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HJ 657-2013 English PDF

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HJ 657-2013: Ambient air and stationary source emission. Determination of metals in ambient particulate matter. Inductively coupled plasma/mass spectrometry (ICP-MS)
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 657-2013	English	549	Add to Cart	4 days [Need to translate]	Ambient air and stationary source emission. Determination of metals in ambient particulate matter. Inductively coupled plasma/mass spectrometry (ICP-MS)	Valid	HJ 657-2013

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Basic data

Standard ID	HJ 657-2013 (HJ657-2013)
Description (Translated English)	Ambient air and stationary source emission. Determination of metals in ambient particulate matter. Inductively coupled plasma/mass spectrometry (ICP-MS)
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z15
Classification of International Standard	13.040
Word Count Estimation	21,214
Quoted Standard	GB/T 16157; HJ/T 48; HJ/T 55; HJ/T 77.2; HJ 93; HJ/T 194; HJ/T 374; " ambient air quality testing (Trial) " SEPA Notice 2007 No. 4
Regulation (derived from)	Department of Environmental Protection Notice No. 50 of 2013
Issuing agency(ies)	Ministry of Ecology and Environment
Summary	This standard specifies: Determination of antimony (Sb), aluminum (Al), arsenic (As), barium (Ba), beryllium (Be), cadmium (Cd), chromium (Cr), cobalt (CO), copper (Cu), of lead (Pb), manganese (Mn), molybdenum (Mo), Nickel (Ni), selenium (Se), silver (Ag

HJ 657-2013: Ambient air and stationary source emission. Determination of metals in ambient particulate matter. Inductively coupled plasma/mass spectrometry (ICP-MS)

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Ambient air and stationary source emission.Determination of metals in ambient particulate matter. Inductively coupled plasma/mass spectrometry (ICP-MS) National Environmental Protection Standard of the People's Republic Metal elements such as lead in air and exhaust particulates Inductively coupled plasma mass spectrometry Ambient air and stationary source emission - Determination of metals In ambient particulate matter – Inductively coupled plasma/mass Spectrometry (ICP-MS) Published on.2013-08-16 2013-09-01 Implementation Ministry of Environmental Protection released

Content

Foreword..i 1 Scope..1 2 Normative references..1 3 Terms and Definitions.1 4 principle of the method..2 5 interference and elimination. 2 6 Reagents and materials.3 7 instruments and equipment.3 8 samples.4 9 Analysis steps..5 10 Results calculation and representation..6 11 Precision and Accuracy..6 12 Quality Assurance and Quality Control 7 13 Disposal of waste 7 14 Notes. 7 Appendix A Normative Appendix.8 Appendix B Informative Appendix.9 Appendix C Informative Appendix. 17

Foreword

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 the Prevention and Control of Air Pollution, protect the environment and protect people This standard is established for the determination of metal elements in air and exhaust particulates. This standard specifies the inductively coupled plasma for the determination of lead and other metal elements in ambient air, unorganized emissions and pollutants. Mass spectrometry. This standard is the first release. Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Shanghai Environmental Monitoring Center. This standard is verified by. National Environmental Analysis and Testing Center, Zhejiang Environmental Monitoring Center, Ningbo Environmental Monitoring Center, Shanghai Baoshan District Environmental Monitoring Station, Shanghai Jiading District Environmental Monitoring Station, and Australia Real Analysis and Testing (Shanghai) Co., Ltd. This standard was approved by the Ministry of Environmental Protection on August 16,.2013. This standard has been implemented since September 1,.2013. This standard is explained by the Ministry of Environmental Protection. Determination of lead and other metallic elements in air and exhaust particulates Inductively coupled plasma mass spectrometry

1 Scope of application

This standard specifies the determination of antimony (Sb), aluminum (Al), arsenic (As), barium (Ba), barium (Be), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), Lead (Pb), manganese (Mn), molybdenum (Mo), nickel (Ni), selenium (Se), silver (Ag), thallium (Tl), thorium (Th), uranium (U), vanadium (V), Zinc (Zn), bismuth (Bi), Inductively coupled plasma mass spectrometry of metal elements such as strontium (Sr), tin (Sn), and lithium (Li). This standard applies to ambient air PM2.5, PM10, TSP and sputum (Sb) in unorganized emissions and pollution source exhaust particulates. Aluminum (Al), arsenic (As), barium (Ba), barium (Be), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn), Molybdenum (Mo), nickel (Ni), selenium (Se), silver (Ag), thallium (Tl), thorium (Th), uranium (U), vanadium (V), zinc (Zn), antimony (Bi), antimony (Sr), tin (Sn), lithium (Li), etc. Determination of metallic elements. When the air sampling amount is 150m3 (standard state) and the sampling source of the pollution source is 0.600m3 (standard dry flue gas), each The method detection limits for metal elements are given in Appendix A.

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard. GB/T 16157 Determination of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants HJ/T 48 soot sampler technical conditions HJ/T 55 Technical Guidelines for the Monitoring of Unorganized Emissions of Air Pollutants HJ/T 77.2 Determination of Dioxins in Ambient Air and Exhaust Gases Isotope Dilution High Resolution Gas Chromatography - High Resolution Spectral method HJ 93 ambient air particulate matter (PM10 and PM2.5) sampler technical requirements and test methods HJ/T 194 Technical Specifications for Manual Air Quality Monitoring HJ/T 374 total suspended particulate sampler technical requirements and testing methods HJ/T 397 Fixed Source Exhaust Gas Monitoring Technical Specification "Regulations on Environmental Air Quality Monitoring (Trial)" (State Environmental Protection Administration Announcement No. 4,.2007)

3 Terms and definitions

The following terms and definitions apply to this standard. 3.1 Calibration Blank (Calibration Blank) The composition should be the same as the solution used to dilute the standard, usually a nitric acid solution at a concentration of (1 99). 3.2 Laboratory Reagent Blank (Laboratory Reagent Blank) The preparation process must be the same as the preparation of the sample, except that the reagents used are the same as those used for the preparation of the sample. 3.3 Washing blank solution (Rinse Blank) Typically a nitric acid solution at a concentration of (2 98) is used primarily to flush residues from the instrument system that may have originated from the previous measurement. 3.4 Field Blank (Field Blank) The blank sample does not need to be evacuated or the source of exhaust gas passes through the blank filter (filter cartridge), but passes through the same place as the actual sample. Management and transportation operations should avoid contamination and loss during sample transportation.

4 Principle of the method

The filter is used to collect the particulate matter in the ambient air, and the filter cartridge is used to collect the particulate matter in the waste gas of the pollution source, and the collected sample is pretreated (micro After wave digestion or electrothermal plate digestion, the content of each metal element was measured by inductively coupled plasma mass spectrometry (ICP-MS).

5 interference and elimination

5.1 Isobaric interference Table B-1 in Appendix B is the method to avoid such interference (except 98Mo and 82Se will still have 98Ru and 82Kr interference) The recommended isotope table. If you want to achieve higher sensitivity, choose other natural abundance isotopes in Table B-1. Can produce one or more isobaric interferences. Such interference can be corrected using mathematical equations, usually measuring interference elements. Another isotope of the element, which is then subtracted from the corresponding signal by the analysis signal. The mathematical equation used must be recorded in the report and The correctness must be verified before use. 5.2 Abundance sensitivity When a large number of isotope signals of other elements appear near the isotope of the element to be tested, peak overlap interference may occur. When to be tested When such interference occurs in the sample, improved resolution, matrix separation, use of other analytical isotopes, or other analytical methods may be used. Ways to avoid interference. 5.3 molecular ion interference Molecular ions that can cause interference are typically formed by a carrier gas or certain components of the sample in a plasma or interface system, such as. 40Ar35Cl+ interferes with the determination of 114Cd by 75As and 98Mo16O+. Most of the literature has confirmed the impact of ICP-MS determination Molecular ion interference is shown in Table B-2 in Appendix B. The method of correcting this interference can be found in the literature to find the abundance of isotopes in nature. Or by adjusting the concentration of the standard solution, the instrument can measure the coefficient of variation of the net isotope signal to less than 1.0%, and accurately obtain the interference. Correction factor (Note). Note 1. The correction coefficient of the instrument can be obtained by converting the ratio of the net isotope signal intensity. In the process of determining the correction coefficient, the appropriate concentration should be The standard solution is measured for isotope ratio and the measured signal precision must be less than 1.0%. 5.4 Physical interference The occurrence of physical interference is related to the atomization and transport process of the sample and is also related to ion transport efficiency. Existence of a large number of sample matrices Will cause the surface tension or viscosity of the sample solution to change, which will cause the sample solution to atomize and transfer efficiency changes, and the analysis signal will be Now inhibit or increase. In addition, a large amount of dissolved solids in the sample solution is deposited on the atomizer nozzle and the sampling cone cavity, which also makes the analysis letter The strength of the number is reduced, so the total dissolved solids content in the sample solution must be less than 0.2% (2000 mg/L). Due to physical interference When the internal standard and the element to be tested change to the same extent, the internal standard can be added to correct the physical interference. When the concentration of the matrix present in the sample is too high, the internal standard standard signal is significantly inhibited (less than 30% of the normal signal value) The sample solution can be re-measured after appropriate dilution to avoid physical interference. 5.5 Memory interference When continuously measuring samples or standards with large differences in concentration, the elements to be tested in the sample are deposited and retained in the vacuum interface and spray chamber. And the nebulizer can cause memory interference, and can avoid the occurrence of such interference by prolonging the washing time before and after the sample is measured.

6 reagents and materials

Unless otherwise stated, all grades of pure or purer grades of chemical reagents that meet national standards are used for analysis. Experimental water is Ultrapure water, specific resistance ≥ 18MΩ ⋅ cm. 6.1 Nitric acid. ρ(HNO3) = 1.42g/ml. Excellent grade pure or high purity (such as microelectronics). 6.2 Hydrochloric acid. ρ(HCl) = 1.19 g/ml. Excellent grade pure or high purity (such as microelectronics). 6.3 Nitric acid-hydrochloric acid mixed solution 55.5 ml of nitric acid (6.1) and 167.5 ml (6.2) of hydrochloric acid were added to about 500 ml of ultrapure water, and then diluted to 1 L with ultrapure water. 6.4 standard solution 6.4.1 Single element standard stock solution. ρ = 1.00 mg/ml. It can be made into high purity metal (purity greater than 99.99%) or metal salt (reference or high purity reagent) to make 1.00mg/ml The standard stock solution, the acidity of the solution is maintained above 1.0% (v/v). A certified standard solution can also be purchased. 6.4.2 Multi-element standard stock solution. ρ = 100 mg/L. It can be prepared by a single element standard stock solution or a certified standard solution. 6.4.3 Multi-element standard use solution The concentration is recommended to be ρ =.200 μg/L. 6.4.4 Internal standard stock reserve solution The internal standard element should be selected according to the mass of the isotope of the element to be tested, and it is generally selected within the range of mass ± 50 amu. The internal standard element used. The recommended internal standard elements are listed in Table B-3 in Appendix B. Can purchase certified standard solution, can also use high purity gold Is a genus (purity greater than 99.99%) or a corresponding metal salt (reference or high purity reagent). The concentration is 100.0μg/L. The medium is 1% nitric acid. 6.4.5 Mass spectrometer tuning solution The concentration is recommended to be ρ = 100 μg/L. The solution needs to contain enough elemental ions to cover the entire mass spectrum, including Li, Be, Mg, Co, In, Tl, Pb, etc. Can be purchased with certified standard solution, or high purity metal (purity greater than 99.99%) or corresponding gold Formulated as a salt (reference or high purity reagent). 6.5 Glass fiber or quartz filter The retention efficiency of particles with a particle size greater than 0.3 μm is not less than 99%; the background concentration value should meet the measurement requirements. 6.6 Glass fiber or quartz filter cartridge The retention efficiency of particles with a particle size greater than 0.3 μm is not less than 99.9%; the background concentration value should meet the measurement requirements. 6.7 Argon The purity is not less than 99.99%.

7 Instruments and equipment

7.1 cutter 7.1.1 TSP cutter. cutting particle size Da50 = (100 ± 0.5) μm, other performance and technical indicators should meet the requirements of HJ/T 374. 7.1.2 PM10 cutter. The cutting particle size is Da50=(10±0.5)μm; the geometric standard deviation of the collection efficiency is σg=(1.5±0.1)μm. Other sex Energy and technical indicators should comply with HJ/T 93 regulations. 7.1.3 PM2.5 cutter. The cutting particle size is Da50=(2.5±0.2)μm; the geometric standard deviation of the collection efficiency is σg=(1.2±0.1)μm. Other performance And technical indicators should comply with the provisions of HJ/T 93. 7.2 Particle sampler 7.2.1 Ambient air (unorganized emissions) sampling equipment Large flow sampler. The sampler operating point flow is 1.05m3/min. Medium flow sampler. The sampler operating point flow is 0.100m3/min. Other performance and technical specifications for high flow and medium flow samplers shall be in accordance with HJ/T 374. 7.2.2 Pollution source exhaust sampling equipment Soot sampler. The sampling flow rate is (5~80) L/min. Other performance and technical indicators should meet the requirements of HJ/T 48. 7.3 Inductively Coupled Plasma Mass Spectrometer The mass range is (5 to 250) amu, and the minimum width at a resolution of 5% peak height is 1 amu. 7.4 Microwave digestion device 7.4.1 Microwave Digestion Device. With programmable power setting function, it can provide output power up to 600W. 7.4.2 Microwave digestion vessel. PFA Teflon or similar material. 7.4.3 Rotating disc. A rotating disc must be used during microwave digestion to ensure that the sample is subjected to microwave uniformity. 7.5 Electric heating plate. 100 °C. 7.6 Ceramic scissors. 7.7 Teflon beaker. 100ml. 7.8 Polyethylene volumetric flask. 50ml, 100ml. 7.9 Polyethylene or polypropylene bottle. 100ml. 7.10 Class A glass measuring device. 7.11 Common instruments and equipment used in general laboratories.

8 samples

8.1 Collection and preservation 8.1.1 Sample collection 8.1.1.1 Ambient air sample The setting of the ambient air sampling point shall comply with the relevant requirements in the Ambient Air Quality Monitoring Regulations (Trial). Sampling process The requirements for particle sampling in HJ/T 194 are performed. The ambient air sample collection volume is not less than 10m3 (standard state) in principle, when heavy gold When the concentration is low or PM10 (PM2.5) sample is collected, the gas volume may be appropriately increased, and the sampling environment conditions shall be recorded in detail at the same time. 8.1.1.2 Unorganized emission samples Unorganized emission sample collection According to the relevant requirements of HJ/T 55, the monitoring points are set, and other environmental air sample collection requirements. 8.1.1.3 Source of waste gas samples The sampling process of the waste gas sample of the pollution source shall be carried out in accordance with the requirements for particle sampling in GB/T 16157. Use the soot sampler to collect The granular sample is in principle not less than 0.600 m3 (standard dry flue gas), and the gas recovery volume can be appropriately increased when the heavy metal concentration is low. If the temperature of the flue gas in the pipeline is higher than the melting point of the relevant metal element to be collected, the cooling measures should be taken to make the temperature of the flue before entering the filter cartridge. The degree is lower than the melting point of the relevant metal element. For the specific method, refer to the relevant content in HJ/T 77.2. 8.1.2 Preservation of samples After collecting the filter sample, the dust surface will be folded inward twice and placed in a sample box or paper bag. The sample of the filter cartridge will be sealed inward after collection. Fold, put it back into the original sampling sleeve and store it in a closed position. Samples were stored at (15 ~ 30) °C before analysis, and the maximum shelf life of the samples was 180 days. 8.2 Preparation of samples 8.2.1 Microwave digestion Take appropriate amount of filter sample. large TSP filter (size is about 20cm × 25cm) take 1/8, small round filter (such as diameter of 90mm Or below) Take the entire sheet. Cut into small pieces with ceramic scissors and place in a digestion tank. Add 10.0 ml of a mixed solution of nitric acid-hydrochloric acid (6.3) to make The filter membrane is immersed in it, capped, placed in the digestion tank assembly and screwed onto the microwave carousel. Set the digestion temperature to.200 ° C, eliminate The solution lasts for 15 minutes and begins to dissolve. After the digestion is completed, the digestion tank assembly is taken out, cooled, and the inner wall is rinsed with ultrapure water. Into about 10ml of ultrapure water, let stand for half an hour for leaching, filtration, and make up to 50.0ml, to be tested. Can also be fixed to 50.0ml, After centrifugation, the supernatant was taken for measurement. Note 2. The sample of the filter cartridge is taken as a whole. After cutting into small pieces, add 25.0 ml of a mixed solution of nitric acid-hydrochloric acid (6.3) to immerse the filter cartridge, and finally make up to 100.0 ml. Other operations are the same as the filter sample; if the sample size of the filter is large, the volume of the nitric acid-hydrochloric acid mixed solution (6.3) can be appropriately increased to make the filter immersed. among them. 8.2.2 Heating plate digestion Take appropriate amount of filter sample. large TSP filter (size is about 20cm × 25cm) take 1/8, small round filter (such as diameter of 90mm Or below) Take the entire sheet. Cut into small pieces with ceramic scissors and place in a Teflon beaker. Add 10.0 ml of a mixed solution of nitric acid-hydrochloric acid (6.3). The filter was immersed therein, covered with a watch glass, heated under reflux at 100 ° C for 2.0 hours, and then cooled. Rinse the inner wall of the beaker with ultrapure water. Add about 10 ml of ultrapure water, let stand for half an hour for leaching, filter, and dilute to 50.0 ml, to be tested. It can also be fixed to 50.0ml. After centrifugation, the supernatant was taken for measurement. Note 3. The filter cartridge sample is taken as a whole, and 25.0 ml of a mixed solution of nitric acid-hydrochloric acid (6.3) is added, and finally the volume is adjusted to 100.0 ml. Other operations are compared with the membrane sample. If the sample volume of the filter sample is large, the volume of the nitric acid-hydrochloric acid mixed solution (6.3) may be appropriately increased to allow the filter membrane to be immersed therein.

9 Analysis steps

9.1 Instrument Tuning After igniting the plasma, the instrument needs to be preheated for 30 minutes. During this time, mass spectrometer tuning solutions can be used for mass calibration and Resolution check. The mass spectrometer tuning solution must be measured at least 4 times to confirm the intensity of the elemental signal contained in the measured tuning solution. The relative standard deviation is ≤ 5%. Quality correction and resolution verification must be performed for the range of masses covered by the element to be tested, such as quality calibration If the difference between the positive result and the true value exceeds 0.1 amu or more, the quality must be corrected to the correct value according to the instruction manual of the instrument; The resolution of the number is about 1 amu at a peak height of 5%. 9.2 Drawing of the calibration curve A series of standard solutions of the elements to be tested are sequentially prepared in a volumetric flask at concentrations of 0 μg/L, 0.100 μg/L, and 0.500 μg/L, respectively. 1.00 μg/L, 5.00 μg/L, 10.0 μg/L, 50.0 μg/L, 100.0 μg/L, and the medium was 1% nitric acid. Internal standard solution (6.4.4) It can be added directly to each sample, or it can be added with another peristaltic pump before the sample is atomized to mix well with the sample. ICP-MS Make a measurement and draw a calibration curve. The concentration range of the calibration curve can be adjusted according to the measurement needs. 9.3 Sample determination Before each sample is measured, flush the system with a wash blank solution until the signal is at a minimum (usually about 30 seconds), the signal to be analyzed The sample can only be measured after stabilization (usually about 30 seconds). The internal standard solution (6.4.4) should be added to the sample. If in the sample The concentration of the element to be tested exceeds the calibration curve and needs to be re-measured after dilution. When measuring on the machine, the acid concentration in the sample solution must be controlled within 2% to reduce the damage of the vacuum interface and reduce Less multi-atomic ion interference. In addition, when the sample solution contains hydrochloric acid, there may be interference of polyatomic ions, which can be passed. The calibration equations listed in Table B-4 in Appendix B are corrected and can also be corrected by means of reaction cell technology. 9.4 Blank experiment A blank test was performed using ultrapure water instead of the sample. The preparation and measurement methods are identical to those of the sample, and the amount of reagent used is also the same. A blank experiment is performed while the sample is being measured, and the blank is a laboratory reagent blank. 10 Calculation and representation of results 10.1 The recommended correction equation for each element is shown in Table B-4 in Appendix B. 10.2 Calculation of results The concentration of metal elements in the particles is calculated as follows. Stdmm VFV/)n10( 3 −×××= −ρρ Where. ρm-mass concentration of metal elements in the particles, μg/m3; Ρ- concentration of metal elements in the sample, μg/L; V-sample sample volume after digestion, ml; The number of parts cut by n-filter paper. If it is a small round filter or a filter cartridge, if the whole sheet is taken during digestion, then n=1; if it is a large filter, Take one eighth of the digestion, then n=8; The average metal content of the Fm-blank filter (filter cartridge), μg. For large-scale filter membranes (filter cartridges), you can choose 20~ 30 sheets were measured to calculate the average concentration; while small batch filters (filter cartridges) were selected for a smaller number (5%). Line measurement Vstd-standard state (273K, 101.325Pa) sample volume, m3. For pollution source exhaust gas samples, Vstd is standard The sampling volume of dry flue gas, m3. 10.3 Results are expressed The final result retains three significant figures. 11 Precision and accuracy 11.1 Precision Six laboratories tested airborne matter standard material simulation samples, exhaust gas cartridge simulation samples and actual filter samples. Three of the laboratories used microwave digestion to process samples, and three laboratories used hot plate digestion to process samples. sample The mean value of each metal element (X), the relative standard deviation in the laboratory (RSDi), the relative standard deviation between the experiments (RSD'), The repeatability limit (r) and the reproducibility limit (R) are shown in Table B-5 in Appendix B. 11.2 Accuracy Six laboratories tested the quality control membrane and particulate matter standards, and three of them used microwave digestion. The samples were processed and the three laboratories used a hot plate digestion method to process the samples. Relative error (REi) and relative error final value (RE2RE S±) See Table B-6 in Appendix B. 12 Quality Assurance and Quality Control 12.1 Instrument The sampler should be periodically calibrated or calibrated and checked as scheduled. Flow and air tightness check before each sampling...

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