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HJ 806-2016: Water quality - Determination of acrylonitrile and acrolein - Purge and trap / gas chromatography
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Water quality - Determination of acrylonitrile and acrolein - Purge and trap / gas chromatography
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HJ 806-2016
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Basic data | Standard ID | HJ 806-2016 (HJ806-2016) | | Description (Translated English) | Water quality - Determination of acrylonitrile and acrolein - Purge and trap / gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 9,990 | | 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 806-2016: Water quality - Determination of acrylonitrile and acrolein - Purge and trap / gas chromatography
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(Water quality - Determination of acrylonitrile and acrolein purge and trap/GC)
Water quality - Determination of acrylonitrile and acrolein
Purge trapping/gas chromatography
Water quality - Determination of acrylonitrile and acrolein - Purge and
Trap/gas chromatography
2016-06-24 released
2016-08-01 implementation
National Environmental Protection Standard of the People 's Republic of China
Ministry of Environmental Protection released
I directory
Preface ii
1 Scope of application 1
2 normative reference document 1
Principle of Method 1
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples
8 Analysis Step 3
Results and Expressions
10 Precision and Accuracy 4
11 Quality assurance and quality control
12 Waste treatment 5
Appendix A (informative) Auxiliary qualitative chromatographic reference conditions
Foreword
In order 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 Water Pollution,
Protection of human health, regulate the determination of acrylonitrile and acrolein in water, the development of this standard.
This standard specifies the purge and trap/gas chromatographic methods for the determination of acrylonitrile and acrolein in water.
This standard is the first release.
Appendix A to this standard is an informative appendix.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. Shanghai Environmental Monitoring Center.
The standard verification unit. Zhejiang Province Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Center, Zhenjiang City Environmental Monitoring Center Station,
Shanghai Textile Energy Conservation and Environmental Protection Center, Shanghai Jiading District Environmental Monitoring Station, Shanghai Qingpu District Environmental Monitoring Station.
This standard is approved by the Ministry of Environmental Protection 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 water quality acrylonitrile and acrolein - Purge and trap/gas chromatography
1 Scope of application
This standard specifies the purge and trap/gas chromatographic methods for the determination of acrylonitrile and acrolein in water.
This standard is applicable to the determination of acrylonitrile and acrolein in surface water, groundwater, seawater, industrial waste water and domestic sewage.
When the sampling volume of 5 ml, the acrylonitrile and acrolein detection limit were 0.003 mg/L, the determination of the lower limit of 0.012
Mg/L.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
GB 17378.3 Marine Monitoring Specification Part 3. Sample collection, storage and transportation
3 Principle of the method
The target compound in the sample is purged by high purity nitrogen (or other inert gas) and adsorbed in the trap, rapidly heated
The tubes were blown back with high purity nitrogen (or other inert gas) and the components removed by heat were separated by gas chromatography,
Detection with hydrogen flame ionization detector. The retention time was qualitative and the peak area (peak height) was quantified.
4 interference and elimination
In the optimized chromatographic and purge conditions, there is no obvious interference material, if the qualitative results in question, can be used
GC/MS or double column characterization. Auxiliary qualitative column characteristics and chromatographic reference conditions are given in Appendix A.
5 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The experimental water is freshly prepared distilled water
Or deionized water.
5.1 Phosphoric acid. ρ (H3PO4) = 1.87 g/ml.
5.2 Phosphoric acid solution. 1 9 (V/V), prepared with phosphoric acid (5.1).
5.3 ascorbic acid.
5.4 Acrylonitrile (CH2CHCN). Chromatographic pure.
5.5 Acrylonitrile Standard Intermediate. ρ (CH2CHCN) = 12500 mg/L.
Prepared with acrylonitrile (5.4) at room temperature at 20 ° C. Remove the appropriate amount of water in a 10 ml volumetric flask and place it on a balance
Weighing; and carefully drop a few drops of acrylonitrile (5.4) to a weight gain of about 125 mg (accurate to 0.1 mg) and weigh again;
The difference between the two weighing weights determines the exact addition of acrylonitrile. With the experimental water volume to the mark, shake, calculate the acrylonitrile
The exact concentration of the standard intermediate solution (accurate to 10 mg/L). Into a brown reagent bottle with a Teflon screw cap,
Mix, with the current allocation. You can also purchase commercially available certified materials.
5.6 acrylonitrile standard use of liquid. ρ (CH2CHCN) = 125 mg/L.
2 Remove 1.00 ml of acrylonitrile standard intermediate (5.5) in a 100 ml volumetric flask containing the right amount of test water.
Test with water dilution volume to the scale, mixing, with the current allocation.
5.7 Acrolein (CH2CHCHO). Chromatographic purity.
5.8 Acrolein Standard Intermediate. ρ (CH2CHCHO) = 12500 mg/L.
Prepared with acrolein (5.7) at room temperature at 20 ° C. Remove the appropriate amount of water in a 10 ml volumetric flask and place it on a balance
Weighing; and carefully drop a few drops of acrolein (5.7) to a weight gain of about 125 mg (accurate to 0.1 mg) and weigh again;
The difference between the two weighing weights determines the exact addition of acrolein. With the experimental water volume to the mark, shake, calculate acrolein
The exact concentration of the standard intermediate solution (accurate to 10 mg/L). Into a brown reagent bottle with a Teflon screw cap,
Mix, with the current allocation. You can also purchase commercially available certified materials.
5.9 Acrolein standard use of liquid. ρ (CH2CHCHO) = 125 mg/L.
Take 1.00 ml of acrolein standard intermediate (5.8) in a 100 ml volumetric flask containing part of the experimental water.
Water volume to the scale, mixing, with the current allocation.
5.10 Carrier gas. nitrogen, purity 99.999%.
5.11 Gas. hydrogen, purity 99.99%.
5.12 to help gas. oil-free compressed air, by 5A0 molecular sieve purification.
6 instruments and equipment
Unless otherwise stated, the use of the national standard A-class glass gauge is used for the analysis.
6.1 Gas Chromatograph. with a capillary column shunt/splitless inlet, programmable temperature, equipped with hydrogen flame ionization detector
(FID).
6.2 Purge and trap device. with 5 ml or 25 ml purge tube, the capture tube generally use 100% Tenax adsorbent, or
Other equivalent adsorbents.
6.3 Column. quartz capillary column, 60 m x 0.53 mm, film thickness 1.0 μm (100% polyethylene glycol stationary phase),
Or other equivalent columns.
6.4 Vials. 40 ml brown glass vials with silicone rubber - polytetrafluoroethylene liner screw cap.
6.5 purge tube. 5 ml or 25 ml.
6.6 Volumetric flask. Class A, 10 ml, 50 ml, 100 ml.
6.7 Microinjector. 10 μl, 100 μl, 1000 μl.
6.8 Air tightness syringe. 5 ml or 25 ml (for purging and trap instrument for manual injection).
6.9 General laboratory equipment and equipment commonly used.
7 samples
7.1 Sample collection
The collection of samples shall be carried out in accordance with the relevant provisions of HJ/T 91, HJ/T 164 and GB 17378.3. Utensils silicone rubber - poly four
Fluoroethylene liner screw cap 40 ml brown glass vial (6.4) Collect the sample. Before sampling, add 0.3 g of bad blood
Acid (5.3) in the vial (6.4); when collecting the sample, the sample should be spilled in the vial without leaving the bubble,
A few drops of phosphoric acid solution (5.2) are fixed so that the pH of the sample is 4 to 5, tighten the cap. Each sample should be collected in parallel,
Each batch should have at least one full program blank.
Full program blank. add 0.3 g of the same batch of ascorbic acid (5.3) vial (6.4) to the sampling site, with the same
3 batches of experimental water filled with vials, add an equal volume of phosphoric acid solution (5.2) fixed, so that the pH value of 4 to 5, tighten the bottle
Cover, with the sample back to the laboratory.
7.2 Transport and storage of samples
After the collection of samples should be refrigerated below 4 ℃, dark, sealed and transported. If not timely analysis, should be at 4 ℃ to
Under cold storage, dark and sealed to complete the analysis within 5 d.
8 Analysis steps
8.1 Instrument reference conditions
8.1.1 Purge and capture reference conditions
Purge temperature is 50 ℃; purge time is 20 min; analytical temperature is 190 ℃; analytical time is 0.5 min;
The temperature is 210 ° C; the baking time is 10 min. The purge gas is high purity nitrogen and the purge flow rate is 30 ml/min. The rest of the Senate
Number of reference instrument operating instructions.
8.1.2 Gas Chromatographic Reference Conditions
Column temperature. initial temperature 40 ° C, rise to 80 ° C for 8 min at a rate of 5 ° C per minute, and then at a temperature of 50 ° C per minute
The rate rose to 190 ℃ for 7 min;
Inlet. no split injection, temperature.200 ℃;
Gas flow. high purity nitrogen for 8.1 ml/min, hydrogen for 30 ml/min, air for 300 ml/min;
Detector. temperature 250 ℃.
8.2 Drawing of working curves
Microcapsules (6.7) were used to remove 0 μl, 2 μl, 5 μl, 10 μl, 20 μl, 50 μl, 100 μl acrylonitrile
Standard use of liquid (5.6) and acrolein standard use of liquid (5.9), quickly added to the amount of experimental water containing a set of 50 ml capacity
Measuring bottle, and constant volume to the scale, shake. The concentration of the target compound was 0.000 mg/L, 0.005 mg/L,
0.013 mg/L, 0.025 mg/L, 0.050 mg/L, 0.125 mg/L, 0.250 mg/L. Accurate removal
5.0 ml standard series to purge tube, in accordance with the instrument reference conditions (8.1), from low to high concentration in turn measured. With propylene
The concentration of nitrile and acrolein is abscissa, and the corresponding peak area (or peak height) of the chromatogram is the ordinate and the working curve is drawn. C
The standard chromatogram of acrylonitrile and acrolein is shown in Fig.
1 - acrolein (9.075 min) 2 - acrylonitrile (13.692 min)
Figure 1 Acrylonitrile, acrolein standard chromatogram
8.3 Determination of samples
4 Remove the sample collected by 5.00 ml (7.1), follow the same instrument reference conditions (8.1) and steps as the plotting work curve
(8.2).
8.4 blank test
Follow the same instrument reference conditions (8.1) and step (8.2) as the plotting curve to remove the 5.00 ml test
Water for blank test.
9 Results calculation and representation
9.1 Results calculation
The concentration of acrylonitrile and acrolein in water samples is calculated according to formula (1)
A) A ( (1)
Where. - mass concentration of acrylonitrile and acrolein in water samples, mg/L;
A - measured peak area (or peak height) of acrylonitrile and acrolein in water samples;
A - the intercept of the standard curve equation;
B - the slope of the standard curve equation.
9.2 The result is shown
When the result is less than 1 mg/L, three decimal places are retained; when the result is greater than or equal to 1 mg/L,
Leaving three valid digits.
10 precision and accuracy
10.1 Precision
6 laboratories were tested for homogeneous samples containing acrylonitrile concentrations of 0.008 mg/L, 0.051 mg/L and 0.203 mg/L, respectively
Ok the test. The relative standard deviations in the laboratory were 6.7% ~ 8.4%, 0.3% ~ 10.4% and 0.4% ~ 7.8% respectively; the laboratory
The relative standard deviations were 10.4%, 4.9% and 2.8%, respectively; the repeatability limits were 0.002 mg/L, 0.009 mg/L and
0.02 mg/L; reproducibility limits were 0.002 mg/L, 0.01 mg/L and 0.03 mg/L, respectively.
6 laboratories were treated with homogeneous samples containing acrolein concentrations of 0.008 mg/L, 0.053 mg/L and 0.210 mg/L, respectively
Ok the test. The relative standard deviations in the laboratory were 5.0% ~ 9.3%, 1.9% ~ 7.2% and 0.4% ~ 6.0%, respectively.
The relative standard deviations were 6.3%, 5.3% and 4.7%; repeatability limits are 0.001 mg/L, 0.009 mg/L and 0.02
Mg/L, and the reproducibility limits were 0.002 mg/L, 0.011 mg/L and 0.03 mg/L, respectively.
10.2 Accuracy
The actual samples of acrylonitrile were quantitatively recovered by six laboratories. The recoveries were 97.5% ~ 126%
The final recoveries were 107% ± 20.8%.
The results showed that the recoveries of acrolein were 86.8% ~ 121%.
The final recoveries were 99.6% ± 23.6%.
11 quality assurance and quality control
11.1 calibration with a linear fitting curve, the correlation coefficient should be greater than or equal to 0.999, otherwise the need to re-draw the work
line.
511.2 Every 20 samples or per batch (less than 20 samples) should make a full blank and lab blank, blank
The results of acrylonitrile and acrolein should be lower than the detection limits.
11.3 Every 20 samples or each batch (less than 20 samples) should be analyzed at least one blank plus one sample and one sample spike
kind. The standard addition of acrylonitrile and acrolein should be 85.0% ~ 115%. The actual sample plus acrylonitrile
The recoveries of the additions should be within the range of 86.2% ~ 128%, and the recoveries of acrolein should be in the range of 76.0% ~ 123%.
11.4 Every 20 samples or each batch (less than 20 samples) should be analyzed at least one parallel sample, parallel sample relative deviation
Should be controlled within 20%.
11.5 Before batch analysis, the calibration test shall be carried out using the standard working solution at the intermediate concentration of the working curve.
Liquid should be temporary with the current; the determination of the results and the working curve of the relative density of the point should be less than 15%. Otherwise, to be repeated
Draw the work curve.
12 Waste treatment
The waste and waste generated in the experiment should be collected and kept collectively, and the corresponding identification shall be made, and the qualified unit shall be entrusted.
6 Appendix A
(Informative)
Auxiliary qualitative chromatographic reference conditions
A.1 column
Capillary column, 30 m x 0.53 mm, 40 μm film thickness (100% styrene-divinylbenzene polymer column), or
Performance similar to the column.
A.2 Assisted chromatographic reference conditions
A.2.1 Column temperature. initial temperature 40 ℃, keep 3 min, at a rate of 10 ℃ per minute rose to 180 ℃ for 2 min, then
The rate of 50 ° C per minute rose to 190 ° C for 3 min.
A.2.2 Detector. Temperature 250 ° C.
A.2.3 Inlet. Splitless injection, temperature.200 ° C.
A.2.4 Gas flow. N2. 8.1 ml/min, H2. 30 ml/min, air. 300 ml/min.
A.3 Standard chromatogram
1 - Acrolein (9.071 min) 2 - Acrylonitrile (9.752 min)
Figure 1 Acrylonitrile, acrolein standard chromatogram
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