HJ 548-2009_English: PDF (HJ548-2009)
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| HJ 548-2016 | English | 229 |
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Stationary source emissions. Determination of hydrogen chloride. Silver nitrate titration
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HJ 548-2016
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| HJ 548-2009 | English | 319 |
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Stationary source emissions. Determination of hydrogen chloride. Silver nitrate titration method
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HJ 548-2009
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Standards related to: HJ 548-2009
| Standard ID | HJ 548-2009 (HJ548-2009) | | Description (Translated English) | Stationary source emissions. Determination of hydrogen chloride. Silver nitrate titration method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Classification of International Standard | 13.040.40 | | Word Count Estimation | 8,830 | | Date of Issue | 2009-12-30 | | Date of Implementation | 2010-04-01 | | Quoted Standard | GB 16157; HJ/T 373; 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 hydrogen chloride silver nitrate volumetric method. This standard applies to stationary source emissions Determination of hydrogen chloride. This standard method detection limit of 0. 03mg. When the sample volume is 15L, the detection limit of 2mg/m ^ 3. |
HJ 548-2009
Stationary source emissions.Determination of hydrogen chloride.Silver nitrate titration method
National Environmental Protection Standard of the People's Republic
Determination of hydrogen chloride in fixed pollution source
Silver nitrate capacity method (provisional)
Stationary source emissions-Determination of hydrogen chloride
-Silver nitrate titration 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);
X. Determination of chlorine gas from fixed pollution sources, iodometric method (provisional) (HJ 547-2009);
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.3
11 Notes 3
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
The body health, standardize the monitoring method of hydrogen chloride in the fixed source of waste gas, and develop this standard.
This standard specifies the silver nitrate volumetric method for the determination of hydrogen chloride in fixed source exhaust 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 hydrogen chloride in fixed pollution source
Silver nitrate capacity method (provisional)
1 Scope of application
This standard specifies the silver nitrate volumetric method for the determination of hydrogen chloride in fixed source exhaust gas.
This standard applies to the determination of hydrogen chloride in fixed pollution source exhaust gas.
The method detection limit of this standard is 0.03 mg. When the sampling volume is 15 L, the detection limit is 2 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
After the hydrogen chloride is absorbed by the sodium hydroxide solution, it is titrated with a silver nitrate standard solution under neutral conditions using potassium chromate as an indicator.
Silver chloride precipitates, and excess silver ions react with potassium chromate indicator to form a light brick red silver chromate precipitate indicating the end point of the titration. The reaction formula is as follows.
3Cl AgNO
− → 3NO AgCl− ↓
42Ag CrO
− → 2 4Ag CrO ↓
(light brick red)
4 interference and elimination
4.1 Sulfide, cyanide, chlorine and other halides interfere with the determination, resulting in higher results.
4.2 When chlorine (Cl2) coexists in the exhaust gas, it reacts with sodium hydroxide to form equal amounts of chloride ions and hypochlorite ions to interfere with hydrogen chloride.
The determination, the hypochlorite is determined by the iodometric method, and the amount is subtracted from the total chloride to obtain the hydrogen chloride content.
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 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.2 Anhydrous ethanol. ρ (CH3CH2OH) = 0.79 g/ml.
5.3 Nitric acid solution. c (HNO3) = 0.10 mol/L.
Dilute 6.25 ml of nitric acid (5.1) to 100 ml with water and mix.
5.4 Ethanol solution. 1 1.
Take 250 ml of absolute ethanol (5.2), dilute to 500 ml with water, and mix.
5.5 Sodium hydroxide absorption solution. c (NaOH) = 0.10 mol/L.
Dissolve 4.0 g of sodium hydroxide in a small amount of water, dilute to 1 000 ml with water, and mix.
5.6 sodium chloride standard solution
Weigh 0.550 0~0.600 0 g of sodium chloride (NaCl, previously burned in porcelain crucible at 400-500 °C until no longer emitted
Burst, slightly cold, transfer to a weighing bottle, weigh to 0.1 mg), dissolve in water, transfer to a 100 ml volumetric flask, dilute to the mark with water, and shake.
Accurately calculate the concentration of sodium chloride standard solution according to formula (1).
10(NaCl)
58.44
Wc ×= (1)
Where. c (NaCl) - concentration of sodium chloride standard solution, mol/L;
W--the amount of sodium chloride, g;
58.44 - molar mass of sodium chloride, g/mol.
5.7 Silver nitrate standard stock solution. c (AgNO3) ≈ 0.10 mol/L.
5.7.1 Preparation
Weigh 17.00 g of silver nitrate, dissolve in water, dilute to 1 000 ml with water, and store in a brown bottle.
5.7.2 Calibration
Pipette 10.00 ml of sodium chloride standard solution (5.6), place in a white porcelain dish, add 25 ml of water. Add potassium chromate indicator (5.9) 1.0 ml,
With the glass rod constantly stirring, titrate with a silver nitrate standard stock solution until a pale brick red color does not disappear. Recording silver nitrate titration
Liquid volume. Another 35 ml of water was taken and blank titration was carried out in the same manner. Calculate the concentration of silver nitrate standard stock solution according to formula (2).
10.00(AgNO ) cc
VV
×= − (2)
Where. c (AgNO3) - silver nitrate standard stock solution concentration, mol/L;
C1--sodium chloride standard solution concentration, mol/L;
V0--the volume of the silver nitrate stock solution consumed by titrating the blank solution, ml;
V--The volume of the silver nitrate stock solution consumed by the titration of the sodium chloride solution, ml.
5.8 Silver nitrate standard use solution
Draw the calibration standard silver nitrate stock solution (5.7) 10.00 ml, place it in a 100 ml volumetric flask, dilute with water to the mark, mix
Evenly, stored in a brown bottle.
5.9 Potassium chromate indicator
Weigh 5.0 g of potassium chromate (K2CrO4) dissolved in a small amount of water, and add the standard solution of silver nitrate (5.8) dropwise to produce a small amount of light brick red.
The color precipitates. After standing overnight, filtering, discarding the precipitate, the filtrate was diluted with water to 100 ml and stored in a brown reagent bottle.
5.10 Phenolphthalein indicator
Weigh 0.50 g of phenolphthalein and dissolve it in 100 ml of ethanol solution (5.4).
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 0~1 L/min.
6.2 Brown acid burette. 25 ml.
6.3 Absorber. Perforated glass absorption bottle, 75 ml.
6.4 Acetate fiber microporous membrane. 0.3 μm.
6.5 sampling tube
Made of hard glass or fluororesin, with appropriate size of pipe material, and should be attached with a thermal insulation jacket that can be heated to above 120 °C.
6.6 Filter Membrane. Teflon, the size is matched with the cellulose fiber microporous membrane.
6.7 connecting pipe
Use a Teflon hose or a silicone rubber tube lined with a Teflon film.
6.8 White porcelain. 75 ml.
7 samples
7.1 Sample collection
According to the "Measurement of particulate matter in fixed pollution source exhaust gas and sampling method of gaseous pollutants" (GB/T 16157). When sampling, connect one
A perforated glass plate absorption bottle containing 30 to 50 ml of sodium hydroxide absorbent (5.5) is sampled at a flow rate of 0.5 L/min for 10 to 30 minutes. in
Keep the temperature of the sample insulation jacket at 120 °C during the sampling process to avoid condensation before the water is absorbed in the bottle.
Note. When the concentration of hydrogen chloride is high, two absorption bottles can be sampled in series, and the sample solutions are combined. After constant volume, an appropriate amount of solution is titrated. If the exhaust contains chloride
For particulate matter, the filter holder should be installed before the absorption bottle.
7.2 Preservation of samples
Sample collection should be analyzed as soon as possible. If it cannot be measured on the same day, the sample should be sealed and stored at 0~4 °C for a period of not more than 48 h.
8 Analysis steps
8.1 Analysis of samples
After sampling, transfer the sample solution to a white porcelain dish, add 1 drop of phenolphthalein indicator (5.10), and add 0.10 mol/L nitric acid solution (5.3).
Until the red just disappeared. Add potassium chromate indicator (5.9) 1.0 ml, keep stirring, use 0.01 mol/L silver nitrate standard solution (5.8)
Titrate until a light brick red color is produced.
8.2 Blank test
Take the same volume of absorbent and perform a blank titration according to 8.1.
9 Calculation of results
Calculate the mass concentration of hydrogen chloride in the fixed source exhaust gas according to formula (3).
Nd
( ) 36.46 1000
HCl
VV c
ρ − × × ×=( ) (3)
Where. ρ (HCl)--the mass concentration of hydrogen chloride in the fixed pollution source exhaust gas, mg/m3;
V1--titration sample solution consumption of silver nitrate standard solution volume, ml;
V0--the titration of the silver nitrate consumed by the titration blank solution standard solution volume, ml;
C2--concentration of silver nitrate standard solution, mol/L;
36.46 - molar mass of hydrogen chloride (HCl), g/mol;
Vnd - the sampling volume of dry gas in the standard state (101.325 kPa, 273 K), L.
10 Quality Assurance and Quality Control
10.1 Quality control and quality assurance are carried out in accordance with HJ/T 373.
10.2 The sampler should be airtight and flow calibrated prior to use. Each batch should have at least one full program blank.
10.3 Used absorbent bottle, connecting tube, etc., after pouring the solution, wash it directly with deionized water, do not wash with tap water;
During the process, pay attention to dustproof, do not touch the mouth of the absorption bottle to prevent the chloride from staining.
11 Precautions
The titration solution should be neutral or slightly alkaline (pH = 6.5 ~ 10.5). In an acidic solution, when the conversion affects the endpoint
Formation of Ag2CrO4 precipitate. Ag will form an Ag2O precipitate in an alkaline solution.
4CrO
− 2
2 7Cr O
......
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