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HJ 712-2014: Solid waste-Determination of total phosphorus. Ammonium metamolybdate spectrophotomtric method
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Solid waste-Determination of total phosphorus. Ammonium metamolybdate spectrophotomtric method
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HJ 712-2014
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Basic data | Standard ID | HJ 712-2014 (HJ712-2014) | | Description (Translated English) | Solid waste-Determination of total phosphorus. Ammonium metamolybdate spectrophotomtric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z13 | | Word Count Estimation | 9,977 | | Date of Issue | 11/27/2014 | | Date of Implementation | 1/1/2015 | | Quoted Standard | HJ/T 20 | | Regulation (derived from) | Ministry of Environmental Protection Notice 2014 No. 77 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of total phosphorus in the solid waste Partial molybdate spectrophotometric method. This standard applies to be crushed solid or semi-solid determination of total phosphorus in the solid waste. When the sample vol | HJ 712-2014: Solid waste-Determination of total phosphorus. Ammonium metamolybdate spectrophotomtric method
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Solid waste-Determination of total phosphorus.Ammonium metamolybdate spectrophotomtric method
People's Republic of China National Environmental Protection Standards
Solid waste - Determination of total phosphorus
Partial molybdate spectrophotometry
Solid waste-Determination of total phosphorus-Ammonium metamolybdate
spectrophotometric method
(release
draft)
Issued on.2014-11-27
2015-01-01 implementation
Ministry of Environmental Protection released
i Table of Contents
Preface .ii
1. Scope .1
2 Normative references .1
3 .1 The principle of the method
4 and eliminate interference 1
5 Reagents and materials 1
6 instruments and equipment 2
Sample 2 7
Analysis Step 8 .3
9 result of the calculation .3
10 precision and accuracy .4
11 Quality assurance and quality control ..4
12 Precautions .4
Foreword
To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Solid Waste Pollution Prevention Law"
Protecting the environment, safeguarding human health, specifications can be crushed in solid, semi-solid determination of total phosphorus in the solid waste of the enactment of this
standard.
This standard specifies the determination of total phosphorus in the solid waste Partial molybdate spectrophotometric method.
This standard is the first release.
This standard is developed by the Ministry of Environmental Protection Science, Technology organization.
Drafting of this standard. Nantong Municipal Environmental Monitoring Center.
The standard verification. Jiangsu Provincial Environmental Monitoring Center, Suzhou Municipal Environmental Monitoring Center, Yangzhou Municipal Environmental Monitoring Center
Station, Zhenjiang Municipal Environmental Monitoring Center, Nantong City Agricultural Products Quality Testing Center and Nantong, Tongzhou District Environmental Monitoring Station.
This standard MEP November 27, 2014 for approval.
This standard since January 1, 2015 implementation.
The standard explanation by the Ministry of Environmental Protection.
Determination of Solid Waste 1 TP Partial molybdate spectrophotometry
1 Scope
This standard specifies the determination of total phosphorus in the solid waste Partial molybdate spectrophotometric method.
This standard applies to be crushed solid or semi-solid determination of total phosphorus in the solid waste.
When the sample volume is 0.5 g, volume by volume of 50 ml, using a 30 mm cuvette when the standard method detection limit of 3
mg/kg, detection limit of 12 mg/kg.
2 Normative references
This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable
For this standard.
HJ/T 20 industrial solid waste sampling sample preparation Technical Specifications
3 PRINCIPLE OF THE METHOD
Solid waste system by nitric acid digestion, in which the phosphorus soluble salts and organic matter is completely converted to soluble orthophosphate
Salt, under acidic conditions to form a yellow heteropoly metavanadate and ammonium molybdate react with acids to measure absorbance at a wavelength of 420 nm
Luminosity. Within a certain range of concentrations, the phosphate content of the absorbance values conform to the Lambert - Beer law.
4 and elimination of interference
Microwave digestion - Partial molybdate spectrophotometric determination of total phosphorus in the solid waste, the color liquid Fe3 concentration of less than 100 mg/L,
Cr6 concentrations below 18 mg/L when measured without interference.
5 Reagents and materials
Unless otherwise indicated, the use of chemical reagents analytical line with national standards of analysis, to test water for the preparation of the new
Ionized or distilled water.
5.1 concentrated nitric acid. ρ (HNO3) = 1.40 g/ml, pure class distinctions.
Concentrated sulfuric acid 5.2. ρ (H2SO4) = 1.84 g/ml.
5.3 sulfuric acid solution. c (H2SO4) = 0.5 mol/L
Measure 5.5 ml of concentrated sulfuric acid (5.2) was slowly poured into a small amount of water and dilute to 200 ml.
5.4 Sodium carbonate solution. w (Na2CO3) = 10%
Weigh 10 g of sodium carbonate (Na2CO3) was dissolved in 100 ml of water.
5.5 potassium dihydrogen phosphate (KH2PO4). pure class distinctions.
Proper amount of potassium dihydrogen phosphate (of KH2PO4) in a weighing bottle is placed 105 ℃ drying 2 h, cooling the oven and set aside.
5.6 ammonium molybdate solution. ρ [(NH4) 6Mo7O24 · 4H2O] = 62.5 g/L
Weigh 25 g of ammonium paramolybdate [(NH4) 6Mo7O24 · 4H2O] was dissolved in 400 ml of water.
5.7 metavanadate solution. ρ [NH4VO3] = 2.27 mg/L
Weigh 1.25 g of ammonium metavanadate (NH4VO3) was dissolved in 300 ml boiling water, after cooling, was added 250 ml of concentrated nitric acid (5.1),
Cooled to room temperature.
25.8 molybdate - a mixed solution of ammonium metavanadate
The ammonium molybdate solution (5.6) was slowly added a solution of ammonium metavanadate (5.7), diluted with water to 1000 ml. Placed in the refrigerator 2 ~
5 ℃ preservation, stable for at least a year, if turbidity occurs, the discarded reconfiguration.
5.9 P standard stock solution. ρ (P) = 1000 mg/L
Weigh 4.3940 g of potassium dihydrogen phosphate (5.5) dissolved in about 200 ml of water, add 5 ml of concentrated sulfuric acid (5.2) to move to 1000
ml volumetric flask, add water to the mark, and mix. The solution was stored in a brown reagent bottle, valid for one year. Or direct
Purchase a commercially available certified reference solution.
5.10 Phosphorus standard solution. ρ (P) = 20 mg/L
Pipette 10.00 ml phosphate standard stock solution (5.9) to 500 ml flask, water volume, and the solution with the existing Pro.
5.11 Indicator. 2,6-dinitrophenol (C6H4N2O5) or 2,4-dinitrophenol (C6H4N2O5)
Weigh 0.2 g 2,6- or 2,4-dinitrophenol dinitrophenol is dissolved in 100 ml of water.
6 instruments and equipment
6.1 Visible Spectrophotometer. with 30 mm glass cuvette.
6.2 Microwave Digestion System. Maximum power 1600 W.
6.3 Electric digester. special microwave digestion tank (50 ~ 200 ℃, the output power of 1600 W).
6.4 Electric board. 50 ~ 200 ℃, the output power of 3000 W.
6.5 Analytical balance. accuracy of 0.0001 g.
6.6 plug colorimetric tube. 50 ml.
6.7 General Commonly used laboratory instruments and equipment.
7 Sample
7.1 collection, preservation and preparation
Collection and preservation of samples were prepared in accordance with HJ/T relevant provisions 20.
7.2 Preparation of the sample
It weighs about 0.2 ~ 0.5 g sample (accurate to 0.0001 g), placed in a microwave digestion vessel, with the amount of water wet sample,
Add 10 ml of concentrated nitric acid (5.1), stamped with a cold digestion overnight (at least 16 hours), and then placed in a microwave digestion digestion (L
Temperature program refer to Table 1), after digestion is complete cooling. The microwave digestion tank into the digester to about 160 ℃ electric rush acid sample was adhered to
Viscous. If after a hot plate to catch the acid digestion solution can be completely transferred to a glass beaker on a hot plate heated to about 160 ℃ sample
It was sticky. As the test solution does not show then the digestion is not completely white, etc., cool to room temperature, plus the amount of concentrated nitric acid (5.1), following the
Continued hurry microwave digestion and acid until the sample was gray. Remove the microwave digestion vessel was cooled to room temperature, the samples were all transferred to
50 ml colorimetric tube, add water to 50 ml, shake, standing, and the supernatant tested.
Table 1 microwave digestion instrument reference temperature program
Heating step heating time (min) digestion temperature (℃) retention time (min)
The first step 5.00 1202
Step 4.00 1605
The third step 4.00 19025
Note 1. The rush acid sample digestion was complete, after digestion solution was allowed to stand colorless, clear shape. If reddish-brown nitrogen oxides do not catch, can continue to catch the acid straight
To reddish brown disappear.
38 analysis steps
8.1 Calibration curve
Pipette 0.00,2.00,4.00,6.00,8.00,10.00,12.00,14.00 ml phosphorus standard solution (5.10) to 50.0
ml colorimetric tube, add water to 25 ml mark. Subsequently, 2 drops of indicator (5.11), with a sulfuric acid solution (5.3) or carbonate
Sodium solution (5.4) solution was adjusted to pale yellow, then add 10 ml ammonium molybdate - ammonium metavanadate mixed solution (5.8), water volume
To 50.0 ml, allowed to stand at room temperature for 30 min. Phosphorus concentrations were 0.00 standard series, 0.80,1.60,2.40,3.20,4.00,
4.80,5.60 mg/L, with water as a reference, at a wavelength of 420 nm at 30 mm with colorimetric cuvette. Deductions from zero concentration
Corrected absorbance value of the vertical axis, the phosphorus concentration (mg/L) as the abscissa, construct a calibration curve.
8.2 Determination
Pipette 10.00 ml sample (7.2) to 50.0 ml colorimetric tubes, diluted to 25 ml mark, add 2 drops of indicator
(5.11), with a sulfuric acid solution (5.3) or sodium carbonate solution (5.4) solution was adjusted to pale yellow, and then follow the calibration (8.1) operation
Procedures to measure absorbance.
Note 2. If the total phosphorus concentration in the sample is too high, may be appropriate to reduce the volume of the sample measured.
Note 3. When a sample has a certain turbidity - when color measurement results of the sample may have an impact. You can plug colorimetric tube, dispensing with the sample in a 50 ml
Product measurement sample of the same volume, according to (8.1) step, without molybdate - ammonium metavanadate mixed solution, corrected absorbance was measured. The absorbance of the sample
Minus the corrected absorbance and calculation.
8.3 Blank test laboratory
Not reinforced waste samples prepared (7.2) and measured (8.2) the same step, color development and measurement of the sample in accordance with.
9 Results Calculation and representation
9.1 Calculation Results
Solid waste samples total phosphorus content (mg/kg), according to the equation (1) is calculated.
Vm
(1)
Where. -- solid waste waste samples total phosphorus content, mg/kg;
ρ-- calculate the sample concentration of total phosphorus, mg/L from the calibration curve;
ρ0-- blank sample calculation of the concentration of total phosphorus, mg/L from the calibration curve;
m-- amount of sample (sample fresh weight), g;
1V - constant volume digestion solution volume, ml;
2V - the determination of the amount of sample volume taken, ml;
50- volume test solution volume, ml.
9.2 The results are shown
The measurement results than or equal to 100 mg/kg, the three significant figures.
410 precision and accuracy
10.1 Precision
6 laboratories at a concentration of 560 mg/kg, 693 mg/kg, 1.03 × 104mg/kg of solid waste unified sample (actual
Sample) were measured in the laboratory relative standard deviation of 1.0% to 1.6%, 1.3% to 2.8%, 3.6% and 6.4% real
Inter laboratory relative standard deviation were 0.7%, 2.8%, 4.6%, repeatability limits of 21 mg/kg, 45 mg/kg, 1.60 × 103
mg/kg, reproducibility limit was 23 mg/kg, 67 mg/kg, 1.96 × 103 mg/kg.
10.2 Accuracy
6 laboratories concentration (560 ± 18) mg/kg of certified standard soil samples were determined relative error in the laboratory
Difference of -0.6% to 1.4% and the relative error of the final value (0.4 ± 1.4)%. 6 laboratories at a concentration of 693 mg/kg, 1.03 × 104
mg/kg of solid waste unified sample was measured recoveries of spiked amount were 50 μg, recoveries were. 97.9%,
96.0%, and the recovery value of the final 97.9% ± 9.4%, 96.0% ± 8.6%.
11 Quality Assurance and Quality Control
11.1 The correlation coefficient of the calibration curve should be greater than or equal 0.999.
11.2 each batch of samples should be done two blank test, the test results should be below the detection limit.
11.3 parallel each batch of samples to be measured at least 10% of the two-sample, the sample is less than 10 should be measured at least a parallel twin-like.
Take the arithmetic mean of the parallel determination results of the measurement results. Two measurements of relative deviation should not exceed 15%.
11.4 10% of each batch of samples spiked sample recovery should be measured at least. Spiked concentration of 0.5 to 2.5 times the original sample concentration, plus
The recovery should be between 80% to 120%.
12 Notes
12.1 All glassware and digestion vessels have been applied, dilute hydrochloric acid or dilute nitric acid immersion.
12.2 Microwave Digestion should be in strict accordance with the instructions to use the instrument to prevent accidents.
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