HJ 541-2009Yellow phosphorus production emission. Determination of gaseous arsenic. Silver diethyldithiocarbamate spectrophotometric method (English PDF)
黄磷生产废气 气态砷的测定 二乙基二硫代氨基甲酸银分光光度法(暂行)
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Issued by
Ministry of Ecology and Environment
Level / Type
National · Mandatory
Issue date
December 30, 2009
Implementation date
April 1, 2010
Scope
HJ 541-2009 is the English-translated version of 黄磷生产废气 气态砷的测定 二乙基二硫代氨基甲酸银分光光度法(暂行).
HJ 541-2009 — This standard specifies the silver diethyldithiocarbamate spectrophotometric method for the determination of gaseous arsenic and its compounds in the exhaust gas from yellow phosphorus production.
This standard applies to the determination of arsenic and its compounds in gaseous form in the exhaust gas of yellow phosphorus production. The detection limit of this method is 1.25 µg/5 ml silver diethyldithiocarbamate absorption.
When the gas volume is 15 L, the detection limit of arsenic is 0.08 mg/m3, the lower limit of determination is 0.32 mg/m3 (both in As).
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Document preview — HJ 541-2009
National Standard of the People's Republic of China
- ICS
- 13.040.40
- Classification
- Z 25
Issued by: Ministry of Ecology and Environment
Contents
- Foreword
- 1 Scope of application
- 2 Normative references
- 3 Principle of the method
- 4 Interference and elimination
- 5 Reagents and materials
- 5.9 Bromide nitric acid absorption solution
- 5.16 Lead acetate cotton
- 6 Instruments and equipment
- 7 Samples
- 7.1 Sample collection
- 7.2 Preservation of samples
- 7.3 Preparation of samples
- 7.4 Preparation of blank blank samples
- 8 Analysis steps
- 8.1 Drawing of standard curves
- 8.2 Sample analysis
- 8.3 Analysis of blank samples of the whole program
- 9 Calculation of results
- 10 Quality Assurance and Quality Control
- 11 Precautions
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 formulated for the health monitoring of arsenic and its compounds in the exhaust gas from yellow phosphorus production.
This standard specifies the silver diethyldithiocarbamate spectrophotometric method for the determination of arsenic and its compounds in the waste gas from yellow phosphorus production.
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.
Determination of gaseous arsenic in waste gas from yellow phosphorus production 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 silver diethyldithiocarbamate spectrophotometric method for the determination of gaseous arsenic and its compounds in the exhaust gas from yellow phosphorus production.
This standard applies to the determination of arsenic and its compounds in gaseous form in the exhaust gas of yellow phosphorus production.
The detection limit of this method is 1.25 µg/5 ml silver diethyldithiocarbamate absorption. When the gas volume is 15 L, the detection limit of arsenic is 0.08 mg/m3, the lower limit of determination is 0.32 mg/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 16157 Determination of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants 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
The gaseous arsenic and its compounds in the waste gas from the production of yellow phosphorus are absorbed by the brominated nitric acid absorption liquid, and the brominated nitric acid oxidizes the low-priced arsenide into pentavalent arsenic.
Compound, in an acidic solution, using potassium iodide and stannous chloride (KI-SnCl2) to reduce pentavalent arsenic to trivalent arsenic, adding zinc particles and acid, producing Producing new ecological hydrogen, further reducing trivalent arsenic to gaseous arsine (AsH3), and diethylamino group dissolved in chloroform (CHCl3) the action of silver dithiocarbamate (Ag·DDC) to form a purple-red complex, the absorbance is measured at 510 nm, and the yellow phosphorus can be calculated.
The content of arsenic and its compounds in the production of exhaust gas.
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.
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 Bromine water. rho (Br2) = 3.12 g/ml.
5.3 Hydrochloric acid. rho (HCl) = 1.19 g/ml, excellent grade pure.
5.4 Nitric acid. rho (HNO3) = 1.42 g/ml, excellent grade pure.
5.5 Hydrochloric acid solution. c (HCl) = 1 mol/L.
Measure 83 ml of hydrochloric acid (5.3) and dilute to 1 000 ml with water.
5.6 Hydrochloric acid solution. 3 2.
5.7 Nitric acid solution. 1 1.
5.8 Sodium hydroxide solution. c (NaOH) = 0.1 mol/L.
Weigh 4 g of sodium hydroxide (analytical grade) dissolved in water and dilute to 1000 ml.
5.9 Bromide nitric acid absorption solution
Nitric acid (5.4) plus bromine water (5.2) to saturation, or 60 ml of nitric acid solution (5.7), add 20 ml of bromine water (5.2). 0 to 4 ° C Store in cold storage.
5.10 Potassium iodide solution. rho (KI) = 150 g/L.
Weigh 15 g of potassium iodide and dissolve in 100 ml of water.
5.11 Stannous chloride solution. rho (SnCl2) = 400 g/L.
Weigh 48 g of stannous chloride (SnCl 2 · 2H 2 O), dissolve in 50 ml of hydrochloric acid (5.3), and add water to 100 ml.
5.12 Lead acetate solution. rho [Pb(CH3COO)2]=100 g/L.
Weigh 10 g of lead acetate and dissolve in 100 ml of water.
5.13 Silver diethylaminodithiocarbamate (Ag·DDC) absorption liquid. w(Ag·DDC)=0.25%.
Weigh 0.25 g of silver diethylaminodithiocarbamate (Ag·DDC), add 1.0 ml of triethylamine, dissolve in 100 ml of trichloromethane.
Shake well in alkane (CHCl3), stand overnight, filter, and store in the dark.
5.14 Standard stock solution of arsenic. rho (As) = 1.00 mg/ml.
Weigh 0.132 0 g arsenic trioxide (AS2O3, benchmark reagent, pre-baked at 105-110 ° C for 2 h), dissolved in 2.0 ml of hydroxide in the sodium solution (5.8), add 50 ml of water and 2.0 ml of hydrochloric acid solution (5.6). Transfer to a 100 ml volumetric flask and dilute with water to the score line. This solution the solution contains 1.00 mg of arsenic per ml.
A standard solution for arsenic can also be used as a standard solution.
5.15 Arsenic standard use solution. rho (As) = 1.00 µg/ml.
When used, the standard stock solution of arsenic (5.14) is diluted with water to a standard solution containing 1.00 µg of arsenic per ml.
5.16 Lead acetate cotton
Immerse 10 g of cotton wool in 100 ml lead acetate solution (5.12), 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 Flue gas sampler. The flow range is 0~2.0 L/min, and the accuracy is better than ±2.5%.
6.2 Flue gas sampler cooling device.
6.3 Impact absorption bottle; 25 ml.
6.4 Visible spectrophotometer. with a 10 mm cuvette.
6.5 Electric heating plate.
6.6 Arsenic hydrogen generation and absorption device. As shown in Figure 1, the connecting pipe and the absorption pipe should be washed and dried before use.
Phi8~9
Grinding mouth 5 ml
Phi8
Phi11
3 unit. mm
D20
1-conical flask; 2-air pipe; 3-absorbent pipe; 4-acetate lead cotton
Figure 1 Arsenic hydrogen generation and absorption device
7 Samples
7.1 Sample collection
The sampling position, sampling point and sampling method are implemented in accordance with the relevant provisions of GB 16157. Sampling with a flue gas sampler, gas in the sampling tube A cooling device is installed at the mouth. Two impact absorption bottles containing 25 ml of brominated nitric acid absorbing solution (5.9) in series, in impact absorption bottles A buffer bottle containing sodium hydroxide solution (5.8) is connected in series with the flue gas sampler. Collect at a flow rate of 0.5 L/min for 15 to 30 minutes.
Record the sampling conditions in detail.
7.2 Preservation of samples
The collected samples should be sealed, stored at 0~4 °C, and measured within 7 days.
7.3 Preparation of samples
Pour the sample (7.1) from the two absorption tubes into a beaker, heat and evaporate on a hot plate, and concentrate to about 10 ml to make it completely Oxidation, add 10 ml of hydrochloric acid solution (5.6), continue to drive bromine until the solution is colorless, and obtain the sample solution. This operation is in the fume hood Row.
7.4 Preparation of blank blank samples
Take the blank absorbent prepared at the same time, transport and store it at the same time, and prepare a blank blank sample according to 7.3.
8 Analysis steps
8.1 Drawing of standard curves
8.1.1 Take 8 sets of arsenic hydrogen generator bottles and prepare standard series according to Table 1.
Table 1 arsenic standard series
Bottle number 0 1 2 3 4 5 6 7 Arsenic standard use solution/ml 0.00 1.00 2.00 3.00 5.00 10.0 15.0 20.0 Water/ml 70 69 68 67 65 60 55 50 Arsenic content/µg 0.00 1.00 2.00 3.00 5.00 10.0 15.0 20.0
8.1.2 Add 30 ml hydrochloric acid solution (5.6), 2.0 ml potassium iodide solution (5.10), 0.4 ml stannous chloride to each bottle in 8.1.1.
Solution (5.11), mix and let stand for 15 min.
8.1.3 Add 5.0 g of arsenic-free zinc (5.1) to the solution of 8.1.2, immediately with a filter containing lead acetate (5.16) and 5.0 ml the absorption tube of Ag·DDC absorption liquid (5.13) was connected, and after reacting for 1 h, chloroform was added to each absorption tube to 5.0 ml.
8.1.4 At a wavelength of 510 nm, use a 10 mm cuvette with chloroform as a reference to measure the absorbance and subtract the blank from the arsenic content.
The absorbance is plotted against a standard curve and the standard curve regression equation is calculated.
8.2 Sample analysis
Transfer the sample (7.3) to the hydrogen arsenide generator bottle, add 20 ml hydrochloric acid solution (5.6), 70 ml water, 2.0 ml potassium iodide solution (5.10).
0.4 ml of stannous chloride solution (5.11), shake well and let stand for 15 min. The following sample steps 8.1.3 to 8.1.4 are drawn with the standard curve.
The absorbance of the solution was calculated from the standard curve to determine the arsenic content in the sample solution.
8.3 Analysis of blank samples of the whole program
The whole procedure blank sample analysis step is the same as the sample analysis (8.2), and the absorbance of the whole program blank sample solution is measured, which is calculated from the standard curve.
The arsenic content in the blank sample solution of the whole program.
9 Calculation of results
Calculate the mass concentration of arsenic and its compounds in the waste gas from yellow phosphorus production according to formula (1).
rho -= (1)
Where. rho (As)--the mass concentration of arsenic and its compounds in the waste gas from yellow phosphorus production, mg/m3;
M--the arsenic content in the sample solution found from the standard curve, µg;
M0--the arsenic content in the whole program blank sample solution found from the standard curve, µg;
Vnd - the volume of gas production in the standard state (101.325 kPa, 273 K), L.
10 Quality Assurance and Quality Control
Quality assurance and quality control measures are implemented in accordance with the relevant provisions of HJ/T 373.
11 Precautions
11.1 AsH3 reacts with Ag·DDC to form red elemental colloidal silver, which promotes reduction when organic base and pyridine are present in chloroform.
And can increase the stability of red elemental colloidal silver in the solvent.
11.2 The rate of occurrence of arsine is greatly affected by the size, surface state and amount of zinc particles, reaction acidity and temperature. Zinc grain is 10~ 20 mesh, the surface is rough, the effect is the same with 3~5 g. The acidity of sulfuric acid during the reaction is preferably 2.3 to 2.5 mol/L. Acidity is too high, anti it should be too fast, the absorption is not complete; the acidity is too low, the reaction is too slow, the agitation of the bubbles in the reactor is not good, and the reaction may be incomplete. But warm the degree is too high and the reaction is too fast, which may result in incomplete absorption of AsH3 and the result is low. If the room temperature is higher than 30 ° C, the bottle can be placed in cold water Cool in the bath.
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Related Standards
GB/T 16157-1996 — Determination of particulates and sampling methods of gaseous pollutants emitted from exhaust gas of stationary source
GB/T 6682-2008 — Water for analytical laboratory use - Specification and test methods
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