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HJ 503-2009 English PDF

HJ 503-2009_English: PDF (HJ503-2009)
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HJ 503-2009English339 Add to Cart 3 days [Need to translate] Water quality. Determination of volatile phenolic compounds. 4-AAP spectrophotometric method Valid HJ 503-2009
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BASIC DATA
Standard ID HJ 503-2009 (HJ503-2009)
Description (Translated English) Water quality. Determination of volatile phenolic compounds. 4-AAP spectrophotometric method
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Classification of International Standard 13.060
Word Count Estimation 13,129
Date of Issue 2009-10-20
Date of Implementation 2009-12-01
Older Standard (superseded by this standard) GB/T 7490-1987
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 surface water, groundwater, drinking water, industrial wastewater and domestic sewage volatile phenols 4 amino antipyrine spectrophotometric method.


HJ 503-2009 Water quality.Determination of volatile phenolic compounds. 4-AAP spectrophotometric method HJ National Environmental Protection Standard of the People's Republic Replace GB 7490-87 Determination of volatile phenols in water 4-aminoantipyrine spectrophotometry Water quality-Determination of volatile phenolic compounds -4-AAP spectrophotometric 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); 2. Determination of brominated volume of volatile phenols in water (HJ 502-2009); 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 Method 1 Extraction Spectrophotometry 4 method principle..1 5 interference and elimination.1 6 reagents and materials. 2 7 instruments and equipment.3 8 samples.3 9 Analysis steps..3 10 result calculation 4 11 Precision and Accuracy 4 12 Quality Assurance and Quality Control.5 Method 2 Direct spectrophotometry 13 Principle of the method 5 14 Interference and elimination..5 15 Reagents and materials..5 16 Instruments and Equipment..5 17 samples. 5 18 Analysis Step 5 19 result calculation 6 20 Precision and Accuracy 6 21 Quality Assurance and Quality Control.6 Appendix A (Normative) Calibration of phenol stocks 7 Appendix B (informative) 4-Aminoantipyrine purification.8 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 spectrophotometric method for the determination of volatile phenols in surface water, groundwater, drinking water, industrial wastewater and domestic sewage. This standard is a revision of the "4-aminoantipyrine spectrophotometric method for the determination of volatile phenols in water" (GB 7490-87). 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. -- Expanded the scope of application of the standard and clarified the applicable objects of the standard; - Increased the optical path of the extraction spectrophotometric cuvette, reducing the detection limit; - Improved the purification method of 4-aminoantipyrine and increased the purification method of phenol; -- Added quality assurance and quality control provisions. 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 4-Aminoantipyrine spectrophotometric method after distillation (GB 7490-87) was abolished. 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. 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 Determination of volatile phenols in water 4-aminoantipyrine spectrophotometry Warning. Ether is a low boiling, flammable and anesthetic organic solvent. There should be no open flame around and be ventilated. In the cabinet operation, when the room temperature is high, the sample and ether should be cooled in the ice bath first, then the extraction operation should be carried out as soon as possible; Alkanes are anesthetic and irritating organic solvents that are harmful to inhalation of vapors. Wear a gas mask and keep them in a ventilated place. use. 1 Scope of application This standard specifies 4-aminoantipyrine fractions for the determination of volatile phenols in surface water, groundwater, drinking water, industrial wastewater and domestic sewage. Photometric method. Surface water, groundwater and drinking water should be determined by extraction spectrophotometry. The detection limit is 0.000 3 mg/L, and the lower limit of determination is 0.001 mg/L. The upper limit of determination is 0.04 mg/L. Industrial wastewater and domestic sewage should be determined by direct spectrophotometry. The detection limit is 0.01 mg/L, and the lower limit of determination is 0.04 mg/L. The upper limit is 2.50 mg/L. For samples with a mass concentration higher than the upper limit of the standard measurement, the sample may be appropriately diluted. 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 It is distilled with water vapor and can react with 4-aminoantipyrine to form a volatile phenolic compound of a colored compound, and the result is based on phenol. Method 1 Extraction Spectrophotometry 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. The distilled phenolic compound reacts with 4-aminoantipyrine in the presence of potassium ferricyanide in a pH (10.0 ± 0.2) medium. The orange-red antipyrine dye was produced and extracted with chloroform and the absorbance was measured at 460 nm. 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 (6.23), indicating the presence of oxidant, and an excess of ferrous sulfate (6.2) 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 (6.24). If the test paper turns black, it indicates that there is a sulfide. presence. At this time, the sample was further added with phosphoric acid, and the aeration chamber was stirred and aerated until the generated hydrogen sulfide completely escaped. 5.3 Elimination of organic or inorganic reducing substances such as formaldehyde and sulfite The appropriate amount of the sample can be separated into a separatory funnel, and the sulfuric acid solution (6.11) is added to make it acidic, and 50, 30, and 30 ml of diethyl ether (6.5) 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 (6.12) in portions to carry out back extraction. The phenols are transferred to a sodium hydroxide solution. Combine the alkali extract, transfer to a beaker, warm on a water bath to remove residual ether, then use water (6.1) Dilute the alkali extract to the original sample volume. At the same time, water (6.1) 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 phenol-free water. phenol-free water can be prepared according to 6.1.1 or 6.1.2. Phenolic-free water should be stored in glass bottles. When used, avoid with rubber. The product (rubber plug or latex tube, etc.) is in contact. 6.1.1 Add 0.2 g of activated carbon powder activated at.200 ° C for 30 min per liter of water, shake well, place overnight, and use double-layer medium speed. Filter paper filter. 6.1.2 Add sodium hydroxide to make the water strong alkaline, and add potassium permanganate until the solution is purple-red, and transfer it to the whole glass distiller for heating and distillation. Collect the distillate for use. 6.2 Ferrous sulfate (FeSO4·7H2O). 6.3 Potassium iodide (KI). 6.4 Copper sulfate (CuSO4·5H2O). 6.5 Ethyl ether (C4H10O). 6.6 Trichloromethane (CHCl3). 6.7 Refined phenol. Take phenol (C6H5OH) in a distillation flask with an air condenser, heat and distill it, and collect the distillation at 182-184 °C. After the fraction is cooled, the fraction should be colorless crystals, stored in a brown bottle, and sealed in a cool dark place. 6.8 Ammonia. ρ (NH3·H2O) = 0.90 g/ml. 6.9 Hydrochloric acid. ρ (HCl) = 1.19 g/ml. 6.10 Phosphoric acid solution, 19. 6.11 Sulfuric acid solution, 14. 6.12 Sodium hydroxide solution. ρ (NaOH) = 100 g/L. Weigh 10 g of sodium hydroxide dissolved in water and dilute to 100 ml. 6.13 Buffer solution. pH = 10.7. Weigh 20 g of ammonium chloride (NH4Cl) dissolved in 100 ml of ammonia water (6.8), stuffed in a refrigerator, and placed in the refrigerator. save. In order to avoid the change of pH caused by the volatilization of ammonia, it should be stored at low temperature, and it should be closed immediately after use, and Formulated in appropriate amount. 6.14 4-aminoantipyrine solution. Weigh 2 g of 4-aminoantipyrine dissolved in water, dissolved and transferred to a 100 ml volumetric flask. Release to the marking line, purify according to Appendix B, collect the filtrate and store in the refrigerator for 7 days. 6.15 Potassium ferricyanide solution. ρ (K3[Fe(CN)6]) = 80 g/L. Weigh 8 g of potassium ferricyanide dissolved in water, dissolve it and transfer it to a 100 ml volumetric flask. Dilute to the mark with water. Store in the refrigerator for one week. 6.16 Potassium bromate-potassium bromide solution. c (1/6KBrO3) = 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. 6.17 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. 6.18 Starch solution. ρ = 0.01 g/ml. Weigh 1 g of soluble starch, make a paste with a small amount of water, add boiling water to 100 ml, and after cooling, Transfer to the reagent bottle and store in the refrigerator. 6.19 phenol standard stock solution. ρ (C6H5OH) ≈ 1.00 g/L. Weigh 1.00 g of refined phenol (6.7), dissolve in water (6.1), and transfer Dilute to the mark with water (6.1) in a 1 000 ml volumetric flask. Calibrate according to Appendix A. Refrigerated in the refrigerator for stable storage for one month. 6.20 Phenol standard intermediate. ρ (C6H5OH) = 10.0 mg/L. Take appropriate amount of phenol standard stock solution (6.19) and dilute to 100 ml with water (6.1) In the volumetric flask, it is prepared on the same day of use. 6.21 Phenol standard use solution. ρ (C6H5OH) = 1.00 mg/L. Measure 10.00 ml of phenol standard intermediate (6.20) in a 100 ml volumetric flask In the middle, dilute to the mark with water (6.1) and use it within 2 hours after preparation. 6.22 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. 6.23 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 well, 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. 6.24 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. 6.25 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 Spectrophotometer. 460 nm wavelength with a cuvette with an optical path of 30 mm. 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 (6.23) 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 (6.2). The sample collection should be greater than 500 ml and stored in a hard glass bottle. The sample after collection should be acidified to pH about 4.0 in time, and an appropriate amount of copper sulfate (6.4) 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 sample into 500 ml full glass distiller, add 25 ml water (6.1), add several glass beads to prevent bumping, add more Drop the methyl orange indicator solution (6.22). If the sample is not orange-red, continue to add phosphoric acid solution (6.10). 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 (6.22). If the residue is not acidic after distillation, it should be resampled, and the amount of phosphoric acid solution (6.10) added is increased to carry out distillation. Note 1. The distillation equipment used should not be mixed with distillation equipment for measuring industrial wastewater or domestic sewage. The entire distillation unit 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 Color rendering Transfer 250 ml of distillate into a separatory funnel, add 2.0 ml of buffer solution (6.13), mix, pH 10.0 ± 0.2, add 1.5 ml 4-aminoantipyrine solution (6.14), mix well, add 1.5 ml potassium ferricyanide solution (6.15), mix well, close the plug, place 10 min. 9.3 Extraction Accurately add 10.0 ml of chloroform (6.6) in the above-mentioned color development (9.2) separatory funnel, tightly shake, shake vigorously for 2 min, and place it upside down. Gas, standing layered. Dry the inner wall of the neck of the separatory funnel with dry absorbent cotton or filter paper, and stuff a small group of dry absorbent cotton or filter paper into the neck tube to dichlorochloride. The methane layer is passed through a dry skim cotton or filter paper, and after discarding the first few drops of the extract, the remaining chloroform is directly placed into the optical path of 30. Mm in the cuvette. 9.4 Absorbance measurement The absorbance of the chloroform layer was determined at 460 nm using chloroform (6.6) as a reference. 9.5 Blank test Replace the sample with water (6.1) and measure the absorbance according to steps 9.1 to 9.4. The blank should be measured simultaneously with the sample. 9.6 Calibration 9.6.1 Preparation of the calibration series Add 100 ml of water (6.1) to a set of 8 separatory funnels, and add 0.00, 0.25, 0.50, 1.00, 3.00, 5.00, 7.00 and 10.00 ml of phenol standard solution (6.21), then add water (6.1) to 250 ml. The measurement was carried out in accordance with the steps 9.2 to 9.4. 9.6.2 Drawing of the calibration curve The absorbance value measured by the calibration series is subtracted from the absorbance value of the zero-concentration tube, and the curve of the absorbance value to the phenol content (μg) is plotted. The correlation coefficient of the quasi-curve regression equation should be above 0.999. 10 result calculation The mass concentration of volatile phenol in the sample (calculated as phenol) is calculated according to formula (1). ρ = s bA A a bV − − (1) Where. ρ - mass concentration of volatile phenol in the sample, mg/L; As--the absorbance value of the sample; Ab--absorbance value of blank test (9.5); A--the intercept value of the calibration curve (9.6.2); B--the slope of the calibration curve (9.6.2); V--the volume of the sample, ml. When the calculated result is less than 0.1 mg/L, it is retained to four decimal places; when it is greater than or equal to 0.1 mg/L, three significant figures are retained. 11 Precision and accuracy 11.1 Precision Five laboratories measured uniform samples containing phenolic concentrations of 0.004 0, 0.020 0, and 0.036 0 mg/L. The relative standard deviations in the experimental room were. 7.4% to 10.1%, 3.3% to 4.5%, and 1.8% to 2.3%; The relative standard deviations between laboratories were. 2.9%, 2.3%, 1.3%; The repeatability limits were. 0.001 0 mg/L, 0.002 3 mg/L, 0.002 0 mg/L; The reproducibility limits were. 0.001 0 mg/L, 0.002 3 mg/L, and 0.001 8 mg/L, respectively. 11.2 Accuracy Five laboratories measured standard substances with a phenol concentration of (45.5 ± 3.6) μg/L. The relative error is. −2.6% to 3.5%; The final error is. 1.8% ± 5.0%. 12 Quality Assurance and Quality Control Each batch of samples should have an intermediate checkpoint, and the relative error of the measured value of the intermediate checkpoint and the corresponding point of the calibration curve should not exceed 10%. Method 2 Direct spectrophotometry 13 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. The distilled phenolic compound reacts with 4-aminoantipyrine in the presence of potassium ferricyanide in a pH (10.0 ± 0.2) medium. An orange-red antipyrine dye is produced. After color development, the absorbance was measured at 510 nm in 30 min. 14 interference and elimination See 5. 15 Reagents and materials See 6. 16 Instruments and equipment 16.1 Spectrophotometer. 510 nm wavelength with a cuvette with an optical path of 20 mm. 16.2 Common instruments used in general laboratories. 17 samples See 8. 18 Analysis steps 18.1 Pre-distillation See 9.1. 18.2 Color development Distill 50 ml of the distillate into a 50 ml colorimetric tube, add 0.5 ml of buffer solution (6.13), and mix, at this time, the pH value is 10.0±0.2. Add 1.0 ml of 4-aminoantipyrine solution (6.14), mix well, add 1.0 ml of potassium ferricyanide solution (6.15), mix well, close the plug, Leave for 10 min. 18.3 Absorbance measurement At 510 nm, the absorbance of the solution was measured in 30 min using a cuvette with an optical path of 20 mm with water (6.1) as a reference. Degree value. 18.4 Blank test Replace the sample with water (6.1) and measure the absorbance according to the procedure of 18.1 to 18.3. The blank should be measured simultaneously with the sample. 18.5 Calibration 18.5.1 Preparation of the calibration series Add 0.00, 0.50, 1.00, 3.00, 5.00, 7.00, 10.00 and 12.50 ml of phenol to a set of 8 50 ml colorimetric tubes Standard intermediate solution (6.20), add water (6.1) to the marking line. The measurement was carried out in accordance with the procedures of 18.2 to 18.3. 18.5.2 Drawing of the calibration curve The absorbance value measured by the calibration series is subtracted from the absorbance value of the zero concentration tube, and the curve of the absorbance value to the phenol content (mg) is plotted. The correlation coefficient of the quasi-curve regression equation should be above 0.999. 19 Calculation of results The mass concentration of volatile phenol in the sample (calculated as phenol) is calculated according to formula (2). ρ = sb 1 000A A a bV − − × (2) Where. ρ--the mass concentration of volatile phenol in the sample, mg/L; As--the absorbance value of the sample; Ab--absorbance value of the blank test (18.4); A--the intercept value of the calibration curve (18.5.2); B--the slope of the calibration curve (18.5.2); V--the volume of the sample, ml. When the calculation result is less than 1 mg/L, it is retained to 3 digits after the decimal point; when it is greater than or equal to 1 mg/L, three significant digits are retained. 20 precision and accuracy 20.1 Precision Five laboratories tested uniform samples with phenol concentrations of 0.25, 1.25 and 2.25 mg/L. The relative standard deviations in the laboratory are. 2.0% to 2.1%, 0.6% to 0.9%, and 0.4% to 0.6%; The relative standard deviations between laboratories were. 2.2%, 0.4%, 0.2%; The repeatability limits were. 0.01 mg/L, 0.02 mg/L, 0.03 mg/L; Reproducibility limits were. 0.02 mg/L, 0.03 mg/L, 0.03 mg/L. 20.2 Accuracy Five laboratories measured standard substances with a phenol concentration of (1.21 ± 0.05) mg/L. The relative error is. −1.7%~0.8%; The final value of the relative error is −0.5%±1.8%. 21 Quality Assurance and Quality Control Each batch of samples should have an intermediate checkpoint, and the relative error of the measured value of the intermediate checkpoint and the corresponding point of the calibration curve should not exceed 10%. Appendix A (normative a... ......