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HJ 696-2014: Water quality. Determination of turpentine. Gas chromatography method
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Water quality. Determination of turpentine. Gas chromatography method
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HJ 696-2014
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PDF similar to HJ 696-2014
Standard similar to HJ 696-2014 GB 5085.7 HJ 694 GB 5085.1 HJ 697 HJ 686 Basic data | Standard ID | HJ 696-2014 (HJ696-2014) | | Description (Translated English) | Water quality. Determination of turpentine. Gas chromatography method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 10,158 | | Date of Issue | 3/31/2014 | | Date of Implementation | 7/1/2014 | | Quoted Standard | HJ/T 91; HJ/T 164 | | Regulation (derived from) | Ministry of Environmental Protection Notice No. 24 of 2014 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the Determination of turpentine gas chromatography. This Standard applies to surface water, groundwater, industrial wastewater and domestic sewage in the determination of turpentine. When the sample size is 100ml when this standard | HJ 696-2014: Water quality. Determination of turpentine. 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.
Water quality.Determination of turpentine.Gas chromatography method
National Environmental Protection Standard of the People's Republic
Water quality turpentine - Determination of gas chromatography
Published on.2014-03-31
2014-07-01 implementation
release
Ministry of Environmental Protection
Content
Preface II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 reagents and materials 1
5 Instruments and equipment 1
6 sample 2
7 Analysis steps. 2
8 Calculation and representation of results.3
9 precision and accuracy. 4
10 Quality Assurance and Quality Control 4
11 Waste treatment.4
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 Water Pollution Prevention and Control, to protect the environment,
This standard is formulated to ensure human health and standardize the determination method of turpentine in water.
This standard specifies gas chromatography for the determination of turpentine in water.
This standard is the first release.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Taizhou Environmental Monitoring Center Station.
This standard is verified by. Jiangsu Environmental Monitoring Center, Wuxi Environmental Monitoring Center Station, Suzhou Environmental Monitoring Center
Station, Changzhou Environmental Monitoring Center, Zhenjiang Environmental Monitoring Center Station and Taizhou Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on March 31,.2014.
This standard has been implemented since July 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Water quality turpentine - Determination of gas chromatography
Warning. The reagents and standard solutions used in this method are volatile toxic compounds. The preparation process should be in the fume hood.
Carry out; protective equipment should be worn as required to avoid contact with skin and clothing.
1 Scope of application
This standard specifies gas chromatography for the determination of turpentine in water.
This standard applies to the determination of turpentine in surface water, groundwater, industrial wastewater and domestic sewage.
When the sample amount is 100ml, the detection limit of this standard is 0.03mg/L, and the lower limit of determination is 0.12mg/L.
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.
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring
3 Principle of the method
The turpentine in the sample is extracted with dichloromethane, and the extract is dehydrated and dried, and the gas phase is detected by a hydrogen flame ionization detector.
The chromatographic test was performed according to the retention time of α-pinene and β-pinene, the main components in turpentine, and quantified by external standard method.
4 reagents and materials
Analytical purification reagents in accordance with national standards were used for analysis, unless otherwise stated.
Sub-water or distilled water.
4.1 Dichloromethane. pesticide residue level.
4.2 Turpentine standard solution. ρ = 20 mg/ml, the solvent is methanol.
4.3 Standard use of turpentine. accurately transfer a certain amount of turpentine standard solution (4.2) with dichloromethane (4.1)
A standard use solution with a mass concentration of 1000.0 mg/L was released.
4.4 Sodium Chloride (NaCl)
After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.
4.5 anhydrous sodium sulfate (Na2SO4)
After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.
4.6 Nitrogen. purity ≥ 99.999%.
4.7 Hydrogen. purity ≥ 99.95%.
4.8 Gas. Compressed air.
5 Instruments and equipment
5.1 Gas Chromatograph. Hydrogen flame ionization detector.
5.2 Column 1. quartz capillary column, 30m × 0.25mm, coated with 5% phenylmethylpolysiloxane, film thickness 0.25μm,
Or other equivalent capillary column.
5.3 Column 2. quartz capillary column, 30m × 0.25mm, internally coated with 35% phenylmethylpolysiloxane, film thickness 0.25μm,
Or other equivalent capillary column.
5.4 Oscillator.
5.5 separatory funnel. 250 ml.
5.6 Microinjectors. 10μl, 100μl, 250μl.
5.7 Drying column. glass column with a length of 250mm and an inner diameter of 20mm, and the glass piston is not coated with lubricating oil. At the lower end of the column, put less
A glass wool or glass fiber filter paper was added, and 10 g of anhydrous sodium sulfate (4.5) was added.
5.8 Box type electric furnace.
5.9 Common instruments and equipment used in general laboratories.
6 samples
6.1 Sample collection and preservation
Samples were taken with reference to the relevant regulations of HJ/T 91 and HJ/T 164.
Samples were taken using a 250 ml hard-ground glass bottle or a brown threaded glass bottle with a Teflon septum. At 4 ° C
Store underneath, extract within 48h, and extract for 7d.
6.2 Preparation of samples
Take 100.0 ml of the sample into a 250 ml separatory funnel, add 2.5 g of sodium chloride (4.4), dissolve and add 10.0 ml.
Dichloromethane (4.1), shaken and vented, placed on a shaker and shaken vigorously for 5 min, allowed to stand for 10 min, layered, and collected dichloro
The methane extract is dehydrated using a dry column or other type of drying equipment and 1.0 ml is to be tested.
Note. For samples with complex composition, if the emulsification phenomenon is serious during the extraction process, mechanical separation should be used to complete the two-phase separation, including
It can be broken by agitating, centrifuging, filtering with glass wool, etc., or it can be broken by freezing.
6.3 Preparation of blank samples
A 100.0 ml portion of distilled water was weighed instead of the sample, and a blank sample was prepared in accordance with the same procedure as in the preparation of the sample (6.2).
7 Analysis steps
7.1 Recommended chromatographic conditions
Inlet temperature. 180 ° C; splitless injection; column flow rate. 1.0 ml/min; oven temperature.
10/ min 30/ min60 min 110 min 230 min⎯⎯⎯→ ⎯⎯⎯→°C °C°C(10) °C(1) °C(5); detector temperature. 260°C; sample
Product. 1.0 μl.
7.2 Drawing a calibration curve
Take 6 10ml volumetric flasks, add appropriate amount of dichloromethane (4.1), and add 0.0, 10.0 with a micro-syringe.
20.0, 50.0, 100.0, 250.0 μl of turpentine standard use solution (4.3), make up to volume with dichloromethane, and mix. Made into pine
The fuel-saving mass concentration is a standard series of 0.0, 1.00, 2.00, 5.00, 10.0, 25.0 mg/L, respectively. Standard solution series
The concentration (mg/L) is the abscissa, and the corresponding peak response value (the sum of the peak height or peak area of α-pinene and β-pinene)
For the ordinate, draw a calibration curve.
7.3 Determination of samples
1.0 μl of the sample to be tested (6.2) was injected into the gas chromatograph and the measurement was carried out under the same chromatographic conditions as the calibration curve.
Record the retention time and peak area (or peak height) of the chromatographic peak.
7.4 Blank test
While the sample is being analyzed, a blank test should be performed. Take 1.0μl blank sample (6.3) into the gas chromatograph, press
7.3 Determine the same steps for analysis.
8 Calculation and representation of results
8.1 Qualitative analysis
Take a certain amount of turpentine standard solution (4.2), dilute to 25.0 mg/L with dichloromethane (4.1), take 1.0 μl injection,
Characterize the retention time of the turpentine chromatographic peak, see Figure 1.
Figure 1 Standard chromatogram of turpentine (column 1)
If the target compound is detected, use column 2 to aid in qualitative confirmation, see Figure 2.
Figure 2 Turpentine-assisted qualitative chromatogram (column 2)
8.2 Quantitative analysis
The mass concentration (mg/L) of turpentine in the sample is calculated according to formula (1).
Ρρ = × (1)
In the formula.
Ρ--the mass concentration of turpentine in the sample, mg/L;
Ρ1-- Calculate the pine in the sample to be tested from the calibration curve based on the sum of the peak areas (or peak heights) of α-pinene and β-pinene
Mass concentration of oil saving, mg/L;
V 1--sample volume, ml;
V2--extract volume, ml.
8.3 result representation
When the measurement result is less than 1.00 mg/L, it is retained to two decimal places; when the measurement result is greater than or equal to 1.00 mg/L,
Keep three significant digits.
9 Precision and accuracy
9.1 precision
Six laboratories tested the uniform samples with turpentine concentrations of 0.10mg/L, 0.50mg/L, and 1.50mg/L, respectively.
The relative standard deviations in the experimental room were. 6.0%~8.1%, 3.8%~10.1%, 2.8%~5.9%; the relative standard between laboratories
The deviations were. 5.7%, 6.6%, 3.9%; the repeatability limits were. 0.02 mg/L, 0.09 mg/L, 0.18 mg/L;
The sexual limits were. 0.03 mg/L, 0.12 mg/L, and 0.23 mg/L, respectively.
9.2 Accuracy
Six laboratories conducted certified standard substances with turpentine concentrations of 0.10 mg/L, 0.50 mg/L, and 1.50 mg/L, respectively.
The relative errors are. -5.6%~7.9%, -8.4%~5.5%, -4.7%~5.8%; the relative error final values are.
-0.58% ± 12.4%, -2.40% ± 11.2%, 1.37% ± 7.3%.
Six laboratories carried out spiked analysis and analysis on surface water, domestic sewage and industrial wastewater samples, respectively.
The recoveries of 0.010mg, 0.050mg and 0.150mg were 83.2%~93.0%, 84.6%~103% and 91.3%~103% respectively.
The final recoveries of the spiked recoveries were 87.6% ± 6.9%, 90.6% ± 13.4%, and 95.0% ± 8.8%, respectively.
10 Quality Assurance and Quality Control
10.1 At least one laboratory blank should be made for each batch of samples, and the blank value should be lower than the method detection limit. Otherwise, the cause should be ascertained.
10.2 The correlation coefficient of the calibration curve should be ≥0.995, otherwise the calibration curve should be redrawn.
10.3 Continuous calibration. For every 20 samples measured, a standard solution of the concentration at the midpoint of the calibration curve shall be determined.
The relative error of this point concentration with the calibration curve should be ≤ 20%. Otherwise, the calibration curve needs to be redrawn.
10.4 At least 10% of parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel should be determined.
Double. When the measurement result is within 10 times the detection limit (including the detection limit of 10 times), the relative deviation of the results of the parallel double sample measurement
Should be ≤ 50%; when the measurement result is greater than 10 times the detection limit, the relative deviation of the parallel double sample measurement results should be ≤ 20%.
10.5 At least one spiked sample shall be determined for each batch of samples, and the spiked recovery rate shall be between 70% and 130%.
11 Waste treatment
The organic waste generated by the experiment should be stored in a centralized manner and entrusted to a qualified unit for processing.
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