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HJ 742-2015: Soil and sediment. Determination of volatile aromatic hydrocarbons. Headspace gas chromatography
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Soil and sediment. Determination of volatile aromatic hydrocarbons. Headspace gas chromatography
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HJ 742-2015
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Basic data | Standard ID | HJ 742-2015 (HJ742-2015) | | Description (Translated English) | Soil and sediment. Determination of volatile aromatic hydrocarbons. Headspace gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Classification of International Standard | 13.080 | | Word Count Estimation | 16,169 | | 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 in soil and sediment of 12 kinds of volatile aromatic hydrocarbons headspace/gas chromatography. This standard applies to 12 kinds of soil and sediment determination of volatile aromatic hydrocarbons. Other volatile aromatic hydrocarbons if verified also apply to this standard. | HJ 742-2015: Soil and sediment. Determination of volatile aromatic hydrocarbons. Headspace gas chromatography
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Soil and sediment. Determination of volatile aromatic hydrocarbons. Headspace gas chromatography
National Environmental Protection Standard of the People 's Republic of China
Determination of volatile aromatic hydrocarbons in soil and sediments
Headspace/gas chromatography
Soil and sediment-Determination of volatile aromatic
Hydrocarbons-Headspace gas chromatography
2015-05-04 release
2015-07-01 implementation
Ministry of Environmental Protection released
I directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 reagents and materials 1
5 instruments and equipment 2
6 Sample 2
7 Analysis steps
8 results are calculated and expressed
9 precision and accuracy
10 Quality assurance and quality control
11 Waste treatment .7
12 Precautions .7
Appendix A (normative appendix) method of detection limit and lower limit of determination
Appendix B (informative) method of precision and accuracy 9
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 aromatic hydrocarbons, the development of this standard.
This standard specifies headspace/gas chromatography for the determination of volatile aromatic hydrocarbons in soil and sediments.
This standard is the first release.
Appendix A of this standard is a normative appendix, Appendix B is an informative appendix.
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 Aromatic Hydrocarbons in Soil and Sediment Headspace/Gas Chromatography
WARNING. The reagents and standard solutions used in the test are volatile, and the preparation process should be carried out in a fume hood
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 12 volatile aromatic hydrocarbons in soil and sediments.
This standard applies to the determination of 12 volatile aromatic hydrocarbons in soil and sediments. Other volatile aromatic hydrocarbons if passed
The certificate also applies to this standard.
When the sampling amount is 2 g, the detection limit of 12 kinds of volatile aromatic hydrocarbons is 3.0 ~ 4.7 μg/kg, the lower limit is 12.0 ~
18.8 μg/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.
GB 17378.3 Marine Monitoring Specification Part 3 Sample Collection Storage and Transportation
GB 17378.5 Marine monitoring regulations 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 volatiles of volatile aromatic hydrocarbons in the headspace bottle evaporate to the liquid space, and the gas-liquid three-phase reaches the heat
Mechanically dynamic equilibrium. The volatile aromatic hydrocarbons 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 ultrapure water preparation. Before use to be blank test test, indeed
There was no interference with the peaks in the retention time interval of the target.
4.2 Methanol (CH3OH). Pesticide level or equivalent level. By blank test, it was confirmed that there was no retention time in the target
There are interference peaks appear.
4.3 sodium chloride (NaCl). excellent grade pure.
In a muffle furnace (or box-type electric furnace) at 400 ℃ baking 4 h, placed in a dryer to cool to room temperature, transferred to the grinding glass
Keep in the bottle.
4.4 phosphoric acid (H3PO4). excellent grade pure.
4.5 saturated sodium chloride solution.
Measure the amount of 500 ml of experimental water (4.1), add a few drops of phosphoric acid (4.4) to adjust to pH ≤ 2, add 180 g of sodium chloride (4.3)
Dissolve and mix. At 4 ℃ under the dark preservation, can be stored for 6 months.
4.6 Standard stock solution. ρ = 1000 μg/ml.
2 volatile aromatic hydrocarbon methanol standard solution can be purchased directly to prove the standard solution can also be prepared with standard materials. Including benzene,
Toluene, ethylbenzene, m-xylene, p-xylene, o-xylene, cumene, styrene, chlorobenzene, 1,3-dichlorobenzene, 1,4-
Dichlorobenzene, 1,2-dichlorobenzene.
Store at or below 4 ° C or refer to the manufacturer's product description. Before use should be restored to room temperature, and shake. After opening
Freeze sealed for up to 14 days. Such as the purchase of high concentrations of standard stock solution, the use of methanol (4.2) for appropriate dilution.
4.7 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.
4.8 Carrier gas. high purity nitrogen (≥99.999%), deoxidized by deoxidizer, dehydrated by molecular sieve.
4.9 Gas. high purity hydrogen (≥99.999%), dehydrated by molecular sieve.
4.10 to help gas. air, dehydrated by silica gel, activated carbon off organic matter.
5 instruments and equipment
5.1 Gas Chromatograph. With split/splitless inlet, programmable temperature rise, with flame ionization detector (FID).
5.2 Column. quartz capillary column, 30 m (length) × 0.32 mm (inner diameter) × 0.25 μm (film thickness), the stationary phase is poly
Diol. Other equivalent capillary columns may also be used.
5.3 Automatic headspace sampler. with headspace bottle (22 ml), gasket (polytetrafluoroethylene/silicone), cap (screw cap or one
Times the use of the gland).
5.4 reciprocating oscillator. oscillation frequency of 150 times/min, can be fixed head empty bottle.
5.5 Balance. A balance of 0.01 g.
5.6 Microinjector. 5 μl, 10 μl, 25 μl, 100 μl, 500 μl, 1000 μl.
5.7 Sampling equipment. shovel and stainless steel spoon.
5.8 portable refrigerated containers. volume 20 L, the temperature below 4 ℃.
5.9 brown dense bottle. 2 ml, with PTFE packing and solid screw cap.
5.10 Sampling Bottle. 60 ml or.200ml threaded brown jar with a Teflon-Silica Tape Screw Cap.
5.11 disposable Pasteur glass pipette.
5.12 General laboratory equipment and equipment commonly used.
6 samples
6.1 Collection and storage of samples
The collection and storage of soil samples were carried out in accordance with the relevant provisions of HJ/T 166. In accordance with the relevant provisions of GB 17378.3
Collection and storage of sediment samples. Collection of samples of the application of iron shovel and stainless steel spoon. All samples should be collected at least 3
Representative sample.
Use a shovel and a stainless steel spoon to collect the sample as soon as possible into the sampling bottle (5.10) and fill it as much as possible. Quickly remove the sample
Bottle threads and samples attached to the outer surface, sealed vials. Placed in a portable freezer and brought back to the laboratory.
The samples in the sampling vials were used for the determination of the dry matter and the moisture content of the sediments.
Note 1. If necessary, the sample can be sieved at the sampling site using a portable instrument for the determination of volatile aromatic hydrocarbons. As if
When the volatile aromatic hydrocarbon concentration in the product is greater than 1000 μg/kg, the sample is considered to be a high content sample.
Note 2. Do not stir soil and sediment when collecting samples, so as to avoid the evaporation of organic matter.
3 samples should be analyzed as soon as possible after being sent to the laboratory. If you can not immediately analyze, sealed below 4 ℃, the shelf life does not exceed
7d. There should be no organic interference in the sample storage area.
6.2 Preparation of the sample
6.2.1 Low content sample
Take the sample vial (5.10) in the laboratory and wait for 2g (accurate to 0.01g) to be returned to room temperature.
In the bottle, add 10.0 ml of saturated sodium chloride solution (4.5) to the headspace bottle immediately, and immediately seal the reciprocating oscillator (5.4)
On the frequency of 150 times/min oscillation 10 min, to be measured.
6.2.2 High content samples
The high content sample is prepared as follows. Remove the sample bottle (5.10) and allow it to return to room temperature. Weigh 2g (accurate to 0.01g)
The sample was placed in a headspace bottle and 10.0 ml of methanol (4.2) was added rapidly, sealed on a reciprocating oscillator (5.4)
/ Min for 10 min. After standing for settling, remove about 1 ml of the extract with a disposable Pasteur glass pipette to 2 ml
Brown dense bottle (5.9). The extract can be stored in the freezer at 4 ℃, the shelf life of 14 d.
Note 3. If the concentration of the target compound in the methanol extract is high, it can be appropriately diluted by adding methanol.
After recovering the extract to room temperature before analysis, add 2 g (accurate to 0.01 g) quartz sand (4.7) to the empty headspace flask,
10.0 ml of saturated sodium chloride solution (4.5) and 0.010 to 0.100 ml of methanol extract. Immediately sealed in reciprocating oscillator (5.4)
On the frequency of 150 times/min oscillation 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 samples
Before sampling, 10.0 ml of saturated sodium chloride solution (4.5) and 2 g (accurate to 0.01 g) of quartz sand (4.7)
Into the top of the bottle sealed, to bring it to the sampling site. Sampling unopened, then shipped back to the laboratory with the sample, in the reciprocating
Oscillator (5.4) at 150 times/min oscillation time for 10 min, to be measured.
6.3.2 Low content blank sample
Weigh 2 g (accurate to 0.01 g) quartz sand (4.7) instead of the sample, prepare a low level blank sample according to 6.2.1.
6.3.3 High content blank samples
Weigh 2 g (accurate to 0.01 g) quartz sand (4.7) instead of high content samples, prepare high levels of air according to 6.2.2
White sample.
Determination of Soil Dry Matter Content and Sediment Moisture Content
The dry matter content of the soil was determined according to HJ 613; the moisture content of the sediment sample was determined according to GB 17378.5.
7 Analysis steps
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 recommended conditions for this instrument are as follows.
7.1 Instrument reference conditions
7.1.1 Headspace sampler reference conditions
Heating equilibrium temperature 85 ℃; heating equilibrium time 50 min; sampling needle temperature 100 ℃; transmission line temperature 110 ℃; transmission
Line was subjected to deactivation, the inner diameter of 0.32 mm quartz capillary column; pressure equalization time 1 min; injection time 0.2 min;
Dial time 0.4 min.
47.1.2 Gas chromatograph reference conditions
Temperature programmed. 35 ° C (for 6 min) 5 ° C/min 150 ° C (for 5 min) 20 ° C/min.200 ° C (for 5 min);
Inlet temperature. 220 ° C; detector temperature. 240 ° C; carrier gas. nitrogen; column flow. 1.0 ml/min; hydrogen flow rate. 45 ml/min;
Air flow. 450 ml/min; injection method. split injection; split ratio. 5. 1.
7.2 Calibration curve drawing
25.0 μl, 50 μl, 100 μl, 250 μl, 500 μl of standard stock solution (4.6) were charged with a small amount of methanol
In a 5 ml volumetric flask, and then equilibrated with methanol to give a standard solution concentration of 5.00 μg/ml, 10.0 μg/ml, 20.0
Μg/ml, 50.0 μg/ml, 100 μg/ml, and frozen (-18 ° C or lower).
Add 2 g (accurate to 0.01 g) quartz sand (4.7), 10.0 ml saturated sodium chloride solution (4.5)
And 10.0 μl of the above standard solution (7.2), the target compound mass was 50.0 ng, 100 ng,.200 ng, 500 ng
And a 1000 ng 5-point calibration curve series. According to the instrument reference conditions (7.1) followed by injection analysis to peak area or peak height
For the ordinate, the quality (ng) for the abscissa, draw the calibration curve. The standard chromatograms of 12 volatile aromatic hydrocarbons are shown in Fig.
7.5 10.0 12.5 15.0 17.5 20.0 22.5 min
0.00
0.25
0.50
0.75
1.00
1.25
1.50
1.75
2.00
2.25
2.50
ΜV (x10,000) 0
2-toluene; 3-ethylbenzene; 4-p-xylene; 5-m-xylene; 6-cumene; 7-o-xylene; 8-chlorobenzene; 3-dichlorobenzene;
-1,4-dichlorobenzene; 12-1,2-dichlorobenzene.
Figure 1 12 kinds of volatile aromatic hydrocarbon standard chromatogram
7.3 Determination
The prepared sample (6.2) was placed on an automatic headspace sampler (5.3) and tested according to instrument reference (7.1)
set.
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
Qualitative analysis was performed based on the retention time of each component of the reference substance.
8.2 Calculation of soil samples
8.2.1 The content of volatile aromatic hydrocarbons in low-content samples (μg/kg) is calculated according to formula (1).
5dmwm
1
0 (1)
Where. - the content of the target compound in the sample, μg/kg;
M0 - Calculate the mass of the target compound based on the calibration curve, ng;
M1 - sample weight (wet weight), g.
Dmw - dry matter content of the sample,%.
8.2.2 The content of volatile aromatic hydrocarbons in high-content samples (μg/kg) is calculated according to formula (2).
DmS wVm
Fm
0 0.10 (2)
Where. - the content of the target compound in the sample, μg/kg;
M0 - according to the calibration curve to calculate the target compound quality, ng;
10.0 - volume of extract, ml;
M1 - sample weight (wet weight), g;
Vs - volume of methanol extract for headspace measurement, ml;
Dmw - dry matter content of sample,%;
F - the dilution factor of the extract.
8.3 Calculation of sediment sample results
8.3.1 Content of volatile aromatic hydrocarbons in low-content samples (μg/kg), calculated according to formula (3).
)1(
OHwm
(3)
Where. - the content of the target in the sample, μg/kg;
M0 - according to the calibration curve to calculate the target compound quality, ng;
M1 - sample weight (wet weight), g;
OHw 2 - moisture content of the sample,%.
8.3.2 The content of volatile aromatic hydrocarbons in high-content samples (μg/kg) is calculated according to formula (4).
SOH Vwm
Fm
)1(
0.10
0 (4)
Where. - the content of the target in the sample, μg/kg;
M0 - according to the calibration curve to calculate the target compound quality, ng;
10.0 - volume of extract, ml;
M1 - sample weight (wet weight), g;
Vs - 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
When the determination result is less than 100 μg/kg, one decimal place is retained; when the result is greater than or equal to 100 μg/kg,
6 Reserved 3 significant digits.
9 precision and accuracy
9.1 precision
Six laboratories tested the soil samples at concentrations of 25.0 μg/kg, 100 μg/kg and 500 μg/kg, respectively
The relative standard deviations in the laboratory were 3.3% ~ 17.8%, 0.9% ~ 11.2% and 1.8% ~ 13.0%, respectively.
The relative standard deviations were between 2.4% and 10.1%, 2.1% to 7.8% and 1.3% to 4.8%, respectively.
1.9 μg/kg to 11.9 μg/kg and 30.2 μg/kg to 60.9 μg/kg; reproducibility limits
Not from 2.0 μg/kg to 3.9 μg/kg, 7.7 μg/kg to 15.0 μg/kg and 30.2 μg/kg to 64.4 μg/kg.
Six samples of the concentration of 25.0 μg/kg, 100 μg/kg, 500 μg/kg of sediment samples were fine
The relative standard deviations in the laboratory were 1.7% to 9.2%, 0.9% to 7.3% and 1.2% to 5.2%, respectively.
The relative standard deviations were 1.7% ~ 6.5%, 2.0% ~ 4.4% and 1.3% ~ 2.6%, respectively.
Not to be 1.8 μg/kg to 4.4 μg/kg, 5.6 μg/kg to 10.3 μg/kg and 23.8 μg/kg to 48.5 μg/kg;
Not 2.7 μg/kg to 4.7 μg/kg, 7.1 μg/kg to 14.9 μg/kg and 27.9 μg/kg to 53.1 μg/kg.
9.2 Accuracy
Six laboratories were tested for spiked samples of soil matrix with 25.0 μg/kg, 100 μg/kg and 500 μg/kg
The recoveries of the 12 target species were 35.3% ~ 68.7%, 49.3% ~ 90.6% and 37.8% ~
73.7%.
Six samples of spiked samples with spiked concentrations of 25.0 μg/kg, 100 μg/kg and 500 μg/kg, respectively
The determination. The recoveries of 12 kinds of targets were 77.9% ~ 102%, 83.8% ~ 106% and 78.6% ~
96.5%.
Refer to Appendix B for summary of precision and accuracy.
10 quality assurance and quality control
10.1 Calibration curve
According to the concentration of the target and the response value of the calibration curve, the correlation coefficient should be greater than or equal to 0.999, if not satisfied
Seek, replace the column or take other measures, and then redraw the calibration curve.
10.2 Calibration Confirmation
Before and after each batch analysis, calibration was carried out using the standard curve intermediate concentration point. The target compound was measured
The relative deviation between the set value and the standard value should be ≤ 20%, otherwise the calibration curve should be redrawn.
10.3 samples
10.3.1 Laboratory Blank Test The concentration of all the test compounds in the results of the analysis should be lower than the method detection limit. Otherwise, should
Identify the cause, timely elimination, to the laboratory blank test results qualified, to continue the sample analysis.
10.3.2 At least one transport blank sample shall be collected for each batch. The results of the analysis should meet the control index of the blank test
(10.3.1), otherwise you need to find the cause, remove the interference after re-acquisition of sample analysis.
10.3.3 Each batch of samples (up to 20) shall be measured with a blank spike, the matrix spike and the matrix
The recoveries of the samples were in the range of 80.0% ~ 120%. The recoveries of the spiked samples were
In the range of 35.0% ~ 110%, the relative deviation of the matrix calibration results should be less than 20%.
711 Waste treatment
Hazardous wastes containing volatile aromatic hydrocarbons produced in the experiment shall be kept in a centralized manner and entrusted with qualified relevant units for processing.
12 Precautions
12.1 In order to prevent contamination by sampling tools, the sampling tool should be thoroughly washed with methanol and purified water before use. In the collection of its
When he samples, pay attention to the replacement of sampling tools and cleaning sampling tools to prevent cross-contamination.
12.2 During sample storage and transportation, to avoid contamination, the sample should be placed in a closed, dark portable refrigerator (5.8)
In the cold storage.
12.3 The necessary instruments, materials, medicines, etc. during the analysis shall be analyzed in advance to confirm that they contain interference with the analytical
The substance to be measured. Equipment, materials can be washed with methanol, as far as possible in the blank to remove the interference material.
8 Appendix A
(Normative appendix)
Method of detection limit, the lower limit of determination
When the amount of soil and sediment samples is 2 g, the detection limits of the 12 target species are determined, and the lower limit of determination is shown in Table A.1.
Table A.1 Method Detection limit, lower limit of determination
Compound name English name
The detection limit
(Μg/kg)
Lower limit
(Μg/kg)
Benzene 3.1 12.4
Toluene toluene 3.2 12.8
Ethylbenzene ethylbenzene 4.6 18.4
P-xylene p-xylene 3.5 14.0
M-xylene 4.4 17.6
Cumene isopropylbenzene 3.4 13.6
O-xylene o-xylene 4.7 18.8
Chlorobenzene 3.9 15.6
Styrene styrene 3.0 12.0
1,3-dichlorobenzene 3.4 13.6
1,4-dichlorobenzene 4.3 17.2
1,2-dichlorobenzene 3.6 14.4
9 Appendix B
(Informative)
Method of precision and accuracy
Table B.1 ~ B.2 gives the method of repeatability, reproducibility limit and spike recovery and other precision and accuracy indicators.
Table B.1 Method Precision
Compounds
name
Spiked concentration
(Μg/kg)
Determination of content
(Μg/kg)
Laboratory relative standard
Quasi-deviation (%)
Inter-laboratory relative
standard deviation(%)
Repeatability limit
(Μg/kg)
Reproducibility limit
(Μg/kg)
Soil Sediments Soil Sediments Soil Sediments Soil Sediments Soil Sediments Soil Sediments
25.0 25.0 17.2 25.6 3.6 to 4.0 2.0 to 3.0 3.6 3.1 1.9 1.9 2.4 2.8
100 100 90.6 105 0.9 to 3.3 1.7 to 4.0 2.1 3.0 5.9 6.8 7.7 10.8
500 500 369 483 1.8 ~ 3.8 1.2 ~ 2.0 1.3 1.4 30.2 23.8 30.5 29.2
Toluene
25.0 25.0 14.7 23.9 3.9 to 5.7 2.1 to 2...
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