HJ 545-2017 (HJ545-2017) & related versions
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Stationary source emission－Determination of total gaseous phosphorus -- Quimociac volumetric analysis
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HJ 545-2017
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HJ 545-2017
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| HJ 545-2009 | English | 359 |
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Stationary source emission. Determination of total gaseous phosphorus. Quimociac volumetric analysis
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HJ 545-2009
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HJ 545-2017: PDF in English
HJ 545-2017
People's Republic of China national environmental protection standards
Replacing HJ 545-2009
Stationary source emissions - Determination of total gaseous phosphorus
Quinocholine capacity method
Stationary source emission-Determination of total gaseous phosphorus
Quimociac volumetric analysis
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 Terms and definitions 1
4 method principle .1
Interference and elimination 2
6 Reagents and Materials 2
7 instruments and equipment 4
8 sample 5
9 Analysis steps .6
10 Results Calculation and Presentation .7
11 precision and accuracy .7
12 Quality Assurance and Quality Control .8
13 Waste treatment .8
14 Matters needing attention .8
Foreword
In order to implement the Law of the People's Republic of China on Environmental Protection and the Law of the People's Republic of China on Prevention and Control of Atmospheric Pollution,
Environment, protect human health, standardize the determination of gaseous total phosphorus in the exhaust gas of fixed sources of pollution, to develop this standard.
This standard specifies the determination of fixed sources of emissions of gaseous total phosphorus Quimociac volume method.
This standard is "a fixed source of emissions of gaseous total phosphorus Determination Quimociac Volume Act (Interim)" (HJ 545
-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 contents of the amendment and amendment are as follows.
- Revised method limits of detection, reagents and materials, apparatus and equipment, sample collection and analysis step clauses.
- Supplement and improve the quality assurance and quality control part of the content.
- Added warning, interference and elimination, precision and accuracy, waste disposal and precautions.
From the date of implementation of this standard, "fixed source of emissions of gaseous total phosphorus Determination Quimociac Volume Act (Interim)"
(HJ 545-2009) Repealed.
This standard is revised by the Ministry of Environmental Protection Environmental Monitoring Department and Science and Technology Standards Division.
This standard was drafted. Beijing Environmental Protection Monitoring Center, Sichuan Institute of Industrial Environmental Monitoring.
This standard verification unit. Sichuan Institute of Industrial Environmental Monitoring, Chaoyang District, Beijing Environmental Protection Monitoring Station, Beijing
Dongcheng District Environmental Monitoring Station, Haidian District, Beijing Environmental Protection Agency monitoring station, Beijing North China Measurement North Detection Technology Co., Ltd.
And Beijing Environmental Protection Monitoring 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 gaseous total phosphorus - Quinocetone volumetric method
Warning. The bromine water and nitric acid used in the experiment are oxidizing and corrosive, and must be handled in a fume hood when formulated
Take care when handling samples and laboratories to avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of fixed sources of emissions of gaseous total phosphorus Quimociac volume method.
This standard applies to the determination of gaseous total phosphorus in fixed sources of exhaust gas.
When the sample volume is 18 L, the detection limit of the method is 2 mg/m3 and the lower limit of determination is 8 mg/m3. When the sample volume is
4.5 L, the detection limit of the method is 7 mg/m3 and the lower limit of determination is 28 mg/m3.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this standard.
Determination of Particulate Matter and Gaseous Pollutants in Exhaust of Fixed Pollution Sources GB/T 16157
HJ/T 373 fixed pollution source monitoring quality assurance and quality control technical specifications (Trial)
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
Total gaseous phosphorus
Fixed pollution sources of gaseous single-phase phosphorus and phosphorus compounds in general.
4 method principle
The gaseous total phosphorus is absorbed by brominated nitric acid absorption liquid and oxidized to orthophosphate. In acidic medium, orthophosphate and quinalocin
Ketone to form a yellow quinoline phosphomolybdate ((C9H7N) 3H3 [PO4 · 12MoO3] · H2O) precipitate. The precipitate is filtered and washed
After dissolving in a known excess sodium hydroxide solution, after the completion of the reaction titration with hydrochloric acid standard solution of the remaining sodium hydroxide,
The gaseous total phosphorus content is calculated based on the amount of sodium hydroxide standard solution consumed.
The reaction is as follows.
Absorption reaction.
P4 16H2O 10Br2 = 4H3PO4 20 HBr
3P4 20HNO3 8H2O = 12H3PO4 20NO ↑
P4O8 8H2O 2Br2 = 4H3PO4 4HBr
PH3 4H2O 4Br2 = H3PO4 8HBr
Precipitation reaction.
H3PO4 3C9H7N 12Na2MoO4 24HNO3 = (C9H7N) 3H3 [PO4 · 12MoO3] · H2O 11H2O 24NaNO3
Dissolution reaction.
(C9H7N) 3H3 [PO4 · 12MoO3] · H2O 26NaOH = Na2HPO4 12Na2MoO4 3C9H7N 15H2O
Titration reaction.
NaOH HCl = NaCl H2O
5 Interference and elimination
Hydrogen sulfide has an impact on the sampling process, discoloration of brominated nitric acid absorption solution, thereby reducing the oxidation of brominated nitric acid, and
Sulfate and elemental sulfur are produced. Increase the first absorption of brominated bromine absorption of the amount of liquid nitrogen so that hydrogen sulfide in the first absorption bottle
Is fully absorbed within, eliminating the interference of hydrogen sulfide on the sampling process. Sulfate does not react with Quimociac because of simple substance
Sulfur can not be dissolved in sodium hydroxide, it does not affect the measurement results.
Fluoride, arsenic and their compounds have no interference with this method.
6 Reagents and materials
Unless otherwise specified, all analytically pure reagents that meet the national standards were used for the analysis. Water used for the experiment was prepared using 6.1.
6.1 Water. No carbon dioxide water, prepared by one of the following methods.
6.1.1 Boiling method.
Take appropriate deionized or distilled water into beakers as needed, boil for at least 10 minutes, or allow water to evaporate 10%
On the cover cold.
6.1.2 aeration method.
Pass inert gas or pure nitrogen into deionized or distilled water to saturation.
6.2 Sodium molybdate (Na2MoO4 · 2H2O).
6.3 Citric acid (C6H8O7 · H2O).
6.4 Sodium hydroxide (NaOH). excellent grade pure.
6.5 Nitric acid. ρ (HNO3) = 1.42 g/ml.
6.6 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.7 Absolute ethanol. ρ (CH3CH2OH) = 0.79 g/ml.
6.8 Bromine water. ω (Br2) = 3%.
6.9 Quinoline. ρ (C9H7N) = 1.09 g/ml.
6.10 Acetone. ρ (CH3COCH3) = 0.79 g/ml.
6.11 potassium hydrogen phthalate (C8H5KO4). reference reagent.
105 ~ 110 ℃ electric oven to constant weight, placed in the dryer spare.
6.12 nitric acid solution. 1 1.
Take 250 ml nitric acid (6.5) into 250 ml water and mix well.
6.13 brominated nitric acid absorption solution. 3 1.
In the absorption bottle by adding 30 ml of nitric acid solution (6.12), then add 10 ml of bromine water (6.8), the absorption of liquid now with the match.
6.14 Quimociac solution.
6.14.1 Weigh 70 g of sodium molybdate (6.2) dissolved in 100 ml of water.
6.14.2 Add 85 ml of nitric acid (6.5) to 150 ml of water and dissolve 60 g of citric acid (6.3) in the above solution.
6.14.3 With constant stirring, slowly pour solution 6.14.1 into solution 6.14.2.
6.14.4 Add 35 ml of nitric acid (6.5) and 5 ml of quinoline (6.9) in 100 ml of water.
6.14.5 The solution 6.14.4 poured into solution 6.14.3, placed in the dark for 12 h, with a No. 4 glass sand funnel (7.4)
Filtration, add 280 ml of acetone (6.10) to the filtrate, dilute to 1000 ml with water, mix and store in a polyethylene bottle.
This solution can be stored for 6 months without light. If it is found that the polyethylene bottle has obvious flatulence, it should be reconstituted.
6.15 sodium hydroxide standard titration solution. c (NaOH) ≈ 0.3 mol/L, the result retained 4 significant figures.
6.15.1 Preparation
Weigh 110 g of sodium hydroxide (6.4), dissolved in 100 ml of water, shake, into the polyethylene container, placed in sealed
The solution is clear. Pipette 16.2 ml supernatant into a volumetric flask, dilute to 1000 ml with water and shake well.
6.15.2 Calibration
Weigh 2.25 g (accurate to 0.1 mg) potassium hydrogen phthalate (6.11), dissolve in 50.0 ml of water, add 2 drops of phenol
Phthalocyanine (6.17) is titrated with sodium hydroxide solution (6.15.1) until the solution is pink and remains unchanged for 30 s.
Another 50.0 ml of water, with the above method for blank titration.
Sodium hydroxide standard titration solution concentration calculated by the formula (1).
204.22
1 2
VV
c NaOH m
(1)
Where. c (NaOH) - sodium hydroxide standard titration solution concentration, mol/L;
m - the mass of potassium hydrogen phthalate, g;
V1 - sodium hydroxide standard titration solution volume, ml;
V2 - blank test volume of sodium hydroxide standard titration solution, ml;
204.22 - The molar mass of potassium hydrogen phthalate, g/mol.
6.16 hydrochloric acid standard titration solution. c (HCl) ≈ 0.1 mol/L, the result retained 4 significant figures.
6.16.1 Preparation
Pipette 9 ml of hydrochloric acid (6.6), diluted with water to 1000 ml, and mix.
6.16.2 Calibration
Accurately aspirate 50.00 ml hydrochloric acid solution (6.16.1) in a 250 ml Erlenmeyer flask, add 50.0 ml of water and 2 drops of phenolphthalein
Indicator (6.17), with sodium hydroxide standard titration solution (6.15) titration to pink, and keep 30 s does not change color, remember
Record consumption of sodium hydroxide standard titration solution volume.
Hydrochloric acid standard titration solution concentration by the formula (2) Calculated.
c HCl c1 V1
(2)
Where. c (HCl) - hydrochloric acid standard titration solution concentration, mol/L;
V-- volume of hydrochloric acid standard titration solution, ml;
c1 - sodium hydroxide standard titration solution concentration, mol/L;
V1 - volume of sodium hydroxide standard titration solution, ml.
6.17 phenolphthalein indicator solution. ρ = 10 g/L.
Weigh 1 g of phenolphthalein dissolved in 100 ml of absolute ethanol (6.7).
6.18 methyl orange indicator solution. ρ = 0.5 g/L.
Weigh 0.05 g of methyl orange dissolved in 100 ml of water.
6.19 Teflon microporous membrane. 0.45 μm, suction filtration.
6.20 Acetate Microporous Membrane. 0.45 μm, used to remove particulate matter.
7 instruments and equipment
Unless otherwise stated, the A-grade glassware in accordance with national standards was used for the analysis.
7.1 flue gas sampler. flow range 0 ~ 1 L/min.
7.2 Brown porous glass absorption bottle. 100 ml, as shown in Figure 1. Requirements glass 2/3 area on the foam fine and uniform,
No bubbles escape from the rim, and resistance should be (5 ± 0.7) kPa at a flow rate of 0.5 L/min.
Figure 1 porous glass absorption bottle (unit. mm)
7.3 Burette. 25 ml.
7.4 glass sand funnel. No. 4, aperture 5 ~ 15 μm.
7.5 Filter Clamp. Size and cellulose acetate microporous membrane (6.20) match.
8 samples
8.1 Sample Collection
According to GB/T 16157 for sample collection. Within 1 h, 3 to 4 samples were collected at equal time intervals, and samples were taken from each group
Connect in series two absorption bottles containing 40 ml Brominated HNO3 (6.13) and place the filter (6.20) in the filter holder (7.5)
Within, pick up in the absorption bottle to remove particulate phosphorus. In order to prevent corrosive sampler of strong oxidizing absorption liquid, measure and control in flow
The middle of the device and the absorption bottle connected to a built-in 40 ml sodium hydroxide standard titration solution (6.15) of the buffer bottle, absorption bottle
Place in an ice water bath, sampling device shown in Figure 2. Each group of samples collected at a flow rate of 0.3 L/min, sampling 10 ~ 15 min.
After the sampling is finished, immediately cut off the gas pipe between the sampling tube and the absorption bottle to prevent reverse suction, and seal the absorption bottle entrance, avoid light
Shipped back to the laboratory.
Note 1. elemental phosphorus ignition point 40 ℃, the sampling tube should not be heated.
NOTE 2 The presence of hydrogen sulfide in the exhaust of the source of pollution can cause complete fading of the brominated nitric acid in the first absorption cylinder during the sampling process and may
Elemental sulfur precipitation. Sampling process, should always ensure that the second absorption of brominated nitric acid bottle does not completely fade, or should be increased
The first absorption of brominated nitric acid in the absorption liquid volume of the resample.
Note 3. In the sampling process, brominated nitric acid absorption solution instability, each sampling time should not exceed 20 min.
Note 4. 5 drops of methyl orange solution (6.18) can be added to the buffer bottle. If the solution in the buffer bottle changes from yellow to orange during sampling,
Description Brominated nitric acid penetration occurs, should immediately stop sampling.
Figure 2 Schematic diagram of gaseous total phosphorus in fixed pollution source exhaust gas
8.2 full program blank
Bring the same batch of two absorption bottles (7.2) each containing 40 ml Brominated Nitric Acid Absorbent Solution (6.13) to the sampling site and not
Connected with the sampler, the sample taken back to the laboratory after the test.
8.3 Sample Storage
After sample collection, stored at 0 ~ 4 ℃ dark, measured within a week.
8.4 Sample Preparation
8.4.1 Respectively, the absorption solution of the two absorption bottles collected in each group were combined, poured into a 250 ml beaker, within the hood
Heat evaporation, concentrated to about 10 ml, make it completely oxidized, then add hydrochloric acid (6.6), continue to catch bromine, until the solution was no
color. Add 10 ml of nitric acid solution (6.5), diluted with water to about 100 ml, cover the surface of the dish, heated to boiling, stirring constantly
Mix 45 ml of QuimocAMP (6.14), continue to heat, keep slightly boiled for 1 min, remove the beaker and allow to cool to
At room temperature, it was filtered with a suction filter and the precipitate was washed with water until neutral.
8.4.2 Concentration of less than 28 mg/m3 of the sample, all 3 to 4 groups of absorbing liquid combined (equivalent to sampling 18 L), into
In a 500 ml beaker, prepare a sample as described in 8.4.1.
8.5 Preparation of blank samples
8.5.1 Laboratory blank sample
Take the same batch, the same volume of absorbent, according to the same sample preparation step (8.4) of the laboratory blank sample
preparation.
8.5.2 full program blank sample
The entire program blank sample (8.2), according to the same steps with the sample preparation (8.4) for the entire program blank sample system
Prepare
9 Analysis steps
9.1 Determination of the sample
Transfer the pellet and filter (6.19) into a 250 ml Erlenmeyer flask and drop a sodium hydroxide standard titration solution (6.15) with a burette.
While adding edge shake until the precipitate is completely dissolved and then add 5.00 ml, accurately record the volume of added sodium hydroxide standard solution. Join
50.0 ml of water and 2 drops of methyl orange indicator solution (6.18) titrated with hydrochloric acid standard titration solution (6.16) until the solution is changed from yellow
Orange, accurate record of the volume of hydrochloric acid standard titration solution.
9.2 Blank test
According to the same procedure as the sample determination (9.1), the blank of the laboratory and the blank of the whole procedure were measured.
10 Results Calculation and Presentation
10.1 Calculation Results
According to the formula (3) to calculate the fixed source of exhaust gas in the total phosphorus content.
nd V
P c V c V
1 1 2 2 () () 1.191 10
(3)
Where. ρ (P) - the total phosphorus content of gaseous pollutants in fixed pollution sources, mg/m3;
c1 - sodium hydroxide standard titration solution concentration, mol/L;
V1 - sodium hydroxide standard titration solution volume, ml;
c2-- hydrochloric acid standard titration solution concentration, mol/L;
V2 - titration consumed hydrochloric acid standard titration solution volume, ml;
1.191 - per mol of hydroxyl corresponding to the mass of phosphorus, g/mol;
Vnd - Sample volume of dry flue gas at standard state (101.325 kPa, 273.15 K), L.
10.2 results indicated
When the total phosphorus content of fixed-source exhaust gas is less than 100 mg/m3, the result is retained to the whole digit; when the fixed pollution
When the total phosphorus content in the source exhaust gas is greater than or equal to 100 mg/m3, the result retains 3 significant figures.
11 precision and accuracy
11.1 precision
6 laboratories were phosphorus levels of 0.20 mg, 2.50 mg and 5.00 mg of brominated nitric acid solution for 6 times
The relative standard deviations in the test ranged from 2.3% to 4.8%, from 0.2% to 2.1% and from 0.4% to 2.0%
The relative standard deviations were 5.0%, 2.2% and 0.9% respectively. The repeatability limits were 0.02 mg, 0.25 mg and 0.18 mg, respectively.
Reproducibility limits were 0.04 mg, 0.18 mg and 0.21 mg, respectively.
11.2 Accuracy
Six laboratories respectively for blank bromide nitric acid absorption liquid spiked with three kinds of determination, the spiked levels were
0.20 mg, 2.50 mg and 5.00 mg. Laboratory standard spiked recoveries were 95.0% to 110%, 96.4% to 102%, respectively
98.0% ~ 101%. The final recoveries of spiked samples were 103% ± 10.5%, 99.3% ± 4.8% and 99.3% ±
2.1%.
12 Quality Assurance and Quality Control
12.1 Each batch of samples to make at least one laboratory blank and a full program blank, the determination of the results should be less than the method of detection
limit. Otherwise, find out the reason and resample the analysis.
12.2 Make at least one blank spiked sample for each batch of samples, the recovery rate should be 90% ~ 110%.
12.3 Sample collection quality assurance and quality control with reference HJ/T 373 implementation.
13 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.
14 Precautions
14.1 For high concentration samples, due to the large amount of precipitation, wash thoroughly with large amounts of water to ensure that the precipitate is washed to neutrality,
In order to avoid titration error, affect the measurement results.
14.2 All glassware must be soaked with dilute hydrochloric acid or dilute nitric acid.
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| Standard ID | HJ 545-2017 (HJ545-2017) | | Description (Translated English) | Stationary source emission��Determination of total gaseous phosphorus -- Quimociac volumetric analysis | | Sector / Industry | Environmental Protection Industry Standard | | Word Count Estimation | 12,162 | | Date of Issue | 2017-12-29 | | Date of Implementation | 2018-04-01 | | Older Standard (superseded by this standard) | HJ 545-2009 | | Drafting Organization | Chinese Academy of Environmental Sciences | | Administrative Organization | Ministry of Environmental Protection | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 86 |
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