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HJ 695-2014: Soil. Determination of organic carbon. Combustion oxidation nondispersive infrared absorption method
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Soil. Determination of organic carbon. Combustion oxidation nondispersive infrared absorption method
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HJ 695-2014
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Basic data | Standard ID | HJ 695-2014 (HJ695-2014) | | Description (Translated English) | Soil. Determination of organic carbon. Combustion oxidation nondispersive infrared absorption method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Word Count Estimation | 9,984 | | Date of Issue | 3/13/2014 | | Date of Implementation | 7/1/2014 | | Quoted Standard | HJ/T 166; HJ 613 | | Regulation (derived from) | Ministry of Environmental Protection Notice No. 17 of 2014 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the determination of soil organic carbon combustion oxidation a non-dispersive infrared method. This Standard applies to the determination of organic carbon in the soil, does not apply to the determination of sludge contaminated so | HJ 695-2014: Soil. Determination of organic carbon. Combustion oxidation nondispersive infrared absorption method
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Soil.Determination of organic carbon.Combustion oxidation nondispersive infrared absorption method
National Environmental Protection Standard of the People's Republic
Determination of soil organic carbon combustion oxidation - non-dispersive
Infrared method
Soil - Determination of organic carbon - Combustion oxidation
Nondispersive infrared absorption method
Published on.2014-03-13
2014-07-01 Implementation
Ministry of Environmental Protection released
Content
Foreword. II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 Interference and elimination 1
5 reagents and materials 1
6 Instruments and equipment 1
7 sample 2
8 Analysis steps. 2
9 Calculation and representation of results. 2
10 precision and accuracy..3
11 Quality Assurance and Quality Control 3
Foreword
To implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and regulate organic carbon in soil
The method of determination is to develop this standard.
This standard specifies the combustion oxidation-non-dispersive infrared method for the determination of organic carbon in soil.
This standard is the first release.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Dalian Environmental Monitoring Center.
This standard is verified by. Fushun Environmental Monitoring Center Station, Heilongjiang Environmental Monitoring Center Station, Panjin City Environmental Monitoring
Central Station, Suzhou Environmental Monitoring Center Station, Shenzhen Environmental Monitoring Center Station and Tianjin Environmental Monitoring Center.
This standard was approved by the Ministry of Environmental Protection on March 13,.2014.
This standard has been implemented since July 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Determination of soil organic carbon - combustion oxidation - non-dispersive infrared method
1 Scope of application
This standard specifies the combustion oxidation-non-dispersive infrared method for the determination of organic carbon in soil.
This standard applies to the determination of organic carbon in soil, and is not applicable to the determination of organic carbon in sludge-contaminated soil.
When the sample amount is 0.050 g, the detection limit of this method is 0.008%, and the lower limit of determination is 0.032%.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate.
Used in this standard.
HJ/T 166 Technical Specifications for Soil Environmental Monitoring
HJ 613 Determination of dry matter and moisture in soils - Gravimetric method
3 Principle of the method
The air-dried soil sample is heated to above 680oC in an oxygen-rich carrier gas, and the organic carbon in the sample is oxidized to dioxide.
Carbon, the carbon dioxide produced is introduced into the non-dispersive infrared detector, and the infrared absorption of carbon dioxide is strong within a certain concentration range.
The degree is proportional to its concentration, and the organic carbon content in the soil is calculated based on the amount of carbon dioxide produced.
4 interference and elimination
When the sample is heated above.200 °C, all carbonates are completely decomposed to produce carbon dioxide.
Positive interference is produced and can be removed by adding an appropriate amount of phosphoric acid.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis.
5.1 Carbon dioxide-free water. It is ready for use, and the conductivity is ≤0.2 mS/m (25°C).
5.2 Concentrated phosphoric acid. φ (H3PO4) = 85 %, excellent grade pure.
5.3 Sucrose (C12H22O12). Reference reagent.
Note 1. Glucose (C6H12O6) can also be used instead of sucrose.
5.4 Sucrose solution. ρ (organic carbon, C) = 10.0 g/L
Weigh 2.375 g of sucrose (5.3) which has been dried at 104 °C for 2 h, dissolved in an appropriate amount of water (5.1), and transferred to a capacity of 100 ml.
In the bottle, dilute to the mark with water (5.1) and mix. Stored at room temperature, valid for two weeks.
5.5 Phosphoric acid solution. φ(H3PO4)= 5 %
Measure 59 ml of concentrated phosphoric acid (5.2) dissolved in 700 ml of water (5.1), cool to room temperature, and dilute with water (5.1) until
1000ml. Stored at room temperature, valid for two weeks.
5.6 Carrier gas. nitrogen, purity 99.99%.
5.7 Gas. oxygen, purity 99.99%.
6 Instruments and equipment
6.1 Total organic carbon analyzer. with solid combustion device, can be heated to above 680 °C, temperature can be adjusted, accuracy 1 °C;
Features a non-dispersive infrared detector with a quartz cup.
6.2 Balance. Accuracy is 0.1 mg.
6.3 Soil screen. 2 mm (10 mesh), 0.097 mm (160 mesh), stainless steel.
6.4 Microinjector..200 μl.
6.5 Common instruments and equipment used in general laboratories.
7 samples
7.1 Sample collection and preservation
The collection and storage of soil samples is carried out in accordance with the relevant provisions of HJ/T 166.
7.2 Preparation of samples
Place the soil sample in the air-drying tray and spread it into a thin layer of 2 ~ 3 cm thick, first removing the residues such as plants, insects, stones, etc.
Crush the clods with a hammer or a porcelain abrasive rod, flip it several times a day, and air dry.
Mix the air-dried soil thoroughly, use the quadruple method, take two parts, one part is retained, one part is ground to all over 2 mm (10
Mesh) soil sieve. Take 10 ~ 20 g of the sieved soil sample and grind it to the entire 0.097 mm (160 mesh) soil sieve.
Load into a brown stoppered glass bottle for testing.
7.3 Determination of dry matter content
The air-dried soil samples after 2 mm (10 mesh) sieve were accurately weighed, and the dry matter content of the soil was determined by reference to HJ 613.
8 Analysis steps
8.1 Instrument Commissioning
Set the condition parameters and debug according to the instructions of the total organic carbon analyzer.
8.2 Drawing of the calibration curve
Use a pipette to accurately measure 0.0, 0.5, 1.0, 2.5, 5.0, 10.0 ml sucrose solution (5.4) in 10.0 ml
In the measuring flask, dilute to the mark with water (5.1) and prepare the concentrations of 0.0, 0.5, 1.0, 2.5, 5.0, 10.0 g/L, respectively.
Calibration series. Use a micro-syringe (6.4) to take.200 μl of the calibration series in a quartz cup with a small amount of glass wool on the pad.
The organic carbon content is 0.00, 0.10, 0.20, 0.50, 1.0, and 2.0 mg, respectively, and the quartz cup is placed in the total organic carbon analyzer (6.1).
The response value of the standard series is determined from low concentration to high concentration in turn, and the organic carbon content (mg) is plotted on the abscissa.
The value should be the ordinate and the calibration curve should be drawn.
8.3 Determination
Weigh 0.05g (7.2) of the sample to the nearest 0.0001 g, put it into a quartz cup with a small amount of glass wool on the pad, and slowly add it.
Phosphoric acid solution (5.5), no bubbles appeared in the sample. The quartz cup was placed in a total organic carbon analyzer (6.1) and the response was measured.
Note 2. When the sample concentration is high, the sample sample size can be appropriately reduced, but should not be less than 0.01g.
8.4 Blank test
Replace the sample with.200 μl of water (5.1) and measure according to step (8.3).
9 Calculation and representation of results
9.1 Calculation of results
The organic carbon content ocω (in terms of carbon, mass fraction, %) in the soil is calculated according to the formulas (1) and (2).
Dmwmm ×= (1)
(2)
0 ×××
−−=
Mb
aAA
Ocω
In the formula.
M1--the mass of dry matter in the sample, g;
M--sample sample amount, g;
Dmw -- dry matter content (mass fraction) of soil samples, %;
Ocω - the content of organic carbon in soil samples (in terms of carbon, mass fraction), %;
A -- sample response value;
0A - blank sample response value;
a -- the intercept of the calibration curve;
b -- The slope of the calibration curve.
9.2 Results representation
When the measurement result is < 1%, it is retained to three decimal places; when the measurement result is ≥1%, three significant figures are retained.
10 Precision and accuracy
10.1 Precision
Six laboratories conducted certified standards for organic carbon content of 0.54% and 1.80% and actual samples of 0.51%.
For the measurement, the relative standard deviations in the laboratory were 3.0% ~ 7.5%, 0.7% ~ 4.5%, 1.8% ~ 7.7%;
The relative standard deviations were 3.0%, 1.2%, and 1.8%, respectively; the repeatability limits were 0.08%, 0.11%, and 0.06%, respectively; reproducibility
The limits are 0.08%, 0.12%, and 0.06%, respectively.
10.2 Accuracy
Six laboratories tested the certified standard samples with organic carbon content of 0.54% and 1.80%, respectively, in the laboratory.
The relative errors were 0% ~ 7.4%, 0.6% ~ 2.2%, respectively; the relative error final values were 1.9% ± 5.7%, 0.9% ± 1.3%.
11 Quality Assurance and Quality Control
11.1 Each batch of samples should be tested at least 10% of parallel samples. When the number of samples is less than 10, each batch should be made at least one.
Parallel sample determination. When the sample organic carbon content is ≤1%, the difference between the parallel sample determination results should be within ±0.10%;
When the sample organic carbon content is >1%, the relative deviation of the parallel sample measurement results is ≤10.0%.
11.2 When testing each batch of samples, a certified standard sample shall be analyzed and its measured value shall be within the guaranteed value range.
11.3 The correlation coefficient of the calibration curve should be greater than or equal to 0.995.
11.4 Each batch of samples shall be tested with a calibration sample at the middle of the calibration curve. The measured values of the calibration samples are relative to the calibration curve.
The relative error of the point concentration should not exceed 10%.
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