|
US$339.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 679-2013: Soil and sediment. Determination of acrolein, acrylonitrile, acetonitrile. Headspace-Gas chromatography method
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 679-2013 | English | 339 |
Add to Cart
|
3 days [Need to translate]
|
Soil and sediment. Determination of acrolein, acrylonitrile, acetonitrile. Headspace-Gas chromatography method
| Valid |
HJ 679-2013
|
PDF similar to HJ 679-2013
Basic data | Standard ID | HJ 679-2013 (HJ679-2013) | | Description (Translated English) | Soil and sediment. Determination of acrolein, acrylonitrile, acetonitrile. Headspace-Gas chromatography method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Classification of International Standard | 13.080 | | Word Count Estimation | 13,153 | | Quoted Standard | GB 17378.3; GB 17378.5; HJ/T 166; HJ 613 | | Regulation (derived from) | Ministry of Environmental Protection Notice No. 70 of 2013 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination in soils and sediments acrolein, acrylonitrile, acetonitrile, a headspace gas chromatography. This standard applies to soils and sediments acrolein, acrylonitrile determination, acetonitrile. When the sample volum | HJ 679-2013: Soil and sediment. Determination of acrolein, acrylonitrile, acetonitrile. Headspace-Gas chromatography 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.
Soil and sediment.Determination of acrolein, acrylonitrile, acetonitrile.Headspace-Gas chromatography method
National Environmental Protection Standard of the People's Republic
Measurement of soil and sediment acrolein, acrylonitrile and acetonitrile
Headspace-gas chromatography
Soil and sediment-Determination of acrolein, acrylonitrile, acetonitrile
Headspace-Gas chromatography method
Released on.2013-11-21
2014-02-01 implementation
Ministry of Environmental Protection released
Content
Foreword. II
Warning 1
1 Scope..1
2 Normative references..1
3 method principle..1
4 Reagents and materials.1
5 instruments and equipment. 2
6 samples. 2
7 Analysis steps..3
8 result calculation and representation..4
9 precision and accuracy..6
10 Quality Assurance and Quality Control 6
11 Waste treatment..7
12 Notes. 7
Precision and Accuracy of Appendix A (Informative) Method 8
Foreword
To implement the Environmental Protection Law of the People's Republic of China, protect the environment, protect human health, and regulate soil and sediment
This standard is formulated for the determination of acrolein, acrylonitrile and acetonitrile.
This standard specifies headspace-gas chromatography for the determination of acrolein, acrylonitrile and acetonitrile in soils and sediments.
This standard is the first release.
Appendix A of this standard is an informative annex.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Ningbo Environmental Monitoring Center.
This standard is verified by. Zhoushan Marine Ecological Environment Monitoring Station, Taizhou Environmental Monitoring Center Station, Hangzhou Environment
Monitoring Center Station, Jiaxing Environmental Protection Monitoring Station, Huzhou Environmental Protection Monitoring Center Station and Jinhua Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on November 21,.2013.
This standard has been implemented since February 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Determination of acrolein, acrylonitrile and acetonitrile in soils and sediments
Headspace-gas chromatography
Warning. The reagents and standard solutions used in the test are volatile and toxic compounds. They should be well ventilated during preparation.
Carry out in the environment; wear protective equipment as required to avoid contact with skin and clothing.
1 Scope of application
This standard specifies headspace-gas chromatography for the determination of acrolein, acrylonitrile and acetonitrile in soils and sediments.
This standard applies to the determination of acrolein, acrylonitrile and acetonitrile in soil and sediment.
When the sampling amount is 2.0g, the detection limit of acrolein is 0.4mg/kg, the lower limit of determination is 1.6mg/kg; the detection of acrylonitrile
The limit is 0.3 mg/kg, the lower limit of determination is 1.2 mg/kg; the detection limit of acetonitrile is 0.3 mg/kg, and the lower limit of determination is 1.2 mg/kg.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate.
Used in this standard.
GB 17378.3 Marine monitoring specification Part 3 Sample collection, storage and transportation
GB 17378.5 Marine monitoring specification Part 5 Sediment analysis
HJ/T 166 Technical Specifications for Soil Environmental Monitoring
HJ 613 Determination of dry matter and moisture in soils - Gravimetric method
3 Principle of the method
The sample sealed in the headspace bottle, under certain temperature conditions, the acrolein, acrylonitrile, acetonitrile contained in the sample volatilize
To the upper space, and achieve thermodynamic dynamic balance in gas-liquid-solid three-phase. Take a certain amount of gas-phase gas injection zone in the headspace bottle
Separation and determination were carried out in a gas chromatograph with a hydrogen flame detector. Characterize by retention time and quantify by external standard method.
4 reagents and materials
4.1 Experimental water
Freshly prepared organic-free deionized or distilled water. A blank test is required before use to confirm that there is no target compound
Or the target compound concentration is below the method detection limit.
4.2 Sodium chloride (NaCl). excellent grade pure. Bake at 400 ° C for 4 h to remove possible interfering substances, cool and store in the grinding
The glass bottle is sealed and stored.
4.3 Methanol (CH3OH). Chromatographic grade. Test before use to confirm that there is no target compound or low concentration of target compound
The method detection limit.
4.4 Phosphoric acid (H3PO4). excellent grade pure.
4.5 Matrix modifier
Measure 500 ml of experimental water (4.1), add a few drops of phosphoric acid (4.4) to adjust pH ≤ 2, and then add 180 g of sodium chloride (4.2).
Dissolve and mix. Sealed and stored below 4 °C in an environment free from organic interference. The shelf life is 6 months.
4.6 Standard solution of acrolein, acrylonitrile and acetonitrile in methanol. ρ=2000mg/L
Prepare with a standard solvent such as acrolein, acrylonitrile or acetonitrile with methanol as solvent, or directly purchase a commercially available certified standard solution.
The standard solution is stored at -18 ° C or less in the dark. The solution was returned to room temperature before use and shaken. Use a dense bottle to protect from light after opening
Save and use within 1 month.
4.7 Quartz sand (SiO2). 20~50 mesh. Test before use to confirm that there is no target compound or low concentration of target compound
The method detection limit.
4.8 Carrier gas. nitrogen, purity ≥99.999%.
4.9 Combustion gas. hydrogen, purity ≥ 99.99%.
4.10 Gas. Air, need to dehydrate and de-organize.
5 Instruments and equipment
5.1 Gas Chromatograph. Capillary split/splitless inlet, programmable temperature, with hydrogen flame ionization detector.
5.2 Capillary column. 30m (length) × 0.53mm (inside diameter) × 1.0μm (film thickness), polyethylene glycol fixative or other
Effective capillary column.
5.3 Headspace Sampler. with headspace bottle, gasket (silicone rubber lined with Teflon) and sealed cap. Headspace bottle, cap
If you need to reuse it, you should first clean it with detergent, then rinse it with tap water and distilled water, and then seal it at 105 °C.
Save for backup.
5.4 Reciprocating Oscillator. The oscillation frequency is 150 times/min, which can fix the headspace bottle.
5.5 Ultrapure water preparation instrument or sub-boiling distiller.
5.6 Balance. The accuracy is 0.01 g.
5.7 Microinjectors. 10μl, 50μl, 100μl.
5.8 Sampler. The soil sampler is made of stainless steel, with an inner diameter of 1cm and a length of 20cm, or it can be used to match the diameter of the sample bottle.
Disposable plastic syringe; the sediment sampler uses a grab or cone type mud collector.
5.9 Portable refrigerator. 20L volume, temperature below 4 °C.
5.10 Brown compact bottle. 2 ml with Teflon liner and solid screw cap.
5.11 Vial. 40 ml brown wide-mouth glass bottle with Teflon-silica liner screw cap (or greater than 40ml other specifications)
Glass bottle).
5.12 Common instruments and equipment used in general laboratories.
6 samples
6.1 Acquisition and preservation
6.1.1 Sample Collection
According to the relevant provisions of HJ/T 166, the collection and preservation of soil samples shall be carried out in accordance with the relevant provisions of GB 17378.3.
Collection and storage of sediment samples. The sample collection tool should be cleaned before use. Portable at the sampling site
The volatile organic matter measuring instrument performs a preliminary screening of the sample at a high concentration. At least 3 parallel samples should be collected for all samples.
The sample should be collected into the sample vial (5.11) as soon as possible and filled up to quickly remove the sampled bottle thread and the adhered sample on the outer surface.
Products, sealed sample bottles. Put it in a portable freezer and bring it back to the lab.
Note 1. Do not stir the soil and sediment during sample collection to avoid the volatilization of organic matter in the soil and sediment. Collected soil or sediment
The sample should be gently placed in the sampling bottle, leaving no space and quickly sealed.
6.1.2 Sample storage
Samples should be analyzed as soon as they are sent to the laboratory. If it cannot be analyzed immediately, the sample should be in an environment below 4 °C without organic interference.
Sealed in the middle. The shelf life of acrolein does not exceed 2d, and the storage period of acetonitrile and acrylonitrile does not exceed 5d.
6.2 Sample preparation
6.2.1 Low content sample
Remove the sample vial and return to room temperature, weigh 2g of sample into the headspace bottle, and quickly add 10ml of matrix modifier (4.5).
Immediately sealed and oscillated on the oscillator at a frequency of 150 times/min for 10 min, to be tested.
6.2.2 High content sample
If the initial screening of volatile organic compounds at the site is high or low, the determination result is greater than 300 mg/kg.
Amount of sample. The high-content sample was prepared as follows. another unopened sample was taken, and after returning to room temperature, 2 g of the sample was weighed and placed on top.
In an empty vial, quickly add 10 ml of methanol (4.3), seal and shake on the shaker for 10 min. After standing to settle, remove 1-2 ml
The methanol extract (if necessary, centrifuge first and remove the supernatant) into a 2 ml brown glass bottle. The extract is protected at 4 ° C in the dark
Storage, acrolein storage period is 2d, if only acetonitrile and acrylonitrile are measured, it can be stored for 7d.
After returning the methanol extract to room temperature before analysis, add 2 g of quartz sand (4.7), 10 ml to the empty headspace vial.
The matrix modifier (4.5) and 10 to.200 μl of the methanol extract were immediately sealed to a frequency of 150 beats/min on the shaker.
Oscillation for 10 min, to be tested.
Note 2. If the concentration of the target compound in the methanol extract is high, it can be appropriately diluted with methanol.
6.3 blank sample preparation
6.3.1 Low content blank sample
Replace the sample with 2g quartz sand (4.7) and prepare a low content blank sample according to the procedure of 6.2.1.
6.3.2 High content blank sample
Replace the sample with 2g quartz sand (4.7) and prepare a high content blank sample according to the procedure in 6.2.2.
6.4 Determination of dry matter content and moisture of samples
The dry matter content of the soil samples was determined according to HJ 613, and the moisture content of the sediment samples was determined according to GB 17378.5.
carried out.
7 Analysis steps
7.1 Instrument Reference Conditions
Different models of headspace sampler and gas chromatograph have different working conditions, and should be operated according to the instrument manual.
For this standard, the recommended reference conditions for the instrument are as follows.
7.1.1 Headspace Reference Conditions
Heating equilibrium temperature. 75 ° C; heating equilibrium time. 30 min; sampling needle temperature. 105 ° C; transmission line temperature. 150 ° C;
Transmission line type. deactivated quartz capillary column with inner diameter of 0.32mm; pressure equalization time. 2min; injection
Time. 0.10 min; needle removal time. 0.2 min; headspace bottle pressure. 8 psi.
7.1.2 Gas Chromatography Reference Conditions
Temperature programmed. 40 ° C (for 5 min) 5 ° C/min 60 ° C 30 ° C/min 150 ° C (for 5 min);
Inlet temperature. 150 ° C; carrier gas. nitrogen, constant current, flow rate of 4.5 ml/min; injection method. split injection, points
Flow ratio 5.1; detector temperature. 250 ° C; hydrogen flow. 40 ml/min; air flow. 450 ml/min; tail gas. 30 ml/min.
7.2 Calibration
7.2.1 Drawing a calibration curve
Add 2 g of quartz sand (4.7), 10 ml of matrix modifier (4.5) and appropriate amount to 6 22 ml headspace bottles.
Quasi-solution (4.6), prepare 5 different concentrations of the standard series, the content of the target compound is shown in Table 1. According to the instrument reference conditions
(7.1), the samples were injected sequentially from low to high concentration, with the peak area or peak height as the ordinate, and the target compound content (μg) as the horizontal
Coordinates, draw a calibration curve. The standard chromatogram of the target compound is shown in Figure 1.
Table 1 Standard series of target compounds in units of content. μg
No. Compound name 1 2 3 4 5
1 Acrolein 2.0 5.0 20.0 40.0 80.0
2 acrylonitrile 2.0 5.0 20.0 40.0 80.0
3 acetonitrile 2.0 5.0 20.0 40.0 80.0
7.2.2 Standard chromatogram
The standard reference chromatogram of the target compound under the chromatographic conditions specified in this standard is shown in Figure 1.
1-acrylaldehyde; 2-acrylonitrile; 3-acetonitrile
Figure 1 Standard reference chromatogram of acrolein, acrylonitrile, acetonitrile
7.3 Determination
The prepared sample (6.2) was placed on the sample tray of the headspace sampler and measured according to the instrument reference conditions (7.1).
7.4 Blank test
Place the prepared blank sample (6.3) on the headspace sampler and measure according to the instrument reference conditions (7.1).
8 Calculation and representation of results
8.1 Calculation of results
8.1.1 Calculation of low soil sample results
The content of the target compound (mg/kg) in the low-content soil sample was calculated according to the formula (1).
Dmwm
×=
1ω (1)
In the formula.
ω -- target compound concentration, mg/kg;
The content of the target compound was found on the m1--calibration curve, μg;
M--sample amount (wet weight), g;
Wdm - dry matter content of the sample, %.
8.1.2 Calculation of high soil sample results
The content of the target compound (mg/kg) in the high-content soil sample was calculated according to the formula (2).
Sdm Vwm
KVm
××
××= c1ω (2)
In the formula.
ω -- target compound concentration, mg/kg;
The content of the target compound was found on the m1--calibration curve, μg;
Vc--the amount of methanol added to the sample, ml;
m -- sample amount (wet weight), g;
Vs--the amount of methanol extract used for headspace determination, ml;
Wdm-the dry matter content of the sample, %;
K - dilution factor of the extract.
8.1.3 Calculation of low-content sediment sample results
The content of the target compound (mg/kg) in the low-content sediment sample was calculated according to the formula (3).
)1(
W−×= m
Mω (3)
In the formula.
ω -- target compound concentration, mg/kg;
The content of the target compound was found on the m1--calibration curve, μg;
M--sample amount (wet weight), g;
W--the moisture content of the sample, %;
8.1.4 Calculation of high-content sediment sample results
The content of the target compound (mg/kg) in the high-content sediment sample was calculated according to the formula (4).
)1(
−××
××=
SVm
KVmω (4)
In the formula.
ω -- target compound concentration, mg/kg;
The content of the target compound was found on the m1--calibration curve, μg;
Vc--the amount of methanol added to the sample, ml;
m -- sample amount (wet weight), g;
Vs--the amount of methanol extract used for headspace determination, ml;
W--the moisture content of the sample, %;
K - dilution factor of the extract.
Note 4. If the soil and sediment sample moisture content is greater than 10%, the extract volume Vc should be the sum of the volume of methanol and water in the sample;
The water content is 10% or less, and the volume Vc of the extract is 10 ml.
8.2 Results representation
8.2.1 When the measurement result is less than 10.0 mg/kg, one digit after the decimal point is retained; when the measurement result is greater than or equal to 10.0 mg/kg,
Leave 3 significant digits.
9 Precision and accuracy
9.1 precision
9.1.1 Soil
Six laboratories tested the uniform samples with spiked amounts of 1.0 mg/kg and 5.0 mg/kg, respectively.
The standard deviation range is. 2.0%~10.3%, 2.4%~9.0%; the relative standard deviation between laboratories is 6.1%~
9.8%, 4.8% to 10.7%; the repeatability limits are. 0.17 mg/kg to 0.18 mg/kg, 0.77 mg/kg to 0.82 mg/kg;
Reproducibility limits range from 0.16 mg/kg to 0.25 mg/kg and from 0.77 mg/kg to 1.20 mg/kg.
9.1.2 Sediment
Six laboratories tested the uniform samples with spiked amounts of 1.0 mg/kg and 5.0 mg/kg, respectively.
The standard deviation range is. 2.9%~10.3%, 2.3%~8.6%; the relative standard deviation between laboratories is. 4.8%~
10.7%, 5.5% to 10.8%; the repeatability limits are. 0.16 mg/kg to 0.18 mg/kg, 0.63 mg/kg to 0.72 mg/kg;
Reproducibility limits range from 0.12 mg/kg to 0.26 mg/kg and from 0.72 mg/kg to 1.30 mg/kg.
9.2 Accuracy
9.2.1 Soil
Six laboratories tested the uniform samples with spiked amounts of 1.0 mg/kg and 5.0 mg/kg, respectively.
The ranges are. 74.5%~115%, 80.0%~113%.
9.2.2 Sediment
Six laboratories tested the uniform samples with spiked amounts of 1.0 mg/kg and 5.0 mg/kg, respectively.
The ranges are. 70.0%~108%, 67.3%~105%.
See Appendix A for the precision and accuracy of the method.
10 Quality Assurance and Quality Control
10.1 Calibration curve
A calibration curve should be drawn before each batch of samples is analyzed. The correlation coefficient of the calibration curve should be ≥0.995. For continuous analysis, every
24h analysis of an intermediate point concentration standard solution, the relative deviation of the measured results from the concentration of the intermediate point of the calibration curve should be ≤ 20%,
The retention time of the target compound should be within the retention time window, otherwise the calibration curve and sample should be redrawn.
10.2 Qualitative
Samples are characterized by retention time. If necessary, use a two-column or temperament online method to characterize.
A retention time window of t ± 3 s should be established prior to sample analysis. t is the flattening time of each concentration standard substance at the initial calibration
Mean, s is the standard deviation of the retention time of each reference material at the initial calibration. Target compound retention time when sample analysis
Should be within the retention time window.
10.3 Blank test
At least one laboratory blank and full program blank should be determined for each batch of samples. The target compound concentration should be lower than the method detection limit.
10.4 Sample determination
Samples that exceed 4 times the upper limit of the calibration curve can be reanalyzed by reducing the sample size. Both results should be reported, minus
The sample concentration after a small sample amount is greater than the concentration at the midpoint of the curve. The minimum sample sample size should not be lower than 0.5g, otherwise it needs to be high.
Concentration method analysis.
10.5 Parallel sample determination
Each batch of samples should be analyzed for 20% of parallel samples. If the sample contains the target compound, the phase of the parallel sample is measured.
The deviation should be within 25%.
10.6 spike recovery rate
At least 10% of the spiked parallel samples were analyzed for each batch of samples, and the relative deviation of the spiked parallel samples should be within 25%.
11 Waste treatment
The toxic wastes generated during the experiment should be stored in a centralized manner and entrusted to qualified units for processing.
12 Precautions
12.1 The sampling tool should be thoroughly washed with methanol and purified water before use, and dried for use. When collecting other samples, note
Replace the sampling tool and the cleaning sampling tool to prevent cross-contamination.
12.2 In the process of preservation and transportation of the sample, to avoid contamination, the sample should be placed in a closed, dark-proof refrigerator (5.9).
Storage.
12.3 The instruments, materials and reagents used in the test shall be analyzed in advance to confirm whether they contain interference with the determination of the target.
substance. Appliances and materials can be cleaned with methanol to remove interfering substances as much as possible.
12.4 After analysis of a high-content sample, the blank sample should be analyzed until the concentration of the target compound in the blank sample is less than the detection limit.
Only subsequent analysis can be performed.
Appendix A
(informative appendix)
Method precision and accuracy
Table A gives the precision and accuracy indicators such as repeatability, reproducibility and spike recovery.
Precision and accuracy of Schedule A methods
Compound
name
content
Level
(mg/kg)
Repeatability limit
(mg/kg)
Reproducibility limit
(mg/kg)
Laboratory room
The relative standard deviation
(%)
Laboratory room
The relative standard deviation
(%)
Scaling recovery final value
(%)
Soil sediments soil sediments soil sediments soil sediments soil sediments
Acrolein
1.0 0.18 0.17 0.28 0.26 4.3~8.5 4.4~8.3 10.7 10.6 90.3±16.6 86.1±19.7
5.0 0.84 0.72 1.34 1.26 3.6~8.9 3.0~8.8 10.0 10.4 93.5±13.1 85.0±20.1
Acrylonitrile
1.0 0.16 0.15 0.19 0.20 2.0~10.0 2.0~10.6 7.4 7.9 93.4±15.0 90.5±11.7
5.0 0.73 0.60 1.15 1.05 2.8~7.4 2.3~6.9 8.5 8.2 95.8±15.4 91.5±15.8
Acetonitrile
1.0 0.18 0.18 0.18 0.12 2.9~8.3 4.3~9.3 6.6 4.7 97.0±7.6 90.5±8.8
5.0 0.76 0.64 0.90 0.79 2.5~8.6 3.2~5.9 6.8 6.1 98.6±11.6 93.2±10.3
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 679-2013_English be delivered?Answer: Upon your order, we will start to translate HJ 679-2013_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 679-2013_English with my colleagues?Answer: Yes. The purchased PDF of HJ 679-2013_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.
|