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HJ 998-2018: Soil and sediment - Determination of volatile phenolic compounds - 4-AAP spectrophotometric method
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Soil and sediment - Determination of volatile phenolic compounds - 4-AAP spectrophotometric method
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HJ 998-2018
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Basic data | Standard ID | HJ 998-2018 (HJ998-2018) | | Description (Translated English) | Soil and sediment - Determination of volatile phenolic compounds - 4-AAP spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Word Count Estimation | 12,125 | | Date of Issue | 12/26/2018 | | Date of Implementation | 6/1/2019 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 998-2018: Soil and sediment - Determination of volatile phenolic compounds - 4-AAP spectrophotometric method
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Soil and sediment - Determination of volatile phenolic compounds - 4-AAP spectrophotometric method
National Environmental Protection Standard of the People's Republic
Determination of volatile phenols in soils and sediments
4-aminoantipyrine spectrophotometry
Soil and sediment-Determination of volatile phenolic compounds-
4-AAP spectrophotometric method
Published on.2018-12-26
2019-06-01 Implementation
Ministry of Ecology and Environment released
i directory
Foreword...ii
1 Scope...1
2 Normative references...1
3 Terms and Definitions...1
4 Principles of the method... 2
5 Interference and elimination... 2
6 Reagents and materials...2
7 Instruments and Equipment...3
8 samples...3
9 Analysis steps...5
10 Results calculation and representation...5
11 Precision and Accuracy...6
12 Quality Assurance and Quality Control...7
13 Waste treatment...7
14 Notes...7
Precision and Accuracy of Appendix A (Informative) Method...8
Foreword
To protect the "Environmental Protection Law of the People's Republic of China" and the Law of the People's Republic of China on Soil Pollution Prevention
This standard is formulated to ensure human health and to regulate the determination of volatile phenols in soils and sediments.
This standard specifies the 4-aminoantipyrine spectrophotometric method for the determination of volatile phenols in soils and sediments.
Appendix A of this standard is an informative annex.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Dalian Environmental Monitoring Center.
This standard is verified by. Shenyang Environmental Monitoring Center Station, Anshan Environmental Monitoring Center Station, Jinzhou City Environmental Monitoring
Xinzhe, Zibo Environmental Monitoring Station, Shaanxi Provincial Environmental Monitoring Center Station and Hunan Environmental Monitoring Center Station.
This standard is approved by the Ministry of Ecology and Environment on December 26,.2018.
This standard has been implemented since June 1,.2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Determination of volatile phenols in soil and sediment
4-aminoantipyrine spectrophotometry
Warning. Phenols are toxic substances, and solution preparation should be carried out in a fume hood; protective equipment should be worn as required during operation.
Avoid breathing into the respiratory tract or direct contact with skin and clothing.
1 Scope of application
This standard specifies the 4-aminoantipyrine spectrophotometric method for the determination of volatile phenols in soils and sediments.
This standard applies to the determination of volatile phenols in soils and sediments.
When the sampling amount is 20 g and the detection optical path is 10 mm, the detection limit of the volatile phenol (based on phenol) is 0.3.
Mg/kg, the lower limit of determination is 1.2 mg/kg.
2 Normative references
This standard refers to the following documents or their terms. For undated references, the valid version applies to this
standard.
GB 17378.3 Marine monitoring specification Part 3. Sample collection, storage and transport
GB 17378.5 Marine monitoring specification Part 5. Sediment analysis
HJ 494 Water Quality Sampling Technical Guidance
HJ 503-2009 Determination of Volatile Phenols in Water - 4-Amino Antipyrine Spectrophotometric Method
HJ 613 Determination of dry matter and moisture in soils - Gravimetric method
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
HJ/T 166 Technical Specifications for Soil Environmental Monitoring
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
Volatile phenolic compounds
It can be extracted from soil and sediment under the conditions stipulated in this standard, can be distilled with water vapor and combined with 4-amino
Antipyrine reacts to form volatile phenolic compounds of colored compounds, with the result being phenol.
Note. Volatile phenols measured under the conditions specified in this standard do not contain 4-cresol, 2,4-xylenol, 3,4-xylenol, 2,4-dinitrophenol, 4,6-
A compound such as dinitro-2-cresol which does not undergo a color reaction with 4-aminoantipyrine.
24 Principles of the method
Extraction of phenolic compounds from soil and sediment with an alkaline solution, the extract is distilled under acidic conditions, and in the distillate
Volatile phenol reacts with 4-aminoantipyrine in an alkaline solution in the presence of potassium ferricyanide catalyst to form orange-red indophenol
Tebulin was measured at a wavelength of 510 nm, and the volatile phenol content was proportional to the absorbance value over a range of concentrations.
5 interference and elimination
Determination of volatile phenols in soils and sediments by aniline containing less than 750 mg/kg and oils of 1.5×104 mg/kg
No interference.
5.2 Sulfide interferes with the determination of volatile phenols. Preparation process before sampling (8.1) and distillation of sample (8.4.2)
The addition of copper sulfate pentahydrate (6.2) eliminates the interference of less than 3.0 x 104 mg/kg sulfide.
6 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis.
6.1 Experimental water. no phenol water, should be stored in glass bottles, when used, should avoid with rubber products (rubber plug or latex tube)
Etc.) Contact. The phenol-free water can be prepared in the following three ways.
Method 1. Newly prepared deionized water or distilled water, blank test is required before use, and the results should be in accordance with blank inspection.
(12.1) Requirements.
Method 2. Add 0.2 g of activated carbon powder activated at.200 ° C for 30 min per liter of water, shake well, and let stand overnight.
Filter with double layer medium speed filter paper.
Method 3. Add sodium hydroxide to make the water strong alkaline, and add potassium permanganate until the solution is purple-red, and transfer to full glass distillation.
The tube was heated and distilled, and the distillate was collected for use.
6.2 Copper sulfate pentahydrate (CuSO4·5H2O).
6.3 Ammonia. ρ(NH3·H2O) = 0.90 g/ml.
6.4 Phosphoric acid. ρ(H3PO4) = 1.87 g/ml.
6.5 sodium hydroxide (NaOH).
6.6 Phenol (C6H5OH).
6.7 Methyl orange (C14H14N3SO3Na).
6.8 Ammonium chloride (NH4Cl).
6.9 4-Aminoantipyrine (C11H13N3O).
6.10 Potassium ferricyanide (K3[Fe(CN)6]).
6.11 Quartz sand.
After burning at 400 ° C for 4 h, cooled to room temperature, transferred to a ground glass bottle and stored in a desiccator.
6.12 Sodium hydroxide solution. ρ (NaOH) = 10 g/L.
Weigh sodium hydroxide (6.5) 10 g dissolved in water, dilute to 1 L, and store in a plastic reagent bottle.
6.13 Refined phenol.
Phenol (6.6) is taken in a distillation flask with an air condensing tube, heated and distilled, and a distillate portion of 182 ° C to 184 ° C is collected.
3 minutes, the fraction should be colorless crystals after cooling, stored in a brown bottle, sealed in a cool dark place, and re-refined after discoloration.
6.14 phenol standard stock solution. ρ (C6H5OH) ≈ 1.00 g/L.
Weigh 0.1 g (accurate to 0.01 g) of refined phenol (6.13), dissolve in 100 ml of water, and store at 4 ° C or less in the dark.
It can be stored stably for one month, and needs to be reconstituted after discoloration. Before use, follow the method specified in Appendix A of HJ 503-2009.
set. Commercially available certified standard solutions can also be purchased.
6.15 Phenol standard use solution. ρ (C6H5OH) = 10.0 mg/L.
Take appropriate amount of phenol standard stock solution (6.14), dilute to 100 ml volumetric flask with water, shake well, and use it now.
6.16 methyl orange indicator solution. ρ (C14H14N3SO3Na) = 0.5 g/L.
Weigh 0.1 g of methyl orange (6.7) in.200 ml of water and store in a glass reagent bottle.
6.17 Buffer solution. pH ≈ 10.7.
Weigh 20 g of ammonium chloride (6.8) dissolved in 100 ml of ammonia (6.3), and store in a plastic reagent bottle at 4 ° C or less.
6.18 4-aminoantipyrine solution
2 g of 4-aminoantipyrine (6.9) was weighed and dissolved in 100 ml of water. In accordance with the method specified in Appendix B of HJ 503-2009
Purification, refrigerated at 4 ° C or less can be stored for one week.
6.19 Potassium ferricyanide solution. ρ(K3[Fe(CN)6])= 80 g/L.
Weigh 8 g of potassium ferricyanide (6.10) dissolved in 100 ml of water and store in a brown reagent bottle at 4 ° C or less for one week.
6.20 Copper sulfate solution. ρ(CuSO4·5H2O)=5 g/L.
Weigh 5 g of copper sulfate pentahydrate (6.2) dissolved in 1 L of water and stored in a glass reagent bottle.
6.21 Glass beads.
7 Instruments and equipment
7.1 Spectrophotometer. equipped with a cuvette with an optical path of 10 mm.
7.2 Ultrasonic instrument. The power is not less than.200 W.
Note. A cleaning ultrasonic or impact ultrasonic system can be used.
7.3 Horizontal oscillator. The frequency is from 100 r/min to 150 r/min. It is verified that the method requirements are met, and other oscillations can also be used.
device.
7.4 Heating device. adjustable power.
7.5 Vial. 30 ml brown glass jar with screw cap.
7.6 Vials. Glass bottles with screw caps and Teflon liners with a capacity of at least 100 ml.
7.7 Wide mouth polyethylene bottle. 500 ml with screw cap.
7.8 Distiller. 500 ml, all glass.
7.9 Common instruments and equipment used in general laboratories.
8 samples
8.1 Preparation before sampling
Before sampling, inject 10.0 ml of copper sulfate solution (6.20) into each 30 ml vial (7.5) with the number (code).
Accurately weigh and record the weight of each vial (with cap) (accurate to 0.1 g).
48.2 Sample Collection and Storage
Soil samples were collected in accordance with the relevant regulations of HJ/T 166. According to the phase of HJ 494, HJ/T 91 and GB 17378.3
The collection of sediment samples is required.
Samples for the determination of volatile phenols in soil and sediment are collected into vials (8.1), filling the vials and quickly
Remove the sample from the vial thread and the attached surface and seal the vial. At least 2 samples should be taken at each point. Pick
The collected samples should be stored at 4 ° C or less and stored for 3 days.
If necessary, replace the sample with a quartz sand (6.11) to fill the weighed vial (8.1) and seal it to the sampling site.
Open the cover, seal it to the site environment according to the sampling time, seal it, and transport and store it under the same conditions as the sample.
As a full program blank sample.
Samples measuring dry matter content (soil) or moisture content (sediment) are collected separately in vials (7.6).
Sample storage was carried out in accordance with the relevant regulations of HJ/T 166, HJ 494, HJ/T 91 and GB 17378.3.
8.3 Determination of moisture
The dry matter content of soil samples was determined according to HJ 613, and the moisture content of sediment samples was measured according to GB 17378.5.
set.
8.4 Preparation of samples
8.4.1 Extraction of samples
The 30 ml vial after sample collection according to 8.2 is returned to room temperature and weighed and recorded (accurate to 0.1 g), vial sampling
The difference between the front and rear weight is the sample amount (m) of the sample.
Take all samples from the vial into a wide-mouth polyethylene bottle (7.7) and use 10 ml of sodium hydroxide solution (6.12).
Clean the sample bottle, pour the cleaning solution into a polyethylene bottle, and then repeat the cleaning twice, then add 260 ml of sodium hydroxide solution.
(6.12), tighten the screw cap, oscillate horizontally for 10 min, or sonicate with a cleansing sonicator for 10 min. If the impact type is used
Sound wave meter, polyethylene bottle can be uncovered, ultrasonic for 10 min. After the sample is shaken or sonicated, let stand for 5 min and take 250 ml of supernatant.
Transfer to a 500 ml full glass distiller (7.8) to be distilled.
If the sample extract is not distilled in time, it should be placed in a polyethylene bottle, refrigerated at 4 ° C, sealed, and stored.
For 14 days.
8.4.2 Distillation of the sample
Add a few drops of methyl orange indicator solution (6.16) to the sample extract (8.4.1) and adjust the pH to the sample with phosphoric acid (6.4).
Obvious orange red (pH< 4), then add 5 g of copper sulfate pentahydrate (6.2), add 25 ml of water, add several glass beads (6.21) to prevent violence
Boiling. Connect the condenser, heat the distillation, adjust the power of the heating device (7.4) during the distillation process, control the distillation rate is not large
At 7 ml/min, collect 250 ml of distillate for testing.
Note. During the distillation process, the distillation system should be kept sealed. If the methyl orange red color is found to be faded, add 1 drop after the end of the distillation.
Base orange indicator solution (6.16). If the residue is not acidic after distillation, it should be resampled to increase the amount of phosphoric acid (6.4) added.
Distillation.
8.5 Preparation of blank samples
5 Replace the sample with quartz sand (6.11) and carry out the laboratory empty according to the same procedure as the sample preparation (8.4.1~8.4.2).
Preparation of white samples.
9 Analysis steps
9.1 Establishment of the standard curve
Add 0 ml, 0.50 ml, 2.00 ml, 5.00 ml, 10.0 ml to 6 50 ml stoppered glass tubes.
And 25.0 ml of phenol standard solution (6.15), the corresponding phenol content is 0 μg, 5.00 μg, 20.0 μg, 50.0 μg,
100 μg and 250 μg, add water (6.1) to the mark. Then add 0.5 ml buffer solution (6.17), mix, then add 1.0 ml
4-aminoantipyrine solution (6.18), mix well, and finally add 1.0 ml potassium ferricyanide solution (6.19), mix well, dense
Plug, place for 10 min.
The absorbance was measured at a wavelength of 510 nm in 30 min using a light path of 10 mm cuvette with water (6.1) as a reference.
The phenol content (μg) in each standard series solution is taken as the abscissa, and the corresponding net absorption after subtracting the absorbance value of the zero concentration point
The luminosity value is the ordinate and a standard curve is established.
9.2 Determination of samples
Measure the sample (8.4.2) 50.0 ml (V2), place it in a 50 ml stoppered glass cuvette, and follow the standard curve.
The same procedure (9.1) was carried out for the measurement.
Note. When the phenol content exceeds 250 μg, the sample size can be reduced and measured after dilution.
9.3 Laboratory blank test
The blank sample (8.5) was measured in the same manner as in 9.2.
10 Calculation and representation of results
10.1 Calculation of results
The mass fraction w (in phenol, mg/kg) of volatile phenol in the soil is calculated according to formula (1).
dmwmVb
VaAAw
10 (1)
Where. w--the mass fraction of volatile phenol in the soil sample (in terms of phenol), mg/kg;
A--the absorbance value of the sample;
0A -- absorbance value of laboratory blank test (9.3);
A--the intercept of the standard curve;
1V - extract volume, 300 ml;
B--the slope of the standard curve;
2V - sample volume for colorimetric, ml;
M--sample amount of sample, g;
6dmw -- soil sample dry matter content, %.
The mass fraction w (in phenol, mg/kg) of volatile phenol in the sediment is calculated according to formula (2).
OHwmVb
VaAAw
(2)
Where. w--the mass fraction of volatile phenol in the sediment sample (in terms of phenol), mg/kg;
A--the absorbance value of the sample;
0A -- absorbance value of laboratory blank test (9.3);
A--the intercept of the standard curve;
1V - extract volume, 300 ml;
B--the slope of the standard curve;
2V - sample volume for colorimetric, ml;
M--sample amount of sample, g;
OHw 2 -- the moisture content of the deposit, %.
Note. When the sample does not need to be diluted, 2V is 50 ml; when the sample needs to be diluted, 2V is the actual sample amount.
10.2 Results are expressed
When the measurement result is less than 100 mg/kg, the result is retained to one decimal place; when the measurement result is greater than or equal to 100 mg/kg,
The result retains three significant digits.
11 Precision and accuracy
11.1 Precision
Six laboratories performed six repeated measurements on low, medium and high concentrations of blank spiked soil and sediment samples.
The relative standard deviations in the laboratory ranged from 2.7% to 4.7%, 1.5% to 3.5%, and 1.3% to 2.1%, respectively;
The deviation ranges from 3.7% to 4.2%, 3.0% to 4.6%, and 2.9% to 3.9%, respectively; the repeatability limits range from 0.2 mg/kg to 0.3, respectively.
Mg/kg, 2.0 mg/kg to 2.6 mg/kg, and 10 mg/kg to 11 mg/kg; the reproducibility limits range from 0.3 mg/kg to 0.4, respectively.
Mg/kg, 3.3 mg/kg to 4.9 mg/kg and 21 mg/kg to 27 mg/kg.
Six laboratories performed six repeated measurements on two different concentrations of uniform soil and sediment samples.
The indoor relative standard deviation ranges from 2.2% to 5.7% and 2.5% to 5.8%, respectively; the relative standard deviations between laboratories are respectively
5.0%~10% and 5.0%~7.8%; the repeatability limits are 2.0 mg/kg~2.7 mg/kg and 2.1 mg/kg~2.8 mg/kg, respectively;
The reproducibility limits ranged from 4.5 mg/kg to 5.4 mg/kg and 4.4 mg/kg to 4.8 mg/kg, respectively.
The method precision summary data is detailed in Appendix A.
11.2 Accuracy
Six laboratories tested the low, medium and high concentrations of soil and sediment blank spiked samples, and the recovery rate was spiked.
The ranges are 83.0%~89.1%, 85.3%~89.9% and 90.5%~94.0% respectively.
Six laboratories performed standard addition analysis on two different concentrations of uniform soil and sediment samples, and added
The recovery rates ranged from 86.0% to 92.0% and 86.0% to 91.5%, respectively.
Refer to Appendix A for details of the method accuracy summary data.
12 Quality Assurance and Quality Control
12.1 Blank check
At least one laboratory blank shall be determined for each batch of samples, and the absorbance value of the blank test shall be ≤0.015.
12.2 Continuous calibration
The correlation coefficient of the standard curve is r≥0.999; for each batch (≤20), a curve intermediate check point should be determined.
The relative error between the result and the corresponding point of the standard curve should be within ±10%.
12.3 Precision Control
At least 10% of the parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel sample should be determined. earth
The relative deviation of the parallel samples of soil should meet the maximum allowable relative deviation of soil monitoring parallel samples specified in HJ/T 166, sediments
The relative deviation of the parallel samples should meet the parallel deviation requirements of GB 17378.5.
12.4 Accuracy Control
Each batch of samples should be measured with a blank spiked sample and 10% matrix spiked sample. When the number of samples is less than 10, it should be
Less determination of a matrix spiked sample, the spike recovery should be between 80% and 110%. If the sample has a matrix effect, spike
When the recovery rate is not satisfactory, a matrix-added parallel sample shall be measured. The relative deviation of the two matrix-added parallel samples shall be
Less than 25%.
13 Waste treatment
The waste generated in the experiment should be collected in a centralized manner and marked and entrusted to a qualified unit for disposal.
14 Precautions
14.1 In order to avoid the change of pH caused by the volatilization of ammonia in the buffer solution (6.17), it should be closed immediately after use.
When you want to use it now.
14.2 If the viscosity of the sample is large, it will agglomerate into a mass. After the extraction process, add sodium hydroxide solution (6.12) and apply the glass rod.
Spread the product and disperse it in the extract.
14.3 The distillation equipment used should not be mixed with distillation equipment for the determination of industrial or domestic sewage. Before and after each test, should
Clean the entire distillation unit.
14.4 Do not use rubber stoppers or rubber hoses to connect the distillation flask and condenser to prevent interference with the measurement.
8 Appendix A
(informative appendix)
Method precision and accuracy
The results of precision and accuracy are shown in Table A.1 and Table A.2.
Table A.1 Precision summary of the method
sample
Types of
average value
(mg/kg)
Experimental room relative
standard deviation(%)
Interlaboratory
standard deviation(%)
Repeatability limit
r(mg/kg)
Reproducibility limit
R (mg/kg)
Blank plus
Standard sample
2.6 3.0~4.7 4.2 0.3 0.4
33.6 2.2~3.5 4.6 2.6 4.9
226 1.3~2.1 3.9 11 27
actual
sample
27.3 2.2~5.7 5.0 2.7 4.5
28.9 2.5~5.7 5.0 2.8 4.8
Blank plus
Standard sample
2.6 2.7~3.5 3.7 0.2 0.3
33.0 1.5~2.4 3.0 2.0 3.3
228 1.3~2.0 2.9 10 21
actual
sample
17.7 2.5~5.1 10 2.0 5.4
18.4 2.5~5.8 7.8 2.1 4.4
Table A.2 Summary of Method Accuracy
Sample type
Background average
(mg/kg)
Sample spike concentration
(mg/kg)
Spike recovery range
iP (%)
Scaling recovery final value
PSP 2 (%)
Blank plus
Standard sample
0 3.0 83.0~87.7 84.8±4.2
0 37.5 85.3~89.1 87.2±2.6
0.200 90.5~92.0 91.3±1.0
actual
sample
27.3 20.0 86.0~89.5 87.9±2.4
28.9 30.0 86.0~90.0 88.4±3.0
Blank plus
Standard sample
0 3.0 85.0~89.1 86.5±3.2
0 37.5 86.7~89.9 88.0±2.2
0.200 91.0~94.0 91.8±2.2
actual
sample
17.7 10.0 88.0~92.0 89.7±3.0
18.4 20.0 87.0~91.5 89.1±3.6
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