|
US$419.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 805-2016: Soil and Sediment - Determination of polycyclic aromatic hydrocarbon by Gas chromatography - Mass Spectrometry Method
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 805-2016 | English | 419 |
Add to Cart
|
4 days [Need to translate]
|
Soil and Sediment - Determination of polycyclic aromatic hydrocarbon by Gas chromatography - Mass Spectrometry Method
| Valid |
HJ 805-2016
|
PDF similar to HJ 805-2016
Basic data | Standard ID | HJ 805-2016 (HJ805-2016) | | Description (Translated English) | Soil and Sediment - Determination of polycyclic aromatic hydrocarbon by Gas chromatography - Mass Spectrometry Method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Word Count Estimation | 18,132 | | Date of Issue | 2016-06-24 | | Date of Implementation | 2016-08-01 | | Regulation (derived from) | Ministry of Environmental Protection Announcement No.47, 2016 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 805-2016: Soil and Sediment - Determination of polycyclic aromatic hydrocarbon by Gas chromatography - Mass Spectrometry Method
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(PAHs in soil and sediment by gas chromatography - mass spectrometry)
National Environmental Protection Standard of the People 's Republic of China
Determination of polycyclic aromatic hydrocarbons in soil and sediments
Gas chromatography - mass spectrometry
Soil and Sediment-Determination of polycyclic aromatic
Hydrocarbon by Gas chromatography-Mass Spectrometry Method
2016-06-24 released
2016-08-01 implementation
Ministry of Environmental Protection
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 3
6 Sample 3
7 Analysis steps
8 Calculation and representation of results
9 Precision and Accuracy
10 Quality assurance and quality control
11 Waste treatment .9
12 Note ..10
Appendix A (normative) method of detection limit and lower limit of determination
Appendix B (informative) Reference parameters for the determination of the target compound
Appendix C (informative) method of precision and accuracy
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 the determination of 16 polycyclic aromatic hydrocarbons in soil and sediments by gas chromatography-mass spectrometry.
This standard is the first release.
Appendix A to 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. Henan Province Environmental Monitoring Center.
The standard verification unit. Henan Province Environmental Science Research Institute, Xinxiang City Environmental Monitoring Station, Zhengzhou City Environmental Monitoring Station, opened
Closed city environmental monitoring station, Chinese Academy of Geological Sciences Institute of hydrogeology and geology, environmental monitoring center in Henan Province.
The Environmental Protection Department of this standard is approved on June 24,.2016.
This standard has been implemented since August 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of polycyclic aromatic hydrocarbons in soil and sediments - Gas chromatography - mass spectrometry
Warning. The organic solvents and reference materials used in the experiment are toxic and hazardous substances, the standard solution preparation and the sample pretreatment process should be
Fume hood; operation should be required to wear protective equipment, to avoid direct contact with skin and clothing.
1 Scope of application
This standard specifies the determination of polycyclic aromatic hydrocarbons in soil and sediments by gas chromatography-mass spectrometry.
This standard is applicable to the determination of 16 polycyclic aromatic hydrocarbons in soil and sediments. The target compounds include naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene,
(A) anthracene, benzo (b) fluoranthene, benzo (k) fluoranthene, benzo (a) pyrene, dibenzo (a, h) anthracene, benzene
And (g, h, i) perylene and indene (1,2,3, -c, d) pyrene.
When the sampling volume is 20.0 g and the volume of volume after concentration is 1.0 ml, the detection limit of the method is
0.08 mg/kg to 0.17 mg/kg, with a lower limit of 0.32 mg/kg to 0.68 mg/kg. See Appendix A. for details.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard
quasi.
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
Extraction of pressurized fluid from soil and sediment organic matter
3 Principle of the method
Polycyclic aromatic hydrocarbons in soil or sediments are extracted using a suitable extraction method (Soxhlet extraction, pressurized fluid extraction, etc.)
Body interference to choose the appropriate purification method (copper powder desulfurization, silica gel column, magnesium silicate column or gel permeation chromatography) on the extract purification,
Concentrated, constant volume, by gas chromatography separation, mass spectrometry. Through the mass spectrometry with the standard material, retention time, fragment ion mass ratio and its abundance
Comparison of qualitative and internal standard method.
4 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water for the new preparation of ultra-pure water or distilled water.
4.1 acetone (C3H6O). pesticide residues.
4.2 n-hexane (C6H14). pesticide residues.
4.3 dichloromethane (CH2Cl2). pesticide residues.
4.4 ethyl acetate (C4H8O2). pesticide residues.
4.5 pentane (C5H12). pesticide residues.
4.6 Cyclohexane (C6H12). Pesticide level.
4.7 Acetone-n-hexane mixed solvent. 1 1.
2 was mixed at a 1. 1 volume ratio with n-hexane (4.2) and acetone (4.1).
4.8 Dichloromethane-pentane mixed solvent. 2 3
Mixed with dichloromethane (4.3) and pentane (4.5) at a volume ratio of 2. 3.
4.9 Dichloromethane-n-hexane mixed solvent. 1 9
Mixed with methylene chloride (4.3) and n-hexane (4.2) at a 1. 9 volume ratio.
4.10 Gel permeation chromatography Mobile phase. Ethyl acetate (4.4) -cyclohexane (4.6) Mixing solvent (1 1), or by instrumentation
His solvent system.
4.11 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
4.12 nitric acid solution. 1 1 (v/v), prepared with nitric acid (4.11).
4.13 copper powder (Cu). purity of 99.5%
Use the nitric acid solution (4.12) to remove the oxide on the surface of the copper powder before use. Rinse the acid with the test water and rinse with acetone (4.1)
After the dry with nitrogen, each pretreatment, keep the copper powder surface bright.
4.14 polycyclic aromatic hydrocarbons standard stock solution. ρ = 1000 mg/L ~ 5000 mg/L, commercially available standard solution.
4.15 Polycyclic Aromatic Hydrochloride Standard Intermediate. ρ =.200 μg/ml to 500 μg/ml
The polycyclic aromatic hydrocarbon standard stock solution (4.14) was diluted with acetone-n-hexane mixed solvent (4.7).
4.16 internal standard stock solution. ρ = 5000 mg/L
Naphthalene-d8, acenaphthene-d10, phenanthrene-d10, -d12 and perylene-d12, commercially available standard solutions. Other properties can also be used similar to the semi-volatile
Organic matter to do internal standard.
4.17 internal standard liquid. ρ =.200 μg/ml ~ 400 μg/ml
The internal standard stock solution (4.16) was diluted with acetone-n-hexane mixed solvent (4.7).
4.18 Substitute stock solution. ρ =.2000 mg/L to 4000 mg/L, commercially available standard solution.
2-fluorobiphenyl and p-terphenyl-d14; also available deuterated polycyclic aromatic hydrocarbons as substitutes.
4.19 Substitute Intermediate. ρ = 500 μg/ml
The stock solution (4.18) was diluted with acetone-n-hexane mixed solvent (4.7).
4.20 decafluorotriphenylphosphine (DFTPP). ρ = 50 mg/L, commercially available standard solution. Can also purchase a higher concentration of DFTPP standard solution, with
Dichloromethane (4.3) was diluted to 50 mg/L.
4.21 Gel Permeation Chromatography Calibration Solution. Contains corn oil (25 mg/ml), di (2-diethylhexyl) phthalate (1 mg/ml)
Methotrexate (200 mg/L), perylene (20 mg/L) and sulfur (80 mg/L). Commercially available.
4.22 desiccant. excellent grade pure anhydrous sodium sulfate (Na2SO4) or granular diatomaceous earth.
Placed in the muffle furnace 400 ℃ bake 4 h, after cooling into the grinding glass bottle sealed in the dryer to save.
4.23 Silica Adsorbent. 75 μm (200 mesh) ~ 150 μm (100 mesh)
Placed in the surface dish, with aluminum foil or tin paper light cover, 130 ℃ activation at least 16 h, remove the dryer into the cooling, stand-by. Before use
activation.
4.24 glass column. about 20 mm in diameter, 10 cm ~ 20 cm long, with PTFE piston.
4.25 Magnesium silicate purification column. filler for the magnesium silicate, 1000 mg, column volume of 6 ml.
4.26 quartz sand. 150 μm (100 mesh) ~ 830 μm (20 mesh)
Placed in the muffle furnace 400 ℃ bake 4 h, after cooling into the grinding glass bottle sealed.
34.27 glass wool or glass fiber filter. before use with dichloromethane (4.3) immersion, to be dichloromethane (4.3) volatile dry, stored in the grinding mouth
The glass bottle is sealed and stored.
4.28 Carrier gas. high purity helium, purity of 99.999% or more.
5 instruments and equipment
5.1 Gas Chromatography/Mass Spectrometer. Electron Impact (EI) Ionization Source.
5.2 Column. quartz capillary column, length 30 m, inner diameter 0.25 mm, film thickness 0.25 m, stationary phase 5% - phenyl-methyl polysiloxane
Alkyl, or other equivalent capillary column.
5.3 Extraction device. Soxhlet extraction or pressurized fluid extractor and other equipment equivalent performance.
5.4 Gel Permeation Chromatography (GPC). A 254 nm fixed wavelength UV detector, filled with gel packing column.
5.5 Concentration device. rotary evaporator, nitrogen blowing instrument or other equivalent equipment.
5.6 Vacuum Freeze Dryer. No load vacuum below 13 Pa.
5.7 solid phase extraction device.
5.8 General laboratory equipment and equipment commonly used.
6 samples
6.1 Collection and storage of samples
Soil samples were collected and preserved in accordance with the relevant requirements of HJ/T 166, and samples of sediments were collected in accordance with the relevant requirements of GB 17378.3
save. Samples should be stored in a clean, ground brown glass bottle. Transport should be sealed, dark, 4 ℃ below the cold storage. If not timely
Analysis, should be below 4 ℃ cold storage, dark, sealed, save time for 10 days.
6.2 Determination of moisture
Determination of dry matter content of soil samples According to HJ 613, the moisture content of sediment samples was measured according to GB 17378.5.
6.3 Preparation of the sample
6.3.1 Sample preparation
The soil or sediment samples taken in enamel or glass tray, remove branches sticks, leaves, stones and other foreign matter, fully mixed. Said
Take 20 g (accurate to 0.01 g) fresh sample for dehydration, add appropriate amount of anhydrous sodium sulfate (4.22), mix evenly, grind into fine particles.
If pressurized fluid extraction is used, it is treated with granular diatomaceous earth (4.22) instead of anhydrous sodium sulfate (4.22).
Note 1. The sample can also be dewatered by means of a vacuum freeze dryer (5.6), and the frozen sample is thoroughly ground to a size of about 1 mm
Particles.
The detailed steps are performed according to HJ 783.
6.3.2 Extraction
6.3.2.1 extraction method can choose Soxhlet extraction, pressurized fluid extraction and other methods.
Soxhlet extraction. 80.0 μl of the substitute intermediate (4.19) was added to the prepared soil or sediment sample and all samples were carefully
Into the paper sleeve, the paper sleeve placed in the Soxhlet extractor tube, in the round bottom of the solvent bottle by adding 100 ml of acetone - n-hexane mixed
Solvent (4.7), extraction for 16 h ~ 18 h, the reflux rate is controlled at 4 to 6 times per hour. Collect the extract.
The pressurized fluid extraction was performed according to HJ 783.
6.3.2.2 If there is significant moisture in the extract (6.3.2.1), filtration and dehydration are required. Place a layer of glass wool or fiberglass on the glass funnel
4-dimensional membrane (4.27), add about 5 g of anhydrous sodium sulfate (4.22), and extract the extract into a concentrated vessel. And then a small amount of acetone - n-hexane
Mixed solvent (4.7) was washed and extracted three times, the washing solution was filtered into a funnel, and finally a small amount of acetone-n-hexane mixed solvent (4.7)
Rinse the funnel, all collected into the concentrated utensils, to be concentrated.
6.3.3 Concentration
Concentration method is recommended in the following two ways.
6.3.3.1 Nitrogen blowing concentration
It is advisable to open the nitrogen gas to the surface of the solvent with gas flow (avoid gas vortices). With n-hexane (4.2)
Exposed concentrator wall. If you do not need to purify, directly concentrated to about 0.5 ml, add the appropriate amount of internal standard liquid (4.17) to its internal standard concentration
And consistent with the internal standard concentration in the calibration curve and fixed to 1.0 ml with acetone-n-hexane mixed solvent (4.7).
For purification, extract the extract (6.3.2) directly to about 2 ml. When gel permeation chromatography was used, about 5 ml was added
Gel permeation chromatography mobile phase (4.10) solvent conversion, and then concentrated to about 2 ml, to be purified; election silica gel column purification,
Continue to add about 4 ml of cyclohexane (4.6) for solvent conversion, and then concentrated to about 2 ml, to be purified; selected magnesium silicate purification column
, The concentration is reduced to about 2 ml directly in the same step without purification.
6.3.3.2 Rotary Evaporation Concentration
According to the instrument instructions set heating temperature conditions, if not purification, the extract concentrated to about 2 ml, with a disposable dropper will be concentrated
The liquid was transferred to a graduated concentrator and the bottom of the rotary vial was rinsed twice with a small amount of acetone-n-hexane mixed solvent (4.7)
The whole concentrate was concentrated to about 0.5 ml with nitrogen, and an appropriate amount of internal standard solution (4.17) was added to the internal standard concentration and calibration curve
The internal standard concentration was consistent and was fixed to 1.0 ml with acetone-n-hexane mixed solvent (4.7)
For purification, extract the extract (6.3.2) directly to about 2 ml and transfer to the graduated concentrator. Was elected with gel permeation
Through the chromatographic method, continue to add about 5 ml gel permeation chromatography mobile phase (4.10) for solvent conversion, and then concentrated to about 2 ml, to be purified;
When purified by silica gel chromatography, add about 4 ml of cyclohexane (4.6) for solvent conversion and concentrate to about 2 ml to be purified;
When purified with a magnesium silicate purification column, concentrate directly to about 2 ml in the same step without purification.
6.3.4 Desulfurization
After the concentrated extract (6.3.3) has a darker color, desulfurization is required. In the prepared silica gel column or activated solid phase extraction
(6.33.1) or 6.3.5.2), so that the extract (6.3.3) is immersed in the copper powder at the top of the column
Desulfurization.
If the gel permeation chromatography is used (6.3.5.3), the desulfurization step can be omitted.
6.3.5 Purification
This method recommends the use of silica gel chromatography column, magnesium silicate purification column and gel permeation chromatography three kinds of purification methods.
6.3.5.1 silica gel column purification
(1) silica gel column preparation
Fill glass wool (4.27) at the bottom of the glass column (4.24), add about 1.5 cm thick anhydrous sodium sulfate (4.22) and 10
G silica gel adsorbent (4.23), tapping the column wall, so that silica gel adsorbent (4.23) filled evenly. Add about 1.5 at the top of the silica gel adsorbent
Cm thick anhydrous sodium sulfate (4.22). Add appropriate amount of dichloromethane (4.3) leaching, tapping chromatography column wall, out of the bubble, so that silica gel filled,
Keep the filler filled with dichloromethane (4.3), close the piston, soak the packing for at least 10 min, release the dichloromethane (4.3), continue slowly
Into the n-hexane (4.2) 30 ml ~ 60 ml leaching, when the top of the anhydrous sodium sulfate layer just before exposure to air, shut off the piston stand.
5 (2) purification
The elution rate was controlled at 2 ml/min by elution with 40 ml of pentane (4.5). The elution rate was controlled at 2 ml/min.
(4.22) or desulfurized copper powder (4.13) layer before exposure to air, close the column piston and discard the eluent. The concentrated extract (6.3.3)
Go to the silica gel column and rinse the concentrator 3 times with 2 ml of cyclohexane (4.6), all into the column (if desulfurization is required,
Liquid immersion in copper powder for about 5 minutes), open the piston, slowly add 25 ml pentane (4.5) elution, discard this part of the pentane eluent.
The mixture was eluted with 25 ml of methylene chloride-pentane mixed solvent (4.8) and the eluate was collected until further concentration (6.3.6).
6.3.5.2 Magnesium silicate purification column
The magnesium silicate purification column (4.25) was fixed on a solid phase extraction device (5.7) and washed with 4 ml of dichloromethane (4.3)
Column, add 5 ml of n-hexane (4.2) to be closed after the column closed flow control valve infiltration 5 min, slowly open the control valve, continue to join 5 ml
N-hexane (4.2), before the filler is exposed to air, close the control valve and discard the effluent. The concentrated extract (6.3.3) was transferred
To the column, with 2 ml of n-hexane (4.2) three times the concentration of washing utensils, lotion all into the column (if desulfurization, this solution should be dissolved
Liquid immersion in copper powder for about 5 minutes). Slowly open the control valve and close the control valve before the filler or copper powder is exposed to air, add 5 ml
Dichloromethane-n-hexane mixed solvent (4.9), slowly open the control valve to be eluted to clean the column after the closure of the control valve,
Run slowly for 2 min, slowly open the control valve, continue to add 5 ml of methylene chloride - n-hexane mixed solvent (4.9), and collect all the eluent
Concentrated again (6.3.6).
6.3.5.3 Gel permeation chromatography purification
(1) Gel permeation column calibration
The gel permeation chromatography (GPC) column was calibrated according to the instrument manual. The chromatographic peaks of the GPC calibration solution (4.21) should be met
The following conditions. all peak shape symmetry; corn oil and phthalic acid bis (2-diethylhexyl) ester between the chromatographic peaks greater than the resolution
85%; the resolution between the bis (2-diethylhexyl) phthalate and the droplets of methaneth drip is greater than 85%; methotrexate and
The resolution between perylene peaks is greater than 85%; the peaks of perylene and sulfur can not be saturated and the baseline separation is greater than 90%.
Polycyclic aromatic hydrocarbon collection time is limited to the corn oil out of the peak to the sulfur before the peak, the perylene peak appears, immediately stop collecting.
(2) purification
Prepare a standard solution for the concentration of polycyclic aromatic hydrocarbons at the midpoint of the calibration curve. According to the collection time determined at the time of calibration,
All the quasi-solution through the purification column, according to the polycyclic aromatic hydrocarbon mixed standard solution peak time, once again adjust the collection time. In accordance with the adjusted income
The concentration of the intermediate point of the mixed standard solution was again passed through the column to determine the recovery rate. When the target (except acenaphthene)
Yield is greater than 90%, you can purify the sample according to this condition, otherwise you need to continue to adjust.
The concentrated extract (6.3.3) was added to the volume required for the GPC dosing ring with GPC mobile phase (4.10).
After the purification conditions of automatic purification, the collection of effluent, to be re-concentrated (6.3.6).
6.3.6 Concentration, plus internal standard
The purified test solution (6.3.5) was concentrated again by the step of nitrogen blowing or rotary evaporation (6.3.3) again,
Standard intermediate (4.17), and set to 1.0 ml, mix and transfer to 2 ml vials, to be tested.
6.4 Preparation of blank samples
A blank sample was prepared by the same procedure as the preparation (6.3) of the sample using quartz sand (4.26) instead of the actual sample.
7 Analysis steps
7.1 Instrument reference conditions
67.1.1 Gas Chromatographic Reference Conditions
Inlet temperature. 280 ° C, splitless, or split injection (sample concentration is high or instrument sensitivity is sufficient);
Injection volume. 1.0 μl, column flow. 1.0 ml/min (constant current);
Column temperature. 80 ℃ for 2 min; at 20 ℃/min rate rose to 180 ℃, keep 5 min; then 10 ℃/min rate rose to 290 ℃,
Keep for 5 min.
7.1.2 Mass Spectral Reference Conditions
Electron bombardment source (EI);
Ion source temperature. 230 ° C;
Ionization energy. 70 eV;
Interface temperature. 280 ℃;
Four pole temperature. 150 ℃;
Quality scanning range. 45 amu ~ 450 amu;
Solvent delay time. 5 min;
Scan mode. full scan Scan or select ion mode (SIM) mode.
7.2 Calibration
7.2.1 Mass Spectrometric Examination
Prior to each analysis, mass spectrometry should be automatically tuned and the gas chromatograph and mass spectrometer set to the instrument conditions required for the analytical method and
In the standby state, through the gas chromatography inlet directly into the 1.0 μl decafluorotriphenylphosphine (DFTPP) (4.20), the operating method,
To the deuterated triphenylphosphine spectrum, the ion abundance of the mass debris should all meet the requirements in Table 1. Otherwise the mass spectrometer ion source should be cleaned.
Table 1 Evaluation of the critical ions and ion abundan...
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 805-2016_English be delivered?Answer: Upon your order, we will start to translate HJ 805-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 805-2016_English with my colleagues?Answer: Yes. The purchased PDF of HJ 805-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|