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HJ 894-2017: Water quality. Determination of extractable petroleum hydrocarbons(C10-C40). Gas chromatography
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Water quality. Determination of extractable petroleum hydrocarbons(C10-C40). Gas chromatography
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Basic data | Standard ID | HJ 894-2017 (HJ894-2017) | | Description (Translated English) | Water quality. Determination of extractable petroleum hydrocarbons(C10-C40). Gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 11,168 | | Date of Issue | 2017-12-21 | | Date of Implementation | 2018-02-01 | | Quoted Standard | GB 17378.3; HJ/T 91; HJ/T 164 | | Regulation (derived from) | Ministry of Environmental Protection Announcement 2017 No. 77 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies gas chromatography for the determination of extractable petroleum hydrocarbons (C10-C40) in water. This standard applies to the determination of extractable petroleum hydrocarbons (C10-C40) in surface water, groundwater, domestic sewage, industrial wastewater and seawater. When the sample volume is 1000 ml, the method detection limit is 0.01 mg/L and the lower limit of determination is 0.04 mg/L. | HJ 894-2017: Water quality. Determination of extractable petroleum hydrocarbons(C10-C40). Gas chromatography
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(Water quality - Determination of petroleum hydrocarbons C10-C40) Determination of gas chromatography)
People's Republic of China national environmental protection standards
Water quality - Determination of petroleum hydrocarbons (C10-C40)
Gas chromatography
Water quality-Determination of extractable petroleum hydrocarbons
(C10-C40) -Gas chromatography
2017-12-21 Published
2018-02-01 implementation
Release MEP
i directory
Foreword .ii
1 Scope 1
2 Normative references 1
3 Terms and definitions
4 method principle 1
5 Reagents and materials .1
6 instruments and equipment
7 samples .2
8 Analysis Step 3
9 Results Calculation and Presentation 4
10 precision and accuracy .5
11 Quality Assurance and Quality Control .6
12 Waste disposal 6
13 Matters needing attention .6
Appendix A (informative) actual samples of petroleum hydrocarbons chromatogram 7
Foreword
In order to implement the "Law of the People's Republic of China on Environmental Protection" and the "Law of the People's Republic of China on Prevention and Control of Water Pollution", protect the environment,
Protection of human health, regulate the determination of water extractable petroleum hydrocarbons, the development of this standard.
This standard specifies the determination of surface water, groundwater, domestic sewage, industrial wastewater and seawater extractable petroleum hydrocarbons (C10-C40)
Gas Chromatography.
Appendix A of this standard is an informative annex.
This standard is released for the first time.
This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop.
This standard was drafted. National Environmental Analysis Test Center.
This standard verification unit. Shanghai Environmental Monitoring Center, Zhejiang Provincial Environmental Monitoring Center, Pearl River Basin Water Environment Monitoring
Heart, Changde City Environmental Monitoring Station, Xiangtan City Environmental Protection Monitoring Station and Beijing Zhongke Yingman Environmental Testing Research Center.
This standard MEP approved on December 21,.2017.
This standard since February 1,.2018 implementation.
This standard is interpreted by the MEP.
1 Water quality extractability Determination of petroleum hydrocarbons (C10-C40) Gas Chromatography
Warning. The solvents and standard samples used in the experiment are all toxic and harmful compounds, the solution should be prepared in the ventilation
Cabinet, the operation should be worn as required provisions of protective equipment, to avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of water extractable petroleum hydrocarbons (C10-C40) by gas chromatography.
This standard applies to surface water, groundwater, domestic sewage, industrial wastewater and seawater extractable petroleum hydrocarbons (C10-C40)
The determination.
When the sample volume is 1000 ml, the detection limit is 0.01 mg/L and the lower limit of determination is 0.04 mg/L.
2 Normative references
This standard references the following documents or the terms of them. For dated references, the effective version
Applicable to this standard.
GB 17378.3 Marine monitoring code Part 3 Sample collection, storage and transport
HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring
HJ/T 164 Groundwater Environmental Monitoring Technical Specifications
3 Terms and definitions
Extractable petroleum hydrocarbons (C10-C40) extractable petroleum hydrocarbons
Refers to the conditions specified in this standard can be extracted by dichloromethane and magnesium silicate is not adsorbed on the gas chromatogram
Retention time between n-C10H22 (included) and n-C40H82 (included).
Note. The extractable petroleum hydrocarbons (C10-C40) under this definition include aliphatic, alicyclic, aromatic or alkylated aromatics and the like.
4 method principle
Extraction of water with dichloromethane extractability of petroleum hydrocarbons, the extract was dehydrated, concentrated, purified, after the volume, with a
Hydrogen flame ionization detector (FID) gas chromatograph detection, according to the retention time qualitative, according to the time window range
Internal (C10-C40) chromatographic peak area and the standard quantitative comparison.
5 Reagents and materials
Unless otherwise specified, all analytical reagents used in the analysis are in accordance with national standards. The experimental water is distilled water.
5.1 Dichloromethane (CH2Cl2).
5.2 n-Hexane (C6H14).
5.3 anhydrous sodium sulfate (Na2SO4).
Burned at 500 ℃ 4h, cooled into the ground glass jar, placed in a desiccator to save.
25.4 silicon magnesium adsorbent.
Chromatography, 250μm-150μm (60 mesh -100 mesh), burning at 500 ℃ 4 h, cooled and then into the ground glass
Bottle, placed in a desiccator to save.
5.5 Concentrated hydrochloric acid. ρ (HCl) = 1.19 g/ml.
5.6 hydrochloric acid solution. 1 1.
Take 50ml concentrated hydrochloric acid (5.5) slowly added to 50 ml of water.
5.7 Dichloromethane - n-hexane solution. 1 4.
5.8 C10-C40 n-alkane standard solution. the concentration of n-alkanes are ρ = 1000 mg/L, the solvent is n-hexane.
You can buy a certified standard solution. Proven, you can also choose a diesel/lubricant certified standard solution.
5.9 Carrier gas. nitrogen, purity ≥ 99.999%.
5.10 combustion gas. hydrogen, purity ≥ 99.99%.
5.11 combustion gas. air, to be removed moisture and organic matter.
6 instruments and equipment
6.1 Sampling bottle. 1 L Brown glass bottle with grind plug.
6.2 Gas Chromatograph. Split/Splitless Inlet, Temperature Programmable, with Flame Ionization Detector (FID).
6.3 Column. Quartz capillary column, 30 m × 0.32 mm, film thickness 0.25 μm, with 5% phenyl-95% methyl
Polysiloxane, or use other equivalent column.
6.4 Concentration device. Rotary evaporation device, KD concentrator or nitrogen blowing device and other enrichment devices.
6.5 Silica-Magnesium Type Purification Column. 60 mm (column length) × 15 mm (ID) glass or polyethylene column with coarse-porous glass at the bottom
Sand core glass.
Purification column filling. 1000 mg activated silicon magnesium adsorbent (5.4) into a 50 ml beaker, add the appropriate amount
N-hexane (5.2), a magnesium silicate adsorbent was prepared as a suspension. The suspension is then poured into the purge column and the purge column is tapped
To fill the adsorbent. You can also use the same type of packing commercial purification column.
6.6 Separation funnel. 2 L Teflon cocks.
6.7 common laboratory equipment.
7 samples
7.1 sample collection and preservation
Water samples were taken according to the relevant provisions of GB 17378.3, HJ/T 91 and HJ/T 164. Sampling bottles (6.1) mining
Intensive 1000ml sample, hydrochloric acid solution (5.6) acidified to pH ≤ 2, the sample was stored at 4 ℃, 14d completed
Extraction, 40d analysis.
Note. When the petroleum hydrocarbon content in the water sample is too high, the sampling volume may be appropriately reduced.
7.2 Sample Preparation
7.2.1 Sample extraction
Transfer the entire sample to a 2 L separatory funnel (6.6), take 60 ml methylene chloride (5.1) and wash the sample vial.
3 all transferred to a separatory funnel, oscillation extraction 5 min (pay attention to deflated), stand for 10 min, until the two phases delamination, collecting the lower
The organic phase. An additional 60 ml of dichloromethane was added and the above procedure was repeated and the extracts were combined. The extract was passed over anhydrous sodium sulfate
(5.3) Dehydration. The entire aqueous phase was transferred to a 1000 ml graduated cylinder, and the sample volume was measured and recorded.
Note. Emulsification occurs during the extraction process, salting out, stirring, centrifugation, freezing and other methods can be used demulsification.
7.2.2 Sample concentration
The extract was concentrated to about 1 ml using a concentration apparatus (6.4) (Concentrated dichloromethane Reference conditions. water bath temperature 35 ° C,
Degree of vacuum of 750 hPa), 10 ml of n-hexane (5.2) was added and concentrated to about 1 ml (n-hexane concentration, reference conditions. water
Bath temperature 35 ℃, vacuum degree 260 hpa), then add 10 ml n-hexane (5.2), and finally concentrated to about 1 ml, to be a net
The
Note. The concentration of the sample volume of not less than 1 ml, otherwise the recovery rate is low.
7.2.3 Sample purification
The column (6.5) was activated with 10 ml of dichloromethane-n-hexane solution (5.7) followed by 10 ml of n-hexane (5.2)
When the column of n-hexane is nearly dry, transfer all the concentrated liquid to the purifying column, wash the collecting bottle with about 2 ml of n-hexane (5.2)
The washings were combined on a column and eluted with 10 ml of dichloromethane-n-hexane solution (5.7). The column was collected by gravity
Eluate in concentrate bottle.
Note. 1g magnesium silicate purification column of petroleum hydrocarbons purification capacity of 5 mg, if the determination of the total amount of petroleum hydrocarbons exceeds 5 mg, the extract required to be combined
Divided after dilution management, re-purification measured.
7.2.4 concentrated volume
Concentrate the eluate to approximately 1 ml using a concentrator (6.4) and dilute to 1.0 ml with n-hexane (5.2) for further testing.
7.3 Blank sample preparation
Replace the sample with distilled water, and follow the same procedure as sample preparation (7.2) to prepare a blank sample.
8 Analysis steps
8.1 GC reference conditions
Inlet temperature. 320 ° C Column flow. 2.0 ml/min Oven temperature. Initial temperature 60 ° C for 1 min,
Raise to 290 ° C at 8 ° C/min and then ramp to 320 ° C at 30 ° C/min for 7 min.
FID detector temperature. 330 ° C, hydrogen flow rate. 40.0 ml/min, air flow rate. 350.0 ml/min, makeup gas
Flow. 30.0 ml/min.
Injection method. Splitless injection, split 0.75min after injection, split ratio 30.1, injection volume. 1.0 μl.
Collection column loss map, used to deduct the column peak area loss.
8.2 Calibration
Take 5 10 ml brown volumetric flask, respectively, add an appropriate amount of n-hexane (5.2), with a micro syringe were added 10.0,
50.0,100,500,1000 μl C10-C40 n-alkane standard solution (5.8), with n-hexane volume, mix. Formulated
The n-alkanes concentration was 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 50.0 mg/L, 100 mg/L,
4 The total mass concentrations were 31.0 mg/L, 155 mg/L, 310 mg/L, 1550 mg/L, 3100 mg/L respectively.
The standard series of total mass concentration (mg/L) as the abscissa, the total peak area corresponding to the vertical axis, the establishment of the calibration curve
line.
8.3 Sample Determination
Specimen (7.2) is measured according to the same GC reference conditions (8.1) as the calibration curve.
8.4 Blank test
The blank sample (7.3) is measured according to the same GC reference conditions (8.1) as the sample.
9 results calculated and expressed
9.1 Qualitative analysis
According to the chromatographic component retention time of the target compound to be qualitative, the chromatogram shown in Figure 1. C10-C40 target compound
The method of determining the total amount of the target compound starts from the peak of n-C10H22 (inclusive) to n-C40H82
(Including) the end of the peak, calculate the total peak area of C10-C40 (here peak area deducts the total peak area after column loss)
The chromatogram of the column is shown in Figure 2.
Figure 1 C10-C40 normal paraffin gas chromatogram
5 Figure 2 8.1 Chromatogram of the column under GC reference conditions
9.2 Quantitative analysis
Based on the total peak area of the target compound in the retention time window (the total peak area here is the total peak after subtracting the column loss
Area), obtained by external standard method of the total concentration of the target compound. Water quality extractable petroleum hydrocarbons (C10-C40) mass concentration
ρ (mg/L), calculated according to formula (1).
a-Axρ 1 (1)
Where. ρ - water extractable petroleum hydrocarbon (C10-C40) mass concentration, mg/L;
Total peak area of the target compound (total peak area here is the total peak area after column loss)
a - the intercept of the calibration curve;
b - the slope of the calibration curve;
V-water sample volume, L;
V1-sample volume, ml;
f - is the dilution factor.
9.3 results show
When the determination result is 1.00 mg/L or more, the data retain three significant figures; when the result is less than 1.00 mg/L,
Keep two decimal places.
10 precision and accuracy
10.1 Precision
Six laboratories, respectively, with extractable petroleum hydrocarbon concentrations of 0.05 mg/L, 0.10 mg/L, 1.00 mg/L of the unification
The samples were measured 6 times in parallel. The relative standard deviations in the laboratory ranged from 6.1% to 6.8%, from 7.0% to 9.6%
9.0% ~ 12%; The relative standard deviation of the laboratory were 6.7%, 9.2%, 10% respectively; The repeatability limits were.
C40C10
60.01 mg/L, 0.02 mg/L and 0.30 mg/L, respectively. The reproducibility limits were 0.01 mg/L, 0.03 mg/L and 0.40 mg/L, respectively.
Six laboratories on domestic sewage, seawater and petrochemical industrial wastewater uniform samples were measured 6 times in parallel, the experiment
Indoor relative standard deviations ranged from 6.6% to 24%, 6.7% to 31% and 6.2% to 29%, respectively; relative standard between laboratories
Deviations range. 29%, 18%, 17%.
10.2 Accuracy
Six laboratories on the surface water, domestic sewage, seawater and petrochemical industrial wastewater uniform samples were spiked analysis
The standard additions were 0.05 mg/L, 0.10 mg/L, 0.10 mg/L and 1.00 mg/L, respectively. The spiked recoveries were.
84% -96%, 78% -101%, 74% -93%, 83% -108%. The final recoveries of spiked samples were 91% ± 11%
85% ± 17%, 86% ± 15%, 90% ± 19%.
11 Quality Assurance and Quality Control
11.1 Blank test
Make at least 1 lab blank for every 20 samples or batches of samples (less than 20 samples/batches) with a blank value below
Method detection limit.
11.2 Calibration curve
The calibration curve for the first calibration should have a correlation coefficient of ≥ 0.995.
11.3 continuous calibration
Each determination of 20 samples should be continuous calibration, determination of a calibration curve intermediate concentration standard solution, the determination of the results and
The relative error of the initial calibration should be within ± 20%.
11.4 blank spike
Make at least one blank spike analysis for every 20 samples or batches of samples. The spike recovery should be between 70% and 120%.
12 Waste treatment
All waste liquid generated during the experiment should be kept in airtight containers and entrusted to qualified units for disposal.
13 Precautions
13.1 Since this method quantifies the total peak area of C10H22 to C40H82, if the column fails to pass the assembly, the result
High, it is necessary to regularly check the column loss of the spectrum, so as to avoid column performance bias.
13.2 Samples with high levels of halogenated hydrocarbons will result in higher results.
7 Appendix A.
(Informative)
The actual sample of petroleum hydrocarbons chromatogram
Figure A.1 petroleum gas chromatogram of an actual water sample
C10 C40
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