HJ 502-2009_English: PDF (HJ502-2009)
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Water quality. Determination of volatile phenolic compounds. Bromine method
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HJ 502-2009
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Standards related to: HJ 502-2009
| Standard ID | HJ 502-2009 (HJ502-2009) | | Description (Translated English) | Water quality. Determination of volatile phenolic compounds. Bromine method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 9,961 | | Date of Issue | 2009-10-20 | | Date of Implementation | 2009-12-01 | | Older Standard (superseded by this standard) | GB/T 7491-1987 | | Quoted Standard | GB/T 7489-1987; HJ/T 91 | | Drafting Organization | Dalian Municipal Environmental Monitoring Center | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 54 of 2009 | | Summary | This standard specifies the determination of volatile phenolic compounds in industrial wastewater bromine method. This standard applies to industrial wastewater containing high concentrations of volatile phenols Determination of Volatile Phenol. This standard detection limit of 0. 1mg/L, detection limit of 0. 4mg/L, measured a maximum of 45. 0mg/L. For the determination of the mass concentration higher than the upper limit of the standard samples, measured after appropriate dilution. | HJ 502-2009
Water quality.Determination of volatile phenolic compounds.Bromine method
HJ
National Environmental Protection Standard of the People's Republic
Replace GB 7491-87
Water quality - Determination of volatile phenols
Water quality-Determination of volatile phenolic compounds
-bromine method
Released on.2009-10-20
2009-12-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 54 of.2009
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve the measurement of total organic carbon in water quality.
Six standards, such as the combustion oxidation-non-dispersive infrared absorption method, are national environmental protection standards and are released.
The standard name and number are as follows.
I. Determination of total organic carbon in water by combustion oxidation-non-dispersive infrared absorption method (HJ 501-2009);
3. Determination of volatile phenols in water - 4-aminoantipyrine spectrophotometric method (HJ 503-2009);
4. Determination of ozone in ambient air - Spectrophotometric method of sodium indigo disulphonate (HJ 504-2009);
V. “Determination of Biochemical Oxygen Demand (BOD5) on the 5th Day of Water Quality Dilution and Inoculation Method” (HJ 505-2009);
6. "Electrochemical Probe Method for Determination of Dissolved Oxygen in Water" (HJ 506-2009).
The above standards have been implemented since December 1,.2009 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
The following seven national rings approved and issued by the former National Environmental Protection Agency or the former State Environmental Protection Administration from the date of implementation of the above standards
The environmental protection standards are abolished. The standard names and numbers are as follows.
1. "Measurement of total organic carbon (TOC) for water quality by non-dispersive infrared absorption method" (GB 13193-91);
2. Determination of total organic carbon in water by combustion oxidation-non-dispersive infrared absorption method (HJ/T 71-2001);
3. Determination of volatile phenols in water quality and bromination capacity after distillation (GB 7491-87);
4. Determination of volatile phenols in water - 4-aminoantipyrine spectrophotometric method after distillation (GB 7490-87);
V. Determination of ozone in ambient air - Spectrophotometric method of sodium indigo disulphonate (GB/T 15437-1995);
6. "Determination of the Biochemical Oxygen Demand (BOD5) on the 5th Day of Water Quality Dilution and Inoculation Method" (GB 7488-87);
VII. Determination of Dissolved Oxygen in Water by Electrochemical Probe Method (GB 11913-89).
Special announcement.
October 20,.2009
Content
Foreword..iv
1 Scope..1
2 Normative references..1
3 Terms and Definitions.1
4 method principle..1
5 interference and elimination.1
6 reagents and materials. 2
7 instruments and equipment.2
8 samples.2
9 Analysis steps..3
10 result calculation 3
11 Precision and Accuracy 3
Foreword
To protect the environment and protect the human body 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 Water Pollution Prevention and Control
Health, standardize national environmental pollutant monitoring methods, and develop this standard.
This standard specifies the bromination capacity method for the determination of volatile phenols in industrial wastewater.
This standard is a revision of the "Bromide Capacity Method after Distillation of Water Quality Volatile Phenol" (GB 7491-87).
This standard was first published in 1987. The original standard drafting unit was Hangzhou Environmental Protection Monitoring Station. This is the first revision.
The main contents of this revision are as follows.
- clarify the scope of the standard measurement;
- Simplified the analysis steps of the bromination capacity method;
-- Added precision and accuracy terms.
The national environmental protection standard “Water quality approved and issued by the former National Environmental Protection Agency on March 14, 1987 since the implementation of this standard.
Determination of volatile phenols The bromination capacity method after distillation (GB 7491-87) is abolished.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Dalian Environmental Monitoring Center.
This standard was approved by the Ministry of Environmental Protection on October 20,.2009.
This standard has been implemented since December 1,.2009.
This standard is explained by the Ministry of Environmental Protection.
Iv
Water quality - Determination of volatile phenols
1 Scope of application
This standard specifies the bromination capacity method for the determination of volatile phenols in industrial wastewater.
This standard applies to the determination of volatile phenols in industrial wastewater containing high concentrations of volatile phenol.
The detection limit of this standard is 0.1 mg/L, the lower limit of determination is 0.4 mg/L, and the upper limit of determination is 45.0 mg/L. For mass concentration higher than standard
The sample having the upper limit measured can be appropriately diluted and then measured.
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.
GB 7489-87 Determination of dissolved oxygen in water - Iodometric method
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
3 Terms and definitions
The following terms and definitions apply to this standard.
Volatile phenolic compounds
A volatile phenolic compound which can be distilled off with steam and which is substituted with bromine, and the result is phenol.
4 Principle of the method
The volatile phenolic compound is distilled off by distillation and separated from the interfering substance and the fixing agent. Since the volatilization rate of phenolic compounds is
It varies with the volume of the distillate, so the distillate volume must be equal to the sample volume.
In a solution containing excess bromine (produced by potassium bromate and potassium bromide), the distilled phenolic compound and bromine form tribromophenol, and
One step produces bromotribromophenol. While the remaining bromine reacts with potassium iodide to release free iodine, bromotribromophenol reacts with potassium iodide to form
Tribromophenol and free iodine, the free iodine released by titration with sodium thiosulfate solution, and the content of volatile phenol was calculated according to the consumption.
5 interference and elimination
Determination of oxidizing agents, oils, sulfides, organic or inorganic reducing substances and aniline interfering phenols.
5.1 Elimination of oxidants (such as free chlorine)
The sample appeared blue on the starch-potassium iodide test paper (6.13), indicating the presence of oxidant, and an excess of ferrous sulfate (6.1) could be added.
Remove.
5.2 Elimination of sulfides
When there is a black precipitate in the sample, a drop of the sample may be placed on the lead acetate test paper (6.14). If the test paper turns black, it indicates that there is a sulfide.
presence. At this point, the sample is continuously added with phosphoric acid, and the aeration chamber is stirred and aerated until the generated hydrogen sulfide completely escapes.
5.3 Elimination of organic or inorganic reducing substances such as formaldehyde and sulfite
The appropriate amount of the sample can be separated into the separatory funnel, and the sulfuric acid solution (6.7) is added to make it acidic, and 50, 30, and 30 ml of diethyl ether (6.4) are added in portions.
To extract phenol, combine the ether layer into another separatory funnel, and add 4, 3, 3 ml of sodium hydroxide solution (6.8) in portions to carry out back extraction to make phenol
The class is transferred to a sodium hydroxide solution. Combine the alkali extract, transfer to a beaker, add water to the bath to remove residual ether, then use alkali to remove the alkali
The extract is diluted to the original sample volume.
At the same time, water should be used as a blank test.
5.4 Elimination of oils
After the sample is allowed to stand to separate the oil slick, follow the 5.3 procedure.
5.5 Elimination of anilines
Aniline can react with 4-aminoantipyrine to interfere with the determination of phenol, generally under acidic conditions (pH< 0.5).
Separated by pre-distillation.
6 reagents and materials
The reagents used in this standard are analytically purified according to national standards unless otherwise stated. The experimental water is newly prepared.
Distilled or deionized water.
6.1 Ferrous sulfate (FeSO4·7H2O).
6.2 Potassium iodide (KI).
6.3 Copper sulfate (CuSO4·5H2O).
6.4 Ethyl ether (C4H10O).
6.5 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.6 Phosphoric acid solution, 19.
6.7 Sulfuric acid solution, 14.
6.8 Sodium hydroxide solution. ρ (NaOH) = 100 g/L. Weigh 10 g of sodium hydroxide dissolved in water and dilute to 100 ml.
6.9 Potassium bromate-potassium bromide solution. c (1/6 KBrO3) = 0.1 mol/L. Weigh 2.784 g of potassium bromate dissolved in water, add 10 g of potassium bromide, dissolve
After dissolving, transfer to a 1 000 ml volumetric flask and dilute to the mark with water.
6.10 Sodium thiosulfate solution. c (Na2S2O3) ≈ 0.012 5 mol/L. Weigh 3.1 g of sodium thiosulfate, dissolve in boiling water, add
Add 0.2 g of sodium carbonate, dissolve it, transfer it to a 1 000 ml volumetric flask, and dilute to the mark with water. Before use, it is calibrated according to GB 7489-87 method.
6.11 Starch solution. Weigh 1 g of soluble starch, make a paste with a small amount of water, add boiling water to 100 ml, cool, and transfer to the reagent bottle.
Store in the refrigerator.
6.12 methyl orange indicator solution. ρ (methyl orange) = 0.5 g/L. Weigh 0.1 g of methyl orange dissolved in water, dissolve it and transfer it to a.200 ml volumetric flask.
Dilute to the mark with water.
6.13 Starch-potassium iodide test paper. Weigh 1.5 g of soluble starch, stir it into a paste with a small amount of water, add.200 ml of boiling water, mix and let cool.
Add 0.5 g potassium iodide and 0.5 g sodium carbonate, dilute to 250 ml with water, immerse the filter paper strip, take it out and dry it in a brown bottle.
Save the plug.
6.14 Lead acetate test paper. Weigh 5 g of lead acetate, dissolve in water, and dilute to 100 ml. Dip the filter paper into the above solution and take it after 1 h.
Dry out, in a jar, preserved.
6.15 pH test paper. 1 to 14.
7 Instruments and equipment
Unless otherwise stated, this standard uses glass gauges that meet national Class A standards.
7.1 Balance. Accuracy 0.000 1 g.
7.2 Common instruments in general laboratories.
8 samples
8.1 Sample Collection
Sample collection is performed in accordance with the relevant regulations of HJ/T 91.
At the sample collection site, the starch-potassium iodide test paper (6.13) was used to detect the presence or absence of oxidants such as free chlorine in the sample. If the test paper changes
Blue, should be added in time to remove excess ferrous sulfate (6.1).
The sample collection should be greater than 500 ml and stored in a hard glass bottle.
The collected sample should be acidified to a pH of about 4.0 in time, and an appropriate amount of copper sulfate (6.3) is added to make the mass concentration of copper sulfate in the sample about
It is 1 g/L to inhibit the biooxidation of phenols by microorganisms.
8.2 Sample storage
The collected samples should be refrigerated at 4 ° C and measured within 24 h.
9 Analysis steps
9.1 Pre-distillation
Transfer 250 ml of the sample into a 500 ml full glass distiller, add 25 ml of water, add several glass beads to prevent bumping, add a few drops of methyl
Orange indicator solution (6.12). If the sample is not orange-red, continue to add phosphoric acid solution (6.6).
Connect the condenser, heat the distillation, and collect 250 ml of distillate into the volumetric flask.
During the distillation process, if the methyl orange red color is found to fade, it should be allowed to cool after the end of the distillation, and then add 1 drop of methyl orange indicator solution (6.12).
If the residue is not acidic after distillation, it should be resampled, and the amount of phosphoric acid solution (6.6) added is increased to carry out distillation.
Note 1. The entire distillation equipment should be cleaned before and after each test.
Note 2. Do not use rubber stoppers or rubber hoses to connect the distillation flask and condenser to prevent interference with the measurement.
9.2 Bromination titration
Divide 100 ml of distillate into an iodine flask, add 5.0 ml of hydrochloric acid (6.5), slowly shake the iodine bottle, and add bromic acid dropwise with a 5 ml burette.
The potassium-potassium bromide solution (6.9) was 3.00 ml, and the sample was bright yellow. If the sample is colorless or pale yellow, the sample should be diluted.
Quickly cap the stopper, mix and let stand for 15 min at room temperature.
Add 1 g of potassium iodide (6.2), cover with a stopper, mix and place in the dark for 5 min. Dissolve sodium thiosulfate with a 25 ml burette
After the solution (6.10) is light yellow, add 1 ml of starch solution (6.11) and continue to titrate until the blue color just fades. Record the dosage.
9.3 Blank test
Replace the sample with water and measure according to steps 9.1 to 9.2.
10 result calculation
The mass concentration of volatile phenol in the sample (calculated as phenol) is calculated according to formula (1).
ρ = 1 2( ) 15.68 1 000V V c
− × × × (1)
Where. ρ - mass concentration of volatile phenol in the sample, mg/L;
V1--the amount of sodium thiosulfate solution in the blank test, ml;
V2--the amount of sodium thiosulfate solution when titrating the sample, ml;
C--sodium thiosulfate solution concentration, mol/L;
V--sample volume, ml;
15.68 - phenol (1/6 C6H5OH) molar mass, g/mol.
When the calculation result is less than 10 mg/L, it is retained to 1 decimal place; when it is greater than or equal to 10 mg/L, three significant figures are retained.
11 Precision and accuracy
11.1 Precision
Five laboratories tested uniform samples with phenol concentrations of 10.0 mg/L and 25.0 mg/L.
The relative standard deviations in the experimental room were. 2.4% to 5.0%, 1.7% to 2.6%;
The relative standard deviations between laboratories were. 1.2%, 1.0%;
The repeatability limits were. 1.0 mg/L, 1.3 mg/L;
Reproducibility limits were. 0.9 mg/L, 1.4 mg/L.
11.2 Accuracy
Five laboratories measured standard substances with phenol concentrations of 10.0 mg/L and 25.0 mg/L.
The relative errors are. −5.0% to −2.0%, −4.4% to −2.4%;
The relative error final values are. −3.4% ± 2.3%, −3.7% ± 2.0%.
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