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HJ 806-2016Water quality - Determination of acrylonitrile and acrolein - Purge and trap / gas chromatography (English PDF)

水质丙烯腈和丙烯醛的测定吹扫捕集气相色谱法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

June 24, 2016

Implementation date

August 1, 2016

Scope

HJ 806-2016 is the English-translated version of 水质丙烯腈和丙烯醛的测定吹扫捕集气相色谱法.

HJ 806-2016 — 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.

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Document preview — HJ 806-2016

National Standard of the People's Republic of China

Classification: Z 16

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Normative reference documents
3 Principle of the method
4 Interference and elimination
5 Reagents and materials
6 Instruments and equipment
7 Samples
7.1 Sample collection
7.2 Transport and storage of samples
8 Analysis steps
8.1 Instrument reference conditions
8.2 Drawing of working curves
8.3 Determination of samples
8.4 Blank test
9 Results calculation and representation
9.1 Results calculation
10 Precision and accuracy
10.1 Precision
10.2 Accuracy
11 Quality assurance and quality control
12 Waste treatment

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. rho (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. rho (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. rho (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. rho (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. rho (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 °C, dark, sealed and transported. If not timely analysis, should be at 4 °C 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 °C; purge time is 20 min; analytical temperature is 190 °C; 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 °C for 7 min;

Inlet. no split injection, temperature.200 °C;

Gas flow. high purity nitrogen for 8.1 ml/min, hydrogen for 30 ml/min, air for 300 ml/min;

Detector. temperature 250 °C.

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 °C, keep 3 min, at a rate of 10 °C per minute rose to 180 °C 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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