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HJ 638-2012Ambient air. Determination of phenolic compounds by high performance liquid chromatography (English PDF)

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

January 1, 1970

Implementation date

January 1, 1970

Scope

HJ 638-2012 (Ambient air. Determination of phenolic compounds by high performance liquid chromatography) is available as an English-translated PDF.

HJ 638-2012 — This standard specifies high performance liquid chromatography for the determination of phenolic compounds in ambient air. This standard applies to the determination of 12 phenolic compounds in ambient air (see Appendix A for specific determination components).

This standard does not Suitable for the determination of phenolic compounds in granules. When the sampling volume is 25L, the detection limit of this method is 0.006~0.039 mg/m3, and the lower limit of determination is 0.024~0.156.

Mg/m3; When the sampling volume is 75L, the detection limit of this method is 0.002~0.013mg/m3, and the lower limit of determination is 0.008~ 0.052 mg/m3. See Appendix A for details.

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Document preview — HJ 638-2012

National Standard of the People's Republic of China

ICS: 13.040.20
Classification: Z 15

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Normative references
3 Principle of the method
4 Interference and elimination
5 Reagents and materials
5.5 Standard stock solution. rho=1000mg/L
5.6 Standard use solution. rho=100mg/L
5.7 XAD-7 Resin. 40~60 mesh
5.8 Glass fiber filter
5.9 Glass wool
5.10 V-shaped wire
6 Instruments and equipment
6.2 Sampling tube. inner diameter 6mm, outer diameter 8 mm, length 11cm
7 Samples
7.1 Sample collection
7.2 Preservation of samples
7.3 Preparation of samples
7.4 Preparation of blank samples
7.5 Penetration test
8 Analysis steps
8.1 Reference chromatographic conditions
8.2 Calibration
8.3 Determination
8.4 Blank test
9 Calculation and representation of results
9.1 Calculation of results
9.2 Results representation
10 Precision and accuracy
10.1 Precision
10.2 Accuracy
11 Quality Assurance and Quality Control
12 Waste treatment

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 the Prevention and Control of Atmospheric Pollution this standard is formulated to ensure human health and to regulate the determination of phenolic compounds in ambient air.

This standard specifies high performance liquid chromatography for the determination of phenolic compounds in ambient air.

This standard is the first release.

Appendix A of this standard is a normative appendix, and Appendix B is an informative appendix.

This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.

This standard is mainly drafted by. Changchun Environmental Monitoring Center Station.

This standard is verified by. Shenyang Environmental Monitoring Center Station, Dalian Environmental Monitoring Center, Jilin Province Environmental Monitoring Center Station, Harbin Environmental Monitoring Center Station, Jilin Entry-Exit Inspection and Quarantine Technology Center and Jilin Province Product Quality Supervision and Inspection hospital.

This standard was approved by the Ministry of Environmental Protection on February 29, 2012.

This standard has been implemented since June 1, 2012.

This standard is explained by the Ministry of Environmental Protection.

Determination of phenolic compounds in ambient air - High performance liquid chromatography Warning. Phenolic compounds are toxic substances. The preparation of samples should be carried out in a fume hood. Operators should avoid them.

Avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies high performance liquid chromatography for the determination of phenolic compounds in ambient air.

This standard applies to the determination of 12 phenolic compounds in ambient air (see Appendix A for specific determination components). This standard does not Suitable for the determination of phenolic compounds in granules.

When the sampling volume is 25L, the detection limit of this method is 0.006~0.039 mg/m3, and the lower limit of determination is 0.024~0.156.

Mg/m3; When the sampling volume is 75L, the detection limit of this method is 0.002~0.013mg/m3, and the lower limit of determination is 0.008~ 0.052 mg/m3. See Appendix A for details.

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.

HJ/T 55 Technical Guidelines for Unorganized Emissions of Air Pollutants HJ/T 194 Technical Specifications for Manual Air Quality Monitoring

3 Principle of the method

The gaseous phenolic compounds collected by XAD-7 resin are eluted with methanol and separated by high performance liquid chromatography. UV detection Detector or diode array detector detection, qualitative time of retention, quantified by external standard method.

4 Interference and elimination

Benzene, toluene, ethylbenzene, styrene, trichlorobenzene, tetrachlorobenzene, benzopyrene, aniline, nitrobenzene, etc. in ambient air the determination of phenolic compounds does not cause interference, and other interferents can be replaced by changing the column or changing the proportion of the mobile phase.

The target is separated.

5 Reagents and materials

Analytical purification reagents in accordance with national standards were used for analysis unless otherwise stated; the experimental water was phenol-free water, liquid the chromatographic test showed no interference peaks.

5.1 Non-phenolic water. It should be stored in a glass bottle. When using it, avoid contact with rubber products (rubber plugs or latex plugs, etc.).

It can be prepared in accordance with 5.1.1 or 5.1.2.

5.1.1 Add 0.2g of activated carbon powder activated at.200 ° C for 30 min per liter of distilled water, shake it thoroughly, and place it.

At night, filter with double-layer medium speed filter paper.

5.1.2 Add sodium hydroxide to make the distilled water weakly alkaline, and add potassium permanganate until the solution is purple-red, and move into the all-glass distiller.

The medium is heated and distilled, and the effluent is collected for use.

5.2 Methanol. HPLC grade.

5.3 Acetonitrile. HPLC grade.

5.4 Acetone. Excellent grade.

5.5 Standard stock solution. rho=1000mg/L

Accurately weigh phenol, 2-methylphenol, 3-methylphenol, 4-methylphenol, 1,3-benzenediol, 4-chlorophenol, 2,6-di 0.050 g of methylphenol, 1-naphthol, 2-naphthol, 2,4,6-trinitrophenol, 2,4-dinitrophenol and 2,4-dichlorophenol in a 50 ml volumetric flask, make up to volume with methanol (5.2) and mix. Store in a 4 ° C refrigerator. Or buy a commercially available certified standard directly Solution.

5.6 Standard use solution. rho=100mg/L

Measure 1.0 ml of standard stock solution (5.5) in a 10 ml volumetric flask, dilute to volume with methanol (5.2), and mix. Ice at 4 ° C Saved in the box.

5.7 XAD-7 Resin. 40~60 mesh

Soak it in acetone (5.4) for 12h, then put it into Soxhlet extractor and extract it with methanol (5.2) for 16h, then put it in vacuum.

Volatilize to dryness in the dryer.

5.8 Glass fiber filter

Placed in a muffle furnace at 350 ° C for 4 h, cooled and then washed with methanol (5.2), the punch is cut vertically into 8 mm the diameter of the disc is placed in a desiccator for later use.

5.9 Glass wool

Each of acetone (5.4) and methanol (5.2) was washed 2 to 3 times, and placed in a vacuum desiccator for use.

5.10 V-shaped wire

6 Instruments and equipment

6.1 Sampler. The flow range is 0.1~1.0L/min with an accuracy of 0.05L/min.

6.2 Sampling tube. inner diameter 6mm, outer diameter 8 mm, length 11cm

Preparation method. as shown in Figure 1, fill a small amount of glass wool (5.9) 2 cm at the end of the sampling tube A, then add 100 Mg XAD-7 adsorbent (5.7), followed by a little glass wool and 75 mg XAD-7 adsorbent (5.7) and a little glass Glass wool (5.9), finally put a glass fiber filter (5.8) from the A end, compact with a glass rod, and then use a V-shaped wire (5.10) Fixed, closed at both ends with a Teflon cap.

Figure 1 Schematic diagram of the glass sampling tube structure

A--the front end of the sampling tube, 2cm long; B--the rear end of the sampling tube, 4.5cm long;

1--glass wool; 2-100 mg XAD-7, 2 cm long; 3-75 mg XAD-7, 1.5 cm long;

4--glass fiber filter; 5-V wire

6.3 High Performance Liquid Chromatograph (HPLC). with UV detector or diode array detector.

6.4 Column. C18 column, 4.60mm × 150mm, particle size 5.0µm, or other equivalent column.

6.5 Soxhlet extractor. 250ml.

6.6 Muffle furnace.

6.7 Vacuum dryer.

6.8 Common instruments and equipment used in general laboratories.

7 Samples

7.1 Sample collection

The position of the sampling point, the sampling frequency, the placement of the sampler, and the sampling record are related to HJ/T 55 and HJ/T 194.

Provisions.

7.1.1 The sampler should be calibrated before sampling. At the sampling site, connect the B end of a sampling tube to the air sampler.

Adjust sampler flow, this sample tube is only used for flow regulation.

7.1.2 Connect the B end of the sampling tube to the sampler. The inlet end of the sampling tube is vertically downward, and the flow rate is recorded. The sampling flow rate is 0.2~.

0.5L/min, the sampling time is determined according to the actual situation.

7.1.3 Record the sample flow after the sampling is completed. The sampling tube was removed and the ends were closed with a Teflon cap.

7.2 Preservation of samples

At the end of the sampling, the sampling tube is placed in a closed container and brought back to the laboratory. If it cannot be measured in time, it should be avoided below 4 °C Light preservation, measured within 14 days.

7.3 Preparation of samples

The sampling tube was returned to room temperature, and 5 ml of methanol (5.2) was gradually added from the B end to rinse, and the eluent naturally flowed out from the A end.

When the eluate was collected in a 2 ml brown volumetric flask to near the mark, the collection was stopped and then the volume was adjusted to the mark with methanol (5.2).

7.4 Preparation of blank samples

7.4.1 Transportation blank

At least one transport blank sample should be taken with each sample taken. Bring the sample tube prepared in the same batch to the sampling site, no Unpacking, after sampling, put it in a closed container and bring it back to the lab. A blank sample was prepared in the same manner as in 7.3.

7.4.2 Laboratory blank

Laboratory blank samples were prepared in the same laboratory as in the same procedure as in 7.3.

7.5 Penetration test

Connect two sampling tubes in series, one end of one sampling tube (front tube) and one end of another sampling tube (rear tube) with hose Connect, the B end of the other sampling tube is connected to the sampler to record the sampling flow rate and time. The suction of the XAD-7 adsorbent in the front tube with efficiency (%), calculate according to formula (1).

1 × = MM

MK (1)

In the formula.

K--the adsorption efficiency of the front tube, %;

M1--the amount of sample of the front tube, mg;

M2--Sampling amount of the back tube, mg.

8 Analysis steps

8.1 Reference chromatographic conditions

Mobile phase. 20% acetonitrile/80% water (V. V) 45% acetonitrile/55% water (V. V) 80 acetonitrile /20% (V.V), reserved for 5 min;

7.5min 2.0min

Detection wavelength. 223 nm;

Flow rate. 1.5 ml/min;

Injection volume. 10.0 µl;

Column temperature. 25 ° C.

8.2 Calibration

8.2.1 Preparation of the standard series

Measure 0µl, 50µl, 100µl,.200µl, 500µl, 1000µl standard use solution (5.6) in 10ml capacity in a bottle, make up to volume with methanol (5.2) and mix. Formulated to a concentration of 0mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L, 5.0mg/L and a standard series of 10.0mg/L.

8.2.2 Drawing of the calibration curve

The 10.0µl standard series is taken from the low concentration to the high concentration, and injected into the high performance liquid chromatograph according to the reference chromatographic strip.

(8.1) is measured, the chromatographic response is the ordinate, and the phenolic compound concentration (mg/L) is plotted on the abscissa.

Quasi-curve. The calibration curve correlation coefficient r is greater than or equal to 0.999. The reference chromatogram of the phenolic compound is shown in Figure 2.

Figure 2 Standard chromatogram of phenolic compounds

1--2,4-dinitrophenol; 2--2,4,6-trinitrophenol; 3-1,3-benzenediol; 4-phenol;

5--3-methylphenol; 6--4-methylcresol; 7--2-methylcresol; 8-4-chlorophenol;

9--2,6-dimethylphenol; 10--2-naphthol; 11--1-naphthol; 12--2,4-dichlorophenol

8.3 Determination

Measure 10.0 µl of sample (7.3) according to the reference chromatographic conditions (8.1), record retention time and peak height (or peak area).

8.3.1 Qualitative analysis

Qualitative according to the retention time of the standard chromatogram of phenolic compounds.

8.3.2 Quantitative analysis

The concentration of phenolic compounds in the samples was quantified using an external standard method.

8.4 Blank test

A 10.0 µl blank sample (7.4) was weighed and measured according to the reference chromatographic conditions (8.1).

9 Calculation and representation of results

9.1 Calculation of results

The concentration of phenolic compound rho (mg/m3) in the ambient air sample was calculated according to formula (2).

Min

V×= rhorho (2)

In the formula.

rho--the concentration of phenolic compounds in the sample, mg/m3;

1-1--Check the concentration of phenolic compounds from the calibration curve, mg/L;

V1--eluent volume to volume, ml;

Vs--the sampling volume under standard conditions (101.3 kPa, 273.2 K), L.

9.2 Results representation

When the measurement result is less than 1 mg/m3, the result is retained three decimal places; when the measurement result is greater than or equal to 1 mg/m3, the knot is If you keep three significant digits.

10 Precision and accuracy

10.1 Precision

Uniformity of phenolic compounds (concentration near the lower limit of determination, 0.32 mg/m3 and 0.64 mg/m3) in six laboratories the samples were measured and the relative standard deviations in the laboratory were. 0.08% to 8.4%; the relative standard deviations between laboratories were.

0.21% to 3.8%; the repeatability limit range is. 0.003mg/m3 to 0.043mg/m3; the reproducibility limit range is. 0.004mg/m3~ 0.039 mg/m3.

10.2 Accuracy

The six laboratories performed the spiked analysis on the actual samples, and the spiked amount was 2.0 µg. The standard addition recovery range was.

85.0% to 93.4%.

The precision and accuracy data are detailed in Appendix B.

11 Quality Assurance and Quality Control

11.1 The deviation of the flow before and after the collection should be less than 5%, otherwise it should be re-acquired.

11.2 At least one laboratory blank and transport blank shall be determined for each batch of samples, and the results shall be lower than the method detection limit.

11.3 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.

As such, the relative deviation of the results of two parallel measurements should be less than or equal to 10%.

11.4 Each batch of samples should be tested at least once, and the adsorption efficiency of the front tube should be greater than or equal to 80%.

12 Waste treatment

Phenolic compounds are toxic substances. All used waste liquids during the experiment cannot be dumped at will and should be disposed of properly.

Appendix A

(normative appendix) Method detection limit and lower limit of measurement when the sampling volume is 25L and 75L respectively, the detection limit and lower limit of the method are shown in Appendix A.1.

Schedule A.1 Method detection limit and lower limit of measurement Unit. mg/m3 Serial number Chinese name English name Detection limit measurement lower limit detection limit lower limit 25L 75L 1 phenol 0.028 0.112 0.009 0.036 2-methylphenol Phenol) 2-Methylphenol 0.029 0.116 0.010 0.040 3-methylphenol Phenol) 3-Methylphenol 0.019 0.076 0.007 0.028 4-methylphenol Phenol) 4-Methylphenol 0.017 0.068 0.006 0.024 5 1,3-benzenediol 1,3-Dihydroxybenzene 0.027 0.108 0.009 0.036 6 2,6-dimethylphenol 2,6-xylenol 0.039 0.156 0.013 0.052 7 4-chlorophenol 4-chlorophenol 0.029 0.116 0.010 0.040 8 2-naphthol 2-naphthol 0.006 0.024 0.002 9 1-naphthol 1-naphthol 0.025 0.100 0.008 0.032 10 2,4,6-trinitrophenol 2,4,6-Trinitrophenol 0.022 0.088 0.007 0.028 11 2,4-Dinitrophenol 2,4-Dinitrophenol 0.019 0.076 0.006 0.024 12 2,4-Dichlorophenol 2,4-Dichlorophenol 0.021 0.084 0.008 0.032 Appendix B (informative appendix) Method of precision and accuracy summary the sampling volume is 25L, and six laboratories have measured three uniform samples of different concentrations and measured the actual samples.

The product was subjected to spike analysis and the precision and accuracy results are shown in Table B.1.

Summary of the precision and accuracy of the method in Schedule B.1 name average value (mg/ m3) laboratory interior phase Standard deviation (%) Laboratory room Relative standard deviation(%) Repeatability limit r (mg/ m3) Reproducibility limit (mg/ m3) average value (mg/ m3) blank sample spike Recovery rate(%) Actual sample spike recovery (scaling amount 2.0µg) (%) %p Sampling volume 25L Sampling volume 25L phenol 0.12 2.67~5.05 2.22 0.012 0.013 0.16 97.7 90.8 0.32 2.82~5.38 0.970 0.033 0.031 0.40 97.5 0.64 1.48~2.87 0.236 0.038 0.035 0.80 95.2 2-methyl phenol 0.12 1.10~4.69 2.14 0.011 0.013 0.16 97.2 88.8 0.32 1.42~5.86 1.47 0.033 0.033 0.40 97.6 0.64 1.48~2.85 0.484 0.036 0.034 0.80 96.9 3-methyl phenol 0.08 2.59 - 0.006 - 0.16 98.5 95.0 0.32 1.89 - 0.017 - 0.40 97.9 0.64 1.11 - 0.020 - 0.80 97.8 4-methyl phenol 0.08 2.02 - 0.006 - 0.16 98.6 95.0 0.32 2.83 - 0.025 - 0.40 98.5 0.64 1.57 - 0.028 - 0.80 98.8 1,3-benzene Diphenol 0.08 2.77~8.38 3.82 0.011 0.013 0.16 97.6 88.2 0.32 0.717~4.12 1.40 0.029 0.030 0.40 97.8 0.64 0.205~2.88 0.721 0.033 0.032 0.80 96.8 2,6-two Methylbenzene 0.16 2.34~6.70 1.40 0.019 0.018 0.16 98.5 86.1 0.32 2.29~3.66 1.02 0.028 0.027 0.40 98.2 0.64 1.45~2.41 0.463 0.035 0.033 0.80 96.9 4-chloro phenol 0.12 2.15~5.02 1.63 0.012 0.013 0.16 98.4 87.0 0.32 2.97~5.18 0.950 0.034 0.032 0.40 97.7 0.64 1.37~2.79 0.592 0.037 0.035 0.80 95.2 2-naphthol 0.024 3.41~6.45 0.905 0.003 0.004 0.16 97.3 85.0 0.32 1.96~4.72 0.761 0.033 0.031 0.40 97.9 0.64 1.60~2.60 0.359 0.039 0.036 0.80 96.5 1-naphthol 0.12 2.55~6.61 1.93 0.016 0.016 0.16 96.5 85.6 0.32 2.74~4.11 0.567 0.032 0.029 0.40 97.8 0.64 1.44~2.98 0.214 0.040 0.037 0.80 95.8 2,4,6-three Nitro phenol 0.08 0.840~7.58 3.17 0.008 0.011 0.16 97.7 93.4 0.32 2.21~4.13 1.35 0.026 0.027 0.40 97.0 0.64 1.46~3.56 0.274 0.043 0.039 0.80 96.5 2,4-dinitrogen 0.08 2.28 - 0.006 - 0.16 93.3 97.5 name average value (mg/ m3) laboratory interior phase Standard deviation (%) Laboratory room Relative standard deviation(%) Repeatability limit r (mg/ m3) Reproducibility limit (mg/ m3) average value (mg/ m3) blank sample spike Recovery rate(%) Actual sample spike recovery (scaling amount 2.0µg) (%) %p Sampling volume 25L Sampling volume 25L Phenol 0.32 3.05 - 0.025 - 0.40 95.7 0.64 1.48 - 0.025 0.80 95.4 2,4-dichloro phenol 0.08 3.11 - 0.006 - 0.16 101.5 91.2 0.32 2.06 - 0.017 - 0.40 98.3 0.64 1.46 - 0.025 - 0.80 98.8

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