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HJ 646-2013

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HJ 646-2013English579 Add to Cart Days<=4 Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons with gas chromatography/mass spectrometry Valid HJ 646-2013
HJ 646-2013Chinese19 Add to Cart <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]

   
Detail Information of HJ 646-2013; HJ646-2013
Description (Translated English): Ambient air and stationary source emissions. Determination of gas and particle-phase polycyclic aromatic hydrocarbons with gas chromatography/mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z11
Classification of International Standard: 13.040.20
Word Count Estimation: 22,230
Quoted Standard: GB/T 16157; HJ/T 48; HJ/T 55; HJ/T 93; HJ/T 365
Drafting Organization: Shenyang Municipal Environmental Monitoring Center Station
Administrative Organization: Ministry of Environment Protection
Regulation (derived from): Department of Environmental Protection Notice No. 33 of 2013
Summary: This standard specifies: Determination of ambient air and exhaust sixteen kinds of polycyclic aromatic hydrocarbons gas chromatography mass spectrometry. This standard applies to: the ambient air, stationary source emission and fugitive emissions from air


HJ 646-2013
Ambient air and stationary source emissions.Determination of gas and particle-phase polycyclic aromatic hydrocarbons with gas chromatography/mass spectrometry
Ambient air and exhaust gas in gaseous and particulate matter
Determination of polycyclic aromatic hydrocarbons - gas chromatography - mass spectrometry
Ambient air and stationary source emissions - Determination of gas and
Particle-phase polycyclic aromatic hydrocarbons with gas
Chromatography/mass spectrometry
Published on.2013-06-03
2013-09-01 Implementation
Ministry of Environmental Protection released
National Environmental Protection Standard of the People's Republic
Content
Foreword..II
1 Scope.1
2 Normative references.1
3 Terms and Definitions..1
4 principle of the method. 2
5 interference and elimination..2
6 reagents and materials..2
7 instruments and equipment..5
8 samples.8
9 Analysis step 10
10 Results calculation and representation..12
11 Precision and Accuracy..13
12 Quality Control and Quality Assurance.13
13 Waste treatment 15
Detection limits, lower determination limits, and DFTPP key ions and their abundance evaluations in Appendix A (Normative)
Appendix B (informative) target compound, internal standard, substitute qualitative and quantitative ions..18
Precision and accuracy of Appendix C (informative) methods 19
Appendix D (informative) Polycyclic Aromatic Hydrocarbon Physical Constants.21
Foreword
To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Atmospheric Pollution
This standard is formulated to ensure human health and to regulate the determination of polycyclic aromatic hydrocarbons in ambient air and exhaust gases.
This standard specifies gas chromatography-mass spectrometry for the determination of sixteen polycyclic aromatic hydrocarbons in ambient air and exhaust gases.
This standard is the first release.
Appendix A of this standard is a normative appendix, and Appendix B, Appendix C and Appendix D are informative appendices.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard was drafted. Shenyang Environmental Monitoring Center Station, Environmental Standards Institute of the Ministry of Environmental Protection.
This standard is verified by. Jiangsu Environmental Monitoring Center, Liaoning Provincial Environmental Monitoring Experimental Center, and Dalian Environmental Monitoring
Heart, Anshan Environmental Monitoring Center Station and Liaoning Provincial Academy of Environmental Sciences.
This standard was approved by the Ministry of Environmental Protection on June 3,.2013.
This standard has been implemented since September 1,.2013.
This standard is explained by the Ministry of Environmental Protection.
Determination of polycyclic aromatic hydrocarbons in gaseous and particulate gases from ambient air and exhaust gases
Gas chromatography-mass spectrometry
Warning. The solvents and reagents used in this method are both toxic and potentially hazardous to health and should be avoided as much as possible.
Direct contact with some chemicals. The sample preparation process should be carried out in a fume hood, and the reagents used and the analyzed samples should be recovered and carried out.
Safe handling.
1 Scope of application
This standard specifies gas chromatography-mass spectrometry for the determination of sixteen polycyclic aromatic hydrocarbons in ambient air and exhaust gases.
This standard applies to sixteen polycyclic aromatic hydrocarbons in gas phase and particulate matter in ambient air, fixed source exhaust and unorganized exhaust air.
Determination of (PAHs). Sixteen polycyclic aromatic hydrocarbons include naphthalene, terpenes, anthracene, anthracene, phenanthrene, anthracene, fluoranthene, anthracene, benzo(a)pyrene, benzene
And (b) fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, anthracene (1,2,3-c,d)芘, dibenzo(a,h)蒽, benzo ( g,h,i)苝. If verified
This standard also applies to the determination of other polycyclic aromatic hydrocarbons.
When ambient air is collected at 100L/min for 24h, it is measured by full scan method. The detection limit of the method is 0.0004~
0.0009μg/m3, the lower limit of determination is 0.0016~0.0036μg/m3; when the ambient air is collected at 225L/min for 24h, the full scan method is adopted.
Determination, the detection limit of the method is 0.0002 ~ 0.0004μg/m3, the lower limit of determination is 0.0008 ~ 0.0016μg/m3; when collecting fixed source exhaust
At 1 m3, the detection limit was 0.05-0.12 μg/m3 and the lower limit of determination was 0.20-0.48 μg/m3. See details
Schedule A.
2 Normative references
The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this standard.
GB/T 16157 Determination of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants
HJ/T 48 soot sampler technical conditions
HJ/T 55 Technical Guidelines for the Monitoring of Unorganized Emissions of Air Pollutants
HJ/T 93 PM10 sampler technical requirements and testing methods
HJ/T 365 Hazardous Waste Incineration (including Medical Waste) Disposal Facilities Dioxin Emission Monitoring Technical Specifications
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1 Full program blank whole program blank
The sealed storage cylinder and the glass fiber filter/cylinder are brought to the sampling site, and are exposed to the sampling site without sampling.
After sampling, the sample is shipped back to the laboratory, processed and measured in the same operating steps as the sample, for inspection from sample collection to analysis.
Whether the whole process is polluted.
3.2 Shipping Blank Trip Blank
The sealed sample cylinder and the glass fiber filter/cylinder are brought to the sampling site, and the sample is not opened during sampling, and the sample is returned to the experiment after sampling.
The chamber is processed and measured in the same operating steps as the sample to check whether the sample transport process is contaminated.
3.3 Internal standards
Compounds not contained in the sample are added to known amounts prior to sample analysis for quantitative analysis of the target compound.
3.4 surrogate standards
A substance that is not contained in the sample but has similar physicochemical properties to the target compound to be tested. Usually added before sample extraction or sampling
In, the recovery rate can be used to evaluate the effect of the sample preparation or sampling process on the analytical results.
3.5 sampling efficiency sampling efficiency
Refers to the ability of the sampler to capture and retain polycyclic aromatic hydrocarbons. Add a certain amount of polycyclic aromatic hydrocarbons to the sampling filter, the same as the sample
The operating conditions are pumped air to determine the retention capacity of the sample medium for polycyclic aromatic hydrocarbons.
3.6 dynamic sampling efficiency
Add a certain amount of polycyclic aromatic hydrocarbons to the surface of the sampling adsorption column, pump air according to the same operating conditions as the sample, and determine the number of sampling media.
Retention capacity of cyclic aromatic hydrocarbons.
4 Principle of the method
Polycyclic aromatic hydrocarbons in gas phase and particulate matter are collected in sampling cylinders and glass (or quartz) fiber membranes/tubes, sampling cylinders and membranes.
10/90 (v/v) diethyl ether/n-hexane mixed solvent extraction, and the extract is purified by concentration, silica gel column or Florisil column.
Gas chromatography-mass spectrometry (GC/MS) detection was performed and characterized by retention time, mass spectrum or characteristic ions, and quantified by internal standard method.
5 interference and elimination
5.1 Heterocyclic polycyclic aromatic hydrocarbons and alkyl-substituted polycyclic aromatic hydrocarbons may pass through mass spectrometry when they peak at the same retention time as the test compound.
Detecting auxiliary qualitative ions to distinguish them;
5.2 During the process of sample collection, storage and treatment, heat, ozone, nitrogen oxides and ultraviolet light will cause degradation of polycyclic aromatic hydrocarbons.
Sealed, low temperature, protected from light.
6 reagents and materials
Unless otherwise stated, analytically pure reagents and distilled water in accordance with national standards were used for the analysis.
6.1 Dichloromethane (CH2Cl2). chromatographically pure.
6.2 n-Hexane (C6H14). Chromatographically pure.
6.3 Ether (C2H6O). Chromatographically pure.
6.4 Acetone (C3H6O). chromatographically pure.
6.5 anhydrous sodium sulfate (Na2SO4)
Bake at 450 ° C for 2 h in a muffle furnace before use, cool, and store in a ground glass bottle.
6.6 Decafluorotriphenylphosphine (DFPTT). 5mg/L (dichloromethane solvent), can be purchased directly from commercially available certified standard solutions, or with high concentration standards
Quasi-solution preparation.
6.7 Alternatives
6.7.1 Alternative 1
2-fluorobiphenyl and p-terphenyl-d14 (P-Terphenyl-d14), purity. 99% or more. Can also use it
He is an analog or deuterated polycyclic aromatic hydrocarbon. Commercially available certified standard solutions can be purchased directly.
6.7.1.1 Substitute 1 Stock solution. ρ =.2000 μg/ml.
Weigh about 0.1g of difluorobiphenyl and p-terphenyl-d14 (6.7.1), accurate to 0.1mg, in a 50ml volumetric flask, with a small amount
After dissolving in dichloromethane, dilute to the mark with n-hexane.
6.7.1.2 Alternative 1 Use solution. ρ = 40 μg/ml.
Take 0.50 ml of the replacement 1 stock solution (6.7.1.1) in a 25 ml volumetric flask and dilute to the mark with n-hexane.
6.7.2 Alternative 2
Fluoranthene-D10, benzo(a)pyrene-D12, purity. 99% or more. Other deuterated polycyclic aromatic hydrocarbons can also be used. Can be purchased directly for sale
Certified standard solution.
6.7.2.1 Substitute 2 Stock solution. ρ =.2000 μg/ml.
Weigh fluoranthene-D10, benzo(a)pyrene-D12 (6.7.2), about 0.1g, accurate to 0.1mg, in a 50ml volumetric flask, use less
After the amount of dichloromethane was dissolved, it was diluted to the mark with n-hexane.
6.7.2.2 Substitute 2 Use solution. ρ = 40 μg/ml.
Take 0.50 ml of the replacement 2 stock solution (6.7.2.1) in a 25 ml volumetric flask and dilute to the mark with n-hexane.
6.8 internal standard solution
6.8.1 Internal standard stock solution. ρ=2000μg/ml.
Directly purchase commercially available certified standard solutions containing naphthalene-d8, 苊-d10, phenanthrene-d10, -d12, and 苝-d12.
6.8.2 Internal standard use solution. ρ=400μg/ml.
The analytical internal standard stock solution (6.8.1) was diluted with n-hexane to 400 mg/L for use.
6.9 standard solution
6.9.1 Standard stock solution of polycyclic aromatic hydrocarbons. ρ=2000μg/ml.
Direct purchase of commercially available certified standard solutions, including naphthalene, terpenes, anthracene, anthracene, phenanthrene, anthracene, fluoranthene, anthracene, benzo (a) pyrene,
Benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene,dibenzo(a,h)pyrene, benzo(ghi)苝,茚(1,2,3-cd )
芘, below 4 ° C, sealed, protected from light, or refer to the manufacturer's recommended storage conditions.
6.9.2 Polycyclic aromatic hydrocarbon standard intermediate solution, ρ=200mg/L.
Transfer the polycyclic aromatic hydrocarbon standard stock solution (6.9.1) and the substitute 1 stock solution (6.7.1.1) 1.00ml to a 10ml volumetric flask.
Dilute to the mark with n-hexane and mix.
6.9.3 Polycyclic aromatic hydrocarbon standard use solution, ρ=20mg/L.
Take 1.00 ml of polycyclic aromatic hydrocarbon standard intermediate solution (6.9.2), dilute with n-hexane into a 10 ml volumetric flask, and mix.
Note 1. All the solutions (6.7, 6.8, 6.9) are transferred to the screw glass bottle with the Teflon gasket on the top cover, sealed and protected from light, and cooled below 4 °C.
Tibetan.
Note 2. If necessary, substitute 2 should be included.
6.10 Sample extract. 1 9 (V/V) diethyl ether/n-hexane mixed solution.
6.11 Eluent
6.11.1 Eluent 1. 2 3 (V/V) dichloromethane/n-hexane mixed solution.
6.11.2 Eluent 2. 1 1 (V/V) dichloromethane/n-hexane mixed solution.
6.12 Column chromatography silica gel. reagent grade, 100-200 mesh, pore size 30 Ao or 60 Ao. Before use, it is baked and activated in a shallow dish at 130 °C.
16h, take it out and put it in a desiccator for cooling, then put it into a glass bottle for use. If necessary, dilute with dichloromethane before activation.
6.13 Silica solid phase column or fluroric silica solid phase column. 1000mg/6ml, can also choose suitable capacity of commercial silica gel according to impurity content
Or a Florisil solid phase column.
6.14 Ultra-fine glass fiber filter or quartz fiber filter
Select the filter of the corresponding specification according to the sampling flow rate. The retention efficiency of the filter on 0.3μm standard particles is not less than 99% at the gas flow rate.
When the degree is 0.45m/s, the resistance of a single filter is not more than 3.5 KPa. At this air flow rate, the air purified by the high-efficiency filter is extracted for 5 hours.
The weight loss per square centimeter is not more than 0.012 mg. Heat in a Mafu furnace at 400 ° C for more than 5 h before use, cool, wrapped in aluminum foil,
Stored in the filter cartridge to ensure that the filter is not stained before and after sampling, and is flat and unfolded before sampling.
6.15 Glass fiber filter cartridge (quartz filter cartridge)
The cut-off efficiency of 0.5μm standard particles is not less than 99.9%, and it is heated at 600 ° C for 6 hours or more in a muffle furnace before use, and is cooled.
Sealed to ensure that the filter cartridge is free of creases. If necessary, the mixture was refluxed with acetone and dichloromethane, and the solvent was evaporated and sealed for use.
6.16 XAD-2 resin (styrene-divinylbenzene polymer).
After refluxing for 16 hours with dichloromethane (6.1) before use, the dichloromethane was replaced and reflux extraction was continued for 16 hours.
/N-hexane extract (6.10) is refluxed for 16 hours, then placed in a fume hood to dry the solvent (can also be dried at 50 ° C vacuum)
Dry 8h). Store in a clean wide-mouth glass bottle and store in a sealed container.
6.17 Polyurethane Foam (PUF)
Polyether type, density 22 ~ 25 mg/cm3, cutting length 10mm ~ 20mm cylindrical (diameter according to the glass sampling tube gauge
Grid OK). Wash with distilled water before the first use, drain the water, wash it three times with acetone (6.4), put it into the Soxhlet extractor, and then
It was extracted with acetone (6.4) for 16 h, and extracted with diethyl ether/n-hexane (6.10) for 16 h, and replaced with diethyl ether/n-hexane for 2 to 3 times.
The liquid was taken (6.10) and refluxed for 16 h each time. Then take out, dry the solvent or blow dry with nitrogen (can also be dried at 50 ° C vacuum)
Dry 8h). Wrap it in aluminum foil and store in a suitable container. If necessary, the PUF is returned to its original form with acetone and the solvent is evaporated.
Commercially available pretreated PUFs can also be purchased.
It can also be extracted by other methods such as rapid solvent extraction (ASE) and automatic Soxhlet extraction.
Note 3. After purification, the amount of PUF, XAD-2 resin and filter/tube blank is less than 50ng for naphthalene and phenanthrene, and other polycyclic aromatic hydrocarbons are less than 10ng.
6.18 Nitrogen. purity ≥ 99.999%.
6.19 Glass wool
Dip with dichloromethane before use, and then store the solvent after removing the solvent.
7 Instruments and equipment
7.1 Gas Chromatography Mass Spectrometry. Gas chromatography with split/splitless inlet with temperature programming; mass spectrometer with electron bombardment
Hit the source.
7.1.1 Column. quartz capillary column, 30m (length) × 0.25mm (inside diameter) × 0.25μm (film thickness), the stationary phase is 5% phenyl
Methyl polysiloxane, or other equivalent column.
7.1.2 Graphite pad. Contains 60% polyimide and 40% graphite to avoid adsorption of PAHs during the analysis.
7.1.3 Helium. purity ≥99.999%
7.2 Ambient air sampling equipment
The sampling device consists of a sampling head, a sampling pump and a flow meter.
7.2.1 Sampling pump. It has automatic accumulative flow, automatic timing, and power-off re-start function. Large flow sampler load under normal sampling conditions
It can reach more than 225L/min, and the medium flow sampler load can reach more than 100L/min. Ability to pump ambient air to the glass
The fiber filter (6.14) and the adsorbent material in the adsorption sleeve behind it can collect at least 144m3 during continuous 24h.
Air sample.
7.2.2 Sampling head
The sampling head consists of a filter cartridge and a sorbent sleeve, as shown in Figure 1. The sampling head is equipped with different cutters to collect TSP,
PM10 or PM2.5 particulate matter.
The filter cartridge consists of a filter holder, a filter, and a stainless steel screen. The filter holder is made of a metal material and can pass through
A stainless steel mesh support frame holds the glass fiber/quartz filter.
The outer sleeve of the sorbent sleeve is made of PTFE or stainless steel, and the inside is equipped with a glass sampling cylinder. The bottom of the glass sampling cylinder is made of glass.
Supported by glass screen or stainless steel screen, the upper and lower layers of the glass sampling cylinder are PUF (6.17) with a thickness of at least 1cm, and the height is in the middle.
It is about 5cm of XAD-2 macroporous resin (6.16). The glass sampling cylinder is sealed between the filter holder and the suction pump. Adsorption during sampling
The air inlet of the sleeve is connected with the filter holder, and the air outlet is connected with the end of the air pump. After sampling, the glass sampling cylinder can also be placed directly into Soxhlet
Extracted from the extractor. Before and after sampling, the sampling cylinder is wrapped in aluminum foil and placed in a storage box to ensure the glass sampling cylinder and its inside.
The adsorbent is not contaminated before and after sampling.
Figure 1 Schematic diagram of the sampling head
7.2.3 Flowmeter
The flow rate can be set to not less than 100 L/min, and the sampling flow rate is calibrated with a standard flow meter before sampling.
7.3 Fixed source exhaust sampling equipment
When collecting polycyclic aromatic hydrocarbons in gas phase and particulates at the same time, the instrument recommended in HJ/T 365 can be selected, which consists of sampling tube and filtration.
The cylinder (or membrane), gas phase adsorption unit, condensing unit, flow metering and control device are shown in Figure 2.
HJ/T 48-compliant soot samplers can be used when collecting only polycyclic aromatic hydrocarbons in fixed source exhaust particulates.
Figure 2 Schematic diagram of the exhaust gas sampling device
1-flue; 2-thermocouple or thermal resistance thermometer; 3-piddle; 4-sampling tube; 5-filter cartridge (or membrane); 6-gas phase adsorption with condensing unit
Unit; 7-micro pressure sensor; 8-pressure sensor; 9-temperature sensor; 10-flow sensor; 11-flow regulator; 12-sampling pump;
Microprocessing system; 14-micro printer or interface; 15-display
7.3.1 Cartridge (or filter) bracket. The filter cartridge (or filter) bracket is made of borosilicate glass or quartz glass and is sized to be used with the filter cartridge (or
The filter membranes should be matched to facilitate the pick-and-place of the filter cartridge (or filter membrane) and the interface is well sealed.
7.3.2 Vapor adsorption unit with condensing unit. The condensing unit is used to separate and store the condensed water in the exhaust gas and store the condensed water capacity.
The volume of the device should be no less than 1L. The gas phase adsorption unit is an adsorption column, and the adsorption column generally has an inner diameter of 30 mm to 50 mm and a length of 70 mm.
200mm, can be loaded with 20g ~ 40g XAD-2 and PUF.
7.3.3 Flow metering and control device. A device for indicating and controlling the sampling flow. It can monitor dynamic pressure, static pressure, pre-meter temperature,
Pre-meter pressure, flow and other parameters. The flow meter should have an accumulative flow meter that automatically performs temperature and pressure correction. The sample flow rate is before sampling.
Calibration should be done using a standard flow meter.
7.3.4 Sampling pump. The pump's no-load suction flow rate should be no less than 6L/min. When the sampling system load resistance is 20kPa, the flow rate should not be low.
At 30L/min.
7.4 Soxhlet extractor. 500 ml, 1000 ml,.2000 ml. Other equivalent extraction devices can also be used.
7.5 Constant temperature water bath. The temperature accuracy is controlled at ±5 °C.
7.6 Rotary evaporation device, equivalent equipment such as KD concentrator and organic sample concentrator can also be used.
7.7 Solid phase extraction purification device.
7.8 Glass column. glass column with a length of 350mm and an inner diameter of 20mm and a PTFE piston at the bottom.
7.9 Microinjectors. 10 μl, 50 μl, 100 μl, 250 μl.
7.10 Airtight syringe. 500μl, 1000μl.
7.11 Volumetric flask. Class A, 5ml, 10ml, 25ml, 50ml.
7.12 Other instruments and equipment commonly used in laboratories.
8 samples
8.1 Sample Collection
Polycyclic aromatic hydrocarbons above the five rings are mainly found in particulate matter, which can be collected by glass fiber (quartz) membrane/filter; two-ring and three-ring
Cycloaromatic hydrocarbons are mainly present in the gas phase and can pass through glass fiber (quartz) membranes/filter cartridges. XAD-2 resin and polyurethane foam (PUF) are available.
Collection; tetracyclic polycyclic aromatic hydrocarbons exist at the same time, and must be simultaneously treated with glass fiber (quartz) membrane/cylinder, resin and polyurethane foam.
Set samples.
8.1.1 Collection of ambient air and unorganized exhaust gas samples
Before the sampling on site, the flow rate of the sampler should be corrected. Install the filter clamp and the adsorbent sleeve in turn, and connect to the sampler.
Sampling the flow and starting sampling. After sampling, open the filter clip on the sampling head, gently remove the filter with tweezers, and sample the face.
Fold, take the sampling cylinder from the sorbent sleeve, wrap it with the folded-fold filter with aluminum foil, and put it in the original box to seal. After sampling
Perform flow correction.
8.1.2 Sample collection of fixed source exhaust
Install the filter cartridge (6.15) and the vapor phase adsorption unit (7.3.2) with the condensing device, connect the instrument, and the sampling tube is made up of the sampling hole.
Insert the flue, place the sampling nozzle on the measuring point, face the airflow, start the sampling pump, adjust the suction speed of the sampling nozzle and the airflow velocity at the measuring point.
Equal (the relative error is controlled within 10%), make the necessary adjustment for the constant velocity sampling flow every 60 minutes, if the filter resistance increases to none
The method maintains constant-speed sampling, and the sampling is continued after replacing the new filter cartridge. After reaching the required sample volume, quickly withdraw the sampling tube and stop sampling at the same time.
Pump, record parameters such as start and end time or sample volume.
When collecting only the particulate matter of the fixed source exhaust, the method for measuring the particulate matter in the exhaust gas of the fixed pollution source and the sampling method of the gaseous pollutant
(GB/T 16157) for sampling.
8.2 Preservation of samples
After sample collection, it should be stored in the dark at 4 °C or less, and extracted within 7 days; or stored below -15 °C, and extracted within 30 days.
8.3 Preparation of samples
8.3.1 Sample extraction
Place the filter or filter cartridge and glass sampling tube directly in the Soxhlet extractor (if the resin and PUF in the glass sampling cylinder are transferred to the cable)
In the extractor, rinse the glass sampling cylinder with a certain amount of ether/n-hexane extract (6.10), and transfer the rinse solution to the extractor).
Add 100 μl of substitute 1 to the solution (6.7.1.2), add appropriate amount of ether/n-hexane extract (6.10), and reflux a lot per hour.
Extracted at 4 times speed for 16h. After the reflux extraction is completed, cool to room temperature, remove the bottom bottle, clean the extractor and the interface, and wash the cleaning solution.
Transfer to the bottom bottle, add a little anhydrous sodium sulfate (6.5) to the sodium sulfate particles can flow freely, and let stand for 30min. Fixed source row
The condensed water of the gas was transferred to a separatory funnel, and the condensed water collection bottle was rinsed with n-hexane, and transferred to a separatory funnel, and n-hexane was added thereto.
The extract is combined with the extract in the above bottom bottle.
Note 4. Other sample extraction methods may be used as long as the quality control requirements specified in this standard can be met. Automatic Soxhlet extraction using the above extract (6.10)
Extraction of 40 cycles; rapid solvent extraction reference conditions. temperature 100 ° C, pressure 1500 ~.2000 Psi, static extraction time 5 min, rinse volume 60% cell body
The product was purged with nitrogen for 60 s and the number of static extractions was 2 times.
8.3.2 Sample concentration
The extract is transferred to a concentration bottle, the temperature is controlled to be below 45 ° C and concentrated to below 5.0 ml, 5-10 ml of n-hexane is added, and the concentration is continued.
The solvent was completely converted to n-hexane and concentrated to less than 1.0 ml. If no purification is required, add 10.0μl internal standard and dilute to 1.0ml.
Move to the vial for analysis. The prepared samples were stored under refrigeration at 4 ° C and analyzed within 30 days.
8.3.3 Purification of samples
8.3.3.1 Silica gel column purification
The glass chromatography column (7.8) was sequentially filled with glass wool (6.18), and 10 g of activated silica gel (6.12) was wet-filled with methylene chloride as a solvent.
Finally, fill 1~2cm high anhydrous sodium sulfate. After the column is installed, rinse the column twice with 20-40 ml of dichloromethane to ensure that the liquid level remains in sulfur.
Above the surface of sodium, do not drain, rinse the column with 40ml of n-hexane, and close the piston. Transfer the sample extract into the column and use
Wash the extract bottle with 1~2ml of n-hexane and transfer it to the column. The effluent is discarded. Elute the column with 25 ml of n-hexane and discard the stream
Drain. The column was eluted with 30 ml of dichloromethane/n-hexane eluent 1 (6.11.1), and the effluent was received at a flow rate of 2-5 ml/min.
Shrink the bottle. The effluent was concentrated, the solvent was changed to n-hexane, concentrated to below 1.0 ml, and 10.0 μl of internal standard (6.8.2) was added, and the volume was adjusted to 1.0 ml.
Transfer to the vial for analysis. The prepared samples were stored under refrigeration at 4 ° C and analyzed within 30 days.
8.3.3.2 Purification of silica gel or Florisil solid phase extraction column
Take 1 g of silica gel or Florisil solid phase extraction column (6.13) and fix it on the solid phase extraction purification unit (7.7). Use sequentially
Rinse the column bed with 4 ml of dichloromethane and 10 ml of n-hexane. After the column is filled with n-hexane, close the flow control valve and infiltrate for 5 min to open the control valve.
Discard the effluent. Close the control valve before the solvent has dried. Transfer all the concentrated sample extraction solution to the column, open the control
Valve, wash the sample concentrate bottle twice with about 2-3 ml of n-hexane, transfer the wash to a solid phase column, with 10 ml of dichloromethane /
The hexane eluent 2 (6.11.2) was eluted on the solid phase column, and the effluent was collected in a concentrate bottle. Turn off the flow rate control after the eluent flows through the silica gel column
Valve, infiltrate for 5 min, then open the control valve and continue to receive the effluent until it completely flows out. The effluent was concentrated to less than 1.0 ml and 10.0 μl was added.
Internal standard, constant volume to 1.0 ml, transferred to the vial for analysis. The prepared samples were stored under refrigeration at 4 ° C and analyzed within 30 days.
Note 5. The liquid in the column cannot be drained during the purification process.
Note 6. Other sample purification methods may be used as long as the quality control requirements specified in this standard can be met.
8.4 Full program blank and shipping blank
For each batch of samples collected, at least one shipping blank and full program blank are guaranteed.
9 Analysis steps
9.1 Reference conditions of the instrument
9.1.1 Reference conditions for gas chromatography
Inlet temperature. 250 ° C; injection method. splitless injection, split at time 0.75min, split ratio 60.1. Programming temperature.
10/min70 (2min) 320 (5.5min) ⎯⎯⎯⎯→°C°C °C; carrier gas. helium (7.1.3), flow rate. 1.0ml/min. Injection volume. 1.0μl
9.1.2 Mass Spectrometry Reference Conditions
Ion source. EI source; ion source temperature. 230 ° C; ionization energy. 70 eV; scanning method. full scan or selective ion scan
(SIM). Scanning range. m/z 35-500 amu; solvent delay. 6.0 min; electron multiplying voltage. consistent with tuning voltage; transmission
Line temperature. 280 ° C. The rest of the parameters are set according to the instruction manual of the instrument.
9.1.3 Performance check of the instrument
The GC/MS system must perform an instrument performance check before daily analysis. 1μL DFTPP solution (6.6), GC/MS system
The critical ion abundance of DFTPP obtained should meet the requirements of Schedule A.2, otherwise some parameters of the mass spectrometer should be adjusted or
Clean the ion source.
9.2 Qualitative and quantitative methods for compounds
9.2.1 Qualitative.
Related standard:   HJ 644-2013  HJ 645-2013
   
 
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