HJ 592-2010 English PDFUS$339.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 592-2010: Water quality. Determination of nitrobenzene-compounds by gas chromatography Status: Valid
Basic dataStandard ID: HJ 592-2010 (HJ592-2010)Description (Translated English): Water quality. Determination of nitrobenzene-compounds by gas chromatography Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z23 Classification of International Standard: 13.060.30 Word Count Estimation: 13,192 Date of Issue: 2010-10-21 Date of Implementation: 2011-01-01 Older Standard (superseded by this standard): GB 4919-1985 Regulation (derived from): Department of Environmental Protection Notice No. 77 of 2010 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the nitrobenzene compounds in water by gas chromatography. This standard applies to industrial wastewater and domestic sewage in the determination of nitrobenzene compounds. When the sample volume is 500ml, the method detection limit, detection limit and determination limit, see Table 1. HJ 592-2010: Water quality. Determination of nitrobenzene-compounds by gas chromatography---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.Water quality.Determination of nitrobenzene-compounds by gas chromatography National Environmental Protection Standard of the People's Republic Replace GB 4919-85 Determination of water quality nitrobenzene compounds Gas chromatography Water quality-Determination of nitrobenzene-compounds By gas chromatography Released on.2010-10-21 2011-01-01 Implementation Ministry of Environmental Protection released Ministry of Environmental Protection announcement No. 77 of.2010 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 ambient air ozone. Six standards, such as the fixed ultraviolet photometry, are national environmental protection standards and are released. The standard name and number are as follows. 1. Determination of ambient air ozone by ultraviolet photometry (HJ 590-2010); 2. Determination of water quality pentachlorophenols by gas chromatography (HJ 591-2010); 4. Determination of water quality, elemental phosphorus, phosphorus molybdenum blue spectrophotometry (provisional) (HJ 593-2010); 5. Determination of the total amount of water-based developer and its oxides - Iodine-starch spectrophotometry (interim) (HJ 594-2010); 6. Determination of the total amount of water color developing agent 169 Coupler spectrophotometry (provisional) (HJ 595-2010). The above standards have been implemented since January 1,.2011 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection. From the date of implementation of the above standards, the following three national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished. The name and number are as follows. 1. Determination of ambient air ozone by ultraviolet spectrophotometry (GB/T 15438-1995); 2. Determination of water quality pentachlorophenols by gas chromatography (GB 8972-88); 3. Determination of Total Nitro Compounds in Industrial Wastewater Gas Chromatography (GB 4919-85). Special announcement. October 21,.2010 ContentForeword..iv 1 Scope..1 2 Method principle..1 3 reagents and materials.1 4 instruments and equipment. 2 5 samples. 2 6 Analysis steps..3 7 Calculation and representation of results..4 8 precision and accuracy..4 9 Quality Assurance and Quality Control 5 Appendix A (Normative Appendix) Sample Purification..6 Appendix B (informative) Precision and accuracy of the method 7 IvForewordTo 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 This standard is formulated for the determination of nitrobenzene compounds in industrial wastewater and domestic sewage. This standard specifies gas chromatography for the determination of nitrobenzene compounds in industrial wastewater and domestic sewage. This standard is a revision of the "Gas Chromatography for the Determination of Total Nitro Compounds in Industrial Wastewater" (GB 4919-85). This standard was first published in 1985. The original standard drafting unit was the Fifth Design Institute of the Ministry of Weapons Industry and the State-owned Qingyang Chemical Plant. This time is First revision. The main contents of the revision are as follows. -- Amend the standard name to "Gas Chromatography for the Determination of Water Nitrobenzene Compounds"; - replacing the packed column with a capillary column; -- changed the extraction solvent and dosage; - modified the quantitative method of nitrobenzene compounds; - Modified the method for determination of 2,4,6-trinitrobenzoic acid; -- Added quality assurance and quality control provisions. From the date of implementation of this standard, the national environmental protection standard “Industry” approved and issued by the former State Environmental Protection Administration on August 1, 1985 Determination of Total Nitro Compounds in Wastewater Gas Chromatography (GB 4919-85) is 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. Qingdao Environmental Monitoring Center Station. This standard is verified by. Jinan Environmental Protection Monitoring Station, Zibo Environmental Monitoring Station, Weifang Environmental Monitoring Center Station, Qingdao Institute of Technology College of Environmental and Municipal Engineering, Agricultural Products Supervision and Inspection Center of the Ministry of Agriculture (Qingdao). This standard was approved by the Ministry of Environmental Protection on October 21,.2010. This standard has been implemented since January 1,.2011. This standard is explained by the Ministry of Environmental Protection. Water quality - Determination of nitrobenzene compounds - Gas chromatography1 Scope of applicationThis standard specifies the gas chromatography of nitrobenzene compounds in water. This standard applies to the determination of nitrobenzene compounds in industrial wastewater and domestic sewage. When the sample volume is 500 ml, the detection limit, lower limit of determination and upper limit of determination of the method are shown in Table 1. Table 1 Method detection limit and upper limit and lower limit unit. mg/L Compound name detection limit determination lower limit upper limit Nitrobenzene 0.002 0.008 2.8 O-nitrotoluene 0.002 0.008 2.4 m-Nitrotoluene 0.002 0.008 2.4 p-Nitrotoluene 0.002 0.008 2.0 2,4-Dinitrotoluene 0.002 0.008 2.8 2,6-dinitrotoluene 0.002 0.008 2.0 2,4,6-trinitrotoluene 0.003 0.012 2.0 1,3,5-trinitrobenzene 0.003 0.012 2.4 2,4,6-trinitrobenzoic acid 0.003 0.012 2.02 Principle of the methodThe nitrobenzene compound in water is extracted with dichloromethane, and the extract is dehydrated and concentrated, and then subjected to a gas chromatography hydrogen flame ionization detector. The measurement was carried out. 2,4,6-trinitrobenzoic acid is highly water-soluble and is converted to 1,3,5-trinitrobenzene upon heating. Therefore, after extracting dichloromethane The aqueous phase was heated and the 2,4,6-trinitrobenzoic acid was separately determined by extraction with dichloromethane.3 reagents and materialsAnalytical purification reagents conforming to national standards were used for the analysis, and the experimental water was freshly prepared distilled water unless otherwise stated. 3.1 Concentrated sulfuric acid (H2SO4). ρ = 1.84 g/ml. 3.2 Dichloromethane (CH2Cl2). Pure by liquid chromatography. 3.3 Ethyl acetate (C4H8O2). pure by liquid chromatography. 3.4 anhydrous sodium sulfate (Na2SO4). Before use, burn in a 350 ° C muffle furnace for 4 h, cool to room temperature, and place in a glass bottle for use. 3.5 nitrobenzene compound standard solution. ρ = 1.00 mg/ml. Store at 4 ° C in the dark. Commercially available certified standards can be used. 3.6 2,4,6-trinitrobenzoic acid. powdered solid particles, purity > 98.5%. 3.7 2,4,6-trinitrobenzoic acid standard solution. ρ = 1.00 mg/ml. Dissolve with ethyl acetate (3.3) during use, prepare a standard solution of ρ=1.00 mg/ml, and store at 4°C in the dark. effective. 3.8 Carrier gas. nitrogen, purity ≥ 99.99% (volume fraction). 3.9 Combustion gas. hydrogen, purity ≥ 99.99% (volume fraction). 3.10 Gas. Air.4 Instruments and equipment4.1 Gas chromatograph. with hydrogen flame ionization detector. 4.2 Column. quartz capillary column, 30 m × 0.32 mm (inside diameter) × 0.25 μm (film thickness), the stationary phase is 5% phenyl-95% A Polysiloxane. Or other equivalent capillary column. 4.3 Rotary evaporator. 4.4 Nitrogen blowing instrument. 4.5 Adjustable temperature electric furnace or electric heating plate. 4.6 Separating funnel. 500 ml. 4.7 Erlenmeyer. 1 000 ml. 4.8 Microinjector. 10 μl. 4.9 Sampling bottle. 1 000 ml brown glass bottle with ground plug. 4.10 Common instruments and equipment used in general laboratories.5 samples5.1 Sample collection and preservation Collect 1 000 ml of sample in the sampling bottle. If the water sample cannot be measured within 24 h, add concentrated sulfuric acid (3.1) to adjust pH≤3. kind The product must be extracted within 7 days, and the extract should be stored in the dark at 4 ° C. It should be analyzed within 30 days. 5.2 Preparation of samples 5.2.1 Extraction of nitrobenzene compounds (except 2,4,6-trinitrobenzoic acid) Measure 500 ml of sample (when the content is high, take as little as possible) in a separatory funnel, add 25 ml of dichloromethane (3.2), shake for 3 min. (Exhaust 2~3 times), after standing for 3 min, collect the lower extract in a triangular flask; repeat the extraction once and combine the extracts. Extract After dehydration of anhydrous sodium sulfate (3.4), the volume was adjusted to 1 ml by a rotary evaporator and a nitrogen blower to be analyzed. After extracting twice with dichloromethane The aqueous phase was transferred to a 1 000 ml Erlenmeyer flask. 5.2.2 Extraction of 2,4,6-trinitrobenzoic acid The above 1 000 ml Erlenmeyer flask was placed in an electric furnace or a hot plate and heated to boil for 20 min, and then cooled to room temperature. Repeat 5.2.1 Procedure, 2,4,6-trinitrobenzoic acid to be determined. Note 1. The experimental procedure should be operated in a fume hood. Note 2. During the boiling process of step 5.2.2, the heating temperature should not be too high to avoid violent boiling; when the water sample is less than 500 ml, the water should be kept during heating. The amount is not less than 100 ml. Note 3. For high-quality sewage and wastewater samples, water samples should be taken less or directly without concentration. Determination of samples affected by chromatographic analysis, water samples It should be cleaned after taking it. See Appendix A for the operation steps.6 Analysis steps6.1 Chromatographic Analysis Reference Conditions Column temperature. 60 ° C for 4 min, 20/min ° C to 220 ° C, for 3 min; detector temperature. 250 ° C; vaporization Room temperature. 230 ° C; carrier gas flow rate. 1 ml/min; hydrogen flow. 30 ml/min; air flow. 400 ml/min; tail gas flow. 20 Ml/min; injection method. splitless injection, split 0.5 min after injection, split ratio is 30.1; injection volume. 1.0 μl. 6.2 Calibration 6.2.1 Drawing of standard curve Diluting each nitrobenzene compound standard solution (3.5) with methylene chloride (3.2) to a mass concentration of 5, 10, 20, 40, 60 and 120 μg/ml mixed standard series, respectively, 1.0 μl of the standard series solution is injected into the gas chromatograph inlet, according to the quality of each component A standard curve is drawn for the degree and peak area (or peak height). 6.2.2 Standard chromatogram A reference chromatogram of each nitrobenzene compound is shown in Figure 1. pA 2 4 6 8 10 min 1-dichloromethane; 2-nitrobenzene; 3-o-nitrotoluene; 4-m-nitrotoluene; 5-p-nitrotoluene; 6-2,6-dinitrotoluene; 7-2,4-dinitrotoluene; 8-1,3,5-trinitrobenzene; 9-2,4,6-trinitrotoluene Figure 1 Standard chromatogram of nitrobenzene compounds 6.3 Determination A 1.0 μl sample (5.2) was injected into the gas chromatograph using a microsyringe and assayed under the same chromatographic conditions as the standard curve. Record the retention time and peak area (or peak height) of the chromatographic peak. 6.4 Blank test While the sample is being analyzed, a blank test should be performed. That is, the test water is used instead of the water sample, and the analysis is performed in the same manner as the sample measurement.7 Calculation and representation of results7.1 Calculation of results 7.1.1 Calculation of results for nitrobenzene compounds (except 2,4,6-trinitrobenzoic acid) The components of the nitrobenzene compound in the sample (except 2,4,6-trinitrobenzoic acid) were calculated according to the formula (1). Ρρ ×= standard (1) Where. iρ - mass concentration of a certain nitrobenzene compound in the sample, mg/L; ρ standard--the mass concentration calculated from the standard curve, mg/L; 1V - the volume of the volume after concentration of the extract, ml; V -- water sample volume, ml. 7.1.2 Calculation of the results of 2,4,6-trinitrobenzoic acid The 2,4,6-trinitrobenzoic acid in the sample was calculated according to the formula (2). 1 1.21V Ρρ × ×= standard (2) Where. ρ--the mass concentration of 2,4,6-trinitrobenzoic acid in the sample, mg/L; ρ standard--the mass concentration of 1,3,5-trinitrobenzene calculated from the standard curve, mg/L; 1V - the volume of the volume after concentration of the extract, ml; V - water sample volume, ml; The ratio of the relative molecular mass of 1.21--2,4,6-trinitrobenzoic acid to 1,3,5-trinitrobenzene. 7.2 Results representation When the sample content is less than 1 mg/L, the result is retained to the third decimal place; when the sample content is greater than or equal to 1 mg/L, the result is guaranteed. Leave three valid numbers.8 precision and accuracy8.1 Precision Five laboratories tested uniform samples containing nitrobenzene compounds at concentrations of 0.020 mg/L and 0.100 mg/L. The relative standard deviations in the experimental room were. 2.1% to 9.4%, 0.55% to 6.2%; The relative standard deviations between laboratories are. 2.5% to 9.8%, 4.0% to 8.8%; The repeatability limit r is. 0.002 ~ 0.003 mg/L, 0.007 ~ 0.011 mg/L; Reproducibility limits R are. 0.002 to 0.006 mg/L, and 0.015 to 0.026 mg/L, respectively. For detailed summary data on the specific target components, see Appendix B. 8.2 Accuracy Sampling analysis of uniform domestic sewage samples containing nitrobenzene compounds with a concentration of 0.035 mg/L in 5 laboratories (scaling amount is 50.0 μg). Standard recovery rate. 81.2% ~ 94.0%; The final value of the spiked recovery was 81.2%±16.8%～94.0%±17.6%. For a summary of the accuracy of the specific target components, see Appendix B.9 Quality Assurance and Quality Control9.1 Qualitative analysis A retention time window of t ± 3S should be established prior to sample analysis. t is the average value of the retention time of each concentration level of the reference material at the initial calibration, S is the standard deviation of the retention time of each reference material at the initial calibration. When the sample is analyzed, the target compound retention time should be in the retention time window. In the mouth. 9.2 Blank test Make at least one blank sample and blank spiked sample for each batch of samples. The blank sample is analyzed and measured using the same method as the actual sample. The compound concentration should be below the detection limit. The recovery rate of the blank sample should be controlled at 80% to 120%. 9.3 The correlation curve of the standard curve should be greater than or equal to 0.995, otherwise the standard curve should be redrawn. 9.4 Intermediate concentration test The intermediate concentration test shall be carried out during sample analysis. The relative deviation between the measured value of the intermediate concentration and the value of the curve shall be less than or equal to 15%, otherwise A new standard curve should be established. 9.5 Matrix addition At least one matrix spiked sample shall be prepared for each batch of samples. The matrix spiked sample and the actual sample shall be analyzed and determined by the same method. The recovery rate should be controlled at 70% to 130%.Appendix A(normative appendix) Sample purification A.1 Instruments and equipment A.1.1 Column. 300 mm (column length) × 10 mm (inner diameter) glass column with a coarse-pored glass core and a Teflon piston at the bottom. A.1.2 muffle furnace. A.1.3 Oven. A.1.4 Dryer. A.2 Reagents and materials A.2.1 n-Hexane (C6H14). pure by liquid chromatography. A.2.2 Acetone (C3H6O). Pure by liquid chromatography. A.2.3 anhydrous sodium sulfate (Na2SO4). burn in a muffle furnace at 350 ° C for 4 h before use, cool to room temperature, and put into a glass bottle for use. A.2.4 Silica-magnesium type adsorbent. for chromatography (60-100 mesh), purchase 677 °C activated product, stored in a glass stopper or belt with a grinding A screw-covered glass container lined with a PTFE mat. Activation of the silica-magnesium type adsorbent. the silicon-magnesium-type adsorbent is placed in a large porcelain crucible and spread out, and the upper part of the porcelain crucible is covered with aluminum foil, and the crucible is placed. Into the oven, dry at 130 ° C for 16 h, then place the silica-magnesium adsorbent in a desiccator to cool to room temperature, then install the sealed glass Waiting for use in the bottle. A.3 Purification step A.3.1 Packing column 10 g of the activated silica-magnesium-type adsorbent (A.2.4) was placed in a 50 ml beaker, and an appropriate amount of dichloromethane-n-hexane (1 9) was added. A silicon magnesium type adsorbent is prepared as a suspension. Then pour the suspension into the column (A.1.1) and tap the column to fill the adsorbent. Then add 1 cm of anhydrous sodium sulfate (A.2.3) to the top and adjust the elution rate to about 2 ml/min. A.3.2 Solvent replacement The dichloromethane extract (5.2) was concentrated to 1 ml in a concentrate bottle, 4 ml of n-hexane was added to the concentrate bottle, and then concentrated to 1 ml. The solvent was replaced with n-hexane. A.3.3 Purification When the solvent in the column is released until the sodium sulfate layer is exposed, the extract (A.3.2) after replacing the solvent is transferred to the column, Rinse the concentrate bottle with 30 ml of dichloromethane-n-hexane (1 9), transfer the solution to the column, and collect the eluate until the sulfuric acid is just exposed. Sodium layer. The fraction of the eluent is eluent I, and the compound contained is m-nitrotoluene and p-nitrotoluene. Then, the column was eluted with 30 ml of acetone-dichloromethane (1 9), and the eluate was collected. The partial eluent is eluent II, containing The compounds are nitrobenzene, o-nitrotoluene, 2,6-dinitrotoluene, 2,4-dinitrotoluene, 1,3,5-trinitrobenzene, 2,4,6-trinitrate Base armor benzene. A.3.4 If the components of eluent I and eluent II need to be determined simultaneously, combine the eluent I and the eluent II, and concentrate to 1 ml. Analysis. Otherwise, eluent I and eluent II to 1 ml should be separately concentrated for analysis.Appendix B(informative appendix) Method precision and accuracy Schedule B.1 Precision measured by five laboratories Component Name Average/(mg/L) Relative standard in the experimental room deviation/% Relative standard between laboratories deviation/% Repeatability limit r/ (mg/L) Reproducibility limit R/ (mg/L) Nitrobenzene 0.018 2.6～9.4 9.0 0.003 0.005 0.101 1.9～5.0 6.7 0.011 0.021 O-nitrotoluene 0.019 2.9～9.2 9.5 0.003 0.006 0.102 1.2～5.4 8.4 0.010 0.026 M-nitrotoluene 0.019 2.1～9.2 8.3 0.003 0.005 0.100 0.75～3.9 6.2 0.008 0.019 P-nitrotoluene 0.019 2.2～7.7 4.8 0.003 0.004 0.101 1.9......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 592-2010_English be delivered?Answer: Upon your order, we will start to translate HJ 592-2010_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. 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