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HJ 546-2009 English PDF

HJ 546-2009_English: PDF (HJ546-2009)
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HJ 546-2009English639 Add to Cart 5 days [Need to translate] Ambient air. Determination of phosphorus pentoxide. Molybdenum blue ascorbiaccid to deoxidize spectrophotometric method Obsolete HJ 546-2009
HJ 546-2015English209 Add to Cart 3 days [Need to translate] Ambient air. Determination of phosphorus pentoxide. Molybdenum blue spectrophotometric method Valid HJ 546-2015
Newer version: HJ 546-2015

BASIC DATA
Standard ID HJ 546-2009 (HJ546-2009)
Description (Translated English) Ambient air. Determination of phosphorus pentoxide. Molybdenum blue ascorbiaccid to deoxidize spectrophotometric method
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z15
Classification of International Standard 13.040.20
Word Count Estimation 16,175
Date of Issue 2009-12-30
Date of Implementation 2010-04-01
Quoted Standard HJ/T 194; 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 ascorbic acid of phosphorus pentoxide in air Molybdenum blue spectrophotometric method. This standard applies to the determination of phosphorus pentoxide in the air.

Standards related to: HJ 546-2009

HJ 546-2009
Ambient air.Determination of phosphorus pentoxide.Molybdenum blue ascorbiaccid to deoxidize spectrophotometric method
National Environmental Protection Standard of the People's Republic
Determination of ambient air phosphorus pentoxide
Ascorbic acid reduction-molybdenum blue spectrophotometry (provisional)
Ambient air-Determination of phosphorus pentoxide
-Molybdenum blue ascorbiaccid to deoxidize spectrophotometric 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);
X. Determination of chlorine gas from fixed pollution sources, iodometric method (provisional) (HJ 547-2009);
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 and elimination.1
5 Reagents and materials.1
6 instruments and equipment..2
7 samples. 2
8 Analysis steps..3
9 result calculation..3
10 Quality Assurance and Quality Control.3
Foreword
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 Atmospheric Pollution
This standard is established for the determination of human body health and the regulation of phosphorus pentoxide in the air.
This standard specifies the ascorbic acid reduction-molybdenum blue spectrophotometric method for the determination of phosphorus pentoxide in air.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. 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 ambient air phosphorus pentoxide
Ascorbic acid reduction-molybdenum blue spectrophotometry (provisional)
1 Scope of application
This standard specifies the ascorbic acid reduction-molybdenum blue spectrophotometric method for the determination of phosphorus pentoxide in air.
This standard applies to the determination of phosphorus pentoxide in air.
The detection limit of this standard is 0.8 μg/50 ml. When the sampling volume is 5 m3, the detection limit is 0.2 μg/m3, and the lower limit of determination is 0.8 μg/m3.
When the sampling volume is 300 L, the detection limit is 0.003 mg/m3 and the lower limit of determination is 0.012 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.
HJ/T 194 Technical Specifications for Manual Air Quality Monitoring
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle of the method
The phosphorus oxide in the air is collected by a filter membrane such as perchloroethylene. After sampling, water and phosphorus pentoxide are added to form orthophosphoric acid. In acidic media
In the presence of bismuth potassium tartrate, orthophosphoric acid reacts with ammonium molybdate to form a phosphorus molybdenum heteropoly acid, which is reduced to a blue complex with ascorbic acid at 700
The absorbance is measured at the nm wavelength to calculate the phosphorus pentoxide content in the air.
4 interference and elimination
When the pentavalent arsenic is greater than 5 μg/ml, the tetravalent silicon is greater than 8 μg/ml, and the hexavalent chromium is greater than 16 μg/ml, there is interference with the determination of this method.
Sodium and sodium thiosulfate solutions eliminate interference.
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 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.2 Potassium dihydrogen phosphate. ρ (KH2PO4) = 2.34 g/ml, the reference reagent.
5.3 Sulfuric acid solution. c (1/2H2SO4) = 5 mol/L.
Measure 140 ml of sulfuric acid (5.1), slowly inject into a beaker containing 500 ml of water while stirring, and then dilute to 1000 ml with water after cooling.
Mix well.
5.4 Ammonium molybdate solution. ρ [(NH4)6Mo7O24] = 40 g/L.
Weigh 43.34 g of ammonium molybdate [(NH4)6Mo7O24·4H2O], dissolve in water, dilute to 1 000 ml, mix and store in polyethylene plastic
In the bottle, keep it in the refrigerator.
5.5 Ascorbic acid solution. ρ (C6H8O6) = 17 g/L.
Weigh 2.60 g of ascorbic acid, dissolve in water, dilute to 150 ml, and store in a brown bottle. Store in the refrigerator, if it does not change color
long-term use.
5.6 Potassium bismuth tartrate solution. ρ [K(SbO)C4H4O6]= 2.70 g/L.
Weigh 2.74 g of bismuth potassium tartrate [K(SbO)C4H4O6·1/2H2O], dissolve in an appropriate amount of water, dilute to 1000 ml with water, and mix.
5.7 Sodium sulfite solution. ρ (Na2SO3) = 100 g/L.
Weigh 100 g of sodium sulfite, dissolve in water, transfer to a 1 000 ml volumetric flask, dilute with water to the score line, and mix.
5.8 Sodium thiosulfate solution. ρ (Na2S2O3) = 10 g/L.
Weigh 15.70 g of sodium thiosulfate (Na2S2O3·5H2O), dissolve in water, transfer to a 1 000 ml volumetric flask, and dilute with water to the engraved line.
Mix well.
5.9 Potassium dihydrogen phosphate standard stock solution
Accurately weigh 0.191 7 g of potassium dihydrogen phosphate (5.2) dried in a 105-110 ° C electric oven to a constant weight, dissolved in water, and transferred to 1 000 ml.
In the measuring flask, dilute with water to the scribe line and mix. This solution is equivalent to 100.0 μg of phosphorus pentoxide per ml.
5.10 Potassium dihydrogen phosphate standard use solution
When ready to use, draw 10.00 ml of potassium dihydrogen phosphate standard stock solution (5.9) in a 100 ml volumetric flask, dilute with water to the engraved line, dissolve
The liquid is equivalent to 10.0 μg of phosphorus pentoxide per milliliter. A certified standard solution can also be used.
5.11 Mixed reducing agent
For use, take 40 ml of sodium sulfite solution (5.7) and sodium thiosulfate solution (5.8), and mix well with 20 ml of water.
5.12 Mixed developer
When used, mix 25 ml of sulfuric acid solution (5.3), 7.5 ml of ammonium molybdate solution (5.4) and 15 ml of ascorbic acid solution (5.5).
Together, add 2.5 ml of bismuth potassium tartrate solution (5.6) and mix. The developer was stable for only 4 h at room temperature.
Note 1. Ammonium molybdate and ascorbic acid solution are mixed and added to avoid the formation of silicon molybdenum blue.
Note 2. The addition of bismuth potassium tartrate accelerates the reaction rate at room temperature.
6 instruments
Unless otherwise stated, the analysis uses a Class A glass gauge that complies with national standards.
6.1 Particle sampler. medium flow sampler, 80 ~ 130 L/min; small flow sampler, 10 ~ 15 L/min or 0 ~ 30 L/min.
6.2 Visible spectrophotometer. has a 3 cm cuvette.
6.3 Filter membrane such as perchloroethylene. 0.45 μm.
6.4 Oven.
7 samples
7.1 Sample collection
7.1.1 Sampling with a medium flow sampler
When sampling, install the filter in the filter holder of the particle sampler, sample at a flow rate of 100 L/min for 45 to 60 minutes, and record the sample.
condition. After sampling, the filter is removed with a clean tweezers and placed in the sample box and brought back to the laboratory.
7.1.2 Sampling with a small flow sampler
When sampling, install the filter in the filter holder of the particle sampler, sample at 10 L/min for 10-20 min, and record the sample.
condition. After sampling, the filter is removed with a clean tweezers and placed in the sample box and brought back to the laboratory.
7.2 Preservation of samples
The sample should be stored dry at 0 to 4 ° C and measured within 1 week.
7.3 Preparation of samples
Use a pair of tweezers to remove the sampling filter from the sample box, place it in a 50 ml beaker, add 10 ml of water, and shake the beaker to allow the water to soak the filter.
Add 1.0 ml of sulfuric acid solution (5.3), stir and soak for more than 15 min, and filter the sample in a 50 ml volumetric flask with medium speed quantitative filter paper.
The beaker and the filter residue were washed in portions with 20 ml of water, and the washings were combined in a volumetric flask.
7.4 Preparation of blank samples
Take the same batch of blank filter membrane and follow the steps 7.3 to prepare a blank sample.
8 Analysis steps
8.1 Drawing of standard curves
Take 8 50 ml volumetric flasks and prepare a standard series according to Table 1.
Table 1 Standard series of phosphorus pentoxide
Bottle number 0 1 2 3 4 5 6 7
Potassium dihydrogen phosphate standard use solution (5.10)/ml 0.00 0.10 0.50 0.90 1.30 1.70 2.10 2.50
Phosphorus pentoxide content/μg 0.00 1.00 5.00 9.00 13.0 17.0 21.0 25.0
Add 5 ml of water, 1.0 ml of sulfuric acid solution (5.3) and 2.5 ml of mixed reducing agent (5.11) to the volumetric flask, mix and let stand for 10 min.
Add water to about 40 ml, add 8.0 ml of mixed color developer (5.12), dilute with water to the scribe line, and mix.
The color was developed at room temperature above 20 ° C for 25 min; when the temperature was below 20 ° C, the color was developed for 35 min. 3 cm colorimetric at 700 nm
Dish, using water as a reference, measuring the absorbance, plotting the standard curve of the absorbance with the phosphorus pentoxide content (μg), and calculating the standard curve
Regression equation.
8.2 Determination
Add 2.5 ml of mixed reducing agent (5.11) to the volumetric flask of sample (7.3) and blank sample (7.4), mix and place for 10 min.
The following steps are plotted with the standard curve.
9 Calculation of results
Calculate the mass concentration of phosphorus pentoxide in air according to formula (1).
Nd
(PO)
Mm
ρ −= (1)
Where. ρ (P2O5) - mass concentration of phosphorus pentoxide in air, μg/m3;
M--calculated from the standard curve, the content of phosphorus pentoxide on the sample filter, μg;
M0--calculated from the standard curve, the content of phosphorus pentoxide on the blank filter, μg;
Vnd - the volume of air extracted under standard conditions (101.325 kPa, 273 K), m3.
10 Quality Assurance and Quality Control
Quality assurance and quality control shall be in accordance with HJ/T 194. The sampler should be air tight and flow calibrated before use.
Do not touch the filter membrane with your fingers during the sample and analysis process to prevent contamination.
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