HJ 539-2015_English: PDF (HJ539-2015)
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| HJ 539-2015 | English | 209 |
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Ambient air. Determination of lead. Graphite furnace atomic absorption spectrometry
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HJ 539-2015
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| HJ 539-2009 | English | 319 |
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Ambient air. Determination of lead. Graphite furnace atomic absorption spectrometry
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HJ 539-2009
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Standards related to: HJ 539-2015
| Standard ID | HJ 539-2015 (HJ539-2015) | | Description (Translated English) | Ambient air. Determination of lead. Graphite furnace atomic absorption spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 9,978 | | Date of Issue | 2015-11-20 | | Date of Implementation | 2015-12-15 | | Older Standard (superseded by this standard) | HJ 539-2009 | | Quoted Standard | GB/T 15432; HJ/T 194; HJ/T 374 | | Drafting Organization | Beijing Environmental Monitoring Center | | Administrative Organization | Ministry of Environmental Protection | | Regulation (derived from) | Ministry of Environment Announcement 2015 No.73 | | Summary | This Standard specifies the determination of lead in the ambient air by graphite furnace atomic absorption spectrophotometry. This Standard applies to the determination of lead in the ambient air. When collecting the ambient air 10 m3 (standard state), the sample volume to 50 ml, the detection limit is 0.009 ��g/m3, measured lower limit of 0.036 ��g/m3. |
HJ 539-2015
Ambient air.Determination of lead.Graphite furnace atomic absorption spectrometry
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 539-2009
Ambient air - Determination of lead in graphite furnace
Absorption spectrophotometry
Ambient air-Determination of lead - Graphite furnace atomic
Absorption spectrometry
2015-11-20 release
2015-12-15 implementation
Ministry of Environmental Protection released
Directory
Preface ..ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples .2
8 Analysis steps
The results are calculated and expressed
10 Precision and Accuracy
Quality assurance and quality control
12 Waste treatment
Preface
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 Atmospheric Pollution,
Environment, the protection of human health, regulate the ambient air lead monitoring methods, the development of this standard.
This standard specifies the determination of lead in ambient air by graphite furnace atomic absorption spectrophotometry.
This standard is the "ambient air lead determination of graphite furnace atomic absorption spectrophotometry (provisional)" (HJ 539-2009)
The revision.
This standard was first published in.2009, the original standard drafting unit for the Beijing Environmental Protection Monitoring Center. This is the first
The main contents of the amendment are as follows.
- choose a more appropriate filter;
- increased the microwave digestion of the pre-treatment and improve the digestion of the hot plate digestion conditions, changing the digestion with acid;
- Increased interference cancellation and quality assurance and quality control.
From the date of implementation of this standard, the original standard "Determination of ambient air lead graphite furnace atomic absorption spectrophotometry (temporary)"
(HJ 539-2009).
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The drafting of this standard. Beijing Environmental Protection Monitoring Center.
The standard verification unit. Beijing Fengtai District Environmental Monitoring Station, Beijing Yanqing County Environmental Monitoring Station, Beijing Miyun
District Environmental Monitoring Station, Beijing China Measurement North Detection Technology Co., Ltd., Beijing Fangshan District Environmental Monitoring Station, Beijing Environmental Protection
Monitoring center.
The Environmental Protection Department of this standard approves on November 20,.2015.
This standard is implemented as of December 15,.2015.
This standard is explained by the Ministry of Environmental Protection.
Ambient air - Determination of lead - Graphite furnace atomic absorption spectrophotometric method
1 Scope of application
This standard specifies the determination of lead in ambient air by graphite furnace atomic absorption spectrophotometry.
This standard applies to the determination of lead in ambient air.
Collect the ambient air 10 m3 (standard state), the sample volume to 50 ml, the detection limit of 0.009 μg/m3,
The lower limit of determination was 0.036 μg/m3.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Ambient air - Determination of total suspended particulates - Gravimetric method GB/T
Technical specification for manual monitoring of ambient air quality
Technical requirements and testing methods for HJ/T 374 total suspended particulate matter sampler
3 Principle of the method
With quartz fiber and other filters to collect ambient air particles in the sample, after digestion, into the graphite furnace atomizer,
After drying, ashing and atomization, the ground state atoms of 283.3 nm at the line of selective absorption, the absorbance value
And the quality of lead is proportional to the concentration.
4 interference and elimination
Ammonium dihydrogen phosphate is added as a matrix modifier to eliminate matrix interference. High concentrations of calcium, sulfate, phosphate, iodine
Chemical, fluoride or acetic acid can interfere with the determination of lead, can be corrected by standard addition method. Background interference can be done by deducting background
The way to eliminate.
5 reagents and materials
Unless otherwise stated, the analytical grade is used in accordance with national standards. Experimental water. specific resistance ≥ 18 M
Ω · 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. φ (H2O2) = 30%.
5.4 nitric acid solution. l9.
Prepared with nitric acid (5.1).
5.5 Nitric acid solution. φ (HNO3) = 1%.
Prepared with nitric acid (5.1).
5.6 Lead standard stock solution. ρ (Pb) = 1.00 mg/ml.
Accurately weighed 1.0000 g Spectrum of pure metal lead placed in 100 ml beaker, in the fume hood by adding 15 ml of nitric acid (5.1),
Slowly heat on the hot plate until it is completely dissolved and set to 1000 ml with nitric acid solution (5.5). Transferred to polyethylene plastic
Bottle, in the refrigerator in the cold storage, at least 30 days can be stable preservation. You can also purchase a certified standard solution.
5.7 lead standard use of liquid. ρ (Pb) = 0.5 μg/ml.
The lead standard stock solution (5.6) was diluted with nitric acid solution (5.5) to prepare a standard containing 0.5 μg/ml of lead
liquid.
5.8 Quartz fiber filter. the particle size of more than 0.3 μm particles retention efficiency ≥ 99%. The background concentration value should meet the determination
Claim.
5.9 Substrate modifier. ammonium dihydrogen phosphate solution.
Weigh 5 g of ammonium dihydrogen phosphate, with 100 ml of nitric acid solution (5.5) dissolved, prepared into a mass concentration of 5% of dihydrogen phosphate
Ammonium solution.
5.10 argon. purity of not less than 99.99%.
6 instruments and equipment
Unless otherwise noted, the use of A-level glassware in accordance with national standards.
6.1 TSP cutter. cutting diameter Da50 = 100 ± 0.5 μm, other performance and technical indicators should be consistent with the provisions of HJ/T 374.
6.2 sampler. large flow sampler operating point flow is generally 1.05 m3/min; in the flow sampler operating point flow is generally
0.100 m3/min. Large flow sampler and medium flow sampler Other performance and technical specifications shall comply with the requirements of HJ/T 374.
6.3 Graphite Furnace Atomic Absorption Spectrophotometer.
6.4 electric plate or microwave digestion. With programmable power setting function, precision control.
6.5 conical flask.
7 samples
7.1 Collection of samples
The sampling of the particles is carried out in accordance with the sampling requirements for particulate matter in GB/T 15432 and HJ/T 194. Sampling should be noted in detail
Recorded environmental conditions.
7.2 Preservation of samples
After collecting the sample filter and the whole program blank filter folded into a clean paper bag or capsule, into the dryer to save.
7.3 Preparation of samples
7.3.1 Heater digestion
The filters were cut into small pieces, placed in a conical flask, and then 10 ml of nitric acid (5.1), 5 ml of hydrochloric acid (5.2) and
3 ml of hydrogen peroxide (5.3), standing for 20 min ~ 30 min or so, until the initial reaction tends to calm, on the hot plate
Heated to micro-boiling for digestion. Steamed to dry, then add 5 ml of nitric acid (5.1), 1.5 ml of hydrogen peroxide (5.3),
Heat to dry and cool. Then add 5 ml of nitric acid (5.4) to dissolve slightly, the solution is filtered into a 50 ml volumetric flask,
And rinse the filter residue with the concentration of 1% nitric acid (5.5) at least three times, the washing liquid and the filtrate combined,
Scale and shake.
7.3.2 Microwave digestion
The filter was cut into small pieces, placed in a digestion tank, and then 8 ml of nitric acid (5.1), 2 ml of hydrochloric acid (5.2)
And 1 ml of hydrogen peroxide (5.3), standing for 2 h ~ 3 h or so, until the initial reaction tends to calm, the digestion. To be eliminated
After completion of the solution, transfer to the beaker and add 5 ml of nitric acid solution (5.4) to dissolve slightly. The solution is filtered to a 50 ml volumetric flask
And mixed with nitric acid solution (5.4).
Microwave digestion instrument parameters can refer to the instructions to choose, refer to the conditions in Table 1.
Table 1 Microwave digestion conditions
Digestion time t (min) digestion power E (W) digestion temperature T1 (℃) tank temperature T2 (℃)
15 1000 120 100
5 1250 185 120
30 1250 185 120
7.4 Preparation of blank sample
7.4.1 Full program blank
Will be the same batch of two filters to the sampling site, do not collect samples. After sampling, bring back to the laboratory, according to the sample system
Prepared (7.3) to prepare a full program blank sample.
7.4.2 Lab blank
The two batches of the same batch were prepared as laboratory blank samples according to the preparation of the sample (7.3).
8 Analysis steps
8.1 Graphite Furnace Atomic Absorption Spectrophotometer Operating Conditions
Instrument measurement parameters can refer to the instructions to choose, refer to the working conditions in Table 2.
Table 2 Graphite Furnace Atomic Absorption Spectrophotometric Working Conditions
The wavelength is 283.3 nm
Lamp current 8 mA
Slit 0.5 nm
Drying temperature and time 90 ℃, 15 s; 120 ℃, 15 s. Two dry
Ashing temperature and time of 700 ℃, 20 s
Atomization temperature and time 1400 ℃, 5 s
Cleaning temperature and time 2500 ℃, 5 s
The argon gas flow rate was 0.2 L/min
Whether the atomic phase is stopped
Injection volume 20 μl
Substrate modifier 2 μl
Background deduction method Zeeman
8.2 Calibration curve
8.2.1 Preparation of standard series
Take 6 50 ml volumetric flasks and prepare lead standard series according to Table 3. Diluted with nitric acid solution (5.5) to the mark, shake.
Table 3 Lead Standard Series
Bottle number 0 1 2 3 4 5
Lead standard use liquid (ml) 0.00 1.00 2.00 3.00 4.00 5.00
Lead concentration (μg/L) 0.00 10.0 20.0 30.0 40.0 50.0
8.2.2 Calibration curve
From low concentration to high concentration, followed by the lead into the graphite tube lead standard solution, adding 2 μl ammonium dihydrogen phosphate matrix modifier
(5.9), according to the selected instrument operating conditions, the determination of lead standard series of absorbance, and the establishment of calibration curve of the linear back
Return equation.
8.3 Determination of samples
The absorbance of the sample (7.3) was measured by the instrument operating conditions and operating procedures when the calibration curve was drawn.
8.4 Determination of blank
The absorbance of the blank sample (7.4) was measured by the instrument operating conditions and operating procedures when the calibration curve was drawn.
9 Results calculation and representation
9.1 Results calculation
Based on the measured absorbance values, the concentration of lead in the sample and the blank sample was calculated from the linear regression equation,
Calculate the concentration of lead in ambient air (μg/m3).
Ρ (Pb) =
Vn
Xxx
× -
50) (1 0ρρ
(1)
Where. ρ (Pb) - ambient air lead concentration (μg/m3);
1ρ - Lead concentration in sample, μg/L.
0ρ - average of lead concentration in laboratory blank samples, μg/L;
50 - sample solution volume, ml;
TS - total area of sample filter, cm2;
AS - the sample area of the sample taken after the measurement, cm2.
NV - standard volume (101.325 kPa, 273 K) under the sampling volume, m3;
9.2 The result is shown
When the measured value is less than 1 μg/m3, the result retains two decimal places. When the measured value is greater than or equal to 1 μg/m3, the result
Expressed in three significant digits, in μg/m3.
10 precision and accuracy
10.1 Precision
6 laboratories with standard value of 403 ± 32 mg/kg lead standard samples for precision experiments, were weighed quality
0.025 g, 0.04 g, 0.05 g three groups of samples were tested in six parallel tests. the relative standard deviation of the laboratory were. 1.84% ~
4.07%, 1.49% ~ 4.52%, 1.61% ~ 6.52% respectively. The relative standard deviations were 4.86%, 4.68% and 5.41% respectively.
The reproducibility limit r was. 38.1 mg/kg, 29.4 mg/kg, 38.4 mg/kg; the reproducibility limit R was 66.2 mg/kg, 58.3 mg/kg,
68.9 mg/kg.
10.2 Accuracy
6 laboratory with standard value of 403 ± 32 mg/kg lead standard sample for the accuracy of the experiment, were weighed
0.025 g, 0.04 g, 0.05 g three groups of samples were tested in six parallel tests. the relative error in the laboratory were -2.48%
11.2%, - 7.69% ~ 4.96%, 8.68% ~ 4.71% respectively. The relative error values were 2.78% ± 0.100%, - 2.11%
± 0.092%, - 2.69% ± 0.104%.
11 quality assurance and quality control
11.1 blank
Each batch of samples should be at least two laboratory blanks and two full program blanks, the determination of the results should be lower than the lower limit of determination.
11.2 Calibration curve
Each batch of samples need to be calibrated curve, with a linear fitting curve calibration, the correlation coefficient should be greater than or equal to 0.995.
11.3 Quantitative calibration control
During the assay, each of the 10 samples should be re-measured the standard solution at the midpoint of the calibration curve concentration. Determination of knot
The relative deviation of the point concentration on the calibration curve should not exceed ± 10%. Otherwise it should find out the cause and correct, to be stable instrument
The first 10 samples were re-measured.
11.4 parallel sample control
Each batch of samples should be 10% of the proportion of parallel sample determination, the number of samples less than 10, should be measured at least one level
Row of the measured results of the relative deviation of not more than 20%.
11.5 blank spike and matrix spike control
Each batch of samples should be at least 10% of the blank spike or matrix spike recovery test, the number of samples less than 10 at least one
The recovery rate should be in the range of 80% ~ 120%.
12 Waste treatment
All waste generated during the experiment should be collected and collected, and sent to a qualified unit for centralized treatment.
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