HJ 540-2016_English: PDF (HJ540-2016)
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| HJ 540-2016 | 229 |
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Stationary source emission - Determination of arsenic- Silver diethyldithiocarbamate spectrophotometric method
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| HJ 540-2009 | 359 |
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Ambient air and waste gas. Determination of arsenic. Silver diethyldithiocarbamate spectrophotometric method
| Obsolete |
| Standard ID | HJ 540-2016 (HJ540-2016) | | Description (Translated English) | Stationary source emission - Determination of arsenic- Silver diethyldithiocarbamate spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 10,130 | | Date of Issue | 2016-07-26 | | Date of Implementation | 2016-10-01 | | Older Standard (superseded by this standard) | HJ 540-2009 | | Regulation (derived from) | Ministry of Environmental Protection Notice No.52 of 2016 |
HJ 540-2016
(Determination of arsenic in fixed sources - Silver diethyldithiocarbamate spectrophotometric method)
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 540-2009
Determination of arsenic in fixed source
Silver dimethyldithiocarbamate spectrophotometric method
Stationary source emission - Determination of arsenic-Silver
Diethyldithiocarbamate spectrophotometric method
2016-07-26 release
2016-10-01 implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
Interference and elimination
5 reagents and materials 2
6 instruments and equipment 3
7 Sample 3
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 fixed source of waste gas in the form of particulate matter and the determination of arsenic and its compounds,
Develop this standard.
This standard specifies the determination of fixed sources of waste gas in the form of particulate matter and its compounds of diethyldisulfide
Substituted carbamate spectrophotometric method.
This standard is for the determination of "ambient air and waste arsenic, silver diethyldithiocarbamate spectrophotometric (provisional)"
(HJ 540-2009).
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.
- According to the scope of application of the standard, the original standard name "Ambient air and arsenic determination of diethyldithioamino
Formic acid silver spectrophotometric method (tentative) "modified to" fixed source of waste gas arsenic determination of diethyldithiocarbamate silver
Spectrophotometry";
- the contents of the ambient air and so on have been removed from the original standard;
- Based on the experimental results, the detection limit was revised from 0.00 μg/m3 to 0.004 mg/m3 and the lower limit of determination was 3.5 μg/m3
Revised to 0.016 mg/m3;
- the collection of samples and the preparation of samples and other content has been revised;
- increased precision and accuracy and other content;
- improve the quality assurance and quality control content;
- Increased waste disposal.
Since the implementation of the standard date, the original standard "Determination of ambient air and arsenic arsenic diethyldithiocarbamate
Photometric method (provisional) "(HJ 540-2009) abolished.
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, Beijing Xicheng District Environmental Protection Monitoring Station.
The standard verification unit. Yunnan Honghe State Environmental Monitoring Station, Beijing Changping District Environmental Protection Monitoring Station, Beijing Feng
Taiwan Environmental Protection Monitoring Station, Beijing Xicheng District Environmental Protection Monitoring Station, Beijing China measured North Detection Technology Co., Ltd.
The environmental protection department of this standard approved on July 26,.2016.
This standard has been implemented since October 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of arsenic in fixed source
Silver dimethyldithiocarbamate spectrophotometric method
Warning. arsine is a highly toxic gas, before the test must check whether the arsine generator is connected to prevent leakage or reaction
The bottle was disintegrated. The reaction shall be carried out in a fume hood, and the operator shall wear protective equipment.
1 Scope of application
This standard specifies the determination of fixed sources of waste gas in the form of particulate matter arsenic and its compounds diethyldithio
Silver phthalate spectrophotometric method.
This standard is applicable to the determination of arsenic and its compounds in the form of particulate matter in fixed waste gas.
When the sampling volume is 0.4 m3 (standard state), the volume of the volume is 50.0 ml, the detection limit of this method is 0.004 mg/m3,
The lower limit of determination is 0.016 mg/m3 (both in As).
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is applicable
In this standard.
Determination of particulate matter and sampling method of gaseous pollutants in exhaust gas of fixed pollution sources GB/T 16157
HJ/T 373 fixed pollution source monitoring quality assurance and quality control technical specifications (Trial)
HJ/T 48 smoke and dust sampler technical conditions
HJ 77.2 Ambient air and exhaust dioxins Determination of isotope dilution High resolution gas chromatography - High resolution mass spectrometry
3 Principle of the method
Using quartz fiber filter cartridge to collect fixed sources of waste gas containing arsenic particles, nitric acid, sulfuric acid, hydrogen peroxide digestion after preparation
The solution of pentavalent arsenic in this solution was reduced to trivalent arsenic with potassium iodide (KI) and stannous chloride (SnCl2 · 2H2O)
Zinc particles and acid, resulting in new ecological hydrogen, the trivalent arsenic further reduced to gaseous arsine (AsH3), and dissolved in trichloromethyl
(CH5H10AgNS2) in the alkylene chloride (CHCl3) to form a magenta complex at 510 nm
Absorbance measured at the wavelength, within a certain range of its absorbance and arsenic content is proportional to.
4 interference and elimination
Mercury, manganese, copper, nickel, cobalt, lead and iron, 100 μg or less of cadmium and antimony below 50 μg, bismuth below 30 μg,
20 μg or less of chromium, 10 μg of the following selenium, no significant interference with the determination. When the content of antimony in the sample is greater than 50 μg, the interference
Arsenic determination, adding 3 ml of stannous chloride and 5 ml of potassium iodide solution, can inhibit 300 μg of antimony interference. Sulfide interference,
Can be removed with lead acetate cotton.
5 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The experimental water is a freshly prepared deionized water
Or distilled water.
5.1 Arsenic free zinc tablets. 10 mesh to 20 mesh.
Note 1. The rate of occurrence of arsine is affected by the size, surface state and dosage of the zinc particles, the reaction acidity and the temperature. Zinc tablets to 10 to 20
The purpose of the surface rough zinc particles to restore the high efficiency, the amount of 3 g ~ 5 g between the effect is better.
5.2 Potassium iodide (KI).
5.3 Stannous chloride (SnCl2 · 2H2O).
5.4 Lead acetate [Pb (CH3COO) 2].
5.5 Diethyldithiocarbamate (C5H10AgNS2).
5.6 Arsenic trioxide (As2O3). Reference reagent.
Before use, in 105 ℃ ~ 110 ℃ bake 2 h, stored in the dryer cooling, spare.
5.7 Sodium hydroxide (NaOH).
5.8 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.9 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.10 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.11 Trichloromethane (CHCl3).
5.12 Triethanolamine [(HOCH2CH2) 3N].
5.13 Hydrogen peroxide. ω (H2O2) = 30%, excellent grade pure.
5.14 sulfuric acid solution. 1 1.
Prepared with sulfuric acid (5.9).
5.15 Potassium iodide solution. ρ (KI) = 150 g/L
Weigh 15 g of potassium iodide (5.2), dissolved in water and diluted to 100 ml beaker.
5.16 Stannous chloride solution. ρ (SnCl2 · 2H2O) = 400 g/L.
Weigh 48 g of stannous chloride (5.3), add 50 ml of hydrochloric acid (5.10), dissolve it by heating, and then diluted with water to 100 ml
Beaker, ready for use.
5.17 lead acetate solution. ρ [Pb (CH3COO) 2] = 100 g/L.
Weigh 10 g of lead acetate (5.4), dissolve in water and dilute to 100 ml beaker.
5.18 Silver diethyldithiocarbamate Absorbate. ω (C5H10AgNS2) = 0.25%.
Weigh 1.25 g of silver diethyldithiocarbamate (5.5), add 100 ml of trichloromethane (5.11) and 4 ml of tri
Alcohol (5.12) was stirred and diluted to 500 ml with trichloromethane (5.11), shaken, left overnight, filtered with absorbent cotton
In the brown reagent bottle, in the 4 ℃ below the cold, dark can be stored for 3 months.
5.19 Sodium hydroxide solution. ω (NaOH) = 40%.
Weigh 40 g of sodium hydroxide (5.7), dissolve with water and dilute to 100 ml beaker.
5.20 arsenic standard stock solution. ρ (As) = 1.00 mg/ml.
Accurately weigh 0.0660 g (accurate to 0.0001 g) arsenic trioxide (5.6), add 10 ml of sodium hydroxide solution (5.19),
Dissolved in heat. The whole volume into the 100 ml volumetric flask, dilute the volume to the mark with water. Store in a brown reagent bottle at 4 ° C or lower
Refrigerated, sealed for 3 months. You can also purchase commercially available certified materials.
5.21 arsenic standard use of liquid. ρ (As) = 1.00 μg/ml.
Arsenic standard stock solution (5.20) placed in room temperature, diluted with water preparation, temporary with the allocation.
5.22 lead acetate
10 g of absorbent cotton immersed in 100 ml of lead acetate solution (5.17), 30 min after the removal, at room temperature to dry, dark
Preserved in the grinding glass bottles, the preservation period of 1 year.
5.23 quartz fiber filter cartridge
Should be pre-baked in the muffle furnace at 300 ℃ for 3 h, placed in a dryer to cool to room temperature. The arsenic in the digestion of the blank filter cartridge
The amoun......
HJ 540-2009
Ambient air and waste gas.Determination of arsenic.Silver diethyldithiocarbamate spectrophotometric method
National Environmental Protection Standard of the People's Republic
Determination of ambient air and exhaust arsenic
Silver diethyldithiocarbamate spectrophotometry
(temporary)
Ambient air and waste gas-Determination of arsenic
-Silver diethyldithiocarbamate spectrophotometric method
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);
4. Determination of gaseous arsenic in the production of yellow phosphorus - Determination of silver diethyldithiocarbamate spectrophotometry (interim) (HJ 541-2009);
V. Determination of mercury in ambient air - Enrichment of sulfhydryl cotton - Cold atomic fluorescence spectrophotometry (interim) (HJ 542-2009);
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 Interference and elimination.1
5 Reagents and materials.1
6 instruments and equipment.2
7 samples.3
8 Analysis steps..3
9 result calculation..3
10 Quality Assurance and Quality Control.4
11 Notes 4
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 monitoring and regulation of arsenic and its compounds in air and exhaust gases.
This standard specifies the silver diethyldithiocarbamate spectrophotometric method for the determination of arsenic and its compounds in air and exhaust gases.
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 ambient air and exhaust arsenic
Silver diethyldithiocarbamate spectrophotometry (interim)
Warning. Arsine is a highly toxic gas. Before the experiment, it is necessary to check whether the hydrogen arsenide generator is connected to prevent air leakage or reverse.
The bottle should be broken. The reaction should be carried out in a fume hood.
1 Scope of application
This standard specifies the determination of silver and diethyldithiocarbamate in the presence of particulate matter in the air and exhaust gases.
Photometric method.
This standard applies to the determination of arsenic and its compounds in the form of particulate matter in air and exhaust gases.
When the method is to prepare a filter cartridge or filter into a 50 ml sample, the detection limit is 0.35 μg/50 ml (as As).
For organized exhaust emissions, the detection limit is 0.9 μg/m3 when the 400 L gas is collected, and the lower limit of determination is 3.5 μg/m3 (both
As count).
For air samples, the detection limit is 0.06 μg/m3 when the 6 m3 gas is collected, and the lower limit of determination is 0.24 μg/m3 (both in As).
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.
GB/T 15432 Determination of total suspended particulate matter in ambient air
GB/T 16157 Determination of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants
HJ/T 194 Technical Specifications for Manual Air Quality Monitoring
HJ/T 373 Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Source Monitoring (Trial)
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle of the method
Collecting particulate matter in organized exhaust gas with a glass fiber filter cartridge or quartz filter cartridge, and collecting particulate matter in the air with a perchloroethylene filter
Samples, the collected samples were treated with mixed acid digestion.
In an acidic solution, potassium pentaoxide and stannous chloride (KI-SnCl2) are used to reduce pentavalent arsenic to trivalent arsenic, and zinc particles are added to the acid to produce
New ecological hydrogen, further reducing trivalent arsenic to gaseous arsine (AsH3), and diethyldisulfide dissolved in chloroform (CHCl3)
The action of silver urethane (Ag·DDC) produces a purple-red complex and the absorbance is measured at a wavelength of 510 nm.
4 interference and elimination
Hydrogen sulfide, hydrogen halide, and phosphine have similar color reaction with Ag·DDC, which produces positive interference with the determination of arsenic. When the sample is digested,
Sulfur and phosphorus have been oxidized and decomposed by nitric acid, no longer affecting. Hydrogen sulfide produced by a small amount of sulfide present in the reagent can be removed by lead acetate absorbent cotton.
锑 can be masked with KI-SnCl2 below 300 μg.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. Water, GB/T 6682, third grade.
5.1 Arsenic-free zinc particles. 10 to 20 mesh.
5.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.4 Perchloric acid. ρ (HClO4) = 1.67 g/ml, excellent grade pure.
5.5 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.6 Sulfuric acid solution. 1 1.
5.7 Potassium iodide solution. ρ (KI) = 150 g/L.
Weigh 15 g of potassium iodide and dissolve in 100 ml of water.
5.8 Stannous chloride solution. ρ (SnCl2) = 400 g/L.
Weigh 48 g of stannous chloride (SnCl 2 · 2H 2 O), add 50 ml of hydrochloric acid (5.5), heat to dissolve, add water to 100 ml, add a few metals
Tin, kept in a brown bottle for later use.
5.9 Lead acetate solution. ρ[Pb(CH3COO)2]=100 g/L.
Weigh 10 g of lead acetate and dissolve in 100 ml of water.
5.10 Silver diethyldithiocarbamate (Ag·DDC) absorption liquid. w(Ag·DDC)=0.25%.
Weigh 1.25 g of silver diethyldithiocarbamate (Ag·DDC), add 100 ml of chloroform, 4 ml of triethanolamine, add four
Mix the carbon chloride to 500 ml, place it overnight, filter it into a brown bottle with absorbent cotton, and store it in the dark.
5.11 Arsenic standard stock solution. ρ (As) = 1.00 mg/ml.
Weigh 0.066 0 g of arsenic trioxide (reference reagent, dried at 105-110 ° C for 1 h), and dissolve with 10 ml of 40% NaOH solution.
solution. Transfer to a 100 ml volumetric flask and dilute to volume with deionized water. Store in brown bottles and store at low temperature. This solution per ml
Contains 1.00 mg of arsenic.
A standard solution for arsenic can also be used as a standard solution.
5.12 Arsenic standard use solution. ρ (As) = 1.00 μg/ml.
When used, the standard stock solution of arsenic (5.11) is diluted with water to a standard solution containing 1.00 μg of arsenic per ml.
5.13 lead acetate cotton
Immerse 10 g of cotton wool in 100 ml lead acetate solution (5.9), remove it after 30 min, dry at room temperature, and store in the dark.
6 Instruments and equipment
Unless otherwise stated, the analysis uses a Class A glass gauge that complies with national standards.
6.1 Soot sampler. The flow range is 5~50 L/min, and the accuracy is better than ±2%.
6.2 Medium flow particle sampler. The flow range is 80~130 L/min, and the accuracy is better than ±2%.
6.3 Visible spectrophotometer. with a 10 mm cuvette.
6.4 Glass fiber filter cartridge or quartz filter cartridge.
6.5 Perchloroethylene membrane. 0.45 μm.
6.6 Electric heating plate.
6.7 Arsenic hydrogen generation and absorption device. As shown in Figure 1, ......
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