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HJ 697-2014: Water quality. Determination of acrylamide. Gas chromatography method
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Water quality. Determination of acrylamide. Gas chromatography method
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HJ 697-2014
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PDF similar to HJ 697-2014
Standard similar to HJ 697-2014 GB 5085.7 HJ 694 GB 5085.1 HJ 698 HJ 696 Basic data | Standard ID | HJ 697-2014 (HJ697-2014) | | Description (Translated English) | Water quality. Determination of acrylamide. Gas chromatography method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 11,158 | | 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 acrylamide in water by gas chromatography. This Standard applies to surface water, groundwater, industrial wastewater and domestic sewage determined propylene amine phthalocyanine. When the sample size is 100ml | HJ 697-2014: Water quality. Determination of acrylamide. 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 acrylamide.Gas chromatography method
National Environmental Protection Standard of the People's Republic
HJ 697-.2014
Water quality - Determination of acrylamide - Gas chromatography
Water quality-Determination of acrylamide
-Gas chromatography method
2 0 1 4 - 0 3 - 3 1 released
2 0 1 4 - 0 7 - 0 1 implementation
release
Ministry of Environmental Protection
Content
Preface II
1 Scope..1
2 Normative references..1
3 method principle..1
4 Interference and elimination.1
5 Reagents and materials.1
6 instruments and equipment.2
7 samples. 2
8 Analysis steps..3
9 Calculation and representation of results..3
10 Precision and Accuracy 5
11 Quality Assurance and Quality Control..5
12 Waste treatment 5
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,
To ensure human health, standardize the determination method of acrylamide in water, and formulate this standard.
This standard specifies gas chromatography for the determination of acrylamide 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 method verification unit. Jiangsu Environmental Monitoring Center, Wuxi Environmental Monitoring Center Station, Suzhou Environmental Monitoring
Central 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 - Determination of acrylamide - 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 acrylamide in water.
This standard applies to the determination of acrylamide in surface water, groundwater, industrial wastewater and domestic sewage.
When the sample amount is 100ml, the detection limit of this standard is 0.07μg/L, and the lower limit of determination is 0.28μg/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
Under the condition of pH 1~2, acrylamide reacts with bromine to form α,β-dibromopropionamide. Acetic acid
Ethyl ester extraction of α,β-dibromopropionamide, the extract is dried over anhydrous sodium sulfate, concentrated, and made up to volume, with electron capture detection
The gas chromatograph of the instrument is separated and detected, and the external time method is used for quantification according to the retention time.
4 interference and elimination
Due to its high sensitivity, the electron capture detector is prone to interference due to a large number of impurity peaks. When the target compound is detected,
Apply column 2 to aid in qualitative confirmation to eliminate interference.
5 reagents and materials
Unless otherwise stated, analytically pure reagents and distilled water in accordance with national standards were used for the analysis.
5.1 Ethyl acetate. pesticide residue grade.
5.2 Acrylamide standard solution (CH2CHCONH2). ρ = 100 mg/L, the solvent is methanol.
5.3 α,β-dibromopropionamide standard solution. ρ = 100 mg/L, the solvent is ethyl acetate.
5.4 Sulfuric acid solution. c (H2SO4) ≈ 3mol/L.
Take about 167 ml of concentrated sulfuric acid, slowly add a small amount of water, and dilute to 1L.
5.5 Potassium Bromide (KBr)
5.6 Potassium bromate solution. c (KBrO3) = 0.1 mol/L.
Weigh 1.67 g of potassium bromate dissolved in a small amount of water and dilute to 100 ml.
5.7 Sodium thiosulfate solution. c (Na2S2O3) = 1.0 mol/L.
Weigh 15.8 g of sodium thiosulfate in a small amount of water and dilute to 100 ml.
5.8 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.
5.9 Silicon Magnesium Adsorbent
60-100 mesh, fired at 300 ° C for 2 h, naturally cooled, placed in a ground glass bottle, and stored in a desiccator.
5.10 Nitrogen. purity ≥ 99.999%.
6 Instruments and equipment
6.1 Gas Chromatograph. With an electron capture detector.
6.2 Column 1. Quartz capillary column, 30m × 0.32mm, coated with polyethylene glycol, film thickness 0.25μm. Or other equivalent hair
Thin tube column.
6.3 Column 2. Quartz capillary column, 30m × 0.32mm, coated with 35% phenyl-methyl polysiloxane, film thickness 0.25μm.
Or other equivalent capillary column.
6.4 Concentration device. Rotary evaporation device, or equivalent equipment such as KD concentrator and concentrator.
6.5 Oscillator.
6.6 Magnetic stirrer (with magnetic stirrer).
6.7 Drying column. glass column with a length of 250 mm and an inner diameter of 20 mm and a glass piston without oil. At the lower end of the column, put
A small amount of glass wool or fiberglass filter paper. Or use other types of drying equipment.
An electronic balance of 6.8 million.
6.9 Separating funnel. 250 ml.
6.10 Bottle with stoppered iodide. 250ml.
6.11 Microinjectors. 10 μl, 50 μl, 250 μl.
6.12 Common instruments and equipment used in general laboratories.
7 samples
7.1 Sample collection and preservation
Samples were taken with reference to the relevant regulations of HJ/T 91 and HJ/T 164.
Collect 250ml samples in clean ground glass bottles or brown threaded glass bottles with Teflon septa at 2°C
Store at ~5 °C, extract within 7 days, and extract for 30 days.
7.2 Preparation of samples
7.2.1 Measure 100.0ml sample into a 250ml iodine measuring flask, add 6.0ml sulfuric acid solution (5.4), mix, 2 ° C ~ 5 ° C
Place for 30 min.
7.2.2 Take out the iodometric flask, add 15.0g potassium bromide (5.5), dissolve and add 10ml potassium bromate solution (5.6) to mix, 2 ° C
Leave at ~5 °C for 2 h.
7.2.3 Take out the iodometric flask and add sodium thiosulfate solution (5.7) dropwise while shaking until the solution becomes colorless.
7.2.4 Add a magnetic stirrer to the iodine flask and slowly add 30g of anhydrous sodium sulfate (5.8) with vigorous stirring of the magnetic stirrer.
After completely dissolved, the stopper was allowed to stand for 10 min.
Note 1. Anhydrous sodium sulfate cannot be agglomerated during the addition of anhydrous sodium sulfate.
7.2.5 Transfer the above test solution to a 250ml separatory funnel, rinse the iodometric flask with about 2ml of water, and transfer the eluent to the liquid separation.
In the funnel, rinse twice.
7.2.6 Add 25 ml of ethyl acetate (5.1) to the separatory funnel, shake it and place it on a shaker for 5 min.
The layers were separated for 10 min and the organic phase was transferred to a 100 ml beaker. Repeat the extraction twice more.
7.2.7 Purification and drying. 10 g of silica-magnesium adsorbent (5.9) and 4 g of anhydrous sodium sulfate (5.8) were added successively to the drying column (6.7).
The dry column was immersed in a small amount of ethyl acetate, and the bubbles were discharged by pressure or vibration. When the ethyl acetate level is close to the dry column packing
At the time, the organic phase (7.2.6) was added and the organic phase was collected in a 150 ml concentrate bottle and washed with a small amount of ethyl acetate (5.1).
Cup, over dry column, repeat 1~2 times, then wash the dry column with 2 times of ethyl acetate for 2~3 times, collect all organic phase to thick
Shrink the bottle.
7.2.8 Using the rotary evaporator (reference conditions. water bath temperature 50 ° C, vacuum 270 mbar) the above organic phase (7.2.7)
The extract is concentrated to about 5 ml, the concentrate is transferred to a 10 ml volumetric flask, and the concentrate bottle is washed with a small amount of ethyl acetate (5.1).
2~3 times, transfer to the volumetric flask, and then make up to 10.0ml with ethyl acetate, to be tested.
7.2.9 Another 100.0ml of the same sample was placed in a 250ml separatory funnel and directly extracted according to the steps 7.2.6 to 7.2.8.
Take, concentrate and make up.
Note 2. This step is used to determine the content of α,β-dibromopropionamide which may be contained in the sample equivalent to acrylamide.
7.3 Preparation of blank samples
A sample of 100.0 ml of distilled water was used instead of the sample, and a blank sample was prepared in accordance with the same procedure as in the preparation of the sample (7.2).
8 Analysis steps
8.1 Recommended chromatographic conditions
Inlet temperature. 225 ° C; split injection, split ratio 10.1; column flow rate. 1.5 ml/min; oven temperature.
30/min 20/min100 min min 240 min⎯⎯⎯→ ⎯⎯⎯→°C °C°C(4) 220°C(5) °C(5); detector temperature. 280°C;
Injection volume. 1.0 μl.
8.2 Drawing the working curve
The working curve should be drawn using acrylamide standard solution (5.2) each time the sample is analyzed. Take 6 250ml iodine
Bottles, add 100ml of pure water, add 0.00μl, 5.00μl, 10.0μl, 25.0μl, 50.0μl, 125.0μl acryloyl
The standard solution of the amine is used (4.12), and the mass concentration of acrylamide is 0.00μg/L, 0.50μg/L, 1.00μg/L, respectively.
2.50 μg/L, 5.00 μg/L, 12.5 μg/L standard series. According to the preparation step (7.2) of the sample, according to the recommendation
The chromatographic conditions (8.1) were determined by using the concentration of the standard solution series (μg/L) as the abscissa and the corresponding chromatographic peak
The working curve is drawn by the value (peak area/peak height) as the ordinate.
8.3 Determination of samples
Take 1.0 μl of the sample to be tested (7.2) into the gas chromatograph, measure according to the recommended chromatographic conditions, and record the chromatographic peak.
Retention time and peak area (or peak height).
8.4 Blank test
While the sample is being analyzed, a blank test should be performed. Take 1.0μl blank sample (7.3) into the gas chromatograph, push
The recommended chromatographic conditions were determined and the retention time and peak area (or peak height) of the chromatographic peaks were recorded.
9 Calculation and representation of results
9.1 Qualitative analysis
During the addition reaction of acrylamide with bromine to form α,β-dibromopropionamide, other brominated products are produced and used.
The sub-capture detector detects impurity peak interference when it is detected, which is inconvenient for the quasi-determinism of acrylamide. Take an appropriate amount of α,β-dibromopropionamide
Standard solution (5.3), diluted to 20 μg/L with ethyl acetate, according to the recommended chromatographic conditions (8.1), according to the
Leave time to characterize, see Figure 1.
Figure 1 Standard chromatogram of α,β-dibromopropionamide (column 1)
Figure 2 Sample Derived Chromatogram (Column 1)
When acrylamide is detected in the sample, it can be confirmed with column 2.
Figure 3 Sample Derived Chromatogram (Column 2)
9.2 Calculation of results
The mass concentration (μg/L) of acrylamide in the sample was calculated according to the formula (1).
ρ ρρ −= × (1)
In the formula.
Ρ--the mass concentration of acrylamide in the sample, μg/L;
Ρ1-- From the sample (7.2.8) found on the working curve, α,β-dibromopropionamide corresponds to the mass concentration of acrylamide.
Gg/L;
Ρ2--α,β-dibromopropionamide corresponding to the mass concentration of acrylamide in the sample (7.2.9) found on the working curve,
Gg/L;
V1--water sample volume, ml;
V2--sample volume, ml.
9.3 Result representation
When the measurement result is ≥1.00μg/L, three significant figures should be retained; when the measurement result is < 1.00μg/L, the result is kept small.
Two points after the number.
10 Precision and accuracy
10.1 Precision
Uniform samples with acrylamide concentrations of 0.50μg/L, 2.00μg/L, and 8.00μg/L were tested in 6 laboratories.
The relative standard deviations in the laboratory are. 1.7%~6.8%, 1.6%~3.1%, 1.2%~2.0%;
The relative standard deviations were 5.6%, 2.8%, and 1.0%, respectively; the repeatability limits were. 0.06 μg/L, 0.14 μg/L, and 0.32 μg/L, respectively;
The reproducibility limits were 0.10 μg/L, 0.21 μg/L, and 0.37 μg/L, respectively.
10.2 Accuracy
Six laboratories conducted uniform standards for acrylamide concentrations of 0.50 μg/L, 2.00 μg/L, and 8.00 μg/L.
For the measurement, the relative errors are 1.2%-5.5%, 2.2%~5.8%, -1.6%~3.2%, respectively; the relative error final values are.
2.76% ± 3.3%. 3.7% ± 3.1%, 1.4% ± 3.7%.
6 laboratories respectively measured the surface water, domestic sewage and industrial wastewater, and the scalar amount was 0.050μg.
0.500μg, 2.00μg, the standard addition recovery rate. 92.8%~108%, 90.7%~105%, 87.2%~112%;
The final yield values were 99.9% ± 12.3%, 100% ± 11.1%, and 100% ± 16.4%, respectively.
11 Quality Assurance and Quality Control
11.1 For each batch of samples, at least one laboratory blank should be made. The blank value should be lower than the method detection limit. Otherwise, the cause should be ascertained.
11.2 The correlation coefficient of the working curve should be ≥0.995, otherwise the working curve should be redrawn.
11.3 Continuous calibration. For every 20 samples measured, a standard solution of the concentration of the middle point of the calibration curve shall be determined.
The relative error of the concentration of the calibration curve at this point should be ≤ 20%. Otherwise, the calibration curve needs to be redrawn.
11.4 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 double should be determined.
kind. 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 determination 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%.
11.5 At least one spiked sample shall be determined for each batch of samples. The recovery rate of the spiked sample shall be between 70% and 130%.
12 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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