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HJ 741-2015: Soil and sediment. Determination of volatile organic compounds. Headspace gas chromatography
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Soil and sediment. Determination of volatile organic compounds. Headspace gas chromatography
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HJ 741-2015
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Basic data | Standard ID | HJ 741-2015 (HJ741-2015) | | Description (Translated English) | Soil and sediment. Determination of volatile organic compounds. Headspace gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Classification of International Standard | 13.080 | | Word Count Estimation | 18,127 | | Date of Issue | 2015-05-04 | | Date of Implementation | 2015-07-01 | | Quoted Standard | GB 17378.3; GB 17378.5; HJ 613; HJ/T 166 | | Regulation (derived from) | Ministry of Environmental Protection Announcement 2015 No. 28 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of soil and sediments inserts 37 kinds of volatile organic compounds headspace/gas chromatography. This standard applies to 37 kinds of soil and sediment determination of volatile organic compounds. If other volatile organic compounds by verifying also applicable to the present standard. When the amount of soil and sediment samples 2g, the 37 kinds of volatile organic compounds in the method detection limit of 0.005 ~ 0.03mg/kg, detection limit of 0.02 ~ 0.12mg/kg, see Appendix A. | HJ 741-2015: Soil and sediment. Determination of volatile organic compounds. Headspace gas chromatography
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Soil and sediment. Determination of volatile organic compounds.Headspace gas chromatography
National Environmental Protection Standard of the People 's Republic of China
Determination of volatile organic compounds in soil and sediments
Headspace/gas chromatography
Soil and sediment-Determination of volatile organic compounds
-Headspace gas chromatography
Ministry of Environmental Protection
2015-07-01 implementation
2015-05-04 release
I directory
Preface .ii
1 Scope of application 1
2 normative reference document 1
Principle of Method 1
4 reagents and materials
5 instruments and equipment
6 samples
7 Analysis Step 4
Calculation and representation of results 4
9 Precision and Accuracy 6
10 Quality assurance and quality control
11 Waste treatment 7
12 Precautions 7
Appendix A (normative appendix) method of detection limit and determination of the lower limit of 8
Appendix B (informative) method of precision and accuracy
Appendix C (informative) Polyethylene glycol-20M chromatographic analysis of the target chromatogram .13
Foreword
To implement the Environmental Protection Law of the People's Republic of China, protect the environment, protect human health, regulate soil and sediment
In the determination of volatile organic compounds, the development of this standard.
This standard specifies the headspace/gas chromatography of volatile organic compounds in soil and sediments.
This standard is the first release.
Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. Anshan City Environmental Monitoring Center Station.
The standard verification unit. Liaoning Province Environmental Monitoring Experimental Center, Shenyang City Environmental Monitoring Center Station, Dalian City Environmental Monitoring
Center, Harbin Environmental Monitoring Center, Fushun City Environmental Monitoring Center Station and Liaoyang City Environmental Monitoring Center Station.
The environmental protection department of this standard approved on May 4,.2015.
This standard has been implemented since July 1,.2015.
This standard is explained by the Ministry of Environmental Protection.
Determination of Volatile Organic Compounds in Soil and Sediments
Headspace/gas chromatography
WARNING. The organic reagents and standard solutions used in the test are volatile, and the procedure should be in the ventilation
Cabinet to operate, should be required to wear protective equipment, to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the headspace/gas chromatographic method for the determination of 37 volatile organic compounds in soil and sediments.
This standard applies to the determination of 37 volatile organic compounds in soil and sediments. Other volatile organic compounds if verified
Can also be applied to this standard.
When the amount of soil and sediment samples is 2 g, the detection limits of 37 volatile organic compounds are 0.005 mg/kg ~ 0.03
Mg/kg, the determination of the lower limit of 0.02 mg/kg ~ 0.12 mg/kg, see Appendix A.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Specification for ocean monitoring - Part 3. Sample collection, storage and transportation GB 17378.3
Specification for marine monitoring - Part 5. Sediment analysis
Determination of Dry Matter and Moisture in Soil
Technical specification for soil environmental monitoring
3 Principle of the method
At a certain temperature, the volumetric organic matter in the sample of the headspace bottle evaporates to the liquid space, and the gas-liquid three-phase reaches the heat
Mechanically dynamic equilibrium. The volatile organic compounds in the gas phase are separated by gas chromatography and detected by flame ionization detector. To protect
Time qualitative, external standard method.
4 reagents and materials
4.1 Experimental water. secondary distilled water or water prepared by pure water equipment.
Before use, subject to a blank test to confirm that the target compound in the retention time interval without interference peaks appear or its
The concentration of the target compound in the method is lower than the method detection limit.
4.2 Methanol (CH3OH). Chromatographic Purification.
Before use, subject to inspection to confirm that the target compound or target compound concentration is lower than the method detection limit.
4.3 sodium chloride (NaCl). excellent grade pure.
Baked in a muffle furnace at 400 ° C for 4 h, placed in a desiccator and cooled to room temperature and transferred to a glass vial.
4.4 phosphoric acid (H3PO4). excellent grade pure.
4.5 saturated sodium chloride solution.
500 ml of experimental water (4.1), add a few drops of phosphoric acid (4.4) to adjust pH ≤ 2, add 180 g of sodium chloride (4.3),
Dissolve and mix. Stored at 4 ℃, can be stored for 6 months.
24.6 standard stock solution. ρ = 1000 mg/L ~ 5000 mg/L.
Can be purchased directly to prove the standard solution can also be prepared with standard substances.
4.7 standard use of liquid. ρ = 10 mg/L ~ 100 mg/L.
The standard compound of the target compound is stored in a dense bottle for a period of 30 days or formulated with reference to the manufacturer's instructions.
4.8 quartz sand (SiO2). analytical grade, 20 mesh to 50 mesh.
Before use, verify that the target compound or target compound concentration is below the method detection limit.
4.9 Carrier gas. high purity nitrogen (≥99.999%), deoxidized by deoxidizer, dehydrated by molecular sieve.
4.10 Gas. high purity hydrogen (≥99.999%), dehydrated by molecular sieve.
4.11 to help gas. air, dehydrated by silica gel, activated carbon off organic matter.
Note 1. All of the above standard solutions are methanol as solvent, the standard solution after preparation or opening should be placed in a dense bottle, below 4 ℃
Deposit, the preservation period is generally 30 d. Before use should be restored to room temperature, mix.
5 instruments and equipment
5.1 Gas chromatograph. with capillary split/splitless inlet, programmable temperature rise, with hydrogen flame ionization detector (FID).
5.2 Column. quartz capillary column. Column 1.60 m x 0.25 mm, film thickness 1.4 m (6% nitrile phenyl, 94% dimethyl
Base polysiloxane fixative), other equivalent capillary columns may also be used. Column 2.30 m x 0.32 mm, film thickness 0.25 m (poly
Diol-20M), other equivalent capillary columns may also be used.
5.3 Automatic headspace sampler. headspace bottle (22 ml), gasket (polytetrafluoroethylene/silicone material), cap (screw cap or
Once used glands).
5.4 reciprocating oscillator. oscillation frequency 150 times/min, can be fixed head empty bottle.
5.5 Balance. Accuracy 0.01 g.
5.6 Microinjector. 5 μl, 10 μl, 25 μl, 100 μl, 500 μl.
5.7 Sampling equipment. shovel or stainless steel spoon.
5.8 portable refrigerated containers. volume 20L, the temperature below 4 ℃.
5.9 brown dense bottle. 2 ml, with PTFE packing and solid screw cap.
5.10 Sampling Bottle. 60 or.200 ml threaded brown wide-mouth glass bottle with polytetrafluoroethylene-silicone pad screw cap.
5.11 disposable Pasteur glass pipette.
5.12 muffle furnace.
5.13 General laboratory equipment and equipment commonly used.
6 samples
6.1 Collection and storage of samples
According to the relevant requirements of HJ/T 166, GB 17378.3 for soil and sediment samples collected and preserved. Collect samples
Of the application of metal products, should be used before the cleaning. All samples should be collected at least 3 representative samples.
6.1.1 Saturated sodium chloride solution is added to the sample collection
22 ml headspace flask was added 10.0 ml of saturated sodium chloride solution (4.5), weighed (accurate to 0.01 g), to the scene.
Approximately 2 g of soil or sediment samples were collected in a headspace bottle with a sampler, sealed immediately, placed in a freezer and returned to the laboratory.
6.1.2 The sample was collected with no saturated sodium chloride solution
3 Collect the sample as soon as possible with a shovel or spoon into the vial (5.10) and fill it as much as possible. Quickly remove the sampling bottle thread
And samples attached to the outer surface, sealed sample bottles. Placed in a portable freezer and brought back to the laboratory. Sampling the sample in the bottle
For the determination of dry matter content, sediment moisture content and high content of samples in soil.
Note 2. Samples can be sieved at the sampling site using a portable instrument for the determination of volatile organic compounds. When the sample is volatile
When the concentration of organic matter is greater than 1000 μg/kg, the sample is considered to be a high content sample.
Note 3. Do not stir soil and sediment when collecting samples so as to avoid the volatilization of organic matter in soil and sediments.
Samples should be returned to the laboratory as soon as possible after the analysis. If you can not immediately analysis, should be sealed below 4 ℃, the shelf life is not exceeded
Over 7 d. The sample storage area should be free of volatile organic matter.
6.2 Preparation of the sample
6.2.1 Low content sample
6.1.1 Procedure The preparation of the sample was carried out. the headspace flask (6.1.1) containing the sample was taken out in the laboratory and returned to room temperature
After weighing, accurate to 0.01 g. On the oscillator at 150 times/min frequency oscillation for 10 min, to be measured.
6.1.2 Procedure Collect the sample preparation. Remove the sample vial (6.1.2) in the laboratory and return to room temperature
, Then weighed 2 g (accurate to 0.01 g). The sample was placed in a headspace bottle and 10.0 ml of saturated sodium chloride solution (4.5)
Immediately sealed, oscillated at 150 times/min for 10 min on the oscillator.
6.2.2 High content samples
If the site of the initial screening of volatile organic compounds for high content or low content of the sample determination results greater than 1000 μg/kg should be regarded as
For high content samples.
Remove the vial containing the high sample (6.1.2) and return to room temperature. Weigh 2 g (accurate to 0.01 g) sample
Placed in the top of the bottle, quickly add 10.0 ml of methanol (4.2), sealed on the oscillator at 150 times/min frequency of oscillation 10
Min. After standing for settling, remove about 1 ml of methanol extract to a 2 ml brown dense bottle (5.9) with a disposable Pasteur glass pipette.
in. The extract can be stored in a cryopreservation and stored for 14 days. If the concentration of the target compound in the methanol extract is high,
It can be appropriately diluted by adding methanol.
Then, add 2 g (accurate to 0.01 g) quartz sand (4.8), 10.0 ml saturated sodium chloride
Solution (4.5) and 10 μl to 100 μl (5.6) of the above methanol extract, immediately sealed on the shaker at 150 times/min
The frequency of oscillation for 10 min, to be measured.
Note 4. If the concentration is too low or not detected by high content method, the sample should be re-analyzed using a low content method.
6.3 Preparation of blank samples
6.3.1 Transport blank
Before sampling, add 10.0 ml of saturated sodium chloride solution and 2 g (accurate to 0.01 g) of quartz sand in the laboratory.
Seal, bring it to the sampling site. Sampling is not open, then shipped back to the laboratory with the sample. On the oscillator at 150 times/min
The frequency of oscillation for 10 min, to be measured. Used to check whether the sample is contaminated during transport.
6.3.2 Low content blank sample
Weigh 2 g (accurate to 0.01 g) of quartz sand (4.8) instead of the sample, placed in a headspace bottle, add 10.0 ml of saturated chlorine
Sodium chloride solution (4.5), sealed immediately, on the oscillator at 150 times/min frequency oscillation 10 min, to be measured.
6.3.3 High content blank samples
A 2 g (exact to 0.01 g) quartz sand (4.8) was used in place of the high content sample and prepared according to 6.2.2.
Determination of Soil Dry Matter Content and Sediment Moisture Content
4 Determination of dry matter content in soil according to HJ 613; moisture content of sediment samples measured according to GB 17378.5.
7 Analysis steps
7.1 Instrument reference conditions
Different models of headspace sampler and gas chromatograph of the best working conditions are different, should be in accordance with the instructions to operate the instrument
For. The reference conditions given in this standard are as follows.
7.1.1 Headspace Autosampler reference conditions
Heating equilibrium temperature 85 ℃; heating equilibrium time 50 min; sampling needle temperature 100 ℃; transmission line temperature 110 ℃;
The transmission line is a quartz capillary column with an inert treatment and an inner diameter of 0.32 mm. The pressure equilibrium time is 1 min and the injection time is 0.2
Min; dial time 0.4 min.
Note 5. Other injections may also be used.
7.1.2 Gas chromatograph reference conditions
Temperature programmed. 40 ° C (5 min) 8 ° C/min 100 ° C (5 min) 6 ° C/min.200 ° C (10
Min). Inlet temperature. 220 ° C. Detector temperature. 240 ° C. Carrier gas. nitrogen; carrier gas flow. 1 ml/min; hydrogen
Flow. 45 ml/min; air flow. 450 ml/min. Injection method. Split injection; Split ratio. 10. 1.
7.2 Calibration curve drawing
To the 5 headspace bottles, 2.00 g of quartz sand (4.8), 10.0 ml of saturated sodium chloride solution (4.5) and a quantity
(4.7), immediately sealed, the target compound was 0.10 μg, 0.20 μg, 0.50 μg, 1.00 μg
And 2.00 μg of 5 points of different concentration series of calibration curve series. The standard series of samples will be configured on the oscillator (5.4)
At a frequency of 150 times/min for 10 min, according to the instrument reference conditions (7.1) followed by injection analysis to peak area or peak height
As the ordinate, the mass (μg) is the abscissa, and the calibration curve is drawn.
7.3 Determination
The prepared sample (6.2) was placed on a headspace sampler and measured according to the instrument reference conditions (7.1). If you play
Organic matter was detected, the application of column 2 to confirm the qualitative.
7.4 blank test
Place the prepared blank sample (6.3) on the automatic headspace sampler (5.3) and follow the instrument reference conditions (7.1)
Line determination.
Calculation and representation of results
8.1 Qualitative analysis
A standard solution with a volatile organic concentration of 0.200 mg/L was prepared and separated using column 1,
Dynamic sampler and gas chromatograph reference conditions were measured to preserve the time qualitative. When using this method is not qualitative, use
Column 2 or GC-MS and other means to assist qualitative. Column 1 The standard chromatogram for the analysis of volatile organic compounds is shown in Figure 1.
Column 2 The standard chromatogram for the analysis of volatile organic compounds is given in Appendix C.
5.0 10.0 15.0 20.0 25.0 30.0 35.0 40.0 min
0.0
1.0
2.0
3.0
4.0
5.0μV (x10,000) chromatography
1-vinyl chloride; 2-1,1-dichloroethylene; 3-dichloromethane; 4-trans-1,2-dichloroethylene; 5-1,1-dichloroethane; 2-dichloroethyl
8-1, 1,1-trichloroethane; 9-carbon tetrachloride; 10-1,2-dichloroethane benzene; 11-trichlorethylene; 12-1,2- Dichloropropane;
16-tetrachloroethane; 17-dibromochloromethane; 18-1,2-dibromoethane; 14-bromodichloromethane;
19-chlorobenzene; 20-1, 1,1,2-tetrachloroethane; 21-ethylbenzene; 22-m-xylene p-xylene; 23-o-xylene;
25-1,2,2-tetrachloroethane; 26-1,2,3-trichloropropane; 27-1,3,5-trimethylbenzene; 28-1,2,4-trimethyl Phenylbenzene; 29-1,3-dichlorobenzene; 30-1,4-
Dichlorobenzene; 31-1,2-dichlorobenzene; 32-1,2,4-trichlorobenzene; 33-hexachlorobutadiene;
Figure 1 column 1 analysis of 37 kinds of volatile organic standard chromatogram
8.2 Calculation of soil samples
8.2.1 The content of volatile organic compounds (mg/kg) in low-content samples is calculated according to formula (1).
Dmwm
1
0 (1)
Where. - the content of volatile organic compounds in the sample, mg/kg;
0m - calibration curve to calculate the target content, μg;
1m - sample volume (wet weight), g;
Dmw - dry matter content of the sample,%.
8.2.2 The content of volatile organic compounds (mg/kg) in high-content samples is calculated according to formula (2).
Sdm Vw
Fm
10 (2)
Where. - the content of volatile organic compounds in the sample, mg/kg;
0m - calibration curve to calculate the concentration of the target, μg;
10 - the amount of methanol added to the sample, ml;
1m - sample volume (wet weight), g;
SV - volume of methanol extract for headspace measurement, ml;
Dmw - dry matter content of sample,%;
F - the dilution factor of the extract.
keep time
Peak height
Calculation of Sediment Sample Results
8.3.1 The content of volatile organic compounds (mg/kg) in low content samples shall be calculated according to formula (1).
)1(
OHwm
(3)
Where. - the content of the target in the sample, mg/kg;
0m - Calculate the concentration of the target according to the calibration curve, μg;
1m - sample volume (wet weight), g;
OHw 2 - moisture content of the sample,%.
8.3.2 The content of volatile organic compounds (mg/kg) in high-content samples is calculated according to formula (2).
SOH Vw
Fm
) 1 (m
0 (4)
Where. - the content of the target in the sample, mg/kg;
0m - Calculate the concentration of the target according to the calibration curve, μg;
10 - the amount of methanol added to the sample, ml;
1m - sample volume (wet weight), g;
SV - volume of methanol extract for headspace measurement, ml;
OHw 2 - moisture content of the sample,%;
F - the dilution factor of the extract.
8.4 The result is shown
The number of decimal places is the same as the detection limit of the method. Up to three valid digits are retained.
9 precision and accuracy
9.1 precision
Six laboratories studied soil concentrations of 0.25 mg/kg (0.1 mg/kg) and 1.0 mg/kg (0.5 mg/kg)
The relative standard deviations in the laboratory were 1.7% ~ 14.4%, 1.0% ~ 11.7%, respectively. The laboratory
The relative standard deviations range from 4.8% to 20.1% and 1.7% to 15.1%, respectively, and the repeatability limits were 0.013 mg/kg ~
0.05 mg/kg, 0.041 mg/kg to 0.15 mg/kg; the reproducibility limits were 0.020 mg/kg to 0.07 mg/kg, 0.044
Mg/kg to 0.30 mg/kg.
Six laboratories were tested for sediment concentrations of 0.25 mg/kg (0.1 mg/kg) and 1.0 mg/kg (0.5 mg/kg)
The relative standard deviations in the laboratory were 0.8% ~ 15.6%, 0.7% ~ 24.7%, respectively.
The relative standard deviations were 7.2% ~ 15.9% and 2.5% ~ 16.6%, respectively. The repeatability limits were 0.012 mg/kg ~
0.06 mg/kg, 0.045 mg/kg to 0.29 mg/kg; the reproducibility limits were 0.033 mg/kg to 0.14 mg/kg, 0.071
Mg/kg to 0.46 mg/kg.
9.2 Accuracy
Six spheres were tested on soil matrix spiked samples with a standard concentration of 0.10 mg/kg (0.25
Mg/kg), the recoveries of 37 kinds of volatile organic compounds were 22.4% ~ 113%, and the concentration of soil samples was 0.50 mg/kg
(1.00 mg/kg). The recoveries of 37 kinds of volatile organic compounds were in the range of 40.7% ~ 94.7%.
Seven of the six laboratories were tested for the spiked samples of sediments, with a sample concentration of 0.10 mg/kg (0.25
Mg/kg), and the recoveries of 37 kinds of volatile organic compounds were in the range of 52.5% ~ 131%. The standard concentration of sediment samples was 0.50
Mg/kg (1.00 mg/kg). The recoveries of 37 volatile organic compounds were 65.1% ~ 116%.
Refer to Appendix B for summary of precision and accuracy.
10 quality assurance and quality control
10.1 calibration curve of the target compound, the correlation coefficient should be greater than 0.99, if not meet the requirements, should find the reasons,
Draw a calibration curve.
10.2 Calibration Confirmation
Within the time of each batch analysis or within 24 h, the calibration curve should be measured in the middle of the concentration point, and the calibration curve of the concentration point response
Value of the change, the retention time of the change does not exceed ± 2 s, the measured value and the standard value of the relative error should be ≤ 20%, or should take school
Positive measures. If the corrective action is invalid, the calibration curve should be redrawn.
10.3 Laboratory Blank Test The concentration of all target compounds in the results of the analysis should be lower than the method detection limit. Otherwise, need to check
The reasons for the elimination, to the laboratory blank determination of qualified results before they can continue to sample analysis.
10.4 Each batch of samples should be collected at least one transport blank. The analysis results should be less than the method detection limit, otherwise you need to find the reasons,
Eliminate the interference and re-collect the sample analysis.
10.5 Each batch of samples (up to 20) should be measured with a blank spiked sample, the matrix plus the standard sample and the matrix plus standard parallel
The recoveries of the blanks in the laboratory were between 80.0% and 120%. If the sample recovery rate is low, indicating that the sample matrix effect,
But the relative deviation of the parallel spiked sample recovery shall not exceed 25%.
11 Waste treatment
Hazardous wastes containing volatile organic compounds should be collected, stored and commissioned by qualified units for processing.
12 Prec...
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