HJ 547-2017 English PDF

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HJ 547-2017: Stationary source emission -- Determination of chlorine--Iodometric method
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HJ 547: Historical versions

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
HJ 547-2017	269	Add to Cart	3 days	Stationary source emission -- Determination of chlorine--Iodometric method	Valid
HJ 547-2009	319	Add to Cart	3 days	Stationary source emission. Determination of chlorine. Iodometric method	Obsolete

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Basic data

Standard ID: HJ 547-2017 (HJ547-2017)
Description (Translated English): Stationary source emission -- Determination of chlorine--Iodometric method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z25
Word Count Estimation: 11,174
Date of Issue: 2017-12-29
Date of Implementation: 2018-04-01
Older Standard (superseded by this standard): HJ 547-2009
Regulation (derived from): Ministry of Environmental Protection Bulletin 2017 No. 86
Issuing agency(ies): Ministry of Ecology and Environment

HJ 547-2017: Stationary source emission -- Determination of chlorine--Iodometric method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
People's Republic of China national environmental protection standards Replacing HJ 547-2009 Stationary sources - Determination of chlorine gas - Iodometric method Stationary source emission - Determination of chlorine-Iodometric method 2017-12-29 Posted 2018-04-01 implementation Ministry of Environmental Protection released Directory Foreword .ii 1 scope of application .1 2 Normative references .1 3 method principle .1 4 Interference and elimination .1 5 Reagents and materials .2 6 instruments and equipment .3 7 samples .3 8 Analysis steps .5 9 results calculated and said .5 10 precision and accuracy 6 11 Quality Assurance and Quality Control .6 12 Waste treatment 6 13 Matters needing attention 7

Foreword

In order to implement "Law of the People's Republic of China on Environmental Protection" and "Law of the People's Republic of China on Prevention and Control of Atmospheric Pollution," Paul Protect the environment, protect human health, standardize the determination of chlorine in exhaust gas pollution sources, the development of this standard. This standard specifies the amount of iodine method for the determination of chlorine emissions from organized sources of emissions of fixed sources of pollution. This standard is "a fixed source of emissions of chlorine gas Determination of iodine method (Interim)" (HJ 547-2009) amendment. This standard was first released in.2009, the original standard drafting unit for the Beijing Municipal Environmental Protection Monitoring Center, this is the first time The main content of the revision and amendment are as follows. - Revised methods of reagents and materials, apparatus and equipment, reagent preparation, sample collection and analysis steps and other articles paragraph. - Complement and improve the method of principle, interference and eliminate some of the content. - Added precision, accuracy, result representation, sample penetration experiments, quality assurance and quality control content. - Added waste disposal content. Since the implementation of this standard, "fixed sources of chlorine emissions Determination of iodine method (Interim)" (HJ 547-2009) Abolished. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Beijing Environmental Protection Monitoring Center. This standard verification unit. Beijing Environmental Protection Monitoring Center, Changping District, Beijing Environmental Protection Monitoring Station, Beijing North Korea Yang District Environmental Protection Bureau, Fengtai District, Beijing Environmental Protection Monitoring Station, Beijing Kangju Environmental Monitoring Station and the Beijing Municipal Physical and Chemical Analysis test Center. This standard MEP approved on December 29,.2017. This standard since April 1,.2018 come into operation. This standard is interpreted by the MEP. Stationary sources - Determination of chlorine gas - Iodometric method Warning. chlorine gas is harmful to the human body. When sampling, wear protective equipment as required to avoid inhalation, contact with skin and eyes.

1 scope of application

This standard specifies the determination of iodine content of chlorine gas emissions from fixed sources of pollution. This standard applies to fixed sources of emissions of organized emissions of chlorine gas, does not apply to the determination of unorganized emissions. When the sampling volume is 10 L, the detection limit is 12 mg/m3 and the lower limit of determination is 48 mg/m3.

2 Normative references

This standard references the following documents in the terms. For undated references, the effective version applies to this book standard. GB/T 16157 fixed emission sources of particulate matter measurement and gaseous pollutants sampling method HJ/T 47 gas sampler technical conditions

3 method principle

Chlorine is absorbed by the sodium hydroxide solution to produce sodium hypochlorite. After the sample was added potassium iodide, acidified with hydrochloric acid, released Free chlorine oxidizes iodide ions to iodine and titrates with sodium thiosulfate standard solution. Based on consumption of sodium thiosulfate standard solution Volume and sampling volume, calculate the concentration of chlorine in the exhaust gas. The reaction is as follows. 2NaOH Cl2 → NaCl H2O NaClO NaClO HCl → NaOH Cl2 Cl2 2KI → 2KCl I2 I2 2Na2S2O3 → 2NaI Na2S4O6

4 Interference and elimination

Hydrogen fluoride in the exhaust gas and hydrogen chloride do not interfere with the determination; particles will affect the determination, can be added in front of the sampling tube filter to remove; Exhaust gases contain other oxidizing or reducing gases that interfere with the assay.

5 Reagents and materials

Unless otherwise specified, analytical grade reagents and distilled water are used in accordance with national standards. 5.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 5.2 potassium iodide (KI). 5.3 potassium iodate (KIO3). reference reagent or excellent grade pure. 5.4 Sodium hydroxide (NaOH). 5.5 Sodium thiosulfate pentahydrate (Na2S2O3 · 5H2O). 5.6 anhydrous sodium carbonate (Na2CO3). 5.7 hydrochloric acid solution. 2 1. Take 250 ml of hydrochloric acid (5.1), add to 125 ml of water and mix well. 5.8 Hydrochloric acid solution. c (HCl) = 1.2 mol/L. Measure 100 ml of hydrochloric acid (5.1) slowly into 900 ml of water. 5.9 Sodium hydroxide absorbent. ρ (NaOH) = 4.0 g/L. Weigh 4.0 g sodium hydroxide (5.4), dissolved in a small amount of water, diluted to 1000 ml. 5.10 potassium iodate standard solution. c (1/6 KIO3) = 0.1000 mol/L. Weigh accurately 3.567 g at 105 ℃ ~ 110 ℃ drying 2 h and cooled in a desiccator potassium iodate (5.3), dissolved in water, Move into a 1000 ml volumetric flask, dilute to the mark, shake well and store in a brown glass stopper. Room temperature preservation, preservation The time is generally not more than two months. When the solution appears cloudy, precipitation, color changes and other phenomena, should be re-formulated. 5.11 sodium thiosulfate standard solution. c (Na2S2O3) ≈ 0.1 mol/L. Weigh 25 g of sodium thiosulfate pentahydrate (5.5), dissolved in freshly boiled and chilled water, add 0.20 g of anhydrous carbonated Sodium (5.6), dissolved, mixed, set to 1000 ml, stored in a brown glass bottle. If the solution is cloudy, it should be added To filter. 0 ℃ ~ 4 ℃ can be stored for 6 months, temporary calibration. Calibration method. Pipette 10.00 ml potassium iodate standard solution (5.10), placed in 250 ml iodine bottle, add 85 ml Freshly boiled and cooled water, add 1.0 g of potassium iodide (5.2), shake to completely dissolve, then add 10.0 ml of hydrochloric acid Liquid (5.8), immediately covered the bottle stopper, mix well. After 5 min in the dark place, with the standard solution of sodium thiosulfate to be calibrated (5.11) Titration to light yellow, add 5 ml of starch indicator (5.13), continue titration until the blue just fade, record consumption of thiosulfuric acid Volume of sodium standard solution (V). According to formula (1) calculate the concentration of sodium thiosulfate standard solution. () 2 2 3 c Na SO = 0.1000 10.00 (1) Where. C (Na2S2O3) - sodium thiosulfate standard solution concentration, mol/L; V - Titration potassium iodate standard solution of sodium thiosulfate standard solution volume, ml. 5.12 sodium thiosulfate standard solution c (Na2S2O3) ≈ 0.01 mol/L. Pipette 50.00 ml of calibrated sodium thiosulfate standard solution (5.11), placed in 500 ml volumetric flask, with a new boil And has been diluted with water cooling to the mark, shake average, Pro use now. 5.13 Starch indicator. p = 0.002 g/ml. Weigh 0.20 g of soluble starch, add a small amount of water into a paste, slowly pour 100 ml boiling water, continue to boil until the solution Clarified, cooled and stored in stoppered glass bottles, ready for use. 5.14 Microporous cellulose acetate membrane or quartz filter. The retention efficiency of particles larger than 0.3 μm is not less than 99.9%.

6 instruments and equipment

Unless otherwise specified, all glassware used in accordance with the national standard Class A was used for the analysis. 6.1 flue gas sampler. the sampling flow 0 L/min ~ 1 L/min, other performance and technical indicators should be consistent with the provisions of HJ/T 47. 6.2 Filter Clip. Teflon material, size and filter (5.14) match. 6.3 sampling tube. hard glass or PTFE material. The inner diameter should be larger than 6 mm, and should be attached to heat up to 120 ° C More insulation jacket. 6.4 Connecting pipe. Teflon hose or silicone rubber tube lined with Teflon film. The connection method is the internal jacket method connection. 6.5 Porous glass absorption bottle. 125 ml scale. Glass panels require 2/3 area of fine and uniform foam, no bubbles at the edge Escape, with a flow rate of 0.5 L/min, the resistance should be (5 ± 0.7) kPa. 6.6 Brown Acid Burette. 25 ml. 6.7 iodine bottle. 250 ml. 6.8 General laboratory equipment and equipment.

7 samples

7.1 Sample Collection 7.1.1 sampling point layout and sampling methods should be consistent with the provisions of GB/T 16157. 7.1.2 Connect in series two porous glass absorption bottles (6.5) containing 40 ml of sodium hydroxide absorbent (5.9), connect to Sampling system, with 0.5 L/min ~ 1 L/min constant current sampling 20 min ~ 30 min. If the exhaust contains solid particles Things should be placed in the filter membrane (5.14) folder (6.2), then mounted on the front end of the sampling tube, the sampling system shown in Figure 1. When waste When the temperature is higher than the ambient temperature or the moisture content is large, it is necessary to heat the filter membrane and the sampling tube in the filter holder to keep the sampling tube insulated Jacket temperature at 120 ℃, to prevent moisture condensation. Record the sampling flow rate, time, temperature, pressure, etc. After sampling, Seal the outlet of the absorbent bottle with a connecting tube (6.4) and back to the laboratory in the dark. Note. When the chlorine concentration, moisture content (flue gas moisture content above 25%), the need for constant speed sampling. Figure 1 Schematic diagram of a chlorine sampling system in a stationary source of exhaust gas 7.2 full program blank sample The same batch of 40 ml of sodium hydroxide solution (5.9) of the two tandem absorption bottle to the sampling site, not with the sample Connection, after the sample is taken with the collected samples back to the laboratory. 7.3 Sample Storage Samples should be analyzed as soon as possible after the sample is collected. If it can not be measured on the same day, it should be refrigerated below 4 ℃ and be measured within 48 h. 7.4 Sample Preparation 7.4.1 Samples The absorption of the first stage absorption bottle was transferred to a 100 ml volumetric flask, the second level with an absorbent absorption of the washing liquid After the first bottle into the volumetric flask, and then a small amount of water to wash the two absorption bottles and absorption tube, washing liquid into the volumetric flask together, plus Water to the mark, mix well. 7.4.2 Blank sample 7.4.2.1 full program blank Preparation of the entire program blank sample was carried out according to the same procedure as for sample preparation (7.4.1). 7.4.2.2 reagent blank Take the same batch of absorbent (5.9) instead of the sample, according to the same steps as the sample preparation (7.4.1) reagent blank Preparation. 7.4.3 penetrate the experimental sample Respectively, the absorption of the first and second absorption bottles were transferred to a 50 ml volumetric flask, then a small amount of water Wash two absorption bottles, washing liquid into the flask, add water to the mark, mix well.

8 Analysis steps

8.1 Determination of the sample Pipette 25.0 ml sample (7.4.1) in iodine bottle, add an equal volume of water, add 2.0 g of potassium iodide (5.2), to be dissolved After the solution, add 10.0 ml hydrochloric acid solution (5.7), plug tightly, mix well and place in dark place for 5 min. With sodium thiosulfate standard make Titration with liquid (5.12) to pale yellow, add 5 ml of starch solution (5.13), continue titration until the blue just disappears, Record consumption of sodium thiosulfate standard use volume (V). 8.2 blank sample determination Follow the same procedure as described for sample determination (8.1) to determine the full program blank and reagent blank. 8.3 Penetration of experimental samples Following the same procedure as for sample determination (8.1), the penetration test sample (7.4.3) was measured and the consumption recorded.

9 results calculated and expressed

9.1 Calculation Results The concentration of chlorine in the exhaust gas is calculated according to equation (2)  (Cl2) = 1000 () 35.5 0      nd V VV c (2) Where. 2  (Cl) - concentration of chlorine in the exhaust gas, mg/m3; Volume of standard sodium thiosulfate consumed by titration of V - titration sample solution, ml; 0 V - titration reagent blank solution consumed sodium thiosulfate standard volume of liquid used, ml; c - sodium thiosulfate standard solution concentration, mol/L; 35.5 - Molar mass of chlorine (1/2 Cl2), g/mol; nd V - Converted to the gas recovery volume of dry exhaust under standard conditions (0 ° C, 101.325 kPa), L t V - total volume of sample solution, ml; a V - volume of sample solution taken during titration, ml. 9.2 results indicated When the measurement is less than 100 mg/m3, retained to the whole digit; when the measurement is greater than or equal to 100 mg/m3, Keep three significant figures. 10 precision and accuracy 10.1 Precision Six laboratories separately treated sodium hypochlorite solution with available chlorine concentrations of 9.01 mg/L, 72.6 mg/L and 181 mg/L The relative standard deviations in the laboratory were 1.2% ~ 2.1%, 0.32% ~ 1.1% and 0.2% ~ 1.5%, respectively. The relative standard deviations (RSDs) of laboratory were 5.7%, 7.3% and 7.5%, respectively. The repeatability limits were 0.40 mg/L, 1.7 mg/L And 4.0 mg/L respectively. The reproducibility limits were 1.5 mg/L, 15 mg/L and 38 mg/L, respectively. Six laboratories performed standard gas concentrations of 22.4 mg/m3, 78.9 mg/m3 and 735 mg/m3 chlorine respectively The relative standard deviations in the laboratory were 3.8% ~ 6.5%, 1.6% ~ 3.6% and 0.6% ~ 2.1%, respectively. The experiment The relative standard deviations (RSDs) were 1.9%, 1.6% and 3.4% respectively. The repeatability limits were 3 mg/m3 and 3 mg/m3, respectively 30 mg/m3; reproducibility limits are 3 mg/m3, 6 mg/m3 and 70 mg/m3, respectively. 10.2 Accuracy Six laboratories performed standard gas concentrations of 22.4 mg/m3, 78.9 mg/m3 and 735 mg/m3 chlorine respectively The relative error in the laboratory was -5.4% -10%, -3.6% -7.5% and -2.0% -9.2% respectively. The experiment The relative error between rooms was -7.5%, -6.0% and -5.5%, respectively. The final relative error values were -7.5% ± 2.0% -6.0% ± 3.2% and -5.5% ± 6.3%. Six laboratories performed standard gas concentrations of 22.4 mg/m3, 78.9 mg/m3 and 735 mg/m3 chlorine respectively Repeated determination, the laboratory absorption efficiency were 91.7% ~ 94.6%, 92.5% ~ 96.8% and 90.8% ~ 98.0%; Laboratory absorption efficiency were 93.2%, 94.0% and 94.5% respectively. 11 Quality Assurance and Quality Control 11.1 Sampling Each batch of samples should be at least 1 full blank and 2 reagent blank. Full program blank and reagent blank The measured value should be below the detection limit of the method. 11.2 Before analyzing the sample, the standard solution of sodium thiosulfate should be calibrated. The relative value of the single titration result should not be too high More than 0.2%, double titration results poor relative value of not more than 0.5%. 11.3 Parallel titration shall be performed on at least 10% of the samples in each batch of samples, with a relative deviation of no more than 2%. 11.4 Penetration test and absorption efficiency analysis of samples collected at low and high concentrations of chlorine (up to 735 mg/m3) From the point of view, the complete absorption of the gas sample can be achieved by connecting two absorption bottles in series, but if the actual sample concentration is high, To increase the penetration of the experimental link, each batch of samples collected should be done through a penetration test, when the second absorption bottle of chlorine content More than 10% of the first absorption bottle content, that has been penetrated, should reduce gas production or gas production time, re-sampling. 12 Waste treatment The waste liquid and waste generated during the experiment shall be stored in categories, centrally stored and entrusted to qualified units for disposal. 13 Precautions Sampling absorption bottle inlet port and the series of two absorption bottle is not available between the latex hose connection should be polytetrafluoroethylene Hose or polyethylene plastic pipe connected to the jacket method, the plastic tube is about to be inserted into the mouth of the absorption bottle, wrapped with PTFE tape Well, then use a silicone rubber pipe outside the mouth. The connecting pipe should be as short as possible. ......

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