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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 777-2015: Ambient air and waste gas from stationary sources emission. Determination of metal elements in ambient particle matter. Inductively coupled plasma optical emission spectrometry Status: Valid
Basic dataStandard ID: HJ 777-2015 (HJ777-2015)Description (Translated English): Ambient air and waste gas from stationary sources emission. Determination of metal elements in ambient particle matter. Inductively coupled plasma optical emission spectrometry Sector / Industry: Environmental Protection Industry Standard Word Count Estimation: 24,267 Date of Issue: 2015-12-04 Date of Implementation: 2016-01-01 Quoted Standard: GB/T 16157; HJ/T 48; HJ/T 55; HJ 93; HJ/T 194; HJ/T 374; HJ/T 397; HJ 664; JJG 768 Regulation (derived from): Ministry of Environment Announcement 2015 No.81 Issuing agency(ies): Ministry of Ecology and Environment Summary: This Standard specifies the inductively coupled plasma measuring the air and exhaust particles of metal elements Emission Spectrometry. This Standard applies to the ambient air, fugitive emissions and stationary source emission particles of silver (Ag), aluminum (Al), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn), sodium (Na), a nickel (Ni), lead (Pb), antimony (Sb), tin (Sn), strontium (Sr), titanium (Ti), vanadium (V), zinc (Zn) and other 24 kinds of metal elements was measured. When the air sample volume of 150 m3 (standard conditions), sample source emission amount of 0.600 m3 (standard state dry flue gas), sample pretreatment volume volume of 50 ml, and the detection limit of the standard measurement of each metal element The lower limit in Appendix A. HJ 777-2015: Ambient air and waste gas from stationary sources emission. Determination of metal elements in ambient particle matter. Inductively coupled plasma optical emission spectrometry---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. Ambient air and waste gas from stationary sources emission. Determination of metal elements in ambient particle matter. Inventive coupled plasma optical emission spectrometry National Environmental Protection Standard of the People 's Republic of China Determination of Metallic Elements in Air and Waste Particulate Matter Inductively Coupled Plasma Atomic Emission Spectrometry Ambient air and waste gas from stationary sources emission-determination Metal elements in ambient particle matter-Inductively coupled plasma optical Emission spectrometry 2015-12-04 released 2016-01-01 Implementation Ministry of Environmental Protection released Directory Preface iii 1 Scope of application 1 2 normative reference document 1 Principle of Method 1 4 interference and elimination5 reagents and materials6 instruments and equipment7 samples .4 8 Analysis Step 5 9 Results Calculations and Representations 6 10 precision and accuracy 11 quality assurance and quality control 12 Waste treatment .8 13 Precautions .8 Appendix A (normative appendix) Element method detection limit and lower limit of measurement 9 Appendix B (informative) Recommended wavelengths for each element Appendix C (informative) Examples of Judgment and Interference Coefficients for Spectral and Matrix Interference Appendix D (informative) Method Precision and method Accuracy 13 Appendix E (informative) Other digestive systemsForewordIn 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 the Prevention and Control of Atmospheric Pollution, Standardize the health of the human body, regulate the ambient air and pollution sources of particulate matter in the determination of metal elements, the development of this standard. This standard specifies the inductively coupled plasma emission spectrometric method for the determination of metal elements in air and particulate matter. This standard is the first release. Appendix A, Appendix B, Appendix D and Appendix E of this Standard are informative appendices. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Sino-Japanese Friendship Environmental Protection Center (National Environmental Analysis and Testing Center). The standard verification unit. Shanghai Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Center, Australia real analysis and testing (Shanghai) limited Company, Chengdu Environmental Monitoring Center Station, Beijing Physical and Chemical Analysis and Testing Center, Beijing Environmental Protection Monitoring Center and National Geological Survey Test center. This standard is approved by the Ministry of Environmental Protection on December 4,.2015. This standard has been implemented since January 1,.2016. This standard is explained by the Ministry of Environmental Protection. Determination of Metallic Elements in Air and Waste Particulate Matter - Inductively Coupled Plasma Emission spectroscopy1 Scope of applicationThis standard specifies the inductively coupled plasma emission spectrometric method for the determination of metal elements in air and particulate matter. This standard applies to ambient air, unorganized emissions and fixed sources of waste particulate matter in silver (Ag), aluminum (Al), Arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), calcium (Ca), cadmium (Cd), cobalt (Co) Copper (Cu), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn), sodium (Na), nickel (Ni) (Sb), tin (Sn), strontium (Sr), titanium (Ti), vanadium (V), zinc (Zn) and other 24 kinds of metal elements. When the air sampling volume is 150 m3 (standard state), the pollution source gas sampling volume is 0.600 m3 (standard state dry flue gas) When the sample pretreatment volume is 50 ml, the detection limit and the determination limit of each metal element are shown in Appendix A.2 normative reference documentsThe contents of this standard refer to the following documents or their terms. Any annotated file that does not specify the date, its valid version Applicable to this standard. Determination of particulate matter and sampling method of gaseous pollutants in exhaust gas of fixed pollution sources GB/T 16157 HJ/T 48 smoke and dust sampler technical conditions Technical Guidelines for Unorganized Emissions Monitoring of Air Pollutants Technical Requirements and Test Methods for HJ 93 Environmental Air Particulate (PM10 and PM2.5) Sampler Technical specification for manual monitoring of ambient air quality Technical requirements and testing methods for HJ/T 374 total suspended particulate matter sampler Technical specification for HJ/T 397 fixed source exhaust gas monitoring HJ 664 ambient air quality monitoring point layout technical specifications (Trial) JJG 768 emission spectrometer verification procedures3 Principle of the methodWill be collected to the appropriate filter on the air and waste particulate samples by microwave digestion or electric plate digestion, with inductively coupled Plasma emission spectrometry (ICP-OES) was used to determine the content of each metal element. The digested sample is atomized into the atomizer of the plasma emission spectrometer and is carried by the argon carrier gas into the plasma torch , The target element is vaporized in the plasma torch, ionized, excited and radiated to the characteristic line. In a certain concentration range, The characteristic line intensity is proportional to the concentration of the element.4 interference and eliminationInductively Coupled Plasma Atomic Emission Spectroscopy usually exists in the interference can be divided into two categories. one is spectral interference, another One is non-spectral interference. 4.1 spectral interference Spectral disturbances mainly include continuous background and overlapping lines. The usual method of correcting spectral interference is the background subtraction method (According to the single element test to determine the location and manner of subtracting the background) and the interference coefficient method. It can also be mixed in standard solutions Using matrix matching method to eliminate its impact. When there is a single element interference, the interference factor can be obtained according to the following formula. Where. tK - interference coefficient; 'Q - interference element plus analysis element content; Q - analysis of the content of elements; TQ - the content of interfering elements. The Q & apos; was determined at the position of the wavelength of the analytical element by preparing a series of solutions of known interfering element content, Formula to find tK, and then artificial deduction or computer automatically deducted. Under normal circumstances, the atmospheric particulate matter in the concentration of each element is low, the interference between the spectral and matrix elements can be ignored slightly. Pollutants Particulate matter Common Target Metal Element Determination Wavelength Spectral interference and its interference coefficient Reference values are given in Appendix C. Note that the interferometric coefficients for different instruments are different. 4.2 Non-spectral interference Non-spectral interference mainly includes chemical interference, ionization interference, physical interference and solvent interference, etc., in the actual analysis The process of interference is difficult to completely separate. Whether it is compensated and corrected, and the concentration of interfering elements in the sample. this , The physical interference is generally caused by the viscosity of the sample and the surface tension changes, especially when the sample contains a large number of soluble Salt, the measurement may interfere. The easiest way to eliminate such interference is to dilute the sample.5 reagents and materialsUnless otherwise stated, all grades of pure or high purity (eg microelectronics) chemical reagents that meet national standards are used for analysis. The test water is deionized water or water with a specific resistance of ≥18 MΩ · cm. 5.1 nitric acid. ρ (HNO3) = 1.42 g/ml. 5.2 Hydrochloric acid. ρ (HCl) = 1.19 g/ml. 5.3 Hydrogen peroxide. ω (H2O2) = 30%. 5.4 hydrofluoric acid. ρ (HF) = 1.16 g/ml. 5.5 perchloric acid. ρ (HClO4) = 1.67 g/ml. 5.6 nitric acid - hydrochloric acid mixed digestion. 55.5 ml of nitric acid (5.1) and 167.5 ml (5.2) of hydrochloric acid were added to about 500 ml of water, diluted with water and allowed to settle to 1 L. 5.7 Nitric acid solution. 1 1. Add 500 ml nitric acid (5.1) to 400 ml of water, dilute with water and set to 1 L. 5.8 nitric acid solution. 1 9. Add 100 ml of nitric acid (5.1) to 400 ml of water, dilute with water and set to 1 L. 5.9 Nitric acid solution. 1 99 (standard series of blank solution). 10.0 ml of nitric acid (5.1) was added to 400 ml of water, diluted with water and allowed to settle to 1 L. 5.10 nitric acid solution. 2 98 (system washing solution). Add 20.0 ml of nitric acid (5.1) to 400 ml of water, dilute with water and set to 1 L. Mainly used for washing equipment Residues in the system. 5.11 hydrochloric acid solution. 1 1. Add 500 ml of hydrochloric acid (5.2) to 400 ml of water, dilute with water and set to 1 L. 5.12 hydrochloric acid solution. 1 4. Add.200 ml of hydrochloric acid (5.2) to 400 ml of water, dilute with water and set to 1 L. 5.13 standard solution. commercially available standard solution. Multi-element standard stock solution. ρ = 100 mg/L. Single element standard reserve Solution. ρ = 1000 mg/L. 5.14 quartz filter, Teflon filter or polypropylene and other organic filter. The particle size of more than 0.3 μm particles of the retention efficiency of not less than 99%. 5.15 quartz filter, glass filter cartridge. The retention efficiency of particles with particle size greater than 0.3 μm is not less than 99.9%. The target metal element content in blank filter cartridge should be Less than or equal to the discharge standard limit of 1/10, does not meet the requirements can not be used. 5.16 argon. purity not less than 99.9%.6 instruments and equipment6.1 Particulate Sampler The use of ambient air particulate samplers (including cutter) performance and technical specifications should be consistent with HJ/T 374 and HJ 93 Regulations. The sampling flow rate of the waste gas particulate sampler is 5 L/min ~ 80 L/min, and its performance and technical indicators should meet HJ/T 48. 6.2 Inductively Coupled Plasma Atomic Emission Spectrometer The main test items and measurement performance of the instrument shall conform to at least the requirements of Class B in JJG 768. 6.3 digestion device 6.3.1 microwave digestion device. a programmable power setting function. 6.3.2 hot plate. temperature control accuracy is better than ± 5 ℃. 6.3.3 Microwave digestion containers. PFA Teflon or similar materials. 6.3.4 high pressure digestion tank (inner tank. Teflon material; outer tank. stainless steel). 6.4 Laboratory equipment and equipment commonly used 6.4.1 Teflon beaker. 100 ml. 6.4.2 Polyethylene or polypropylene bottles. 100 ml. 6.4.3 ceramic scissors.7 samples7.1 Acquisition and storage 7.1.1 Sample collection Set the ambient air sampling point according to the requirements of HJ 664. When collecting filter samples, use a flow sampler at least Collect 10 m3 (standard state). When the metal concentration is low or PM10 (PM2.5) samples are collected, the sample can be increased as appropriate Product, sampling should be recorded in detail sampling conditions. Unorganized emissions of atmospheric particulate samples were collected according to HJ/T 55 The requirements related to the installation of monitoring points, other with the ambient air sample collection requirements. Sampling process of pollutant source gas samples according to GB/T 16157 in the implementation of particulate matter requirements. Use a soot sampler to collect filter cartridges at least 0.600 m3 (standard state dry Flue gas). When the concentration of heavy metals can be appropriate to increase the sampling volume. Such as the flue gas temperature in the pipeline is higher than the relevant gold to be collected Is the melting point of the element, should take the cooling measures, so that the flue gas into the filter before the temperature is lower than the melting point of the relevant metal elements. 7.1.2 Sample storage Filter samples collected after the dust will be twice inward fold, into the sample box or paper bag to save; filter sample collection will be Sealed inward folding, vertical put back to the original sampling sleeve closed preservation. Samples were stored in a dry, ventilated, dark, room temperature environment. 7.2 Sample preparation 7.2.1 nitric acid - hydrochloric acid mixed solution digestion system 7.2.1.1 Microwave digestion Take a suitable filter or cartridge sample (eg large flow sampler rectangular filter 1/4, or cut diameter of 47 mm Of the wafer; small flow sampler round filter take the whole, the filter to take the whole), with ceramic scissors (6.4.3) cut into small pieces placed in the micro (6.3.3), add 20.0 ml of nitric acid-hydrochloric acid mixed digest (5.6), so that the filter (filter) debris Immersed in, capped, placed in the digestion tank assembly and tighten, put on the microwave turntable. Set the digestion temperature to.200 ℃, The duration of digestion was 15 min. After digestion, remove the digestion tank assembly, cool, rinse with water to digest the inner wall of the container, Add about 10 ml of water, put it aside for 0.5 h for extraction. The extract was filtered into a 100 ml volumetric flask and set to 100 ml with water Scale, to be tested. When the organic content is too high, can be added in the digestion of hydrogen peroxide (5.3) to decompose organic matter. 7.2.1.2 Heater digestion Take a suitable filter or cartridge sample (eg large flow sampler rectangular filter 1/4, or cut diameter of 47 mm Of the wafer; small flow sampler round filter to take the whole, the filter to take the whole), with ceramic scissors (6.4.3) cut into small pieces placed Polytetrafluoroethylene beaker (6.4.1), 20.0 ml of nitric acid-hydrochloric acid mixed digest (5.6) was added to make the filter (filter) Debris immersed, covered with a surface dish, heated at 100 ± 5 ℃ reflux 2 h, cooling. Rinse the inner wall of the beaker with water About 10 ml of water, put it aside for 0.5 h for extraction. The extract was filtered into a 100 ml volumetric flask and set to 100 ml with water Scale, to be tested. When the organic content is too high, can be digested by adding the right amount of hydrogen peroxide (5.3) digestion to decomposition Organic matter. 7.2.2 Other digestion systems In addition to the above nitric acid - hydrochloric acid mixed solution digestion system (7.2.1), according to the actual work needs to choose other to meet Accuracy and precision requirements of the digestion system and digestion method. Such as nitric acid (Appendix E.1), nitric acid - hydrofluoric acid - Hydrogen peroxide/perchloric acid) system (Appendix E.2; Appendix E.3; Appendix E.4) and the determination of Si, Al, Ti, Mn and other constant elements of the alkali melting method (Appendix E.5) and other full digestion system and high pressure sealing tank digestion method. Nitric acid-hydrofluoric acid- Hydrogen peroxide/perchloric acid, alkali melting and other full amount of digestion system suitable for atmospheric particle source analysis for the purpose of collecting pollution sources Determination of Elements in Samples and Environmental Samples. 7.2.3 Laboratory samples are blank Take the same lot as the sample, the same area of the blank filter or filter cartridge, according to the same steps as the preparation of the sample (7.2.1 or 7.2.2) Preparation of laboratory blank samples.8 Analysis steps8.1 Instrument parameters Using the instrument manufacturer recommended instrument operating parameters. Table 1 gives the reference analysis conditions for measurement. Table 1 ICP-OES measurement reference analysis conditions Ignite the plasma, according to the manufacturers to provide the operating parameters set, until the instrument preheat to the indicators after the stability of the open Start the measurement. 8.2 Wavelength selection In the laboratory equipment manufacturers recommended by the best measurement conditions, for each selected element selected 2 to 3 lines for The best analysis spectrum of each element was selected on the basis of the strength, spectrum and interference of each line. line. The recommended wavelengths for each metal element are shown in Appendix B. 8.3 Analysis and determination 8.3.1 Calibration curve Based on the actual chemical composition of the particulate matter, Table 2 gives the standard solution concentration reference range. Suggestions within this range Standard series of blank solution (5.9), followed by the addition of multi-element standard stock solution (5.13) preparation of 3 to 5 concentrations of the standard series. The concentration points were rinsed with nitric acid solution (5.9) to 50.0 ml. Can be adjusted according to the actual sample concentration of the element to be measured Whole calibration curve concentration range. The standard solution is sequentially introduced into the emission spectrometer for measurement, with the concentration as the abscissa, the element response intensity is the ordinate Line linear regression, the establishment of calibration curve. Table 2 Calibration Curve Standard Solution Reference Concentration Range Element concentration range (mg/L) Co, Cr, Cu, Ni, Pb, As, Ag, Be, Bi, Cd, Sr 0.00 to 1.00 Ba, Mn, V, Ti, Zn, Sn, Sb 0.00 to 5.00 Al, Fe, Ca, Mg, Na, K 0.00 to 10.0 8.3.2 Sample determination Before analyzing the sample, rinse the system with the system wash solution (5.10) until the blank strength value is minimized and the signal to be analyzed After stabilization, the sample is analyzed. During sample measurement, if the concentration of the element to be measured in the sample exceeds the calibration curve, Diluted after re-determination.9 Results calculation and representation9.1 Results calculation The concentration of the metal elements in the particles is calculated by the following formula. Where. ρ - concentration of metal elements in particles, μg/m3; C - concentration of metal elements in the sample, μg/ml; 0c - the concentration of metal elements in the blank sample, μg/ml. SV - volume or volume after digestion of sample or sample; N - the number of copies of the filter (ie, the ratio of the area of the sample filter to the area taken during digestion, for the cartridge n = 1). StdV - sampled volume (m3) in standard (273 K, 101.325 Pa). On the source of waste gas samples, stdV The volume of dry flue gas in the standard state (m3). 9.2 The result is shown When the measurement is greater than or equal to 1.00 μg/m3, the data retains three significant digits. When the result is less than 1.00 Μg/m3, the retention of the effective digits after th......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 777-2015_English be delivered?Answer: Upon your order, we will start to translate HJ 777-2015_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. 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