HJ 534-2009 (HJ534-2009) & related versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | See Detail | Status | Similar PDF |
| HJ 534-2009 | English | 289 |
Add to Cart
|
3 days
|
Ambient air. Determination of ammonia. Sodium hypochlorite-salicylic acid spectrophotometry
|
HJ 534-2009
| Valid |
HJ 534-2009
|
HJ 534-2009: PDF in English
HJ 534-2009
Ambient air.Determination of ammonia.Sodium hypochlorite-salicylic acid spectrophotometry
National Environmental Protection Standard of the People's Republic
Replace GB/T 14679-93
Determination of ambient air ammonia
Sodium hypochlorite-salicylic acid spectrophotometry
Ambient air-Determination of ammonia
-Sodium hypochlorite-salicylic acid spectrophotometry
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.
I. Determination of Ammonia Reagent Spectrophotometry for Ambient Air and Exhaust Gas Ammonia (HJ 533-2009);
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..2
8 result calculation..3
9 Accuracy and precision..3
10 Quality Assurance and Quality Control.4
Appendix A (Normative) Preparation method of sodium hypochlorite solution and calibration of available chlorine concentration and free alkali concentration..5
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 sodium hypochlorite-salicylic acid spectrophotometric method for the determination of ammonia in ambient air.
This standard amends the determination of air quality ammonia by sodium hypochlorite-salicylic acid spectrophotometry (GB/T 14679-93).
This standard was first published in.1993. The original standard drafting unit was Shenyang Institute of Environmental Sciences. This is the first revision. This revision
The main contents are as follows.
-- Increased sampling of ambient air.
-- Identify the detection limits and lower limits of the method.
-- Added a full blank of sampling.
-- Combine the calculation formula.
-- Added normative appendices.
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
Sodium hypochlorite-salicylic acid spectrophotometry (GB/T 14679-93) is abolished.
Appendix A of this standard is a normative appendix.
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 ammonia - Sodium hypochlorite - salicylic acid spectrophotometric method
1 Scope of application
This standard specifies the sodium hypochlorite-salicylic acid spectrophotometric method for the determination of ammonia in ambient air.
This standard is applicable to the determination of ammonia in ambient air, and also to the determination of ammonia in the air of the foul odor source.
The method detection limit of this standard is 0.1 μg/10 ml of absorption liquid. When the total volume of the absorption liquid is 10 ml and the sampling volume is 1 to 4 L, ammonia
The detection limit was 0.025 mg/m3, the lower limit of determination was 0.10 mg/m3, and the upper limit of determination was 12 mg/m3. When the total volume of the absorbent is 10 ml,
When the sampling volume is 25 L, the detection limit of ammonia is 0.004 mg/m3, and the lower limit of determination is 0.016 mg/m3.
2 Principle of the method
After the ammonia is absorbed by the dilute sulfuric acid absorption liquid, ammonium sulfate is formed. In the presence of sodium nitroferricyanide, ammonium ions are opposite to salicylic acid and sodium hypochlorite
A blue complex should be formed and the absorbance measured at a wavelength of 697 nm. The absorbance is proportional to the ammonia content, and the ammonia content is calculated based on the absorbance.
the amount.
3 interference and elimination
If the concentration of organic amine is greater than 1 mg/m3, it will interfere with the determination and it is not applicable to this standard.
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 Sulfuric acid absorption liquid, c(1/2 H2SO4)=0.005 mol/L.
2.8 ml of sulfuric acid (4.2) was added to the water and diluted to 1 L to obtain a stock solution of 0.1 mol/L. Dilute 20 times when it is ready.
4.4 Salicylic acid-sodium potassium tartrate solution
Weigh 10.0 g of salicylic acid [C6H4(OH)COOH] in a 150 ml beaker, add appropriate amount of water, and add 5 mol/L sodium hydroxide solution.
15 ml, stir to dissolve completely. Also weigh 10.0 g of sodium potassium tartrate (KNaC4H6O6·4H2O), dissolved in water, heated to boil
The ammonia was removed, and after cooling, it was combined with the above solution and transferred to a.200 ml volumetric flask, diluted with water to the mark, and shaken. The pH of this solution is 6.0~
6.5, stable in brown bottles at 2 to 5 ° C for 1 month.
4.5 sodium nitroferricyanide solution, ρ = 10 g/L.
Weigh 0.1 g of sodium nitrosodium ferricyanide {Na2[Fe(CN)6NO]·2H2O}, place it in a 10 ml plug colorimetric tube, add water to dissolve it,
Constant volume to the marking line, ready to use.
4.6 sodium hypochlorite
Commercial reagents can be purchased, or they can be prepared by themselves. For detailed preparation methods, see Appendix A.1.
Sodium hypochlorite solution (stock solution) stored in plastic bottles, the effective chlorine concentration and free alkali concentration should be calibrated before each use (with NaOH)
For the calibration method, see Appendix A.2 and Appendix A.3.
4.7 sodium hydroxide solution, c (NaOH) = 2 mol/L.
Weigh 8.0 g of sodium hydroxide and dissolve in 100 ml of water.
4.8 sodium hypochlorite use solution, ρ (effective chlorine) = 3.5 g/L, c (free base) = 0.75 mol/L.
Take appropriate amount of calibrated sodium hypochlorite (4.6), dilute with water and 2 mol/L sodium hydroxide solution (4.7) to contain the effective chlorine concentration
3.5 g/L, sodium hypochlorite use solution with a free base concentration of 0.75 mol/L (as NaOH) (calculated the required dilution ratio based on the calibration results)
The number or the volume of sodium hydroxide that needs to be added is stored in a brown dropper bottle. This reagent is stable for 1 week.
4.9 Standard stock solution of ammonium chloride, ρ = 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 and store at 2 to 5 ° C for 1 month.
4.10 Standard use solution of ammonium chloride, ρ=10 μg/ml.
Pipette 5.0 ml of ammonium chloride standard stock solution (4.9) in a 500 ml volumetric flask and dilute to the mark with water.
5 Instruments and equipment
5.1 Gas sampling pump. The flow rate ranges from 0.1 to 1.0 L/min.
5.2 Large bubble absorber. 10 ml.
5.3 with colorimetric tube. 10 ml.
5.4 Spectrophotometer. with a 10 mm pathlength cuvette.
5.5 Drying tube. Built-in color changing silica gel or glass wool.
6 samples
6.1 Preparation of the absorption 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 drying tube (5.5), an absorption tube and a gas sampling pump with 10 ml of absorption liquid (4.3). When sampling
Sampling the entire blank sampling tube.
Smell source plant sampling. at a flow rate of 1.0 L/min, gas production is 1 to 4 L. Pay attention to the wind direction under the source of malodor, and capture the stench.
A sample of the time.
Ambient air sampling. gas production at a flow rate of 0.5 to 1.0 L/min for at least 45 minutes.
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 standard curve
Take 7 plugs of 10 ml colorimetric 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 (4.10)/ml 0.00 0.20 0.40 0.60 0.80 1.00 1.20
Ammonia content/μg 0.0 2.0 4.0 6.0 8.0 10.0 12.0
Dilute each tube to 10 ml with water, add 1.00 ml of salicylic acid-sodium potassium tartrate solution (4.4), and 2 drops of sodium nitroferricyanide solution.
(4.5), 2 drops of sodium hypochlorite use solution (4.8), shake and place for 1 h. Use a 10 mm cuvette at a wavelength of 697 nm with water as a reference.
The absorbance was measured. The standard curve was drawn by taking the absorbance of the reagent blank as the ordinate and the ammonia content (μg) as the abscissa.
7.2 Sample determination
After sampling, add appropriate amount of water and bring the sample solution to a volume of 10 ml. Accurately draw a certain amount of sample solution (the amount of suction depends on the concentration of the sample)
In a 10 ml colorimetric tube, dilute to 10 ml with the absorption solution (4.3), add 1.0 ml of salicylic acid-sodium potassium tartrate solution (4.4), 2 drops
Sodium nitroferricyanide solution (4.5), 2 drops of sodium hypochlorite solution (4.8), shake and place for 1 h. Use a 10 mm cuvette at a wavelength of 697
At nm, the absorbance was measured using water as a reference.
7.3 Blank test
7.3.1 Absorbent blank. Replace the sample with an 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 the sample solution, ml;
V0--the volume of the sample solution taken during the analysis, ml;
Vnd--the volume of the sample taken 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 standards containing 1.44 to 1.50 mg/L of ammonia were analyzed by five laboratories with a repeatability limit of 0.007 mg/L and a coefficient of variation of 5.0%;
The limit was 0.046 mg/L, and the coefficient of variation was 3.1%. The recoveries were 92.4%-104%.
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 Proper use of the sampling pump
Before turning on the sampling pump, confirm that the sampling system is connected correctly, and the inlet end of the sampling pump passes through the drying tube or the buffer tube and the outlet of the sampling tube.
The mouth is connected, if it is reversed, it will cause the acid absorption liquid to suck up, pollute and damage the instrument. In case of reverse suction, the flowmeter should be dismantled in time.
Wash it down, dry it with alcohol, reinstall it, and continue to use it after passing the flow calibration.
10.4 Preventing the absorption tube from being contaminated
In order to avoid contamination of the absorption liquid in the absorption tube, do not tilt or invert the absorption tube during transportation and storage, and replace the absorption tube in time.
Seal the joint.
Appendix A
(normative appendix)
Preparation method of sodium hypochlorite solution and calibration of available chlorine concentration and free alkali concentration
A.1 Preparation method of sodium hypochlorite solution
Hydrochloric acid (ρ=1.19 g/L) was applied dropwise to the potassium permanganate solid, and the evolved chlorine gas was introduced into the 2 mol/L sodium hydroxide absorption liquid.
Collect, produce a pale green green sodium hypochlorite solution and store in a plastic bottle. Since the solution is unstable, its available chlorine concentration should be calibrated before use.
A.2 Determination of available chlorine content in sodium hypochlorite solution
Pipette 10.0 ml sodium hypochlorite (4.6) into a 100 ml volumetric flask, dilute with water to the mark, and mix. Pipette 10.0 ml of diluted
Sodium hypochlorite solution in a 250 ml iodine measuring flask, add 40 ml of distilled water, 2.0 g of potassium iodide, and mix. Add 6 mol/L sulfuric acid solution 5
Ml, dense, mix. After 5 min in the dark, add 0.10 mol/L sodium thiosulfate solution to pale yellow, add about 1 ml starch indication.
Continue to drop until the blue color disappears. Its effective chlorine concentration is calculated according to formula (A.1).
Available chlorine (g/L, in Cl2) = 35.45 10010.0 10
c V× × × (A.1)
Where. c--concentration of sodium thiosulfate solution, mol/L;
V--titration consumption volume of sodium thiosulfate solution, ml;
35.45 - molar mass of available chlorine (1/2 Cl2), g/mol.
Determination of free base (as NaOH) in A.3 sodium hypochlorite solution
A.3.1 Calibration of hydrochloric acid solution
Sodium carbonate standard solution. c (1/2Na2CO3) = 0.100 0 mol/L. Weighed anhydrous sodium carbonate 2.650 0 g dried at 180 ° C for 2 h, dissolved
In freshly boiled cold water, transfer to a 500 ml volumetric flask and dilute to the mark.
Methyl red indicator. ρ = 0.5 g/L. 50 mg of methyl red was weighed and dissolved in 100 ml of ethanol (ρ = 0.99 g/ml).
Hydrochloric acid standard titration solution. c (HCl) = 0.10 mol/L. Take 8.5 ml of hydrochloric acid (ρ=1.19 g/L) in a 1 000 ml volumetric flask with water
Dilute to the mark. Calibration method. Pipette 25.00 ml sodium carbonate standard solution into a 150 ml vertebra bottle, add 25 ml water and 1 drop of methyl red
The indicator was titrated to a reddish color with a standard hydrochloric acid titration solution. Calculate the concentration of the hydrochloric acid standard solution using formula (A.2).
1 1(HCl) c Vc
V2
×= (A.2)
Where. c--hydrochloric acid standard titration solution concentration, mol/L;
C1--sodium carbonate standard solution concentration, mol/L;
V1--sodium carbonate standard solution volume, ml;
V2--HCl standard titration solution volume, ml.
A.3.2 Determination of free alkali (calculated as NaOH) in sodium hypochlorite solution
Pipette sodium hypochlorite (4.6) 1.0 ml into a 150 ml Erlenmeyer flask, add 20 ml of water, use phenolphthalein as an indicator, and use 0.10 mol/L salt.
The acid standard titration solution is titrated until the red color completely disappears. If the color change at the end point is not obvious, add 1 drop of phenol to the titrated solution.
酞 indicator, if the color is still red, continue to use a standard hydrochloric acid titration solution to drop to colorless.
Free base concentration (mol/L, in NaOH) = (HCl) (HCl) cv
× (A.3)
Where. c (HCl) - concentration of hydrochloric acid standard solution, mol/L;
v(HCl)--the volume of hydrochloric acid solution consumed by titration, ml;
V - the volume of sodium hypochlorite solution taken by titration, ml.
......
| Standard ID | HJ 534-2009 (HJ534-2009) | | Description (Translated English) | Ambient air. Determination of ammonia. Sodium hypochlorite-salicylic acid spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040.20 | | Word Count Estimation | 11,195 | | Date of Issue | 2009-12-31 | | Date of Implementation | 2010-04-01 | | Older Standard (superseded by this standard) | GB/T 14679-1993 | | Drafting Organization | Shenyang Municipal Environmental Monitoring Center Station | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 77 of 2009 | | Summary | This standard specifies the determination of ammonia in ambient air of sodium hypochlorite salicylic acid spectrophotometry. This standard applies to the determination of ammonia in ambient air, but also for odor source plant boundary determination of ammonia in the air. |
|