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HJ 685-2014: Stationary source emission. Determination of lead. Flame atomic absorption spectrophotometric method
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Stationary source emission. Determination of lead. Flame atomic absorption spectrophotometric method
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HJ 685-2014
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Basic data | Standard ID | HJ 685-2014 (HJ685-2014) | | Description (Translated English) | Stationary source emission. Determination of lead. Flame atomic absorption spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 9,981 | | Quoted Standard | GB/T 16157; HJ/T 373; HJ/T 48 | | Regulation (derived from) | Department of Environmental Protection Notice No. 4 of 2014 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the determination of particulate matter emissions from stationary sources of lead by flame atomic absorption spectrophotometry. This Standard applies to the determination of particulate matter emissions from stationary sources of l | HJ 685-2014: Stationary source emission. Determination of lead. Flame atomic absorption spectrophotometric method
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Stationary source emission.Determination of lead.Flame atomic absorption spectrophotometric method
People's Republic of China National Environmental Protection Standards
Stationary source emission measurement of lead
Flame atomic absorption spectrophotometry
Stationary source emission-Determination of lead-Flame atomic absorption
spectrophotometric method
(release
draft)
2014-1-13 release
2014-4-1 implementation
release
Ministry of Environmental Protection
Table of Contents
Preface .II
1. Scope .1
2 Normative references ..1
3 .1 The principle of the method
4 and eliminate interference .1
5 Reagents and materials .1
6 .2 instruments and equipment
Sample 2 7
Analysis Step 8 .2
9 Results Calculation and representation .. 3
10 precision and accuracy .. 3
11 Quality Assurance and Quality Control 4
12 Precautions .4
Foreword
To implement the "People's Republic of China Environmental Protection Law", "People's Republic of China Air Pollution Prevention Law," to protect the environment,
Protection of human health, standardized method for measuring the exhaust gas from stationary sources of lead in the development of this standard.
This standard specifies the determination of the exhaust particulate matter from stationary sources of lead by flame atomic absorption spectrophotometry.
This standard is the first release.
This standard is developed by the Ministry of Environmental Protection Science, Technology organization.
This standard is mainly drafted by. China National Environmental Monitoring Center.
The standard verification unit. Anhui Provincial Environmental Monitoring Center Station, Henan Province Environmental Monitoring Center, Zhejiang Environmental Monitoring
Heart, Chongqing Municipal Environmental Monitoring Center, Jiangsu Provincial Environment Monitoring Center, Nanjing Environmental Monitoring Center.
This standard MEP January 13, 2014 for approval.
This standard since April 1, 2014 implementation.
The standard explanation by the Ministry of Environmental Protection.
Stationary source emission flame atomic absorption spectrophotometry lead
WARNING. Lead and its compounds belong to toxic substances, the test should be carried out in a well-ventilated environment.
1 Scope
This standard specifies the determination of the exhaust particulate matter from stationary sources of lead by flame atomic absorption spectrophotometry.
This standard applies to the determination of the exhaust particulate matter from stationary sources of lead.
When the sample size is 0.5 m3, volume volume of 50.0 ml, the detection limit of this method was the standard 1.0 × 10-2 mg/m3,
Detection limit of 4.0 × 10-2 mg/m3.
2 Normative references
This standard refers to the contents of the following documents or the terms. For undated references, the latest valid version
This is suitable for this standard.
GB/T 16157 Stationary source emission-Determination of particulates and gaseous pollutants sampling methods
HJ/T 373 from stationary sources to monitor quality assurance and quality control techniques (Trial)
HJ/T 48 dust sampling technology
3 PRINCIPLE OF THE METHOD
Quartz fiber cartridge collection stationary source emissions of particulate matter, nitric acid - hydrogen peroxide digestion to prepare a solution.
Solution of lead in the air - acetylene flame atomic ground state atoms of lead hollow cathode lamp emission characteristic lines (283.3
nm) of laser light. Within a certain range, the absorbance and mass concentration is linear.
4 and elimination of interference
500mg/L of iron, aluminum, bismuth, chromium, cadmium, copper, zinc, cobalt, tin, manganese, magnesium, silver, sodium, potassium, and calcium silicate
The determination of no significant interference.
5 Reagents and materials
The reagents used in this standard, unless otherwise noted, are in line with national standards for the use of analytical reagent analysis, test water
Deionized water or equivalent purity.
5.1 nitric acid. ρ (HNO3) = 1.42 g/ml, pure class distinctions.
5.2 Hydrogen peroxide. w (H2O2) = 30%.
5.3 nitric acid solution, 199.
5.4 nitric acid solution, 11.
5.5 lead standard stock solution. ρ (Pb) = 1000 mg/L
Accurately weigh 1.0000 g spectroscopically pure metallic lead placed in 100ml beaker, add nitric acid in a fume hood (5.1) 15 ml,
Slowly heated on a hot plate until completely dissolved, nitric acid solution (5.3) and dilute to 1000ml. Into polyethylene plastic
Bottle, stored in the refrigerator, at least stable for one month. It can also be purchased commercially available certified reference materials/substances.
5.6 lead standard solution. ρ (Pb) = 100 mg/L
Imbibe lead standard stock solution (5.5) 10.00 ml to 100 ml volumetric flask, dilute to the mark with a solution of nitric acid (5.3),
Mix well.
5.7 acetylene, purity of not less than 99.6%
6 instruments and equipment
Unless otherwise indicated, all using the national standard of Class A glassware analysis.
6.1 Flame atomic absorption spectrophotometer
6.2 Lead hollow cathode lamp.
6.3 dust sampler, sampling flow rate (5 ~ 80) L/min, performance and other technical indicators in line with the provisions of HJ/T 48's.
6.4 quartz fiber cartridge
Lead content of not more than 5μg. Barrier efficiency particle size greater than 3 μm is not less than 99.9%.
6.5 thermostat electric hot plate, (40 ~ 200) ℃.
6.6 filtration device, 0.45 μm cellulose acetate material or similar properties of the membrane.
6.7 Teflon scissors.
6.8 General Commonly used laboratory instruments and equipment.
7 Sample
Samples collected 7.1
GB 16157 in accordance with the relevant requirements, sample collection using the isokinetic sampling method.
7.2 field blank
With each sample batch taking at least two cartridges, sampling site to site as a blank sample.
Save 7.3 sample
Sampling is completed, carefully remove the cartridge seal inwardly folded back into the original cartridge box vertically, back to the lab for analysis.
7.4 Preparation of the sample
PTFE scissors Shredded cartridge, into 250 ml Erlenmeyer flask, moistened with a little water, add 50 ml
Nitric acid solution (5.4), 15 ml of hydrogen peroxide (5.2), inserted into the small funnel, a hot plate heated to a boil, held 2 h,
To be cooled and then carefully added dropwise 5 ml of hydrogen peroxide (5.2), can be supplemented with a small amount of water, if necessary, continue to boil for half an hour, cooling
After filtration. The filtrate was transferred to a beaker, the above solution of nitric acid (5.3) washing the flask, residues and suction flask three times. wash
After the wash liquid and the filtrate were combined, evaporated on a hot plate to boil nearly dry. Then add 2 ml of nitric acid solution (5.4), heating residue
Residue is dissolved, all transferred to a 50 ml volumetric flask with water to volume (V), shake test.
7.5 Preparation of the laboratory sample blank
Take the same batch number two blank cartridge, 7.4 reference laboratory method for preparing a blank sample.
Analysis Step 8
8.1 reference measurement instrument conditions
Reference instrument conditions were as follows.
Wavelength. 283.3 nm; slit width. 0.5 nm; the flame type. air - acetylene; burner height. 8 mm.
8.2 Calibration
Take seven 100 ml flask, were added to the lead standard solution (5.6) 0.00,0.50,1.00,2.00,4.00,
8.00 and 10.00 ml, then diluted to the mark with a solution of nitric acid (5.3), this series of standard concentration of 0.00,0.50,
1.00,2.00,4.00,8.00 and 10.00 mg/L. Procedure Set up the instrument according to the manufacturer's instructions and select the instrument parameters,
Absorbance measurement standard series to draw absorbance of lead concentration (mg/L) calibration curve.
8.3 Determination
Press the calibration curve drawn when the instrument conditions and measured the concentration of the sample (7.4) of (ρ) calculated. When the sample response
When in the upper range other than the calibration curve should be used nitric acid solution (5.3) was diluted to an appropriate multiplier (F.), So that the response value
Falls within the linear range of the calibration curve.
8.4 blank test
Press the calibration curve drawn when the working conditions of the instrument measured and calculated concentration laboratory blank sample (7.5) of (ߩ തതത).
9 Results Calculation and representation
9.1 Calculation Results
Calculate stationary source exhaust particles of lead content.
) (
× - × =
ndV
) Ρ (0
ρρ fPb
Where. ρ (Pb) - stationary source exhaust particles of lead concentration, mg/m3
ρ- sample lead concentration, mg/L;
ߩ തതത- laboratory blank sample lead concentration, mg/L;
Volume V- sample volume, ml;
Dilution f- sample;
Vnd- standard conditions (273 K, 101.325 kPa) dry flue gas sample volume, m3.
9.2 The results are shown
When the measured value is less than 0.1 mg/m3, the results of two decimal places when measured value is greater than 0.1 mg/m3, results
Three significant digits expressed in units of mg/m3.
10 precision and accuracy
10.1 Precision
6 laboratories lead concentration of 115 μg/m3,230μg/m3,574 μg/m3 simulated exhaust gas sample (sample volume
To 0.5 m3 meter) were measured precision.
Laboratory relative standard deviation of 1.2% ~ 5.7%, from 0.8% to 7.3% and 1.6% ~ 8.5%;
Interlaboratory relative standard deviations were 14.0%, 12.7% and 20.9%;
Repeatability limits were. 12.1 μg/m3,25.5 μg/m3 and 53.1 μg/m3;
Reproducibility limits were. 42.5 μg/m3,76.0 μg/m3 and 134.5 μg/m3.
10.2 Accuracy
Six laboratories using standard samples of fly ash (w (Pb) = 1149mg/kg) group of preparation provided, weighed 0.050g, 0.100g
And 0.250g, respectively, added to a blank cartridge, the as lead concentrations were 115μg/m3,223μg/m3,574μg/m3 three
Concentration simulated exhaust gas sample (sample volume to 0.5m3 meter) accuracy of the experiment were.
Relative error were. -31.6% to 3.4% - to 0.9% and 28.1% -21.0% -3.7%;
The relative error of the final values were. (- 9.2 ± 12.8) 0.050%, (- 11.6 ± 11.2) 0.100%, and (-11.4 ± 10.5) 0.250%.
11 Quality Assurance and Quality Control
11.1 per sample should be done at least two field blank sample, a blank sample lead concentrations should be less than the method detection limit.
11.2 each batch of samples (samples 10 to 20 as a batch) should be done at least two laboratories blank, blank sample concentration of lead
The method for determining the degree should be less than the lower limit.
11.3 During the assay, each sample was measured 10 standard solution should retest a calibration curve of the concentration of the intermediate point. Measurement results
The concentration point on the calibration curve relative deviation fruit should not exceed ± 10%. Otherwise, we should find out the reasons to be corrected,
And re-measured before the 10 samples after the instrument is stable.
11.4 Other quality assurance and quality control of work performed in HJ/T 373 relevant regulations.
12 Notes
12.1 in the sample solution was evaporated to near dryness, the temperature is not too high, so as not to collapse splash.
Glass and plastic containers 12.2 experimental detergent washed, soaked in nitric acid (5.3) solution, washed with water before use
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