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HJ 593-2010 English PDF

HJ 593-2010_English: PDF (HJ593-2010)
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HJ 593-2010English239 Add to Cart 3 days [Need to translate] Water quality. Determination of phosphorus. Phosphomolybdenum blue spectrophotometric method Valid HJ 593-2010


BASIC DATA
Standard ID HJ 593-2010 (HJ593-2010)
Description (Translated English) Water quality. Determination of phosphorus. Phosphomolybdenum blue spectrophotometric method
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Classification of International Standard 13.060.01
Word Count Estimation 9,926
Date of Issue 2010-10-21
Date of Implementation 2011-01-01
Quoted Standard 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. 77 of 2010
Summary This standard specifies the determination of elemental phosphorus molybdenum blue spectrophotometric method. This standard applies to surface water, groundwater, industrial wastewater and domestic sewage in the determination of elemental phosphorus. When the sample volume is 100ml, direct colorimetric method detection limit of 0. 003mg/L, detection limit of 0. 010mg/L, measured a maximum of 0. 170mg/L.

Standards related to: HJ 593-2010

HJ 593-2010
Water quality.Determination of phosphorus.Phosphomolybdenum blue spectrophotometric method
National Environmental Protection Standard of the People's Republic
Water quality - Determination of phosphorus - Molybdenum blue spectrophotometric method
(temporary)
Water quality-Determination of phosphorus-phosphomolybdenum blue
Spectrophotometric method
Released on.2010-10-21
2011-01-01 implementation
Ministry of Environmental Protection released
I directory
Foreword. II
1 Scope.1
2 Normative references.1
3 principle of the method.1
4 Interference and elimination 1
5 reagents and materials 1
6 Instruments and equipment 3
7 sample 3
8 Analysis steps.3
9 result calculation.4
10 Notes.5
Foreword
In order to implement the "Environmental Protection Law of the People's Republic of China" and the "Water Pollution Prevention and Control Law of the People's Republic of China"
The body health, standardize the determination method of elemental phosphorus in water, and develop this standard.
This standard specifies the phosphorus molybdenum blue spectrophotometric method for the determination of elemental phosphorus in water.
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 October 21,.2010.
This standard has been implemented since January 1,.2011.
This standard is explained by the Ministry of Environmental Protection.
1Water quality - Determination of phosphorus - Molybdenum blue spectrophotometric method
Warning. Toluene is toxic, perchloric acid, potassium bromate-potassium bromide solution is corrosive, and the mixture of perchloric acid and organic matter may explode when heated.
Operation must be carried out in a fume hood, the operator must be careful
1 Scope of application
This standard specifies the phosphorus molybdenum blue spectrophotometric method for the determination of elemental phosphorus in water.
This standard applies to the determination of elemental phosphorus in surface water, groundwater, industrial wastewater and domestic sewage.
When the sampling volume is 100ml, the detection limit of the direct colorimetric method is 0.003mg/L, and the lower limit of determination is 0.010 mg/L.
The upper limit of the measurement was 0.170 mg/L.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate.
Used in this standard.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Principle of the method
The toluene is used as an extractant to extract elemental phosphorus from the water sample. The extract is oxidized into elemental phosphorus by potassium bromate-potassium bromide solution.
Orthophosphate, under acidic conditions, the phosphomolybdate heteropoly acid formed by the reaction of orthophosphate with ammonium molybdate is reduced by the reducing agent stannous chloride
To a blue complex, the absorbance is proportional to the content of elemental phosphorus, and the absorbance is measured by a spectrophotometer to calculate the elemental phosphorus.
The content.
When the content of elemental phosphorus in water is less than 0.05mg/L, the coloration determination after enrichment with butyl acetate can reduce the dryness.
Disturbance, improve sensitivity and reliability of detection.
4 interference and elimination
When the amount of arsenide, silicide and sulfide in the water sample is 100 times,.200 times and 300 times of the elemental phosphorus content, respectively,
There is no significant interference with this method.
5 reagents and materials
Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. The test water is in accordance with GB/T 6682.
Three levels.
5.1 Toluene. ρ (C7H8) = 0.867 g/ml, excellent grade pure.
5.2 Hydrochloric acid. ρ (HCl) = 1.19g/ml, excellent grade pure.
25.3 Perchloric acid. ρ (HClO4) = 1.67g/ml, excellent grade pure.
5.4 Ascorbic acid (C6H8O6), excellent grade.
5.5 Glycerol. ρ (C3H8O3) = 1.26g/ml, excellent grade pure.
5.6 Anhydrous ethanol. ρ (CH3CH2OH) = 0.789 g/ml, excellent grade pure.
5.7 butyl acetate. ρ (C8H16O2) = 0.776 g/ml, excellent grade pure.
5.8 Potassium dihydrogen phosphate (KH2PO4). excellent grade pure.
5.9 Nitric acid solution. 1 5.
5.10 Sulfuric acid solution. 1 1.
5.11 Sodium hydroxide solution. ω (NaOH) = 20%.
20.0 g of sodium hydroxide was weighed and dissolved in 100 ml of water.
5.12 Potassium bromate-potassium bromide solution.
10 g of potassium bromate (KBrO3) and 8 g of potassium bromide (KBr) were weighed and dissolved in 400 ml of water.
5.13 Ammonium molybdate solution I. ω [(NH4)6Mo7O24 · 4H2O] = 2.5%.
2.5 g of ammonium molybdate was weighed, and 70 ml of a 1.1 sulfuric acid solution (5.10) was added. After the ammonium molybdate was dissolved, it was diluted with water to 100 ml.
5.14 Ammonium molybdate solution II. ω[(NH4)6Mo7O24 ·4H2O]=5%.
Weigh 12.5g of ammonium molybdate, dissolve it in 150ml of water, stir constantly, add it slowly to 100ml (1 5)
Acid solution (5.9).
5.15 Stannous chloride solution. ω (SnCl2) = 1%.
Weigh 1g of stannous chloride, dissolve it in 15ml of hydrochloric acid (5.2), add 50ml of water, and weigh 1.5g of ascorbic acid.
(5.4), dissolved in the above solution, diluted with water to 100ml, stored in a brown bottle, can be stored in the refrigerator for 4 to 5 days.
5.16 Stannous chloride glycerol solution. ω (SnCl2) = 2.5%.
2.5 g of stannous chloride was weighed and dissolved in 100 ml of glycerol (5.5). This solution can be heated in a water bath to promote dissolution
solution.
5.17 Potassium dihydrogen phosphate standard stock solution. ρ (P) = 50.0 μg/ml.
Accurately weigh 0.2197g potassium dihydrogen phosphate (5.8) (previously dried in an electric oven at 105 ° C ~ 110 ° C for 2 h to constant weight),
Dissolve in water, transfer to a 1000 ml volumetric flask, dilute with water to the score line, and mix.
5.18 Potassium dihydrogen phosphate standard use solution. ρ (P) = 2.00 μg/ml.
For use, draw 10.00 ml of potassium dihydrogen phosphate standard stock solution (5.17) in a 250 ml volumetric flask and dilute with water until now.
line.
5.19 Phenolphthalein indicator solution. ρ = 10 g/L.
3 Weigh 1 g of phenolphthalein and dissolve it in 100 ml of absolute ethanol (5.6).
6 Instruments and equipment
6.1 Visible spectrophotometer. equipped with a cuvette with an optical path of 30 mm.
6.2 Electric heating plate.
6.3 with colorimetric tube. 50ml.
6.4 Separating funnel. 100ml, 250ml.
6.5 Grinding cone. 250ml.
6.6 Explosion-proof boiling glass beads.
7 samples
7.1 Sample collection and preservation
Samples were collected into plastic bottles or hard glass bottles. After sampling, the pH of the samples was adjusted to 6-7, measured within 48 hours.
7.2 Sample preparation
7.2.1 Extraction
Pipette 10.0 ~ 100ml (depending on the phosphorus content in the sample) sample in a 250ml separatory funnel, add 25ml toluene
(5.1), fully oscillate for 5 min, and often open the piston exhaust. After standing and layering, move the lower aqueous phase to another 250ml
The separatory funnel was added to 15 ml of toluene (5.1) and extracted repeatedly for 2 min, then allowed to stand, the aqueous phase was discarded, and the organic phase was incorporated into the first branch.
Separating funnel. Add 15 ml of water to the first separatory funnel, shake for 1 min, let stand, discard the aqueous phase, and repeat the organic phase.
Washed 6 times.
7.2.2 Oxidation
Add 10-15 ml potassium bromate-potassium bromide solution (5.12) to the first separatory funnel containing the organic phase, 2 ml
(1 1) Sulfuric acid solution (5.10), oscillate for 5 min, and often open the piston exhaust. 2ml perchloric acid after standing for 2 minutes
(5.3), after shaking for another 5 minutes, transfer into a 250ml grind cone, add several glass beads, slowly add on the hot plate
Heat to drive off excess perchloric acid and remove bromine (be careful not to spill or evaporate the sample). When the white smoke is reduced, remove the cooling. plus
Into 10ml of water and 1 drop of phenolphthalein indicator (5.19), neutralized with 20% sodium hydroxide solution (5.11) until pink, add dropwise
(1 1) The sulfuric acid solution (5.10) disappeared to the pink color, transferred to a 50 ml volumetric flask, and diluted to the mark with deionized water.
8 Analysis steps
8.1 Drawing of the calibration curve
8.1.1 Direct colorimetry. For samples with an elemental phosphorus content greater than 0.05 mg/L, the calibration curve is followed by the following procedure.
4 Take 8 50 ml plug colorimetric tubes and prepare a calibration series according to Table 1.
Table 1 Elemental Phosphorus Direct Colorimetric Calibration Series
Bottle number 0 1 2 3 4 5 6
Potassium dihydrogen phosphate standard use solution (5.18), ml 0.00 0.50 1.00 3.00 5.00 7.00 8.50
Elemental phosphorus content, μg 0.00 1.00 2.00 6.00 10.0 14.0 17.0
Add water to each colorimetric tube to 50ml, add 2ml ammonium molybdate solution I (5.13) and 1ml stannous chloride
Mix the oil solution (5.16).
Room temperature is above 20 ° C, color development for 20 min; room temperature below 20 ° C, color development for 30 min. At a wavelength of 690 nm,
The absorbance was measured using a 30 mm cuvette with water as a reference. The absorbance corresponding to the blank of the reagent is plotted against the elemental phosphorus content.
Calibration curve.
8.1.2 Extraction colorimetry. For samples with an elemental phosphorus content of less than 0.05 mg/L, the calibration curve is followed by the following procedure.
Take 6 100 ml separatory funnels and prepare a calibration series according to Table 2.
Table 2 Elemental Phosphorus Extraction Colorimetric Calibration Series
Bottle number 0 1 2 3 4 5
Potassium dihydrogen phosphate standard use solution (5.18), ml 0.00 0.50 1.00 1.50 2.00 2.50
Elemental phosphorus content, μg 0.00 1.00 2.00 3.00 4.00 5.00
Add water to each separatory funnel to 50ml, add 3ml (1 5) nitric acid solution (5.9), 7ml ammonium molybdate solution
Liquid II (5.14) and 10 ml of butyl acetate (5.7) were shaken for 1 min and the aqueous phase was discarded. Add 2ml of chlorination to the organic phase
Stannous solution (5.15), shake well, add 1ml of absolute ethanol (5.6), gently rotate the separatory funnel to lower the water droplets.
The aqueous phase was drained, and the organic phase was poured into a 30 mm cuvette, and the absorbance was measured at a wavelength of 720 nm using butyl acetate as a reference.
A calibration curve is drawn by subtracting the absorbance of the reagent blank from the elemental phosphorus content.
8.2 Sample Analysis
8.2.1 For samples with an elemental phosphorus content greater than 0.05 mg/L, direct colorimetry is used.
Pipette an appropriate amount of sample prepared by extraction and oxidation (7.2) (depending on the content of elemental phosphorus in the sample) in 50ml
In the case of a plug colorimetric tube, the following steps are the same as in 8.1.1.
8.2.2 Samples with an elemental phosphorus content of less than 0.05 mg/L are extracted by organic phase.
Pipette an appropriate amount of sample prepared by extraction and oxidation (7.2) (depending on the content of elemental phosphorus in the sample) in 100ml
In the separatory funnel, the following steps are the same as in 8.1.2.
9 Calculation of results
The elemental phosphorus content ρ in the sample is calculated according to formula (1)
VV
mV (1)
Where. ρ—the content of elemental phosphorus in the sample, mg/L;
M-calculated the content of elemental phosphorus in the sample according to the calibration curve, μg;
V1 - sample volume, ml;
V2—the volumetric volume of the sample, V2=50ml;
V3—The volume of the sample taken during the color reaction, ml.
10 Precautions
10.1 The glassware used for the operation can be soaked with (1 5) hydrochloric acid for 2 hours or with a detergent containing no phosphorus;
10.2 The cuvette should be soaked in a dilute nitric acid or chromic acid solution for a while to remove the adsorbed molybdenum blue colored material.
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