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HJ 542-2009: Ambient air. Determination of mercury and its compounds. Cold atomic fluorescent spectrophotometry after sulfhydryl cotton preconcentraction
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Ambient air. Determination of mercury and its compounds. Cold atomic fluorescent spectrophotometry after sulfhydryl cotton preconcentraction
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Basic data | Standard ID | HJ 542-2009 (HJ542-2009) | | Description (Translated English) | Ambient air. Determination of mercury and its compounds. Cold atomic fluorescent spectrophotometry after sulfhydryl cotton preconcentraction | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 11,133 | | Date of Issue | 2009-12-30 | | Date of Implementation | 2010-04-01 | | Quoted Standard | HJ/T 194; GB/T 6682 | | Regulation (derived from) | Department of Environmental Protection Notice No. 74 of 2009 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of mercury and its compounds in ambient air thiol cotton enrichment cold vapor atomic fluorescence spectrophotometry. This standard applies to the ambient air Determination of mercury and its compounds. This standard method detection limit is 0. 1ng/10ml sample solution. When the sample volume is 15L, the detection limit is 6. 6 �� 10 ^ (-6) mg/m ^ 3, detection limit is 2. 6 �� 10 ^ (-5) mg/m ^ 3. | HJ 542-2009: Ambient air. Determination of mercury and its compounds. Cold atomic fluorescent spectrophotometry after sulfhydryl cotton preconcentraction
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Ambient air.Determination of mercury and its compounds.Cold atomic fluorescent spectrophotometry after sulfhydryl cotton preconcentraction
National Environmental Protection Standard of the People's Republic
Determination of mercury in ambient air
Sulfhydryl Cotton Enrichment-Cold Atomic Fluorescence Spectrophotometry
(temporary)
Ambient air-Determination of mercury and its compounds-Cold atomic
Fluorescent spectrophotometry after sulfhydryl cotton preconcentraction
Released.2009-12-30
2010-04-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 74 of.2009
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve the lead gas of fixed pollution sources.
The four standards, such as the determination of flame atomic absorption spectrophotometry (tentative), are national environmental protection standards and are released.
The standard name and number are as follows.
I. Determination of lead in fixed pollution sources - Flame atomic absorption spectrophotometry (tentative) (HJ 538-2009);
2. Determination of lead in ambient air by graphite furnace atomic absorption spectrophotometry (tentative) (HJ 539-2009);
III. Determination of arsenic in ambient air and exhaust gases - Spectrophotometric method of silver diethyldithiocarbamate (interim) (HJ 540-2009);
4. Determination of gaseous arsenic in the production of yellow phosphorus - Determination of silver diethyldithiocarbamate spectrophotometry (interim) (HJ 541-2009);
6. Determination of mercury in fixed pollution sources - Cold atomic absorption spectrophotometry (provisional) (HJ 543-2009);
VII. Determination of Sulfuric Acid Fog of Fixed Pollution Sources by Ion Chromatography (Provisional) (HJ 544-2009);
VIII. Determination of gaseous total phosphorus in fixed pollution sources - Determination of quinolinol ketone capacity (provisional) (HJ 545-2009);
IX. Determination of Phosphorus Pentoxide in Ambient Air Ascorbic Acid Reduction - Molybdenum Blue Spectrophotometry (Provisional) (HJ 546-2009);
X. Determination of chlorine gas from fixed pollution sources, iodometric method (provisional) (HJ 547-2009);
XI. Determination of hydrogen chloride in fixed source pollution. Silver nitrate capacity method (provisional) (HJ 548-2009);
12. Determination of hydrogen chloride in ambient air and exhaust gas Ion chromatography (interim) (HJ 549-2009);
XIII. Determination of total cobalt in water quality 5-chloro-2-(pyridylazo)-1,3-diaminobenzene spectrophotometry (provisional) (HJ 550-2009);
14. Determination of Chlorine Dioxide in Water Quality Iodometric Method (Provisional) (HJ 551-2009).
The above standards have been implemented since April 1,.2010 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
Special announcement.
December 30,.2009
Content
Foreword..iv
1 Scope..1
2 Normative references..1
3 method principle..1
4 Reagents and materials.1
5 instruments and equipment. 2
6 samples.3
7 Analysis steps..3
8 result calculation..4
9 Quality Assurance and Quality Control 4
10 Notes 4
Appendix A (informative) Determination of adsorption efficiency of sulfhydryl cotton 5
Appendix B (informative appendix) Mercury removal method.6
Foreword
To protect the environment and protect people 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
This standard is established for the health of the body and the monitoring methods for the regulation of mercury and its compounds in the ambient air.
This standard specifies the enthalpy-based cotton enrichment cold atomic fluorescence spectrophotometry for the determination of mercury and its compounds in ambient air.
Appendix A and Appendix B of this standard are informative annexes.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard was drafted. Beijing Environmental Protection Monitoring Center.
This standard was approved by the Ministry of Environmental Protection on December 30,.2009.
This standard has been implemented since April 1,.2010.
This standard is explained by the Ministry of Environmental Protection.
Iv
Determination of mercury in ambient air
Sulfhydryl Cotton Enrichment-Cold Atomic Fluorescence Spectrophotometry (Provisional)
1 Scope of application
This standard specifies the sulfhydryl cotton enrichment-cold atomic fluorescence spectrophotometry for the determination of mercury and its compounds in ambient air.
This standard applies to the determination of mercury and its compounds in ambient air.
The detection limit of this standard method is 0.1 ng/10 ml sample solution. When the sampling volume is 15 L, the detection limit is 6.6×10−6 mg/m3.
The lower limit is 2.6 × 10−5 mg/m3.
2 Normative references
The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this standard.
HJ/T 194 Technical Specifications for Manual Air Quality Monitoring
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle of the method
In a slightly acidic medium, mercapto cotton is used to enrich mercury and its compounds in ambient air.
The inorganic mercury reaction formula is as follows.
Hg2 2H SR Hg
SR
SR
2H
The organic mercury reaction formula is as follows.
CH3HgCl H-SR CH3Hg-SR HCl
When elemental mercury passes through the sulfhydryl cotton sampling tube, it is mainly physical adsorption and chemical adsorption of monolayers.
After sampling, total mercury was desorbed with a 4.0 mol/L hydrochloric acid-sodium chloride saturated solution, reduced to metallic mercury by stannous chloride, and measured by cold atomic fluorescence.
The mercury meter measures the total mercury content.
4 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. Water, GB/T 6682, two.
4.1 High purity nitrogen. φ = 99.999%.
4.2 Potassium dichromate (K2Cr2O7). excellent grade pure.
4.3 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
4.4 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
4.5 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
4.6 Potassium dichromate solution. w (K2Cr2O7) = 1.0%.
Weigh 1.0 g of potassium dichromate (4.2), dissolve in water, and dilute to 100 ml.
4.7 Sulfuric acid solution. φ (H2SO4) = 10%.
Measure 10 ml of concentrated sulfuric acid (4.3) and slowly add 90 ml of water.
4.8 Hydrochloric acid solution. c (HCl) = 4.0 mol/L.
Measure 123 ml of hydrochloric acid (4.4), dilute to 1 000 ml with water, and mix.
4.9 Hydrochloric acid solution. c (HCl) = 2.0 mol/L.
Measure 12 ml of hydrochloric acid (4.4), dilute to 1 000 ml with water, and mix.
4.10 Hydrochloric acid solution. pH=3.
Pipette 2.0 mol/L hydrochloric acid (4.9) 0.50 ml, dilute with water to 1 000 ml, and mix.
4.11 Nitric acid solution. φ (HNO3) = 10%.
Measure 10 ml of concentrated nitric acid (4.5), dilute to 100 ml with water, and mix.
4.12 Hydrochloric acid-sodium chloride saturated solution
Add an appropriate amount of solid sodium chloride (NaCl) to a 4.0 mol/L hydrochloric acid solution (4.8) and heat to boiling until the sodium chloride is supersaturated.
until.
4.13 Potassium bromate-potassium bromide solution
Weigh 2.8 g of potassium bromate (KBrO3) and 10.0 g of potassium bromide (KBr), dissolve in water, and dilute to 1 000 ml.
4.14 Hydroxylamine Hydrochloride-Sodium Chloride Solution
Weigh 12.0 g of hydroxylamine hydrochloride (NH2OH·HCl) and 12.0 g of sodium chloride, dissolve in water, and dilute to 100 ml.
4.15 Stannous chloride hydrochloride solution. w = 10%.
Weigh 11.9 g of stannous chloride (SnCl2·2H2O) in a 150 ml beaker, add 10 ml of concentrated hydrochloric acid (4.4), and heat until completely dissolved.
Thereafter, it was diluted with water to 100 ml, and high-purity nitrogen (4.1) was introduced at a flow rate of 1.0 L/min to remove background mercury.
4.16 Standard stock solution of mercury chloride. ρ (HgCl2) = 1 000 μg/ml.
Accurately weigh 0.135 3 g of mercuric chloride (HgCl2), dissolved in 5.0 ml of 10% sulfuric acid solution (4.7) and 1.0 ml of 1.0% weight
In a potassium chromate solution (4.6), transfer to a 100 ml volumetric flask and dilute to the mark with water. This solution contains 1 000 μg of mercury per ml.
4.17 Standard use of mercury chloride. ρ (HgCl2) = 0.50 μg/ml.
Pipette 1.00 ml of standard stock solution of mercuric chloride (4.16), place in a.200 m1 volumetric flask, add 10.0 ml of 10% sulfuric acid solution (4.7)
And 2.0 ml of 1.0% potassium dichromate solution (4.6), diluted with water to the mark, this solution contains 5 μg of mercury per ml. Before use, suck
Take 10.00 ml of the above solution in a 100 ml volumetric flask, add 5.0 mL of 10% sulfuric acid solution (4.7) and 1.0 ml of 1.0% heavy chromium.
Potassium acid solution (4.6), diluted with water to the mark, this solution contains 0.50 μg of mercury per ml.
4.18 巯 base cotton
Add 20 ml of thioglycolic acid (HSCH2COOH), 17.5 ml of acetic anhydride [(CH3CO)2O], 8.5 ml of 36% acetic acid
(CH3COOH), 0.10 ml of sulfuric acid (4.3) and 1.6 ml of water in a 150 m1 beaker and mix well. When the solution temperature drops to 40 ° C
After that, transfer to a brown jar containing 5 g of absorbent cotton, soak the cotton evenly and cover with a stopper. Place in an oven and place at 40 ° C for 4 d
After removal, it was placed in a Buchner funnel with two layers of medium-speed quantitative filter paper, suction filtered, and washed with water until neutral. Drain the water and transfer it to the Petri dish.
It is dried in an oven at 40 ° C, stored in a brown bottle, and placed in a desiccator for 3 months.
5 Instruments and equipment
Unless otherwise stated, the analysis uses a Class A glass gauge that complies with national standards.
5.1 Air sampler. The flow range is 0~1 L/min.
5.2 Cold atomic fluorescence mercury detector.
5.3 巯 base cotton sampling tube. quartz, as shown in Figure 1.
4~5
Unit. mm
Figure 1 Quartz sampling tube
Weigh 0.1 g of sulphur-based cotton, insert it into the tube from the large diameter end of the quartz sampling tube, and press it into the tube section with an inner diameter of 6 mm.
It is about 3 cm. The sulfhydryl cotton was acidified with 0.40 ml of a hydrochloric acid solution (4.10) of pH=3 immediately before use. The ends of the sulphur-based cotton sampling tube shall be sealed with a sleeve.
Store in a mercury-free container.
5.4 Buchner funnel.
5.5 Filtering device.
5.6 Oven.
5.7 Mercury reaction bottle. 5 ml.
5.8 Syringe. 50 μl, 1 ml.
6 samples
6.1 Sample collection
The sample should be collected in accordance with the requirements of HJ/T 194. The sampler should be airtight and flow calibrated before use. The sampling system consists of
The air sampler and the sulphur-based cotton sampling tube are composed.
Connect the fine end of the sputum-based cotton sampling tube to the sampler, and the large-diameter end is facing downward, with a flow rate of 0.3-0.5 L/min, sampling for 30-60 min,
Avoid using fingers to smear the end of the tube of cotton.
6.2 Preservation of samples
After sampling, the ends are sealed and stored at 0~4 °C in cold storage.
6.3 Preparation of samples
Fix the sampled sputum-based cotton sampling tube and insert the thin end into the bottle mouth of the 10 ml volumetric flask, and add 4.0 mol/L at 1-2 ml/min.
Hydrochloric acid-sodium chloride saturated solution (4.12), eluting mercury and its compounds, diluted with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12) to
Mark the line and shake it.
6.4 Preparation of blank samples
Take a blank sputum-based cotton sampling tube and perform the same step at the same time as (6.3) sample processing to prepare a blank sample.
7 Analysis steps
7.1 Preparation of samples
Draw an appropriate amount of sample solution (6.3) into a 5 ml mercury reaction flask and dilute with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12).
Marking.
7.2 Preparation of blank samples
Draw an appropriate amount of blank sample solution (6.4) in a 5 ml mercury reaction flask and dilute with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12).
Released to the marking line.
7.3 Drawing of standard curve
7.3.1 Take 7 5 ml mercury reaction bottles and prepare a standard series according to Table 1.
Table 1 Standard series of mercury chloride
Bottle number 0 1 2 3 4 5 6
Standard use of mercury chloride/μl 0.00 5.00 10.0 20.0 30.0 40.0 50.0
Mercury content/ng 0.00 2.50 5.00 10.0 15.0 20.0 25.0
7.3.2 Dilute to 5 ml mark with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12).
7.3.3 Add 0.10 ml potassium bromate-potassium bromide (4.13) solution to each bottle, place it for 5 min, then appear yellow, add 1 drop of hydroxylamine hydrochloride-
Sodium chloride solution (4.14), let the yellow fade and shake.
7.3.4 Add 1.0 ml of stannous chloride hydrochloride solution (4.15) to the bottle with a syringe. After shaking for 0.5 min, use high purity nitrogen (4.1).
Mercury vapor is blown into a cold atomic fluorescence mercury analyzer to measure the mercury value (ng) of the mercury meter, draw a standard curve, and calculate the standard curve.
The regression equation of the line.
7.4 Determination
The measurement of the sample (7.1) and the blank sample (7.2) was carried out according to the drawing procedure of the standard curve, 7.3.3 to 7.3.4, and the response value was recorded. root
According to the measured values of the sample and the blank sample, the mercury content in the sample and the blank sample was calculated from the regression equation of the standard curve.
8 Calculation of results
Calculate the mercury content in ambient air according to formula (1).
ρ (Hg)= 0
And 1000
WWV
VV
T− ×× (1)
Where. ρ (Hg) - the amount of mercury in the ambient air, mg/m3;
W--the amount of mercury in the sample taken during the measurement, ng;
W0--the content of mercury in the blank taken during the measurement, ng;
Vt--the total volume of the sample solution, ml;
Va--the volume of the sample solution taken during the measurement, ml;
Vnd - the sampling volume under standard conditions (101.325 kPa, 273 K), L.
9 Quality Assurance and Quality Control
9.1 Quality assurance and quality control are carried out in accordance with HJ/T 194.
9.2 Test reagents, including sulfhydryl cotton (4.18), 10% stannous chloride solution (4.15), pH=3 hydrochloric acid solution (4.10),
Potassium bromate-potassium bromide solution (4.13), hydroxylamine hydrochloride-sodium chloride solution (4.14) and 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12)
Etc., all need to be checked by cold atomic fluorescence mercury detector in advance, the blank value of mercury in the reagent should not exceed 0.1 ng.
9.3 The mercury recovery test is carried out after the preparation of each batch of thiol cotton (see Appendix A).
10 Precautions
10.1 Hydroxylamine hydrochloride often contains mercury and must be purified. When the mercury content is low, the mercapto-based cotton fiber tube is used for mercury removal; when the mercury content is high, first press
The extraction method removes a large amount of mercury and then removes mercury according to the sulfhydryl cotton fiber tube method (see Appendix B).
10.2 If the organic mercury and inorganic mercury are to be separately measured, after sampling, place the sulphur-based cotton sampling tube on the bottle mouth of the 5 ml volumetric flask at 1 ml/min.
At the flow rate, 2.0 mol/L hydrochloric acid solution (4.9) was added dropwise to desorb organic mercury. Dilute to the mark with 2.0 mol/L hydrochloric acid solution (4.9), the following steps
The same drawing of the standard curve. Continue to desorb the inorganic mercury from the above sampling tube with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12).
The same as before.
10.3 The method can also measure particulate mercury and gaseous mercury separately, and can add an organic cellulose microporous membrane to capture the sulfhydryl cotton sampling tube.
Granular mercury. It was dissolved in a 10% nitric acid solution (4.11), and mercury was measured by the above method.
Appendix A
(informative appendix)
Determination of adsorption efficiency of sulfhydryl cotton
Add mercury chloride standard solution (4.17) to stannous chloride hydrochloric acid solution (4.15), and then use nitrogen (4.1) to produce
Elemental mercury is introduced into the sulphur-based cotton sampling tube. Desorbed with 4.0 mol/L hydrochloric acid-sodium chloride saturated solution (4.12), and the recovery was determined to obtain a sulfhydryl group.
The adsorption efficiency of cotton on mercury.
Place 1 000 mg/kg methylmercury (CH3HgCl) in a 100 ml polyethylene bottle with a silicone rubber stopper, sealed and kept at temperature
It is 22 ° C. At this time, the concentration of methylmercury in the vapor is 27.8 ng/ml±4.1 ng/ml, and a certain volume of vapor is extracted with a gas-tight syringe.
The sample gas flow is injected into the sputum-based cotton sampling tube, and the organic mercury is desorbed with a 2.0 mol/L hydrochloric acid (4.9) solution, and the recovery rate is determined to obtain a thiol cotton pair.
The adsorption efficiency of organic mercury.
Appendix B
(informative appendix)
Mercury removal method
Mercury-based cotton fiber tube mercury removal method. a glass tube with an inner diameter of 6 to 8 mm and a length of about 100 mm, one end of which is thinned, or a liquid leakage of 500 ml
Fill the liquid pipe with 0.1~0.2 g sulphur-based cotton fiber (4.18), and remove the reagent to be purified by flowing once or twice at a rate of 10 ml/min.
Do not use mercury.
Extraction method. 250 ml of hydroxylamine hydrochloride solution was injected into a 500 ml separatory funnel, each time adding 15 ml of diphenylthiobarium (disulfide)
腙C13H12N4S) 0.1 g/L carbon tetrachloride (CCl4) solution, repeated extraction until the dithizone-containing carbon tetrachloride solution remains green
The color remains the same. It is then extracted with carbon tetrachloride to remove excess dithizone.
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