HJ 547-2009_English: PDF (HJ547-2009)
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Stationary source emission -- Determination of chlorine--Iodometric method
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HJ 547-2017
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| HJ 547-2009 | English | 319 |
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Stationary source emission. Determination of chlorine. Iodometric method
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HJ 547-2009
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Standards related to: HJ 547-2009
| Standard ID | HJ 547-2009 (HJ547-2009) | | Description (Translated English) | Stationary source emission. Determination of chlorine. Iodometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Classification of International Standard | 13.040.40 | | Word Count Estimation | 8,857 | | Date of Issue | 2009-12-30 | | Date of Implementation | 2010-04-01 | | Quoted Standard | HJ/T 373; GB/T 16157; GB/T 6682 | | Drafting Organization | Beijing Municipal Environmental Monitoring Center | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 74 of 2009 | | Summary | This standard specifies the determination of stationary source emissions of chlorine iodometric method. This standard applies to stationary source emissions Determination of chlorine. The detection limit is 0. 03��g, sampling volume is 10L, the detection limit is 12mg/m ^ 3. |
HJ 547-2009
Stationary source emission.Determination of chlorine.Iodometric method
National Environmental Protection Standard of the People's Republic
Determination of chlorine gas from fixed pollution source
Iodometric method (provisional)
Stationary source emission-Determination of chlorine
-Iodometric 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);
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);
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);
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.1
5 Reagents and materials.1
6 instruments and equipment.2
7 samples. 2
8 Analysis steps..3
9 result calculation..3
Foreword
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 prevention of human health and the regulation of chlorine in the fixed source of waste gas.
This standard specifies the method of determining the amount of chlorine in the fixed source of waste gas.
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 chlorine in fixed waste gas sources - Determination of iodometric method (interim)
Warning. When sampling at the site, if the chlorine concentration is high, the operator should be in the upwind direction and take the anti-virus mask operation.
Anti-chlorine gas poisoning.
1 Scope of application
This standard specifies the method of determining the amount of chlorine in the fixed source of waste gas.
This standard applies to the determination of chlorine in fixed source exhaust gas.
The detection limit of this method is 0.03 μg; when the sampling volume is 10 L, the detection limit is 12 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.
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 chlorine gas is absorbed by the sodium hydroxide solution to form sodium hypochlorite, which is acidified with hydrochloric acid to release free chlorine. The reaction formula is as follows.
22NaOH Cl → 2NaCl HO NaClO
NaClO HCl → 2NaOH Cl
Free chlorine reoxidizes the iodide to form iodine, which is titrated with a sodium thiosulfate standard solution to calculate the amount of chlorine.
2Cl 2KI → 22KCl I
2 2 2I 2Na SO 3→ 2 4 62NaI Na SO
4 interference
When hydrogen chloride is contained in the exhaust gas, the measurement is not disturbed; there is interference when it contains oxidizing and reducing gases.
5 reagents and materials
Unless otherwise stated, analytically pure reagents in accordance with national standards were used for the analysis; experimental water, GB/T 6682, grade 3.
5.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.2 Potassium iodide crystal (KI). excellent grade pure.
5.3 Potassium iodate (KIO3). excellent grade pure.
5.4 Hydrochloric acid solution. 2 1.
Formulated with hydrochloric acid (5.1).
5.5 Hydrochloric acid solution. c (HCl) = 1.2 mol/L.
Measure 100 ml of concentrated hydrochloric acid (5.1) and dilute to 1 000 ml with water.
5.6 Sodium hydroxide absorption solution. w (NaOH) = 0.4%.
Weigh 4.0 g of sodium hydroxide, dissolve in water and dilute to 1 000 ml.
5.7 Potassium iodate standard solution. c (1/6KIO3) = 0.100 0 mol/L.
Weigh 3.567 g of potassium iodate (5.3) which is dried at 105-110 ° C for 2 h and cooled. Dissolve in water, transfer to a 1 000 ml volumetric flask, and dilute.
Shake to the mark, shake it, and store in a brown stoppered glass bottle.
5.8 Sodium thiosulfate standard solution. c (Na2S2O3) ≈ 0.1 mol/L.
Weigh 25 g of sodium thiosulfate (Na2S2O3·5H2O), dissolve in freshly boiled and cooled water, add 0.20 g of anhydrous sodium carbonate, dilute
Release to 1 000 ml and store in a brown glass bottle. If the solution is cloudy, it should be filtered. 0 to 4 ° C can be stored for 6 months, Pro
Use calibration.
Calibration method. Pipette 10.00 ml of potassium iodate standard solution (5.7), place it in a 250 ml iodine measuring flask, add 85 ml of new boiled and
Cool the water, add 1.0 g potassium iodide (5.2), shake to complete dissolution, then add 10.0 ml hydrochloric acid solution (5.5), immediately cover the bottle
Plug and mix. After 5 min in dark treatment, titrate with sodium thiosulfate solution (5.8) until pale yellow, add 5 ml starch indicator (5.10),
Continue titration until the blue color just fades and record the volume (V) of the sodium thiosulfate solution consumed. Calculate sodium thiosulfate solution according to formula (1)
concentration.
0.01 10.00(Na SO )c
×= (1)
Where. - concentration of sodium thiosulfate solution, mol/L; 2 2 3 (Na SO ) c
V--The volume of the sodium thiosulfate solution used to calibrate potassium iodate, ml.
5.9 sodium thiosulfate standard use solution
Pipette 50.00 ml of the calibrated sodium thiosulfate solution (5.8) into a 500 ml volumetric flask and dilute with freshly boiled and cooled water.
Released to the marking line, shaken, and ready to use.
5.10 Starch indicator. w = 0.20%.
Weigh 0.20 g of soluble starch, add a small amount of water to make a paste, slowly pour into 100 ml of boiling water, continue to boil until the solution is clear, cold
However, it is stored in a fine mouth bottle and is ready for use.
6 Instruments and equipment
Unless otherwise stated, the analysis used a Class A glass instrument in accordance with national standards.
6.1 Flue gas sampler. 0~1 L/min.
6.2 Sampling tube. glass or Teflon.
Note. Chlorine gas produces hydrochloric acid and hypochlorous acid in the presence of water vapor, which is highly corrosive. Therefore, the sampling tube should be made of glass or Teflon.
Work.
6.3 Porous glass plate absorption bottle. 125 ml.
6.4 Brown acid burette. 25 ml or 50 ml.
6.5 Iodometric flask. 250 ml.
7 samples
7.1 Sample Collection
The sampling point layout and sampling method are performed according to GB/T 16157. When sampling, two porous glass plate absorption bottles are connected in series, and each bottle is packed with 30~
40 ml sodium hydroxide absorption solution (5.6), sample at a flow rate of 0.5 to 1 L/min, and sample for 10 to 30 minutes.
7.2 Sample storage
Sample collection should be analyzed as soon as possible. If it cannot be measured on the same day, the sample should be sealed and placed in the refrigerator, stored at 0~4 °C, and measured within 5 days.
8 Analysis steps
8.1 Sample preparation
After sampling, transfer all the two sample solutions to a 100 ml volumetric flask, and wash the absorption tube and the absorption bottle with the absorbent (5.6).
And transfer to this volumetric flask, add the absorption liquid to the marking line, and mix.
8.2 Determination of samples
Pipette 25.00 ml of sample (8.1) into an iodine measuring flask, add an equal volume of water, add 2.0 g of potassium iodide (5.2), add to dissolve, add
10.0 ml hydrochloric acid solution (5.4), tightly packed, mixed, placed in the dark for 5 min. Titrate to pale yellow with sodium thiosulfate standard solution (5.9).
Add 5 ml of starch solution (5.10), continue titration until the blue color just disappears, and record the consumption (V).
8.3 Blank sample determination
Take 25.00 ml of the absorption solution, add an equal volume of water, and perform a blank titration to record the consumption (V0).
9 Calculation of results
The chlorine content is calculated according to formula (2)
0 t
Nd a
( ) 35.5
(Cl ) 1000
VV c V
VV
ρ − × ×= × × (2)
Where. - chlorine content, mg/m3; 2 (Cl ) ρ
V--the volume of the sodium thiosulfate standard solution consumed by the titration sample solution, ml;
V0--the volume of the sodium thiosulfate standard solution consumed by titrating the blank sample solution, ml;
C--sodium thiosulfate standard use liquid concentration, mol/L;
35.5- molar mass of chlorine (1/2Cl2), g/mol;
Vt--the total volume of the sample solution, ml;
Va--the volume of the sample solution taken by the titration, ml;
Vnd--the gas production volume of dry exhaust gas converted to the standard state (101.325 kPa, 273 K), L.
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