CN111239276A - Method for measuring organic matter content of soil and sludge - Google Patents
Method for measuring organic matter content of soil and sludge Download PDFInfo
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Abstract
The invention relates to the technical field of environmental monitoring and analysis, and discloses a method for measuring organic matter content of soil and sludge. The process is based on the headspace gas chromatography (HS-GC) technique of redox reactions (i.e. OM is converted to carbon dioxide using dichromate). For soil samples (lower OM content), it was measured directly by HS-GC. For the sludge sample (with higher OM content), the method comprises the following steps: (1) sample pretreatment; (2) digesting a sample; (3) detecting the digestion sample by adopting HS-GC; (4) and (6) calculating a result. The invention determines the residual quantity of the potassium dichromate in the reaction solution, thereby calculating the OM content in the sample. The result shows that the method has good reproducibility and high accuracy, the relative standard deviation is less than 5%, and the recovery rate is between 97.9% and 106%. On the basis of headspace automatic sample introduction, batch analysis for high-throughput determination of OM content of a sample is realized.
Description
Technical Field
The invention relates to the technical field of environmental monitoring and analysis, in particular to a method for measuring organic matter content of soil and sludge.
Background
The organic matter content (OM) in soil and municipal sludge is an important parameter to characterize fertility levels. The organic matters in the soil have important influence on improving the coefficient performance and the buffering performance of the soil, enriching the growth environment of microorganism species and improving the fertility and the structure of the soil. Municipal sludge is a by-product of sewage treatment in sewage treatment plants, and is commonly used for landfilling, incineration and land utilization. As municipal sludge contains a large amount of organic matters, the method has a good effect of improving soil and can be used as resources. The organic matter content in soil and sludge is directly related to its ecological functions, such as: biological growth, nutrient decomposition and transformation, pollutant migration and the like. Therefore, the analysis method capable of effectively measuring the content of the organic matters in the soil and the municipal sludge has important guiding significance for realizing resource utilization of the sludge and improving the soil.
At present, the method for measuring the content of organic matters in soil and municipal sludge mainly comprises a burning method and a chemical oxidation method. The burn method is to dry the sample at 105 deg.C (2h) and then weigh the sample. And directly burning the sample at the high temperature of 350-1000 ℃ for 2-5 h so as to completely decompose the organic matters in the sample. According to the weight of the sample before and after burning, the weight lost in burning can be calculated, namely: the content of organic matter. The biggest problem with this approach is some inorganic components, such as: carbonate, etc. are also lost when the sample is burned, thus making the measurement value by the burn method large. Obviously, the process is time consuming and laborious. Although the Elemental Analyzer (EA) can effectively analyze many non-metallic elements, including carbon, it cannot be easily applied to OM analysis due to interference from inorganic carbon. Studies have shown that a very time consuming pre-treatment procedure (6-12 hours, depending on the sample properties) must be employed to eliminate inorganic carbon interference before the EA test is performed.
The invention patent application with application publication number CN110470665A discloses a method for measuring soil organic matters, firstly, a soil sample is put into a dry triangular flask, potassium dichromate sulfuric acid solution with preset molar concentration is added into the triangular flask, and the triangular flask containing the mixed solution is put into an oven to be heated; taking out the heated triangular flask, cooling, and adding distilled water with a preset volume to enable the volume of the mixed solution in the triangular flask to reach a preset volume; and adding an o-phenanthroline ferrous indicator with the capacity matched with the acidity of the mixed solution according to the acidity of the mixed solution, and titrating the mixed solution in the triangular flask by using a ferrous sulfate solution, thereby calculating the organic matter content of the soil. The invention patent application with application publication number CN110470665A discloses a method for measuring the content of organic matters in soil, which is characterized in that: the method comprises the following steps: (1) sampling soil to be measured; (2) preparing a potassium dichromate-sulfuric acid solution, wherein the concentration of the solution is 1 mol/L; (3) carrying out titration; (4) and measuring and calculating. The invention patent application with the application publication number of CN110470665A discloses a method for measuring organic matters in soil, which comprises the following steps: (1) sampling and carrying out sample treatment; (2) preparing a standard solution for later use; (3) transferring 0.5-1 g of the sample treated in the step (1) into a test tube, adding 5ml of potassium dichromate standard solution, adding 5ml of concentrated sulfuric acid, shaking up, placing a condensation funnel at the opening of the test tube, heating to 180-200 ℃, and preserving heat for 5-8 minutes; (4) after cooling, the inner walls of the funnel and the test tube are washed by distilled water, the total volume of the washing liquid is controlled within 50ml, then 3 drops of the o-phenanthroline indicator are added, and the standard working solution prepared in the step (2) is used for titration.
The above existing technologies have the following disadvantages: the operation process is time-consuming and labor-consuming, and the measured value is easily large, and the method is easily interfered by inorganic carbon and reducing substances, and cannot be simply applied to organic matter analysis.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for measuring the organic matter content of soil and sludge.
The purpose of the invention is realized by the following technical scheme:
a method for measuring the content of organic substances in soil and sludge includes such steps as measuring the content of CO generated by the reaction between soil or sludge and strong oxidizing acid by headspace gas chromatograph2The method for indirectly measuring the organic matter is realized according to the following steps:
1. soil sample assay
(11) Sample pretreatment: weighing 0.05-0.2 g of soil sample in a headspace bottle, and adding K2Cr2O7A solution; in addition, samples of the same mass were acidified with hydrochloric acid as a blank;
(12) sample redox reaction: immediately covering the headspace bottle in the step (11), shaking up, placing the headspace bottle in a condition of 120-140 ℃ for oxidation-reduction reaction, taking out the test tube, and cooling to normal temperature;
(13) establishing a standard curve: respectively measuring organic matter standard solutions with different volumes into a headspace bottle, and respectively preparing low-content organic matter standard solutions with the concentration of 0, 10, 20, 40,80 and 100 g/kg; placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
(14) sample detection: placing the headspace bottle in the step (12) into a headspace sample injector, performing headspace gas chromatography analysis by using the same operation conditions of the headspace sample injector and the gas chromatograph as those in the step (13), and recording CO of the sample2The resulting signal value;
(15) and (4) calculating a result: comparing the gas chromatography signal value obtained in the step (14) with the standard curve obtained in the step (13), and calculating to obtain the content of organic matters in the soil;
1.2 sludge sample determination
(21) Sample pretreatment: weighing 0.05-0.2 g of sludge sample in a digestion tube, and adding K2Cr2O7Solution and concentrated sulfuric acid solution with the same volume;
(22) sample digestion: preheating a graphite digestion instrument to 170-180 ℃ in advance, putting the digestion tubes in the step (21), timing when bubbles are generated in the liquid in the digestion tubes when the liquid is boiled, boiling for 5-10min, taking out the digestion tubes, and cooling;
(23) establishing a standard curve: respectively measuring organic matter standard solutions with different volumes into a headspace bottle, and respectively preparing high-content organic matter standard solutions with the contents of 0, 100, 200, 400 and 800 g/kg; placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
(24) sample detection: putting the digestion solution after digestion in the step (22) into a small test tube, and then putting the small test tube into a headspace bottle; slowly adding oxalic acid solution into the headspace bottle, immediately covering the headspace bottle, shaking, analyzing with headspace gas chromatograph, and recording CO2The resulting signal value;
(25) and (4) calculating a result: CO obtained in step (24)2Comparing the signal value with the standard curve obtained in the step (23), and calculating to obtain the content of organic matters in the sludge;
preferably, the sampling mass of the soil sample in the step (11) is 0.05-0.2 g, and the soil sample is filled in a 20ml headspace bottle.
Preferably, the concentration of the hydrochloric acid is 0.001-0.01 mol/L, K2Cr2O7The concentration of the solution is 0.136mol/L, and the volume is 1-5 mL.
Preferably, the time of the oxidation-reduction reaction in the step (12) is 10-40 min.
Preferably, the conditions for the analysis by headspace gas chromatograph in step (13) are:
headspace operating conditions: the furnace temperature is 50-100 ℃, the pipeline temperature is 60-110 ℃, the transmission line temperature is 70-120 ℃, the balancing time is 3-10 min, the shaking degree is a strong level, and the sample interval is 3-15 min;
the gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the pressure of a sample inlet is 6kPa, the temperature of a column box is 30-100 ℃, the running time is 3-10 min, and the temperature of a TCD detector is 150-250 ℃.
Preferably, the amount of the sludge sample in the step (21) is 0.05-0.2 g, 5-10ml of 0.136mol/L potassium dichromate is added, the concentration of concentrated sulfuric acid is 18.4mol/L, and 5-10ml of concentrated sulfuric acid solution is added.
And (3) putting 0.1-2 mL of digested liquid into a headspace bottle, slowly adding 1-5mL of 0.5-2mol/L oxalic acid solution into the headspace bottle, immediately covering the headspace bottle, shaking up, and analyzing by a headspace gas chromatograph.
Preferably, the headspace gas chromatograph analyzes the headspace operating conditions in step (23): 50-100 ℃, the pipeline temperature is 60-110 ℃, the transmission line temperature is 70-120 ℃, the balancing time is 5-10min, the shaking degree is a strong level, and the sample interval is 6-12 min. The gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the pressure of a sample inlet is 6kPa, the temperature of a column box is 30-100 ℃, the running time is 2-10 min, and the temperature of a TCD detector is 150-250 ℃.
Preferably, the soil comprises sandy soil, brown soil and laterite soil; the sludge comprises excess sludge of a sewage treatment plant and sediment sludge of rivers, lakes and reservoirs.
And (3) determining by using HS-GC according to standard solutions with different organic matter contents to respectively obtain calibration curves of the soil sample and the sludge sample. The standard curve is fitted linearly using a mathematical representation, that is:
the linear regression equation of the organic matter standard curve with low content (0-100 g/kg) is as follows:
A＝29782(±854)×c+84793(±51946)(n＝6,R2＝0.997)
the linear regression equation of the organic matter standard curve with high content (0-800 g/kg) is as follows:
A＝3955.75(±51.5)×c+2892(±21219)(n＝6,R2＝0.999)。
according to the invention, by utilizing the headspace gas chromatography, potassium dichromate can oxidize organic matters to generate CO under an acidic condition2Thus can be used to treat CO in the process2And detecting to quantitatively analyze the organic matters.
Under the strong acid environment, organic matters in soil and sludge can be oxidized by potassium dichromate, and Cr6+Reduction to Cr3+That is:
3C (for organic substance) +2Cr2O7 2-+16H+→3CO2↑+4Cr3++8H2O。
The inventors have unexpectedly discovered that more carbon dioxide is produced in the headspace bottle when the organic content of the sample is higher. The high pressure caused by carbon dioxide may cause problems with gas leakage and non-linearity in the process calibration. Therefore, a small amount of digestion solution after reaction is taken, oxalic acid is added into the digestion solution, and the digestion solution and potassium dichromate are subjected to oxidation-reduction reaction, namely: 2Cr2O7 2-+3C2H2O4+8H+→6CO2↑+2Cr3++7H2O。
Therefore, after the sludge is digested, organic matters are oxidized as shown in the formula, and CO can be measured through headspace gas chromatography2To quantify.
Compared with the prior art, the invention has the following technical effects:
the invention relates to a method for measuring organic matters in soil and sludge, which is suitable for samples with organic matter content in any range. The method has the advantages of high determination speed, high accuracy of analysis results, good reproducibility and simple operation, and realizes the analysis of batch samples.
The invention establishes a method for measuring OM content in soil and sludge samples based on a chemical reaction headspace gas chromatography. The result shows that the method has good reproducibility and high accuracy, the relative standard deviation is less than 5%, and the recovery rate is between 97.9% and 106%. On the basis of a headspace automatic sampler, the OM content in soil and sludge is rapidly determined, and the analysis of batch samples is realized.
Drawings
FIG. 1 is a schematic diagram of an analysis experiment of a soil sample;
FIG. 2 is a schematic diagram of an analysis experiment of a sludge sample.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto.
Example 1 testing of soil samples
A method for measuring the organic matter content of soil comprises the following steps:
(11) pretreating a soil sample: grinding a natural air-dried soil sample of a farmland at Guangxi university, and sieving the ground sample with a 60-mesh sieve; the soil was laterite, pH 4.9. 0.05g of soil sample is weighed into a headspace bottle and 2ml of K is added quantitatively by means of a pipette2Cr2O7Putting the solution 2 into a small test tube into a centrifuge tube, and adding 2mL of concentrated sulfuric acid into a headspace bottle in advance, wherein a sample with the same mass is acidified by hydrochloric acid (0.005mol/L, 4mL) to serve as a blank control;
(12) sample redox reaction: immediately covering the headspace bottle, shaking to make K in the small test tube2Cr2O7Fully and uniformly mixing the solution with a concentrated sulfuric acid solution in a headspace bottle, performing oxidation-reduction reaction for 20min at the temperature of 120-140 ℃, taking out a test tube, and cooling to normal temperature;
(13) establishing a standard curve: preparing a series of low-content organic matter standard solutions; placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
headspace operating conditions: the furnace temperature is 60 ℃, the pipeline temperature is 70 ℃, the transmission line temperature is 80 ℃, the balancing time is 3min, the shaking degree is a strong level, and the sample interval is 4 min.
Gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the injection port pressure is 6kPa, the split ratio is 0.1: 1, the temperature of a column box is 30 ℃, the running time is 3min, and the temperature of a TCD detector is 250 ℃.
(14) Sample detection: analyzing by headspace gas chromatograph, recording CO2The resulting signal value;
(15) and (4) calculating a result: substituting the gas chromatography signal value band obtained in the step (4) into the following formula to obtain the content OM of organic matters in the soil;
example 2 testing of sludge samples
A method for measuring the organic matter content of sludge comprises the following steps:
(21) sample pretreatment: a0.05 g sample of the sludge was weighed into a digestion tube, and 10mL of 0.136mol/L potassium dichromate solution and 10mL of concentrated sulfuric acid solution were added slowly and accurately with a pipette (when about 3mL was added, the tube was shaken to disperse the soil).
(22) Sample digestion: preheating a graphite digestion instrument to 170-180 ℃ in advance, putting the digestion tubes in the step (21), timing when bubbles are generated in the liquid in the digestion tubes when the liquid is boiled, boiling for 5-10min, taking out the digestion tubes, and cooling;
(23) establishing a standard curve: preparing a series of organic matter standard solution with high content; and (3) placing the headspace bottle containing the standard solution to be detected in a headspace sample injector, setting the operating conditions of the headspace sample injector and the operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration.
Headspace operating conditions: the furnace temperature is 60 ℃, the pipeline temperature is 70 ℃, the transmission line temperature is 80 ℃, the balancing time is 10min, the shaking degree is a strong level, and the sample interval is 11 min.
Gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the injection port pressure is 6kPa, the split ratio is 0.1: 1, the temperature of a column box is 30 ℃, the running time is 3min, and the temperature of a TCD detector is 250 ℃.
(24) Sample detection: putting 1mL of the digested liquid obtained in the step (22) into a small test tube, and then putting the small test tube into a headspace bottle; slowly adding 5mL oxalic acid solution (1mol/L) into the headspace bottle, immediately covering the headspace bottle, shaking, analyzing by headspace gas chromatograph, and recording CO2The resulting signal value;
(25) and (4) calculating a result: CO obtained in step (24)2Signal value and the mark obtained in step (23)Comparing the standard curves, and calculating to obtain the content of organic matters in the sludge
Standard curve:
measuring organic matter standard solutions with different volumes in a headspace bottle respectively to prepare 0, 10, 20, 40,80 and 100g/kg of low-content organic matter standard solution and 0, 100, 200, 400 and 800g/kg of high-content organic matter standard solution. Placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
wherein the low content was measured according to the method for measuring the organic matter content in the soil sample of example 1;
the high content was measured according to the method for measuring the organic content in the organic solid waste sample of example 2.
And (4) determining by using HS-GC according to standard solutions with different organic matter contents. Calibration curves for the soil sample and the sludge sample were obtained, respectively. They can be expressed mathematically as by linear regression fitting to the standard curve above, giving the following equations, respectively:
A＝29782(±854)×c+84793(±51946)(n＝6,R2＝0.997) (1)
A＝3955.75(±51.5)×c+2892(±21219)(n＝6,R2＝0.999) (2)
wherein A is a gas chromatography signal value; c is the organic matter content. The formulas (1) and (2) are linear regression equations of organic matter standard curves with low content (0-100 g/kg) and high content (0-800 g/kg), respectively.
Based on the formulas (1) and (2), the organic matters in the soil and the sludge can be calculated by the following formulas:
in the formula, A and A. -gas chromatographic signal values of sample and blank.
Examples 3 to 5 examination of various samples
Examples 3 to 5 were conducted on different samples, and the conditions of the respective testing processes are shown in table 1, and the other non-listed working soils were the same as example 1, and the sludge was the same as example 2.
TABLE 1 detection conditions for each of the samples of examples 3 to 5
Note: N/A in the table indicates that this step is absent
Comparative examples 1 to 3
The process conditions of comparative examples 1 to 3 are shown in Table 2, the same operation soil as example 1 and the same sludge as example 2 are not shown.
TABLE 2 Process conditions for comparative examples 1 to 3
Note: N/A in the table indicates that this step is absent
Method accuracy
(1) Reproducibility test
The examples and comparative examples each were measured in 5 replicates by headspace gas chromatography. As can be seen from Table 3, the relative standard deviation of organic matter content of soil and sludge obtained by headspace gas chromatography was less than 4.71%. Therefore, the method can be considered to have better repeatability for detecting the organic matter content. However, as can be seen from comparative example and table 4, if the operational test parameter conditions are not within the range of the method, the method accuracy cannot be guaranteed, and the method cannot exert the test advantages of the soil or sludge sample, specifically, the standard deviation is more than 15%.
Table 3 example repeated tests for headspace gas chromatography
Table 4 repeatability test for comparative example headspace gas chromatography
(2) Spiked recovery test
The accuracy of the method is verified by a standard addition recovery test, namely adding a known amount of OM into an actual soil or sludge sample, and determining the recovery amount. Tables 5 and 6 show the result of the spiking recovery test, and the spiking recovery rate of the headspace gas chromatography for determining the organic matter content is 97.9-106%, which shows that the method has good accuracy in the OM content determination of soil and sludge samples.
TABLE 5 recovery by spiking of headspace gas chromatography
TABLE 6 recovery by spiking of headspace gas chromatography
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (9)
1. A method for measuring the organic matter content of soil and sludge is characterized in that a headspace gas chromatograph is used for measuring the content of CO generated by the reaction of a soil sample or a sludge sample and a strong oxidizing acid2The method for indirectly measuring the organic matter is realized according to the following steps:
1.1 soil sample determination
(11) Sample pretreatment: weighing 0.05-0.2 g of soil sample in a headspace bottle, and adding K2Cr2O7A solution; in addition, samples of the same mass were acidified with hydrochloric acid as a blank;
(12) sample redox reaction: immediately covering the headspace bottle in the step (11), shaking up, placing the headspace bottle in a condition of 120-140 ℃ for oxidation-reduction reaction, taking out the test tube, and cooling to normal temperature;
(13) establishing a standard curve: respectively measuring organic matter standard solutions with different volumes into a headspace bottle, and respectively preparing low-content organic matter standard solutions of 0-100 g/kg; placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
(14) sample detection: placing the headspace bottle in the step (12) into a headspace sample injector, performing headspace gas chromatography analysis by using the same operation conditions of the headspace sample injector and the gas chromatograph as those in the step (13), and recording CO of the sample2The resulting signal value;
(15) and (4) calculating a result: comparing the gas chromatography signal value obtained in the step (14) with the standard curve obtained in the step (13), and calculating to obtain the content of organic matters in the soil;
1.2 sludge sample determination
(21) Sample pretreatment: weighing 0.05-0.2 g of sludge sample in a digestion tube, and adding K2Cr2O7Solution and concentrated sulfuric acid solution with the same volume;
(22) sample digestion: preheating a graphite digestion instrument to 170-180 ℃ in advance, putting the digestion tubes in the step (21), timing when bubbles are generated in the liquid in the digestion tubes when the liquid is boiled, boiling for 5-10min, taking out the digestion tubes, and cooling;
(23) establishing a standard curve: respectively measuring organic matter standard solutions with different volumes into a headspace bottle, and respectively preparing high-content organic matter standard solutions of 0-800 g/kg; placing a headspace bottle containing a standard solution to be detected in a headspace sample injector, setting operating conditions of the headspace sample injector and operating conditions of a gas chromatograph, then carrying out headspace gas chromatography analysis and detection, and obtaining a standard curve according to the corresponding relation between the obtained carbon dioxide chromatographic peak area signal value and the organic matter standard solution with known concentration;
(24) sample detection: putting the digestion solution after digestion in the step (22) into a small test tube, and then putting the small test tube into a headspace bottle; slowly adding oxalic acid solution into the headspace bottle, immediately covering the headspace bottle, shaking, analyzing with headspace gas chromatograph, and recording CO2The resulting signal value;
(25) and (4) calculating a result: CO obtained in step (24)2And (4) comparing the signal value with the standard curve obtained in the step (23), and calculating to obtain the content of organic matters in the sludge.
2. The method for measuring the organic matter content of the soil and the sludge according to claim 1, wherein the sampling mass of the soil sample in the step (11) is 0.05-0.2 g, and the soil sample is filled in a 20mL headspace bottle.
3. The method for determining the organic matter content of soil and sludge according to claim 1, wherein K is determined in step (11)2Cr2O7The concentration of the solution is 0.136mol/L, the concentration of the hydrochloric acid is 0.001-0.01 mol/L, and the volume is 1-5 mL.
4. The method for measuring the organic matter content of the soil and the sludge according to claim 1, wherein the time of the oxidation-reduction reaction in the step (12) is 10-40 min.
5. The method for determining the organic matter content of soil and sludge according to claim 1, wherein the conditions of the headspace gas chromatograph analysis in the step (13) are as follows:
headspace operating conditions: the furnace temperature is 50-100 ℃, the pipeline temperature is 60-110 ℃, the transmission line temperature is 70-120 ℃, the balancing time is 3-10 min, the shaking degree is a strong level, and the sample interval is 3-15 min;
the gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the pressure of a sample inlet is 6kPa, the temperature of a column box is 30-100 ℃, the running time is 2-10 min, and the temperature of a TCD detector is 150-250 ℃.
6. The method for measuring the organic matter content of the soil and the sludge according to claim 1, wherein the amount of the sludge sample in the step (21) is 0.05-0.02 g, 5-10mL of 0.136mol/L potassium dichromate solution is added, the concentration of concentrated sulfuric acid is 18.4mol/L, and 5-10mL of concentrated sulfuric acid solution is added.
And (3) putting 0.1-2 mL of digested liquid into a headspace bottle, slowly adding 1-5mL of 0.5-2mol/L oxalic acid solution into the headspace bottle, immediately covering the headspace bottle, shaking up, and analyzing by a headspace gas chromatograph.
7. The method for determining the organic matter content of the soil and the sludge according to claim 1, wherein the analysis conditions of the headspace gas chromatograph in the step (23) are as follows:
headspace operating conditions: 50-100 ℃, the pipeline temperature is 60-110 ℃, the transmission line temperature is 70-120 ℃, the balancing time is 5-10min, the shaking degree is a strong level, and the sample interval is 6-12 min;
the gas chromatography operating conditions comprise that a GS-Q type capillary chromatographic column (30m multiplied by 0.53mm) is used in the gas chromatography operating conditions, the pressure of a sample inlet is 6kPa, the temperature of a column box is 30-100 ℃, the running time is 2-10 min, and the temperature of a TCD detector is 150-250 ℃.
8. The method of claim 1, wherein the soil comprises sandy soil, brown soil and laterite soil; the sludge comprises excess sludge of a sewage treatment plant and sediment sludge of rivers, lakes and reservoirs.
9. The method for determining the organic matter content of soil and sludge according to claim 1, wherein the calibration curve of the soil sample and the sludge sample is:
0-100 g/kg is a linear regression equation of a low-content organic matter standard curve:
A＝29782(±854)×c+84793(±51946)(n＝6,R2＝0.997)
0-800 g/kg is a linear regression equation of a high-content organic matter standard curve:
A＝3955.75(±51.5)×c+2892(±21219)(n＝6,R2＝0.999)。
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