HY/T 147.4-2013 Technical Regulations for Ocean Monitoring Part 4 Marine Atmosphere HY/T147.4-2013 |tt||Standard compression package decompression password: www.bzxz.net
This part of HY/T147 specifies the analysis methods for monitoring items in marine atmospheric total suspended particulate matter samples and precipitation samples. This part is applicable to the analysis and testing of atmospheric total suspended particulate matter samples and precipitation samples in nearshore waters, offshore and offshore areas.
HY/T147 "Ocean Monitoring Technical Regulations" is divided into seven parts:
———Part 1: Seawater;
———Part 2: Sediment;
———Part 3: Organisms;
———Part 4: Marine atmosphere;
———Part 5: Marine ecology;
———Part 6: Marine hydrology, meteorology and sea ice;
———Part 7: Satellite remote sensing technology methods. This
part is Part 4 of HY/T147.
This part is drafted in accordance with the rules given in GB/T1.1-2009.
This part is proposed by the National Marine Environmental Monitoring Center.
This part is under the jurisdiction of the National Marine Standardization Technical Committee (SAC/TC283).
The responsible drafting unit of this part: National Marine Environmental Monitoring Center.
Participating drafting units of this part: South China Sea Environmental Monitoring Center, State Oceanic Administration East China Sea Environmental Monitoring Center, State Oceanic Administration North China Sea Environmental Monitoring Center.
Main drafters of this part: Han Gengchen, Zhang Zhifeng, Yao Ziwei, Wang Juying, Ma Yongan, Jiang Wenbo, Yang Zhengxian, Wang Lijun, Liu Guangyuan, Hu Yingying, Zhao Shilan, Wang Zhen, Wang Yanjie, Chen Shumei, Lin Zhongsheng, Xu Hengzhen, Huang Chuguang, Yu Hansheng, Li Xiaomin, Wu Shiwei, Lu Chuqian, Zhou Peiyu, Lu Dapeng, Cheng Xiangsheng, Kong Dingjiang, Yang Qing, Qin Banghui, Liu Fuping, Qiu Jinkun, Zhang Shugang, Cui Wenlin, Xie Li, Sun Xiaodong, Wu Shengqing, Xia Youlin, Wang Youliang, Wang Mei.
The following documents are indispensable for the application of this document. For any dated referenced document, only the dated version applies to this document. For any un-dated referenced documents, the latest version (including all amendments) shall apply to this document.
GB/T13580.2 Collection and preservation of atmospheric precipitation samples
GB/T13580.3 Determination of electrical conductivity of atmospheric precipitation
GB/T13580.4 Determination of pH value of atmospheric precipitation-Electrode method
GB/T13580.5 Determination of fluoride, chlorine, nitrite, nitrate and sulfate in atmospheric precipitation-Ion chromatography method
GB/T13580.7 Determination of nitrite in atmospheric precipitation-N-(1-naphthyl)-ethylenediamine photometric method
GB/T13580.8 Determination of nitrate in atmospheric precipitation
GB/T13580.11 Determination of ammonium salt in atmospheric precipitation
GB/T15432 Determination of total suspended particulate matter in ambient air-Gravimetric method
GB17378.1 Marine monitoring specifications Part 1: General provisions GB17378.2
Marine monitoring specifications Part 2: Data processing and analysis quality control
Foreword III
1 Scope 2
Normative references 3
Terms and definitions
4 General provisions
5 Simultaneous determination of copper, lead, zinc, cadmium, chromium, arsenic and iron 6
Determination of nitrite 7 Determination of
nitrate 10
Determination of ammonium salt 14
Determination of phosphate 17
Determination of total phosphorus 10
Determination of polycyclic aromatic hydrocarbons 11
Determination of polychlorinated biphenyls 12
Appendix A (Normative Appendix) Record table37
Appendix B (Informative Appendix) Detection limit of determination method46
Figure 1 Liquid chromatogram of 15 PAHs standard solutions27
Figure 2 Gas chromatogram of 8 PCBs standard solutions33
Table 1 Reference working conditions of microwave digestion instrument4
Table 2 Repeatability and reproducibility of ICP-MS determination of elements in atmospheric filter samples5
Table 3 Repeatability and reproducibility of ICP-MS determination of elements in precipitation samples7
Table 4 HPLC mobile phase gradient program26
Table 5 Peak sequence, excitation wavelength and emission wavelength of PAHs determined by HPLC26
Table 6 Repeatability and reproducibility of HPLC determination of PAHs in atmospheric samples28
Table 7 Repeatability and reproducibility of HPLC determination of PAHs in precipitation samples30
Table 8 Repeatability and reproducibility of PCBs in atmospheric samples determined by GC-ECD34
Table 9 Repeatability and reproducibility of PCBs in precipitation samples determined by GC-ECD36
Table A.1 Sampling record sheet for total suspended particulate matter in the ocean atmosphere (shore-based fixed point) 37
Table A.2 Sampling record sheet for total suspended particulate matter in the ocean atmosphere (underway) 38
Table A.3 Analysis record sheet for total suspended particulate matter in the ocean atmosphere39
Table A.4 Sampling record sheet for precipitation in the ocean atmosphere (shore-based fixed point) 40
Table A.5 Analysis record sheet for precipitation in the ocean atmosphere41
Table A.6 Standard curve record sheet for polycyclic aromatic hydrocarbons in suspended particulate matter (or precipitation) samples in the ocean atmosphere42
Table A.7 Table A.8 Record of polycyclic aromatic hydrocarbons analysis in marine atmospheric suspended particulate matter (or precipitation) samples
Table A.9 Record of polychlorinated biphenyls analysis in marine atmospheric suspended particulate matter (or precipitation) samples Table B.1 Detection limit of determination method Table B.1 Detection limit of
polychlorinated biphenyls analysis in marine atmospheric suspended particulate matter (or precipitation) samples

ICS 07.060
Marine Industry Standard of the People's Republic of China
HY/T 147.4—2013
Code of practice for marine monitoring technology-Part 4 : Marine atmosphere
aimosphere
2013-04-25 Issued
State Oceanic Administration
2013-05-01 Implementation
Normative reference documents
Terms and definitions
General provisions
Simultaneous determination of copper, lead, zinc, cadmium, chromium, arsenic and iron... Determination of nitrate
Determination of nitrate
Determination of ammonium salt
Determination of phosphate
Determination of total phosphorus
Determination of polycyclic aromatic hydrocarbons
Determination of polyoxybiphenyls
Appendix A (Normative Appendix) Record Clothing
Appendix B (Informative Appendix)
Determination method detection limit
Figure 115 PAIIs Liquid chromatogram of standard solution Figure 2 Gas chromatogram of standard solution of 8 PCBs Figure 1 Reference working conditions of microwave digester
Table 21 Protein refolding and reproducibility of each element in atmospheric filter samples determined by CP-MSTable 3 Repeatability and reproducibility of each element in precipitation samples determined by ICP-MSTable 4 Gradient program of HPLC mobile phase
Table 5 Peak sequence, excitation wavelength and emission wavelength of PAHs determined by HPLCTable 6 Repeatability and reproducibility of PAHs in atmospheric samples determined by HPLCTable 7
Repeatability and reproducibility of PAIIs in precipitation samples determined by HPILCTable 8 GC ECD determination of PCRs in atmospheric samples Repeatability and reproducibility Table 9 Repeatability and reproducibility of GC-ECD determination of PC:B5 in precipitation samples Table A.
Sampling record of total suspended particles in the ocean atmosphere (shore-based fixed point) Table A.2 Sampling record of total suspended particles in the ocean atmosphere (underway) Table A.3
Analysis record of total suspended particles in the ocean atmosphere samples
Table A.4 Record of precipitation in the ocean atmosphere (shore-based fixed point) A.5 Analysis record of precipitation samples in the ocean atmosphere
HY/T 147.4—2013
HY/T147.4—2013
Table A.6 Record table of standard curve of polycyclic aromatic hydrocarbons in marine atmospheric suspended particles (or precipitation) samples Table A.7
Record table of analysis of polycyclic aromatic hydrocarbons in marine atmospheric suspended particles (or precipitation) samples Table A8
Record table of standard curve of polychlorinated biphenyls in marine atmospheric suspended particles (or precipitation) samples Table A.9 Record table of standard curve of polychlorinated biphenyls in marine atmospheric suspended particles (or precipitation) samples PCB analysis record table in samples Table 1 Determination method detection limit
HY/T147 "Ocean Monitoring Technical Regulations" is divided into seven parts: Part 1: Seawater;
Part 2: Sediment;
Part 3: Organisms;
Part 4: Marine atmosphere;
Part 5: Marine ecology;
Part 6: Marine hydrology, meteorology and sea ice: Part 7: Satellite sensing technology methods.
This part is Part 4 of HY/T1.47.
This part was drafted in accordance with the rules given in GB/T1.1·-2009. This part was proposed by the National Marine Environmental Monitoring Center. This part was submitted by the National Marine Standardization Technical Committee (SAC/TC283). The responsible drafting unit of this part: National Marine Environmental Monitoring Center. HY/T147.4—2013
Participating drafting units of this part: South China Sea Environmental Monitoring Center of State Oceanic Administration, East China Sea Environmental Monitoring Center of State Oceanic Administration, North China Sea Environmental Monitoring Center of State Oceanic Administration.
Main drafters of this part: Han Gengchen, Zhang Zhi, Yao Ziwei, Wang Juying, Ma Yongan, Jiang Wenbo, Yang Zhengguang, Xia Lijun, Liu Guangyuan, Hu Tangying, Zhao Shilan, Tu Zhen, Wang Yanjie, Chen Shumei, Lin Zhongsheng, Xu Hengzhen, Huang Chuguang, Yu Hansheng, Li Xiaomin, Wu Shiwei, Lu Chuqian, Zhou Peiyu, Lu Dapeng, Cheng Xiangsheng, Kong Dingjiang, Yang Qing, Tai Banghui, Liu Fuping, Qiu Jinkun, Zhang Shugang, Cui Wenlin, Xie Li, Sun Xiaodong, Wu Shengqing, Xia Youlin, Wang Youliang, Wang Mei. bzxz.net
1 Scope
Technical regulations for marine monitoring
Part 4: Marine atmosphere
HY/T 147.4—2013
This part of HY/T147 specifies the analytical methods for monitoring items in total suspended particulate matter and precipitation samples in the marine atmosphere. This part is applicable to the analysis and testing of total suspended particulate matter samples and precipitation samples in coastal waters, offshore and offshore areas. 2 Normative references
The following documents are indispensable for the application of this document. For all dated references, only the dated version applies to this document. For all undated references, the latest version (including all amendments) applies to this document. GB/T13580.2 Collection and preservation of atmospheric precipitation samples GB/T13589.3 Determination of electrical conductivity of atmospheric precipitation - Electrode method GB/T13580.4 Determination of pHI value of atmospheric precipitation - Electrode method GB/T13580.5 Determination of fluorine, chlorine, nitrite, nitrate and sulfate in atmospheric precipitation - Ion chromatography method GB/T13580.7 Determination of nitrate in atmospheric precipitation - N-(1-naphthyl)-ethylamine photometric method GB/T13580.8 Determination of nitrate in atmospheric precipitation GB/T13580.11 Determination of ammonium salt in atmospheric precipitation GB/T15432 Determination of total suspended particulate matter in ambient air - Gravimetric method GB 17378.
Ocean Monitoring Specifications Part 1: General Principles
GB17378.2 Marine Monitoring Specifications Part 2: Data Processing and Analysis Quality Control 3 Terms and Definitions
The terms and definitions defined in GB17378.1 and GB17378.2 and the following terms and definitions apply to this document. 3.1
Total suspended particulate matter; TSP is the general term for particles with aerodynamic equivalent diameter of less than 100 μm suspended in the air, referred to as TSP. 3.2
Precipitation
Liquid water and solid water that fall from the atmosphere to the lower surface (land, water surface, etc.), including rain, snow, fog, etc. 3.3
Sample membrane
Filter membrane carrying total suspended particulate matter.
4 General provisions
4.1 The total suspended particulate matter concentration is determined by the weight method, see GB/T15432. 4.2 The conductivity of precipitation is determined by the electrode method, see G3/T13580.3.1
HY/T 147.4—2013
4.3 The pH of precipitation is determined by the electrode method, see GB/T 13580.1. 4.4 The following methods are available for the determination of nitrite in precipitation: a) Flow analysis method, see 6.2; 6) Ion chromatography method, see GB/T 13580.5; c) N-(1-naphthyl)ethylenediamine photometric method, see CB/T 13580.7. 4.5 The following methods are available for the determination of nitrate in precipitation: z) Flow analysis method, see 7.2; ion chromatography method, see CB/T 13580.5; c) UV photometric method, see GB/T 135 80.8; d) Column reduction photometry, see GB/T 13580.8. 4.6 There are several methods for determining ammonium hydride in precipitation; a) Flow analysis method: see 8.2; Nessler's reagent photometry, see GB/T 13580.11; c) Sodium hypochlorite-salicylic acid photometry, see GB/T 13580.11. 5 Simultaneous determination of copper, lead, zinc, cadmium, chromium, arsenic and iron 5.1 Determination of total suspended particulate matter samples - Inductively coupled plasma mass spectrometry (ICP-MS) 5.1. 1 Scope of application This method is applicable to the simultaneous determination of copper, lead, zinc, cadmium, chromium, arsenic and iron in total suspended particulate matter samples in the marine atmosphere. See Table B.1 for the detection limit of the method.
5.1.2 Principle of the method
Use a high-flow sampler to collect atmospheric total suspended particulate matter samples. After the sample filter membrane is digested, the digestion solution is atomized and enters the plasma area in the form of aerosol. After evaporation, dissociation, atomization, ionization and other processes, it is introduced into the high-vacuum mass spectrometry part. The ions to be measured are filtered and separated by the mass analyzer according to the mass-to-charge ratio (m/), and then enter the ion detector. The concentration of the element to be measured in the sample is calculated based on the ion intensity.
5. 1.3 Reagents and their preparation
5.1.3.1 Unless otherwise specified, all reagents used in this method are of high purity, and water is ultrapure water or water of equivalent purity. 5.1.3.2 Nitric acid (HNO,): 0 = 1.42 g/mL. 5.1.3.3 Perchloric acid (HCl): 0 = 1.67 g/mL. 5.1.3.4 Hydrochloric acid (HCl): 0 = 1.19 g/mL. 5.1.3.5 Nitric acid solution (1 + 99): Mix nitric acid (5.1.3.2) and water in a volume ratio of 1:99. 5.1.3.6 Nitric acid solution (1 + 1): Mix nitric acid (5.1.3.2) and water in equal volumes. 5.1.3.7 Internal standard solution (10, mg/1.): contains one or more elements selected from Li, Sc, Ge, Y, 10 Rh, In, t55 Tb, 0°Bi and the concentration of each element is 1.0.0 g/L. 5.1.3.8 Multi-element mixed tuning solution (1.00 μR/L): contains a multi-element mixed tuning solution with the concentration of Li, Co, YBa, 40Ce, 2Ti and other elements being 1.00 μg/L. 5.1.3.9 Standard stock solution (100.01 mg/L): contains a single element or multi-element standard stock solution with the concentration of Cu, Zr, Zn, Pb, Cr, Zn and Fe being 100.0 mg/L respectively, and the solvent is an acid solution. Refrigerate at 4℃, valid for 1 year. 5.1.3.1 (Standard intermediate solution (10.00 mg/L): Pipette 10.00 mL of standard stock solution (5.1.3.9) into a 10 cm3 volumetric flask 2
, and fill to the mark with nitric acid solution (5.1.3.6). HY/T: 147.4—2013
5.1.3.11 Standard working solution (1.000mg/1.): Pipette 10.00ml of standard intervening solution (5.1.3.10) into a 100ml volumetric flask and dilute to the mark with nitric acid solution (5.1.3.6). 5.1.4 Instruments and equipment
5.1.4.1 High-flow total suspended particulate sampler, its physical requirements and flow calibration method are shown in GB/T15432.5.1.4.2 Sampling filter: Whatm&n No. 41 or equivalent low background value ash-free filter paper, size: 20.3cm×25.4cm5.1. 4.3 Inductively coupled plasma mass spectrometer (ICP-MS), composed of the following parts: - sample introduction system, plasma gas is fluorine gas (99.999%) ICP ion source; - interface and ion focusing system; - mass analyzer: detector. - when using ICP ion source, pay attention to protect high frequency radiation. 5.1.4.4 Electronic balance: sensitivity is 0.1mg. 5.1.4.5 Microwave digestion instrument. 5.1.4.6 Microwave digestion tank. 5.1.4.7 Polytetrafluoroethylene ground: 5.1.4.8 High-precision micropipette (10 μJ.~100 ±L, 100 μ.~-1 000 μ1.). 5.1.4.9 Electric heating plate (or electric furnace).
5.1.4.10 Other common laboratory equipment. 5.1.5 Collection and preservation of filter membrane samples
For the collection and preservation of atmospheric filter membrane samples, please refer to (J3/T15432, select the time when the wind speed conditions between winds meet the requirements of directional sampling for sampling, and record the sampling information in Table A1 (shore-based fixed point) or Table A, 2 (navigation). 5.1.6 Analysis steps
5.1.6.1 Sample digestion
The digestion of atmospheric filter membrane samples is carried out according to one of the following methods: a) Electric heating plate digestion: Cut the sample membrane at the effective sampling part of the sample filter membrane, cut it into pieces and place it in a 50ml. polytetrafluoroethylene crucible, moisten the sample with a little water, add 5ml. nitric acid solution (5.1.3.2), let it stand at room temperature for 2h, and then add 2ml. high acid (5.1, 3. 3) Place the electric heating plate on the stove and raise the temperature to 180 ℃. After heating and reflux for 4 hours, remove the acid and add 1 mL nitric acid solution (5.1.3.6). Heat and extract. Transfer the digestion solution and residue into a 25 mL colorimetric tube with water. Adjust the volume and leave it for 24 hours. Take the clear solution for testing. At the same time, randomly take two blank filter membranes with the same production batch number as the sample filter membrane to prepare analytical blanks. b) Microwave digestion: Cut a sample of a certain area at the effective sampling position of the sample membrane, cut it into pieces and place it in a micro-digestion tank. Moisten it with a little water, add 6 mL nitric acid (5.1.3.2) and 3 mL hydrochloric acid (5.1.3.4). After the reaction is stable, tighten the bottle cap and put it into the microwave digestion tank. Refer to the instrument conditions given in Table 1 for two-step digestion. After the digestion is completed, take it out after cooling to room temperature. Carefully unscrew the lid and place the digestion tank on the acid removal device. Heat to remove the acid: or transfer the entire amount of the digestion solution to a polytetrafluoroethylene crucible and place it on a hot plate for heating. After the acid is completely removed, add 1.0 mL of nitric acid solution (5.1.3.6). Slightly heat and extract, transfer the digestion solution and the remaining amount into a 25 L colorimetric tube with water, make up to volume, mix and let stand, take the supernatant for testing, and randomly select two blank filter membranes with the same production batch number as the sample filter membrane to prepare the analysis space, 3
HY/T 147.4—2013
5.1.6.2 Sample determination
5.1.6.2.1 Optimization of instrument working conditions
Table 1 Reference working conditions of microwave digestion instrument
Heating time
Holding time
After the instrument runs stably, introduce multi-element mixed tuning solution (5.1.3.8) to adjust the parameters of the instrument, select low, medium and high mass band elements to tune the sensitivity of the instrument, and at the same time adjust the oxide and double charge indicators to meet the measurement requirements. The following measures can be used to reduce or eliminate interference: select isotope erythrocytes that are not affected by interference as the quantitative mass number of the element to be measured; perform interference correction during quantification:
Use collision/reaction cell technology. ：
5.1.6.2.2 Preparation of standard series solutions
Take 8 100mL volumetric flasks and add 0ml..0.050mL0.1C1nL.0.50mlL, 1.0CmL.2.00mL.5.00mL10.0mL standard working solution (5.1.3.11) respectively, and dilute to the mark with nitric acid solution (5.1.3.5). The concentrations of the prepared standard series solutions are 0 ug/1.0.500 μg/1, 1.00μp/1.5.00μg/L, 10.0μg/L.20.0 μg/1.,50.0μg/1, 100 μg/L respectively. 5.1.6.2.3 Sample determination
Directly determine the analytical blank and sample digestion solution according to the conditions set by the instrument: the measured values ​​are X, and X5. 1.7 Calculation and recording
The content of heavy metals in the atmosphere is calculated according to formula (1), and the results are recorded in Table A.3, C, = (XXo)X0. 025×S
Where:
The content of heavy metals in the atmosphere per unit volume, in micrograms per cubic meter (ug/m\): - The measured value of heavy metals in the sample filter membrane digestion solution, in micrograms per liter (/.): The measured value of heavy metals in the analytical blank digestion solution, in micrograms per (/1.); - The volume of sample digestion solution, in liter (1); - The effective sampling area of ​​the sample membrane, in square centimeters (cm\); The cut area of ​​the sample filter membrane, in square centimeters (cm\) Under standard conditions (0 ℃ and 191.3 hPa maximum pressure) sampling volume, in cubic meters (m3). Wherein, V is calculated according to formula (2):
or:
V×P×273
(T+273)×P,
The atmospheric sampling volume measured by the gas cumulative flow meter, in cubic meters (m3): P--the average atmospheric pressure during the sampling period, in hectopascals (hPa): 4
T--the average air temperature during the sampling period, in degrees Celsius (℃) P. --Standard atmospheric pressure, 101.3hPa, 5.1.8 Precision
HY/T 147.4--2013
Five laboratories measured atmospheric filter membrane samples, and the relative standard deviation of repeatability and reproducibility are shown in Table 2. Table 2 Repeatability and reproducibility of elements in atmospheric filter membrane samples determined by ICP-MS Element name
Sample concentration
1 0. 575
0,C210
5.1.9 Quality assurance and control
The following quality control measures should be observed during the operation of this method: Repeatability Relative standard deviation
During the digestion process of batch samples, at least two blank samples should be prepared: When analyzing large batches of samples, a double parallel sample should be analyzed for every 10 samples; Reproducibility Relative standard deviation
For every 20 samples analyzed, a solution in the standard series should be selected for inspection. If the error between the measured value and the original value exceeds 10%, the standard curve should be redrawn:
During the analysis process, when using internal standard elements for correction, the internal standard solution can be added online or offline (5.1.3.7). And the content of the internal standard element in the sample should be equivalent to the content of the element to be measured. The selection of internal standard elements should follow the following principles: the internal standard element does not exist in the sample or the content in the sample will not affect the internal standard element; a) the mass number and ionization energy of the element to be measured should be as close as possible to those of the internal standard element; b) the internal standard element should not be interfered by isotopes or polyatomic ions or interfere with the isotope determination of the element to be measured; the internal standard element should have good test sensitivity. d
5.1.10 Precautions
The following matters should be noted during the operation of this method: Avoid using metal materials for the filter membrane holder of the large-flow total suspended particulate sampler; use a stainless steel tube knife or ceramic knife with a diameter of 3.00 cm to cut the sample filter membrane; soak the vessel in nitric acid solution (1 + 3) for more than 48 hours, and then rinse with ultrapure water for more than 5 times before use; the reagent blank can be reduced by repeated distillation and purification of the reagent; when digesting the sample, the amount of acid can be appropriately increased or decreased according to the sample amount; when the content of the element to be measured is high, the standard curve range can be adjusted according to the content of the element to be measured or the sample can be diluted to ensure that the sample concentration is within the range of the drawn standard curve. 5
HY/T 147.4—2013
5.2 Determination of precipitation samples—Inductively coupled plasma mass spectrometry (ICP-MS) 5.2.1 Scope of application
This method is applicable to the simultaneous determination of copper, lead, zinc, chromium, arsenic and iron in marine atmospheric precipitation samples. The detection limit of the method is shown in Table B.1. 5.2.2 Principle of the method
The precipitation sample is collected by a precipitation sampler. After atomization, the sample enters the plasma area in the form of aerosol. After evaporation, dissociation, atomization, ionization and other processes, it is introduced into the high vacuum mass spectrometry part. The ions to be measured are filtered and separated by the mass analyzer according to the size of the mass-to-charge ratio (I/I) and enter the ion detector. The concentration of the element to be measured in the sample is calculated based on the size of the ion intensity. 5.2.3 Reagents and their preparation
See 5.1.3.
5.2.4 Instruments and equipment
5, 2, 4. 1
Precipitation sampler. For the technical requirements of precipitation automatic sampler, see GB/T13580.2. 5.2.4.2 Inductively coupled plasma mass spectrometer, see 5.1.4.3, 5.2.4.3 Electronic balance: sensitivity is 0.1mg. 5.2.4.4 Beaker.
5.2.4.5 Electric heating plate (or electric furnace).
5.2.4.6 High-precision micropipette (10~100ul, 100gl.~1000). 5. 2. 4.7
Other common laboratory equipment.
5.2.5 Collection and preservation of precipitation samples
The collection and preservation of precipitation samples shall be carried out in accordance with the provisions of B/I13580.2 and recorded in Table A.4. 5.2.6 Analysis steps
5.2.6.1 Sample digestion
Measure 5c.0mL precipitation sample and add it to a 100rmE beaker. Add 2mL nitric acid (5.1.3.2) to the water sample and heat it on a hot plate at 85℃ for digestion. When the sample volume is 20mL, cover it with blood and heat it at 85℃ for 30min. Remove the beaker and transfer it to a 50ml colorimetric tube after cooling. Make up to volume with water and let it stand overnight for testing. At the same time, prepare the analytical blank solution with water according to the above steps. 5.2.6.2 Sample determination
See 5.1. (, 2.
5.2.7 Record and calculation
The content of heavy metals in precipitation samples is calculated according to formula (3), and the results are recorded in Table A.5. C = X, X,
Where:
C.-the content of heavy metals in unit volume of atmospheric precipitation sample, in micrograms per liter (/L); X.-the concentration of heavy metals in sample digestion, in micrograms per liter (ug/L); X.-the concentration of heavy metal i in the analytical blank digestion solution, in micrograms per liter (ug/L). 6
5.2.8 Precision
HY/T 147.4--2013
Five laboratories measured the same atmospheric precipitation sample. The relative standard deviation of repeatability and reproducibility is shown in Table 3. Table 3 Repeatability and reproducibility of elements in precipitation samples determined by ICP-MIS Element name
Quality assurance and control
See 5.1.9,
Precautions
Sample concentration
The following matters should be noted during the operation of this method Relative standard deviation of repeatability
Contact part between precipitation sampler and sample Avoid using metal materials; soak the instrument in nitric acid solution (1-3) for more than 481°C and rinse with ultrapure water before use; the reagent blank can be reduced by repeated distillation and purification of the reagent: Reproducibility Relative Standard Deviation
When the content of the element to be measured is high. Adjust the range of the standard curve according to the content of the element to be measured, or dilute the sample to ensure that the sample concentration is within the range of the drawn standard curve. 6 Determination of nitrite
6.1 Determination of total suspended particulate matter samples
6.1.1 Scope of application ||tt ||Flow analysis method
This method is applicable to the determination of nitrate in marine atmospheric total suspended particulate matter samples. The detection limit of the method is shown in Table 13.1. 6.1.2 Principle of the method
Use a large flow sampler to collect atmospheric total suspended particulate matter samples. After the sample filter membrane is extracted, the nitrite in the extract solution reacts with sulfonamide under acidic medium conditions for diazotization. The product is then coupled with diethylenediamine hydrochloride to form a red azo dye, which is measured at a wavelength of F5nm.
6.1.3 Reagents and their preparation
6.1.3.1 Unless otherwise specified, this method uses analytical reagents, and water is secondary deionized water or ultrapure water of equivalent purity. The preparation of reagents depends on the working conditions required by the specific instruments and equipment. t-
HY/T147.4—2013
6.1.3.2 Sodium nitrite (NaNO.): high-grade pure, dried at 110℃~115℃ for 2h, and placed in a desiccator to cool. 6.1.3.3 Polyoxyethylene lauryl ether (Brij-35): Cs:IInsO24+30%. 6.1.3.4 System cleaning solution: Take 6 ml of Brij-35 (6.1.3.3) and dissolve it in water and dilute to 1 T. 6.1.3.5 Color developer: Add 100 mL phosphoric acid (JI.PO) to about 700 mL water, add 10.0 g sulfonamide (CHN,0,S). After it is completely dissolved, add 0.5 g naphthalene diamine hydrochloride (C2HV,Cl), dilute to 1 L with water, mix well, add 4 ml 3rij-35 (6.1.3.3), mix well. Store in a brown reagent bottle. This solution can be stored at 4 ° C for 1 month. The prepared solution should be colorless, otherwise it should be re-prepared. Note: If the solution is pink, it may be that the phosphoric acid is not pure enough. 6.1.3.6 Nitrite standard preparation solution (100.0 mg/L. In terms of nitrogen): Weigh 0.4926 g sodium nitrite (6.1.3.2) and dissolve it in 50 mL water. Then transfer the whole amount to a 1000 mL volumetric flask, add water to the mark, and mix well. Add 1 mL of chloroform (CHCl3), mix well, and store in a brown reagent bottle. This solution can be stored at 4°C for 2 months. 6.1.3.7 Nitrite standard working solution (5.00 μ/mL. in terms of nitrogen): Pipette 5.0 mL of nitrite standard stock solution (6.1.3.6) into a 100 mJ volumetric flask, add water to the mark, mix well: prepare before use. 6.1.4 Instruments and equipment
6.1.4.1 Sampling equipment
See 5.t.4.1.
6.1.4.2 Sample filter membrane
See 5.1, 4, 2.
6.1.4.3 Flow analyzer
The flow analyzer consists of the following parts:-Automatic sampler:
-End-acting pump;
---Gas injection valve:
-Heating cell;
-Circulation cell;
Detector filter.
6.1.4.4 Volumetric flask: 100 mL and 1 000 mL.6.1.4.5 Pipette: 100μL~1000L; 1000μl~5000μl6.1.4.6 Beaker: 100mL, 50cmL and 1000mL6.1.4.7 Commonly used equipment in general laboratories.
6. 1.5 Collection and storage of atmospheric filter membrane samples For the collection of atmospheric filter membrane samples, refer to CB/T15432. Sampling is carried out when the wind direction and wind speed conditions meet the requirements of directional sampling. The samples are sealed in sealed plastic bags and stored at 2℃. The sampling information is recorded in Table A.1 (shore-based fixed point) or Table A.2 (underway). 6.1.6 Analysis steps
6.1.6.1 Preparation of standard series solutions
Take 7 50 mL volumetric flasks. Add 0 mL, 0.10 mL, 0.20 mL, 0.30 mL, 0.40 mL, 0.50 mL, 1.00 mL of nitrate standard solution (6.1.3.7) respectively, add water to the mark, and mix well. The concentrations of the standard series solutions are 0ug/L10.0ug/L, 20.0 μg/1.30.0 μg/L., 40.0μg/1..50.0 μg/L.100 μg/Lc6.1.6.2 System installation and commissioning
Install the flow system for nitrite testing and perform system commissioning according to the following steps: 8
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