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HJ 784-2016: Soil and sediment. Determination of polycyclic aromatic hydocabons. High performance liquid chromatography
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Soil and sediment. Determination of polycyclic aromatic hydocabons. High performance liquid chromatography
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HJ 784-2016
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Basic data | Standard ID | HJ 784-2016 (HJ784-2016) | | Description (Translated English) | Soil and sediment. Determination of polycyclic aromatic hydocabons. High performance liquid chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z13 | | Word Count Estimation | 18,117 | | Date of Issue | 2016-02-01 | | Date of Implementation | 2016-03-01 | | Quoted Standard | GB 17378.3; GB 17378.5; HJ 613; HJ/T 166 | | Regulation (derived from) | ?Ministry of Environment Protection Bulletin 2016 No.10 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies high performance liquid chromatography (HPLC) for the determination of PAHs in soils and sediments. This standard applies to the determination of 16 PAHs in soils and sediments including naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [a], anthracene, Benzo [a] pyrene, dibenzo [a, h] anthracene, benzo [g, h, i] pyrene, indeno [1, 2, 3-c, d] pyrene. | HJ 784-2016: Soil and sediment. Determination of polycyclic aromatic hydocabons. High performance liquid chromatography
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Soil and sediment. Determining of polycyclic aromatic hydocabons. High performance liquid chromatography
National Environmental Protection Standard of the People 's Republic of China
Determination of polycyclic aromatic hydrocarbons in soil and sediments
High performance liquid chromatography
Soil and sediment - Determination of polycyclic aromatic hydocabons
- High performance liquid chromatography
2016-02-01 release
2016-03-01 implementation
Ministry of Environmental Protection released
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
Precision and accuracy
10 Quality assurance and quality control
11 Waste treatment 8
Appendix A (normative appendix) method of detection limit and lower limit of determination
Appendix B (informative) method of precision and accuracy 11
Foreword
For the implementation of the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate soil and sediment
Preparation of polycyclic aromatic hydrocarbons, the development of this standard.
This standard specifies high performance liquid chromatography for polycyclic aromatic hydrocarbons (PAHs) compounds 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. Henan Province Environmental Monitoring Center.
This standard is verified by. Institute of Hydrogeology and Geology and Environmental Geology, Chinese Academy of Geological Sciences, Zhengzhou Environmental Protection Monitoring Center
Station, Kaifeng City Environmental Monitoring Station, Luoyang City Environmental Monitoring Station, Xinxiang City Environmental Monitoring Station.
This standard is approved by the Ministry of Environmental Protection on February 1,.2016.
This standard has been implemented since March 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of polycyclic aromatic hydrocarbons in soil and sediments - High performance liquid chromatography
Warning. part of the polycyclic aromatic hydrocarbons are strong carcinogens, the operation should be required to wear protective equipment, to avoid contact with the skin
And clothes. Solution preparation and sample pretreatment should be carried out in a fume hood.
1 Scope of application
This standard specifies high performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons in soil and sediments.
This standard is applicable to the determination of 16 polycyclic aromatic hydrocarbons in soil and sediments, including naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene,
(A) pyrene, dibenzo (a, h) anthracene, benzo (a) pyrene, benzo (a) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, G, h, i)
Perylene, indene (1,2,3-c, d) pyrene.
When the sampling volume is 10.0 g and the volume of volume is 1.0 ml, the method of 16 kinds of polycyclic aromatic hydrocarbons is determined by UV detector.
And the limit of determination was 12 μg/kg ~ 20 μg/kg. The 16 kinds of polycyclic aromatic compounds
The detection limit of the method is 0.3 μg/kg ~ 0.5 μg/kg, and the limit of determination is 1.2 μg/kg ~ 2.0 μg/kg. See Appendix A. for details.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Any unspecified date of the reference file, the effective version of the appropriate
For this standard.
Specification for ocean monitoring - Part 3. Sample collection, storage and transport
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
The polycyclic aromatic hydrocarbons (PAHs) in soil and sediment samples were extracted with a suitable extraction method (Soxhlet extraction, pressurized fluid extraction, etc.)
According to the sample matrix interference to take appropriate purification methods (silica gel column, silica gel or magnesium silicate solid phase extraction column, etc.)
Extraction solution for purification, concentration, constant volume, equipped with UV/fluorescence detector high-performance liquid chromatography separation test to protect
Time qualitative, external standard method.
4 reagents and materials
Unless otherwise stated, analytical analytical reagents and experimental water are used in accordance with national standards.
4.1 acetonitrile (CH3CN). HPLC grade.
4.2 n-hexane (C6H14). HPLC grade.
4.3 dichloromethane (CH2Cl2). HPLC grade.
4.4 Acetone (CH3COCH3). HPLC grade.
4.5 Acetone-n-hexane mixed solution. 1 1.
Mix with acetone (4.4) and n-hexane (4.2) in a 1. 1 by volume ratio.
4.6 Dichloromethane-n-hexane mixed solution. 2 3.
Mixed with dichloromethane (4.3) and n-hexane (4.2) at a volume ratio of 2. 3.
4.7 Dichloromethane-n-hexane mixed solution. 1 1.
2 was mixed with methylene chloride (4.3) and n-hexane (4.2) in a 1. 1 by volume ratio.
4.8 Polycyclic aromatic hydrocarbon standard stock solution. ρ = 100 mg/L ~.2000 mg/L.
Purchase a commercially available standard solution, store it at 4 ° C, store it in a dark place, or store it with reference to a standard solution certificate. Make
Use should be restored to room temperature and shake.
4.9 Polycyclic aromatic hydrocarbons standard use of liquid. ρ = 10.0 mg/L ~.200 mg/L.
Remove the 1.0 ml polycyclic aromatic hydrocarbon standard stock solution (4.8) in a 10 ml brown flask, diluted with acetonitrile (4.1) and set
To the scale, shake, transferred to the dense bottle at 4 ℃ in the cold, dark preservation.
4.10 Diphenyl biphenyl (C12F10). 99% purity.
Alternatives, other analogues may also be used.
4.11 Decafluorobenzene stock solution. ρ = 1000 mg/L.
Weigh decamerobenzene (4.10) 0.025 g (exact to 0.001 g), dissolve with acetonitrile (4.1) and set to 25 ml
Color volume bottle, shake, transfer to a dense bottle in the 4 ℃ cold storage, dark preservation. Or purchase a commercially available standard solution.
4.12 Use of decafluorobenzene. ρ = 40 μg/ml.
Remove the 1.0 ml solution of tetradecafluorobenzene (4.11) in a 25 ml brown volumetric flask, dilute with acetonitrile (4.1) and set the volume
To the scale, shake, transferred to the dense bottle at 4 ℃ in the cold, dark to save.
4.13 Desiccant. anhydrous sodium sulfate (Na2SO4) or granular diatomaceous earth
Placed in the muffle furnace 400 ℃ bake 4 h, after cooling placed in the grinding glass bottle sealed preservation.
4.14 Silica gel. particle size 75 μm ~ 150 μm (200 mesh ~ 100 mesh).
Before use, should be placed in a flat bottom tray, with aluminum foil loosened, 130 ° C activated at least 16 h.
4.15 glass column. diameter of about 20 mm, length 10 cm ~ 20 cm, with PTFE piston.
4.16 silica gel solid phase extraction column. 1000 mg/6 ml.
4.17 magnesium silicate solid phase extraction column. 1000 mg/6 ml.
4.18 quartz sand. particle size 150 μm ~ 830 μm (100 mesh ~ 20 mesh), before use to be tested to confirm that no interference.
4.19 glass wool or glass fiber filter. muffle furnace in 400 ℃ baking 1 h, after cooling placed in the grinding glass bottle sealed.
4.20 Nitrogen. Purity ≥99.999%.
5 instruments and equipment
5.1 High Performance Liquid Chromatograph. equipped with UV detector or fluorescence detector, with gradient elution function.
5.2 Column. ODS (octadecyl silane bonded silica gel), particle size 5 μm, column length 250 mm, inner diameter 4.6 mm
Of the reversed-phase column or other similar performance of the column.
5.3 Extraction device. Soxhlet extractor or other equivalent equipment.
5.4 Concentration devices. nitrogen blowing concentrator or other equivalent equipment.
5.5 Solid phase extraction device.
5.6 Common laboratory equipment and equipment.
6 samples
6.1 Collection and storage of samples
According to the relevant requirements of HJ/T 166 collection and preservation of soil samples, in accordance with the relevant requirements of GB 17378.3 collection and security
3 deposits of sediments. Samples should be stored in a clean brown jar glass bottle, the transport process should be dark, sealed, refrigerated.
If you can not timely analysis, should be below 4 ℃ cold storage, dark and sealed preservation, storage time is 7 d.
6.2 Determination of moisture
Soil sample dry matter was measured in accordance with HJ 613, and the moisture content of sediment samples was carried out in accordance with GB 17378.5.
6.3 Preparation of the sample
Remove the sample of sticks, leaves, stones and other foreign matter, weighed the sample 10 g (accurate to 0.01 g), adding the amount of no
Water sodium sulfate (4.13), grinding homogenization into quicksand. If pressurized fluid is used, it is treated with granular diatomaceous earth (4.13)
water.
Note 1. The sample may also be dewatered by freeze drying, and the lyophilized sample may be ground, sieved, and homogenized to about 1 mm of granules.
6.3.1 Extraction
Place the prepared sample in a glass tube or paper tube and add 50.0 μl of the solution (4. 12)
The sleeve is placed in a Soxhlet extractor. Add 100 ml of acetone-n-hexane mixed solution (4.5) to no less than 4 times per hour
Reflux rate extraction 16 h ~ 18 h.
Note 2. Other methods of extraction may also be used if the quality control requirements of this standard are verified and met.
Note 3. The casing size depends on the sample size.
6.3.2 Filtration and dehydration
Add a layer of glass wool or glass fiber filter (4.19) to the glass funnel and add about 5 g of anhydrous sodium sulfate (4.13)
The extract was filtered into a concentrated vessel. The extraction vessel was washed three times with an appropriate amount of acetone-n-hexane mixed solution (4.5)
The acetone-n-hexane mixed solution (4.5) rinses the funnel and the lotion is incorporated into the concentrate vessel.
6.3.3 Concentration
Nitrogen blowing concentration method. open the nitrogen to the solvent surface with airflow fluctuations (to avoid the formation of gas vortex), with n-hexane (4.2)
The walls of the concentrator that have been exposed during the nitrogen blowing process are concentrated and the filtered and dehydrated extracts are concentrated to about 1 ml. If you do not need to clean,
Add about 3 ml of acetonitrile (4.1) and concentrate to about 1 ml to completely convert the solvent to acetonitrile. For purification, add about 5 ml
N-hexane and concentrated to about 1 ml. This concentration was repeated three times, the solvent was completely converted to n-hexane and concentrated to about 1 ml,
To be purified.
Note 4. Rotary Evaporation Concentration or other enrichment may also be used.
6.3.4 Purification
6.3.4.1 silica gel column purification
(1) silica gel column preparation
Glass wool (4.19) was added to the bottom of the glass column (4.15), 10 mm thick anhydrous sodium sulphate (4.13) was added,
Rinse with a small amount of dichloromethane (4.3). A glass funnel was placed on a glass column and dichloromethane (4.3) was added until
Filled with chromatography column, the funnel to retain part of the dichloromethane, weighed about 10 g silica gel (4.14) by adding a funnel column to the glass
The rod is tapped and the column is removed to remove the bubbles. Dichloromethane was added and 10 mm thick was added to the top of the column
Anhydrous sodium sulfate (4.13). Columns are shown in Figure 1.
4 Fig.1 Schematic diagram of chromatographic column
(2) purification
The elution rate was controlled at 40 ml of n-hexane (4.2), and the rinse rate was controlled at 2 ml/min.
Before exposure to air, close the column bottom polytetrafluoroethylene piston, discard the effluent. Approximately 1 ml of the extract was concentrated
(6.3.3) into the column, washed with 2 ml of n-hexane (4.2) 3 times, and the lotion was completely transferred to the column,
Before the top anhydrous sodium sulfate was exposed to air, add 25 ml of n-hexane (4.2) to continue rinsing and discard the effluent. use
25 ml of methylene chloride-n-hexane mixed solution (4.6). The eluate was collected in a concentrated vessel and purged with nitrogen
Other concentrated methods) The eluate was concentrated to about 1 ml, about 3 ml of acetonitrile (4.1) was added, and then concentrated to below 1 ml.
The solvent is completely converted to acetonitrile and is accurately set to 1.0 ml. After the test sample if the test can not be timely analysis, should be
4 ℃ under refrigeration, dark, sealed, 30 d to complete the analysis.
6.3.4.2 Solid phase extraction column purification (filler for silica gel or magnesium silicate)
The solid phase extraction column (4.16 or 4.17) was used as a purification column and fixed on a solid phase extraction apparatus (5.5). With 4 ml
Dichloromethane (4.3) Wash the column and equilibrate the column with 10 ml of n-hexane (4.2) to close the column
Control valve infiltration 5 min, open the control valve, discard the effluent. Approximately 1 ml of the concentrated solution was concentrated before the solvent was dried
(6.3.3) into the column, 3 ml of n-hexane (4.2) 3 times to wash the concentrated utensils, lotion all into the column, with 10
Ml of methylene chloride-n-hexane mixed solution (4.7), and the eluent was immersed in the purification column to close the flow rate control valve,
Run 5 min, then open the control valve, receive the eluent to complete outflow. Wash with a nitrogen blowing method (or other enrichment)
Disintegrate to about 1 ml, add about 3 ml of acetonitrile (4.1), then concentrate to below 1 ml, convert the solvent to acetonitrile,
And accurate to 1.0 ml to be measured. After the test sample if the test can not be timely analysis, should be frozen at 4 ℃, dark, dense
Sealed, 30 days to complete the analysis.
6.4 Preparation of blank sample
A blank sample was prepared in the same manner as in the preparation (6.3) of the sample using quartz sand (4.18) instead of the actual sample.
7 Analysis steps
7.1 Instrument reference conditions
Injection volume. 10 μl.
Column temperature. 35 ° C.
5 Flow rate. 1.0 ml/min.
Mobile phase A. acetonitrile; mobile phase B. water.
Table 1 gradient elution program
Time (min) A% B%
28.5 60 40
Detection wavelength. According to the peak time of different objects to choose its UV detection wavelength, the best excitation wavelength and the best emission
Wavelength, the preparation of wavelength conversion procedures. 16 polycyclic aromatic hydrocarbons in the UV detector on the corresponding maximum absorption wavelength and in the fluorescence inspection
The optimum excitation and emission wavelengths for specific conditions are shown in Table 2.
Table 2 corresponds to the target UV detection wavelength and fluorescence detection wavelength
No. Component name Maximum UV absorption wavelength
Recommended UV
Absorption wavelength
Recommended excitation wavelength λex
/ Emission wavelength λem
Optimal excitation wavelength λex
/ Emission wavelength λem
1 naphthalene 220 220 280/324 280/334
2 acenaphthylene 229 230 -
3 acenaphthene 261 254 280/324 268/308
4 fluorene 229 230 280/324 280/324
5 Philippines 251 254 254/350 292/366
6 anthracene 252 254 254/400 253/402
7 fluoranthene 236 230 290/460 360/460
8 pyrene 240 230 336/376 336/376
9 benzo (a) anthracene 287 290 275/385 288/390
10 䓛 267 254 275/385 268/383
11 benzo (b) fluoranthene 256 254 305/430 300/436
12 benzo (k) fluoranthene 307,240 290 305/430 308/414
13 benzo (a) pyrene 296 290 305/430 296/408
14 dibenzo (a, h) anthracene 297 290 305/430 297/398
15 benzo (g, h, i) perylene 210 220 305/430 300/410
16 indene (1,2,3-c, d) pyrene 250 254 305/500 302/506
17 Fluorobiphenyl 228 230 - -
Note. Fluorescence detectors are not suitable for the determination of acenaphthylene and decaphenyl.
7.2 Calibration
7.2.1 Drawing of calibration curves
(4.9) and diluted with acetonitrile (4.1) to prepare at least 5 concentration points
6 standard series, the concentration of polycyclic aromatic hydrocarbons were 0.04 μg/ml, 0.10 μg/ml, 0.50 μg/ml, 1.00 μg/ml
And 5.00 μg/ml (this is the reference concentration), while taking 50.0 μl of decafluorobenzene using the liquid (4.12), added to the standard series
At any concentration point, the mass concentration of tetradecafluorobenzene was 2.00 μg/ml, stored in a brown vial and tested.
From the low concentration to high concentration followed by the standard series of solution into the standard series of solution concentration of the target component for the sitting
Standard, with its corresponding peak area (peak height) as the ordinate, the establishment of calibration curve. The correlation coefficient of the calibration curve is ≥0.995,
Otherwise re-draw the calibration curve.
7.2.2 Chromatogram of standard sample
Figure 2 and Figure 3 for the standard equipment in this standard conditions, 16 polycyclic aromatic hydrocarbons chromatogram.
Figure 2 16 polycyclic aromatic hydrocarbons UV detector chromatogram
Fig.3 Chromatogram of 16 kinds of polycyclic aromatic hydrocarbons fluorescence detector
1-naphthalene; 2-acenaphthylene; 3-acenaphthene; 4-fluorene; 5-phenanthrene; 6-anthracene; 7-fluoranthene; 8-pyrene;
11-benzo (b) fluoranthene; 13-benzo (k) fluoranthene; 14-benzo (a) pyrene; 15-dibenzo (a, h) anthracene; G, h, i) perylene;
17-indeno (1,2,3-c, d) pyrene. (Where. acenaphthylene and decaphene are not detected by fluorescence detectors.)
7.3 Determination
7.3.1 Specimen determination
The measurement was carried out according to the same instrument analysis conditions (7.1) as the drawing calibration curve.
77.3.2 Blank test
The measurement of the blank sample (6.4) was carried out according to the same instrumental analysis condition (7.1) as the sample measurement.
Calculation and representation of results
8.1 Qualitative analysis of the target compound
The target compound retention time qualitative, if necessary, can be used standard sample addition method, the absorption ratio at different wavelengths,
Ultraviolet spectrum scanning and other methods to assist qualitative.
8.2 Calculation of results
8.2.1 The content of polycyclic aromatic hydrocarbons in soil samples (μg/kg) is calculated according to formula (1).
Dm
I Wm
(1)
Where.
I - the content of component i in the sample, μg/kg;
I - the concentration of the resulting component i calculated from the standard curve, μg/ml;
V - constant volume, ml;
M - sample weight (wet weight), kg;
DmW - dry matter content of soil samples,%.
8.2.2 The content of polycyclic aromatic hydrocarbons (PAHs) in sediments samples is calculated according to formula (2).
Wm
Vi
I
(2)
Where.
I - the content of component i in the sample, μg/kg;
I - the concentration of the resulting component i calculated from the calibration curve, μg/ml;
V - constant volume, ml;
M - sample weight (wet weight), kg;
W - sediment sample moisture content,%.
8.2.3 Recovery of decafluorobenzene (%), calculated according to equation (3).
221
VA
VAP
(3)
Where.
8P - recovery rate of 10 - fluorobiphenyl,%;
1A - peak area of tetradecafluorobenzene in sample;
2A - Standard area of the peak area of tetradecafluorobenzene;
1 _ - the concentration of the solvent used in decaphenyl fluoride, 40 μg/ml;
2 - mass concentration of tetradecafluorobenzene in standard series, 2 μg/ml;
1V - the volume of the solution used in the addition of decafluorobenzene in the sample, 50.0 μl;
2V - volume of sample volume, ml.
8.3 results show
When the determination result is greater than or equal to 10 μg/kg, the three effective digits are retained; when the result is less than 10 μg/kg,
Reserved to 1 decimal place. The acenaphthene retains the integer number and retains up to three significant digits.
9 precision and accuracy
9.1 precision
The concentration of the target compound was 1 μg/kg ~ 10 μg/kg, 5 μg/kg ~ 100 μg/kg, 10 μg/kg ~
200 μg/kg of the same sample for 6 times the repeated determination. the relative standard deviation of the laboratory were 4.3% to 15%, 4.1% ~
14%, 4.1% ~ 12.3%, respectively. The relative standard deviations were 9.7% ~ 22%, 6.2% ~ 12% and 4.2% ~ 13%, respectively.
The reproducibility limits were. 0.3 μg/kg to 5.6 μg/kg, 2.2 μg/kg to 28 μg/kg, 2.4 μg/kg to 45 μg/kg, respectively.
The present limits were. 0.5 μg/kg to 8.0 μg/kg, 1.5 μg/kg to 34 μg/kg, 2.8 μg/kg to 56 μg/kg, respectively.
9.2 Accuracy
Six laboratories were tested with soil and sediment as the substrate, and the spiked concentration was
100 μg/kg ~.200 μg/kg, each sample was repeated 6 times, the recoveries were 59.3% ~ 98.7%, 57.4% ~
91.9%, and the final recoveries were. 69.5% ± 13.1% ~ 92.5% ± 14.9%, 70.3% ± 17.4% ~
90.9% ± 4.3%.
The accuracy and accuracy of the results are given in Appendix B.
10 quality assurance and quality control
10.1 blank analysis
Each analysis is done at least one lab blank experiment and a full program blank to check for possible interference, its head
The measured value of the compound is not higher than the detection limit of the method.
10.2 parallel sample determination
A parallel sample should be analyzed for every 20 samples or per batch (less than 20 samples/batch). Results of parallel sampling
Relative deviation should be ≤ 30%.
10.3 matrix spikes
Every 20 samples or each batch (less than 20 samples/batch) to be a matrix plus standard sample, the recovery rate of each component in 50% ~
120% between. The recoveries of te...
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