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HJ 533-2009

Chinese Standard: 'HJ 533-2009'
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HJ 533-2009English229 Add to Cart Days<=3 Ambient air exhaust gas. Determination of ammonia. Nesslerreagent spetcrophotometry Valid HJ 533-2009
HJ 533-2009Chinese14 Add to Cart <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]

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Detail Information of HJ 533-2009; HJ533-2009
Description (Translated English): Ambient air exhaust gas. Determination of ammonia. Nessler's reagent spetcrophotometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 9,954
Date of Issue: 2009-12-31
Date of Implementation: 2010-04-01
Older Standard (superseded by this standard): GB/T 14668-1993
Drafting Organization: Shenyang Municipal Environmental Monitoring Center Station
Administrative Organization: Ministry of Environment Protection
Regulation (derived from): Department of Environmental Protection Notice 2009 No. 77
Summary: This standard specifies the determination of ambient air and industrial emissions of ammonia Nessler's reagent spectrophotometry. This standard applies to the determination of ammonia in ambient air, but also for the pharmaceutical, chemical, coking and other industries Determination of ammonia in the exhaust gas.


HJ 533-2009
Ambient air exhaust gas.Determination of ammonia.Nesslerreagent spetcrophotometry
National Environmental Protection Standard of the People's Republic
Replace GB/T 14668-93
Determination of ambient air and exhaust ammonia
Nessler reagent spectrophotometry
Ambient air and exhaust gas-Determination of ammonia
-Nessler's reagent spetcrophotometry
Published on December 12,.2009
2010-04-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 77 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 "Ammonia of ambient air and exhaust gas.
The five standards, such as the determination of Nessler's reagent spectrophotometry, are national environmental protection standards and are released.
The standard name and number are as follows.
2. Determination of Ammonia in Ambient Air - Sodium Hypochlorite - Salicylic Acid Spectrophotometry (HJ 534-2009);
3. Determination of Ammonia Nitrogen in Water Quality by Nessler Reagent Spectrophotometry (HJ 535-2009);
4. Determination of Ammonia Nitrogen in Water Quality by Salicylic Acid Spectrophotometry (HJ 536-2009);
V. Determination of Ammonia Nitrogen in Water Quality - Neutralization and Titration (HJ 537-2009).
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.
From the date of implementation of the above standards, the following five national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The name and number are as follows.
I. Determination of Air Quality Ammonia by Nessler Reagent Colorimetric Method (GB/T 14668-93);
2. Determination of Ammonia for Air Quality - Sodium Hypochlorite - Salicylic Acid Spectrophotometry (GB/T 14679-93);
Third, "the determination of ammonium water quality Nessler reagent colorimetric method" (GB 7479-87);
4. Determination of Ammonium in Water Quality by Salicylic Acid Spectrophotometry (GB 7481-87);
V. Determination of Distillation and Titration of Ammonium Water (GB 7478-87).
Special announcement.
December 31,.2009
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 interference and elimination.1
4 Reagents and materials.1
5 instruments and equipment. 2
6 samples. 2
7 Analysis steps..3
8 result calculation..3
9 Accuracy and precision..4
10 Quality Assurance and Quality Control.4
Foreword
To protect the environment and protect the human body in order to implement the "Environmental Protection Law of the People's Republic of China"
Health, standard ammonia monitoring methods, the development of this standard.
This standard specifies the Nessler's reagent spectrophotometric method for the determination of ammonia in ambient air and industrial waste gases.
This standard amends the "Air Quality Ammonia Determination of Nessler Colorimetric Method" (GB/T 14668-93).
This standard was first published in.1993, and the original standard drafting unit is the Shanghai Environmental Protection Monitoring Center. This is the first revision. this time
The main contents of the revision are as follows.
-- Added warnings.
-- Increased sampling method and detection limit of 10 ml of absorbent volume.
-- Added quality assurance and quality control provisions, including. no ammonia water check, sampling full blank, reagent preparation and sampling
Precautions, etc.
-- Combine the calculation formula of the result.
As of the date of implementation of this standard, the air quality ammonia test approved and issued by the former National Environmental Protection Agency on October 27,.1993
The Dina reagent colorimetric method (GB/T 14668-93) is abolished.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Shenyang Environmental Monitoring Center Station.
This standard was approved by the Ministry of Environmental Protection on December 31,.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 ammonia - Nessler reagent spectrophotometry
WARNING. Mercury dichloride (HgCl2) and mercury iodide (HgI2) are highly toxic substances and are protected from skin and oral contact.
1 Scope of application
This standard specifies the Nessler's reagent spectrophotometric method for the determination of ammonia in ambient air and industrial waste gases.
This standard is applicable to the determination of ammonia in ambient air, and is also applicable to the determination of ammonia in the exhaust gas of pharmaceutical, chemical, coking and other industrial industries.
The method detection limit of this standard is 0.5 μg/10 ml of absorption solution. When the volume of the absorbent is 50 ml and the gas is 10 L, the detection limit of ammonia is
0.25 mg/m3, the lower limit of determination is 1.0 mg/m3, and the upper limit of determination is 20 mg/m3. When the volume of the absorbent is 10 ml and the gas is 45 L, the ammonia
The detection limit was 0.01 mg/m3, the lower limit of determination was 0.04 mg/m3, and the upper limit of determination was 0.88 mg/m3.
2 Principle of the method
Absorption of ammonia in the air with a dilute sulfuric acid solution, the resulting ammonium ions react with the Nessler reagent to form a yellow-brown complex, and the absorbance of the complex
The degree is proportional to the ammonia content, the absorbance is measured at a wavelength of 420 nm, and the ammonia content in the air is calculated based on the absorbance.
3 interference and elimination
Interference measurement when metal ions, sulfides, and organics such as ferric iron are contained in the sample can be eliminated by the following methods.
3.1 Metal ions such as trivalent iron
In the analysis, 0.50 ml of sodium potassium tartrate solution (4.6) was used to form a mask to eliminate the interference of metal ions such as ferric iron.
3.2 Sulfide
If the sample is disturbed by the occurrence of a heterochromatic color (such as green when the sulfide is present), dilute hydrochloric acid may be added to the sample solution to remove the dry matter.
Disturb.
3.3 Organics
Some organic substances (such as formaldehyde) produce precipitation interference measurement, and the absorption liquid can be used with 0.1 mol/L hydrochloric acid solution (4.7) before colorimetry.
Acidify to a pH not greater than 2 and then boil it.
4 reagents and materials
Unless otherwise stated, the reagents used in the analysis were analyzed analytical reagents in accordance with national standards, and the experimental water was prepared according to 4.1.
water.
4.1 No ammonia water, prepared in one of the following ways in an ammonia-free environment (see 10.1 for inspection without ammonia).
4.1.1 Ion exchange method
The distilled water was passed through a column of strongly acidic cation exchange resin (hydrogen type), and the effluent was collected in a ground glass bottle. Per liter of effluent
Add 10 g of strong acid cation exchange resin (hydrogen type) for easy storage.
4.1.2 Distillation method
0.1 ml of sulfuric acid (4.2) was added to 1 000 ml of distilled water and redistilled in a full glass distiller. Discard the first 50 ml of distillate, then
Approximately 800 ml of distillate was then collected in a ground glass vial. 10 g of strong acid cation exchange resin (hydrogen) per liter of distillate collected
Type), in order to save.
4.1.3 Water Purifier Method
Prepared with a commercially available water purifier before use.
4.2 Sulfuric acid, ρ(H2SO4) = 1.84 g/ml.
4.3 Hydrochloric acid, ρ(HCl) = 1.18 g/ml.
4.4 Sulfuric acid absorption solution, c(1/2H2SO4)=0.01 mol/L.
2.8 ml of sulfuric acid (4.2) was added to the water and diluted to 1 L to obtain a 0.1 mol/L stock solution. Dilute 10 times with water when it is ready.
4.5 Nessler Reagent
Weigh 12 g of sodium hydroxide (NaOH) dissolved in 60 ml of water and cool;
Weigh 1.7 g of mercury dichloride (HgCl2) dissolved in 30 ml of water;
Weigh 3.5 g of potassium iodide (KI) in 10 ml of water, and slowly add the above mercury dichloride solution to the potassium iodide solution while stirring.
Until the red precipitate formed is no longer dissolved;
Slowly add the sodium hydroxide solution cooled to room temperature to the above mixture of mercury dichloride and potassium iodide while stirring, and then add
The remaining mercury dichloride solution was mixed and allowed to stand in the dark for 24 h. The supernatant was decanted, stored in a brown bottle, and stoppered with a rubber stopper, 2 to 5
°C can be stored for 1 month.
4.6 Potassium sodium tartrate solution, ρ = 500 g/L.
Weigh 50 g of sodium potassium tartrate (KNaC4H6O6·4H2O) dissolved in 100 ml of water, heat and boil to drive off ammonia, and then cool to volume.
100 ml.
4.7 Hydrochloric acid solution, c (HCl) = 0.1 mol/L.
Take 8.5 ml of hydrochloric acid (4.3), add a certain amount of water, and dilute to 1 000 ml.
4.8 Ammonia standard stock solution, ρ(NH3)=1 000 μg/ml.
Weigh 0.785 5 g of ammonium chloride (NH4Cl, pure grade, dried at 100-105 ° C for 2 h), dissolve in water, and transfer to a 250 ml volumetric flask.
Dilute to the mark with water.
4.9 Ammonia standard use solution, ρ(NH3)=20 μg/ml.
Pipette 5.00 ml of ammonia standard stock solution (4.8) into a 250 ml volumetric flask, dilute to volume, and shake well. Prepare before use.
5 Instruments and equipment
5.1 Gas sampling device. The flow rate ranges from 0.1 to 1.0 L/min.
5.2 Glass tube absorption tube or atmospheric impact absorption tube. 125 ml, 50 ml or 10 ml.
5.3 with colorimetric tube. 10 ml.
5.4 Spectrophotometer. with a 10 mm pathlength cuvette.
5.5 Glass containers. certified volumetric flasks, pipettes.
5.6 Teflon tube (or glass tube). inner diameter 6 ~ 7 mm.
5.7 Drying tube (or buffer tube). Contains discolored silica gel or glass wool.
6 samples
6.1 Preparation of sampling tube
The absorbent tube with good air tightness, resistance and absorption efficiency should be cleaned and dried for use. Fill the absorbent and seal it before sampling
Keep away from light.
6.2 Sample Collection
The sampling system consists of a sampling tube, a drying tube and a gas sampling pump. Sampling should be carried out with a full blank absorbing tube.
Ambient air sampling. Collect with a 10 ml absorption tube at a flow rate of 0.5 to 1 L/min for at least 45 minutes.
Industrial waste gas sampling. Use a 50 ml absorption tube to collect at a flow rate of 0.5 to 1 L/min. The gas collection time depends on the specific conditions. If industry
When the temperature of the exhaust gas (such as flue gas) is significantly higher than the ambient temperature, the sampling line should be heated to prevent condensation of flue gas in the sampling line.
6.3 Sample storage
It should be analyzed as soon as possible after sampling to prevent absorption of ammonia from the air. If it can not be analyzed immediately, it can be stored for 7 days at 2~5 °C.
7 Analysis steps
7.1 Drawing a calibration curve
Take 7 10 ml plug color tubes and prepare a standard series according to Table 1.
Table 1 Standard series
Pipe number 0 1 2 3 4 5 6
Standard solution (4.9)/ml 0.00 0.10 0.30 0.50 1.00 1.50 2.00
Water/ml 10.00 9.90 9.70 9.50 9.00 8.50 8.00
Ammonia content/μg 0 2 6 10 20 30 40
Accurately remove the corresponding standard volume of liquid (4.9) according to Table 1, add water to 10 ml, and add 0.50 ml of potassium tartrate to each tube.
Sodium solution (4.6), shake well, then add 0.50 ml of Nessler reagent (4.5) and shake well. After 10 minutes of placement, at a wavelength of 420 nm,
The absorbance was measured using a 10 mm cuvette with water as a reference. Taking the ammonia content (μg) as the abscissa, the absorbance of the reagent blank is taken as the vertical sitting
Draw a calibration curve.
7.2 Sample determination
Take a certain amount of sample solution (depending on the sample concentration) in a 10 ml colorimetric tube and dilute to 10 ml with the absorption solution (4.4).
Add 0.50 ml of sodium potassium tartrate solution (4.6), shake well, add 0.50 ml of Nessler's reagent (4.5), shake well, leave for 10 min, then
The absorbance was measured at a wavelength of 420 nm using a 10 mm cuvette with water as a reference.
7.3 Blank test
7.3.1 Absorbent blank. Replace the sample with the absorbent prepared in the same batch as the sample and measure the absorbance according to 7.2.
7.3.2 Sampling the whole process blank. the corresponding volume of the absorption liquid prepared in the same batch as the sample is added to the sampling tube and brought to the sampling site.
For the sampled absorbent, measure the absorbance according to 7.2.
8 Calculation of results
The ammonia content is calculated by equation (1).
Nd 0
( )
(NH ) s
AA a V
b VV
ρ − − ×= × × (1)
Where. ρ(NH3)--ammonia content, mg/m3;
A--the absorbance of the sample solution;
A0--the absorbance of the blank of the absorption liquid prepared in the same batch as the sample;
A--calibration curve intercept;
B--the slope of the calibration curve;
Vs--the total volume of sample absorption liquid, ml;
V0--the volume of the absorbent taken during the analysis, ml;
Vnd--the volume of the gas sample under standard conditions (101.325 kPa, 273 K), L.
The volume Vnd in the standard state of the gas sample is calculated according to formula (2).
Nd
101.325 (273 )
V PV
× ×= × (2)
Where. V - sampling volume, L;
P--atmospheric pressure during sampling, kPa;
t--Sampling temperature, °C.
9 Accuracy and precision
Uniform samples containing 1.33 to 1.55 mg/L ammonia were analyzed by five laboratories with a repeatability limit of 0.018 mg/L and a coefficient of variation of 1.2%;
The limit was 0.05 mg/L, and the coefficient of variation was 3.4%. The recoveries were 97%-103%.
10 Quality Assurance and Quality Control
10.1 Inspection without ammonia
Replace the sample with water. Measure the absorbance according to 7.2. The blank absorbance value should not exceed 0.030 (10 mm cuvette), otherwise check the water and
The purity of the reagent.
10.2 Sampling full blank
It is used to check whether the sample is contaminated during sample collection, transportation and storage. If the sampling blank is significantly higher than the same batch of suction
When the liquid is blank, the samples collected in the same batch are discarded.
10.3 Preparation of Nessler's reagent
In order to ensure good color development of Nessler's reagent, it is necessary to control the amount of HgCl2 added during the preparation, until the trace amount of HgI2 is not precipitated.
Soon when dissolved. The ratio of HgCl2 to KI required to prepare 100 ml of the Nessler reagent is about 2.3.5. In order to speed up the reaction during preparation
Speed, saving preparation time, can be heated at low temperature to prevent the early precipitation of HgI2 red precipitate.
10.4 Preparation of potassium sodium tartrate
When the ammonium salt of sodium potassium tartrate reagent is high, only the boiling of the boiling or the precipitation of the drug is not completely removed. At this time, use less to join
The amount of sodium hydroxide solution is boiled to remove 20% to 30% of the volume of the solution, and after cooling, it is diluted to the original volume with ammonia-free water.
10.5 Proper use of the sampling pump
Before turning on the sampling pump, confirm that the sampling system is connected correctly. The inlet end of the sampling pump passes through the drying tube (or buffer tube) and the sampling tube.
The gas outlets are connected, and if they are reversed, the acid absorption liquid will be sucked up, contaminating and damaging the instrument. In case of reverse suction, the flow should be timely
Remove it, wash it with alcohol, dry it, and reinstall it. Continue to use it after passing the flow calibration.
10.6 Prevent the sampling tube from being contaminated
In order to avoid contamination of the absorption liquid in the sampling tube, do not tilt or invert the sampling tube during transportation and storage, and replace the sampling tube in time.
Seal the joint.
Related standard:   HJ 535-2009  HJ 536-2009
   
 
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