and Agroecology of CAS
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Abstract

A method for extracting black carbon from peat soil relates to a method for extracting black carbon from peat soil. The invention aims to solve the technical problems of removal of black carbon to be detected and organic matter interference in the existing black carbon extraction method. The method comprises the following steps: firstly, weighing peat soil, putting the peat soil into a centrifugal tube, then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching, adding an HCl solution, and centrifuging; adding a mixed solution consisting of an HF solution and an HCl solution into the residue, and centrifuging; adding HCl solution into the residue, centrifuging, adding NaOH solution into the residue, and centrifuging; adding K to the residue2Cr2O4And H2SO4The reaction is carried out for 60 hours, and when the solution turns green in the reaction process, K is immediately replaced2Cr2O4And H2SO4Centrifuging the mixed solution to obtain the black carbon. The method is simple and quick, has low laboratory requirements, can greatly save cost, reduce the interference of high-content organic matters, and effectively extract the black carbon in the peat soil. The invention belongs to the field of extraction of black carbon in peat soil.

Description

Method for extracting black carbon from peat soil
Technical Field
The invention relates to a method for extracting black carbon from peat soil.
Background
Black carbon is produced from incomplete combustion of fossil fuels and biomass. Black carbon emitted by human and natural sources can be firstly emitted into the atmospheric environment, and influences global climate change. The black carbon stays in the atmosphere for several days and eventually settles into the soil. Because of its chemical stability, it can be stored in soil carbon reservoir for thousands of years. To better understand the black carbon emission laws and the effects on climate change, the work of reconstructing the black carbon deposition flux during the historical period by the black carbon content of different soils and deposition species has been gradually carried out on a global scale. Currently, there are many methods for testing the black carbon content in soils and sediments, such as direct observation through a microscope, potassium dichromate oxidation, 375 ℃ thermal oxidation, TOT/R methods, etc. (Han et al, 2012; Paroissien et al, 2012; Morales-Molino et al, 2013; Wang et al, 2013). Hammes et al (2007) uses seven international testing methods to measure the black carbon content in twelve testing materials in 2007, and the testing results show that when the black carbon content in the same material is measured, the results measured by different testing methods are different, so that no method can be used for measuring the black carbon in all environmental materials. Currently, there are few studies on the determination of black carbon in peat soils. The existing literature is read to find that only Leifeld et al (2007) measures the content of black carbon in peat soil by a differential thermal analyzer, but the application of the method is not popularized. Therefore, a method suitable for determining the content of black carbon in peat soil needs to be found. Through existing research, it is found that the 375 ℃ thermal oxidation method has a destructive effect on low-temperature generated black carbon (black carbon generated by incomplete combustion), and the 375 ℃ thermal oxidation method removes the black carbon generated by combustion in the peat soil, and the black carbon is often a non-negligible main source in the peat soil. Due to the fact that the peat soil contains high content of organic matters, a large amount of organic matters still remain in the peat soil after the organic matters are removed by the 0.1mol/L NaOH solution in one step, the original oxidation time cannot be achieved when the potassium dichromate is used for oxidizing the organic matters which are not black carbon, and the result is affected. Therefore, a special black carbon pretreatment method is needed to be designed for the soil with high content of organic matters, such as peat soil, on the basis of the traditional chemical oxidation method, and finally the content of the peat soil is measured.
Disclosure of Invention
The invention aims to solve the technical problems of removal of black carbon to be detected and organic matter interference in the conventional black carbon extraction method, and provides a method for extracting black carbon from peat soil.
A method for extracting black carbon from peat soil comprises the following steps:
firstly, weighing 0.5-1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out supernatant;
thirdly, adding a mixed solution consisting of 5ml of HF solution with the concentration of 17mol/L and 5ml of HCl solution with the concentration of 3mol/L into the residue of the second step, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fourthly, adding 10ml of HCl solution with the concentration of 1mol/L into the residue obtained in the third step, reacting for 10 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fifthly, adding 30ml of NaOH solution with the concentration of 0.1mol/L into the residue obtained in the fourth step, reacting for 12 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
sixthly, repeating the step five for 2-4 times;
seventhly, adding 10ml of K into the residue in the step six2Cr2O4The concentration is 0.1mol/L, H2SO42mol/L mixed solution is reacted for 60 hours, and when the solution turns green in the reaction process, 10ml of K is immediately replaced2Cr2O4The concentration is 0.1mol/L, H2SO4And (3) centrifuging the mixed solution with the concentration of 2mol/L for 5 minutes at the centrifugal speed of 3500 rpm to obtain the black carbon.
The method is simple and quick, has low laboratory requirements, can greatly save cost, reduce the interference of high-content organic matters, and effectively extract the black carbon in the peat soil.
The method does not cause extra loss to the black carbon, the step of adding the NaOH solution in the method does not influence the content of the black carbon, and the black carbon in the peat soil can be measured. In the organic soil, a large amount of organic matters are quickly removed, the consumption of chemical reagents in the later period is reduced, the method is green and environment-friendly, the operation is simple, the requirements on the chemical reagents and the experimental environment are low, the method is convenient to develop in most laboratories, and the method is easy to understand by technicians in the field.
Drawings
FIG. 1 is a graph showing the comparison of the results of extracting black carbon from peat soil in experiment one and experiment two
Figure BDA0002335513770000021
Shows the result of extracting black carbon in peat soil by potassium dichromate oxidation in the first experiment,
Figure BDA0002335513770000022
the result of extracting black carbon from peat soil by a thermal oxidation method at 375 ℃ in the second experiment is shown;
FIG. 2 is a graph comparing the results of the extraction process of black carbon from peat soil in experiment one and experiment three.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: in this embodiment, the method for extracting black carbon from peat soil comprises the following steps:
firstly, weighing 0.5-1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant (removing carbonate);
thirdly, adding a mixed solution consisting of 5ml of HF solution with the concentration of 17mol/L and 5ml of HCl solution with the concentration of 3mol/L into the residue of the second step, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant (removing silicate);
fourthly, 10ml of HCl solution with the concentration of 1mol/L is added into the residue of the third step, the reaction is carried out for 10 hours, the mixture is centrifuged at the centrifugal speed of 3500 rpm for 5 minutes, and the supernatant is poured out (the CaF generated in the previous step is removed)2);
Fifthly, adding 30ml of NaOH solution with the concentration of 0.1mol/L into the residue obtained in the fourth step, reacting for 12 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant (removing humic acid twice);
sixthly, repeating the step five for 2-4 times;
seventhly, adding 10ml of K into the residue in the step six2Cr2O4The concentration is 0.1mol/L, H2SO42mol/L mixed solution is reacted for 60 hours, and when the solution turns green in the reaction process, 10ml of K is immediately replaced2Cr2O4The concentration is 0.1mol/L, H2SO4And (3) centrifuging the mixed solution with the concentration of 2mol/L at a centrifugal speed of 3500 rpm for 5 minutes (removing kerogen), and measuring the content of the final residue by an element analyzer (Flash 2000series) to obtain the black carbon.
The second embodiment is as follows: the difference between the first embodiment and the second embodiment is that 1g of peat soil is weighed in the first step. The rest is the same as the first embodiment.
The third concrete implementation mode: the difference between this embodiment and the first or second embodiment is that the fifth step is repeated 3 times in the sixth step. The others are the same as in the first or second embodiment.
The following experiments are adopted to verify the effect of the invention:
a typical peat profile (Shen shop profile) was selected to represent varying degrees of development of peat soil (table 1) for use as the test material in the study.
TABLE 1
Type of soil Ignition loss (%) Degree of humification Dry volume weight g/cm3 Colour(s) Classification
A 69.42±1.71 34.53±0.03 0.24±0.02 Yellow-brown color Peat coal
B 65.12±4.98 40.87±0.87 0.17±0.005 Brown colour Peat soil
C 16.68±4.39 22.80±1.76 0.55±0.08 Black color Deposit material
Experiment one:
the method for extracting black carbon in peat soil by potassium dichromate oxidation comprises the following steps:
firstly, weighing 1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out supernatant;
thirdly, adding a mixed solution consisting of 5ml of HF solution with the concentration of 17mol/L and 5ml of HCl solution with the concentration of 3mol/L into the residue of the second step, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fourthly, adding 10ml of HCl solution with the concentration of 1mol/L into the residue obtained in the third step, reacting for 10 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fifthly, adding 30ml of NaOH solution with the concentration of 0.1mol/L into the residue obtained in the fourth step, reacting for 12 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
sixthly, adding 10ml of K into the residue in the fifth step2Cr2O4The concentration is 0.1mol/L, H2SO42mol/L mixed solution is reacted for 60 hours, and when the solution turns green in the reaction process, 10ml of K is immediately replaced2Cr2O4The concentration is 0.1mol/L, H2SO4And (3) centrifuging the mixed solution with the concentration of 2mol/L at the centrifugal speed of 3500 rpm for 5 minutes, and measuring the content of the final residue by an element analyzer (Flash 2000series) to obtain the black carbon.
Experiment two:
the method for extracting black carbon in peat soil by a thermal oxidation method at 375 ℃ comprises the following steps:
firstly, weighing 1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out supernatant;
thirdly, transferring the residue obtained in the second step into a crucible, heating the crucible in a muffle furnace at 375 ℃ and reacting for 24 hours;
and fourthly, measuring the content of the final residue by using an element analyzer (Flash 2000series) to obtain the black carbon.
The black carbon content of the peat soil was measured using a conventional potassium dichromate oxidation method and a 375 ℃ thermal oxidation method, and the results are shown in fig. 1. The content of black carbon determined by potassium dichromate oxidation method is higher than that determined by thermal oxidation method at 375 ℃. The difference in the material a located above the peat profile is most pronounced. It can be seen that the 375 ℃ thermal oxidation method has a destructive effect on black carbon generated by low-temperature incomplete combustion (below 1000 ℃). And the main source of the black carbon in the peat land is the black carbon generated by natural fire or artificial biomass combustion. Whereas the temperature of a natural fire is usually around 800 ℃. The conventional 375 ℃ thermal oxidation method removes black carbon generated by combustion in the peat soil, and the black carbon is often a non-negligible main source in the peat soil. Due to the fact that the peat soil contains high content of organic matters, a large amount of organic matters still remain in the peat soil after the organic matters are removed by the 0.1mol/L NaOH solution in one step, the original oxidation time cannot be achieved when the potassium dichromate is used for oxidizing the organic matters which are not black carbon, and the result is affected.
Experiment three:
the method for extracting the black carbon in the peat soil comprises the following steps:
firstly, weighing 1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out supernatant;
thirdly, adding a mixed solution consisting of 5ml of HF solution with the concentration of 17mol/L and 5ml of HCl solution with the concentration of 3mol/L into the residue of the second step, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fourthly, adding 10ml of HCl solution with the concentration of 1mol/L into the residue obtained in the third step, reacting for 10 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fifthly, adding 30ml of NaOH solution with the concentration of 0.1mol/L into the residue obtained in the step five, reacting for 12 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
sixthly, repeating the step five for 2 times;
seventhly, adding 10ml of K into the residue in the step six2Cr2O4The concentration is 0.1mol/L, H2SO42mol/L mixed solution is reacted for 60 hours, and when the solution turns green in the reaction process, 10ml of K is immediately replaced2Cr2O4The concentration is 0.1mol/L, H2SO4And (3) centrifuging the mixed solution with the concentration of 2mol/L for 5 minutes at the centrifugal speed of 3500 rpm to obtain the black carbon.
The black carbon content was determined using the international general black carbon reference material (Hammes et al, 2006) purchased from zurich university and compared to the potassium dichromate oxidation method of experiment one. The results are shown in FIG. 2.
As can be seen from fig. 2, the results of the test of the black carbon content in the carbon dust by the method of experiment three and the potassium dichromate oxidation method in experiment one are close to each other, and no significant reduction occurs. The method does not cause extra loss to the black carbon, so that the step of adding the NaOH solution in the method does not influence the content of the black carbon, and the black carbon in the peat soil can be measured. In the organic soil, a large amount of organic matters are quickly removed, the consumption of chemical reagents in the later period is reduced, the method is green and environment-friendly, the operation is simple, the requirements on the chemical reagents and the experimental environment are low, the method is convenient to develop in most laboratories, and the method is easy to understand by technicians in the field.

Claims (3)

1. The method for extracting the black carbon from the peat soil is characterized by comprising the following steps of:
firstly, weighing 0.5-1g of peat soil, putting the peat soil into a 50ml centrifugal tube, and then putting the centrifugal tube into a 55 ℃ water bath kettle for leaching;
secondly, adding 10ml of HCl solution with the concentration of 1mol/l into a centrifuge tube, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out supernatant;
thirdly, adding a mixed solution consisting of 5ml of HF solution with the concentration of 17mol/L and 5ml of HCl solution with the concentration of 3mol/L into the residue of the second step, reacting for 24 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fourthly, adding 10ml of HCl solution with the concentration of 1mol/L into the residue obtained in the third step, reacting for 10 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant;
fifthly, adding 30ml of NaOH solution with the concentration of 0.1mol/L into the residue obtained in the fourth step, reacting for 12 hours, centrifuging for 5 minutes at the centrifugal speed of 3500 rpm, and pouring out the supernatant; .
Sixthly, repeating the step five for 2-4 times;
seventhly, adding 10ml of K into the residue in the step six2Cr2O4The concentration is 0.1mol/L, H2SO42mol/L mixed solution is reacted for 60 hours, and when the solution turns green in the reaction process, 10ml of K is immediately replaced2Cr2O4The concentration is 0.1mol/L, H2SO4And (3) centrifuging the mixed solution with the concentration of 2mol/L for 5 minutes at the centrifugal speed of 3500 rpm to obtain the black carbon.
2. The method for extracting black carbon from peat soil according to claim 1, wherein 1g of peat soil is weighed in the first step.
3. The method of claim 1, wherein step six is repeated five or 3 times.
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