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HJ 489-2009: Water quality. Determination of silver. Spectrophotometric method with 3, 5-Br2-PADAP
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Water quality. Determination of silver. Spectrophotometric method with 3, 5-Br2-PADAP
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HJ 489-2009
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Basic data | Standard ID | HJ 489-2009 (HJ489-2009) | | Description (Translated English) | Water quality. Determination of silver. Spectrophotometric method with 3, 5-Br2-PADAP | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 9,967 | | Date of Issue | 2009-09-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | GB 11909-1989 | | Regulation (derived from) | Department of Environmental Protection Notice No. 47 of 2009 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of silver in water and wastewater 3, 5-Br (2)-PADAP ([2 (3, 5) dibromo-2 pyridyl azo ] -5 diethylaminophenol) spectrophotometry. This standard applies to surface water contamination by silver and photographic materials production, film processing, silver, smelting and other industries determination of silver in industrial wastewater. | HJ 489-2009: Water quality. Determination of silver. Spectrophotometric method with 3, 5-Br2-PADAP
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Water quality.Determination of silver.Spectrophotometric method with 3, 5-Br2-PADAP
HJ
National Environmental Protection Standard of the People's Republic
Replace GB 11909-89
Determination of water quality silver
3,5-Br2-PADAP spectrophotometry
Water quality-Determination of silver
-Spectrophotometric method with 3,5-Br2-PADAP
Published on.2009-09-27
2009-11-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 47 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 measurement of water quality polycyclic aromatic hydrocarbons.
Eighteen standards, such as fixed liquid extraction and solid phase extraction high performance liquid chromatography, are national environmental protection standards and are released.
The standard name and number are as follows.
I. Determination of Polycyclic Aromatic Hydrocarbons by Liquid-Liquid Extraction and Solid Phase Extraction High Performance Liquid Chromatography (HJ 478-2009);
2. Determination of nitrous oxides (nitrogen oxides and nitrogen dioxide) - Determination of naphthalene diamine hydrochloride spectrophotometric method (HJ 479-
2009);
III. Determination of Fluoride in Ambient Air Filtration of Fluoride Ion Selective Electrode Method (HJ 480-2009);
IV. Determination of fluoride in ambient air Determination of fluoride ion-selective electrode method for lime filter paper (HJ 481-2009);
V. Determination of Sulfur Dioxide in Ambient Air - Formaldehyde Absorption - Pararosaniline Spectrophotometry (HJ 482-2009);
6. Determination of Sulfur Dioxide in Ambient Air - Tetrachloromercury Salt Absorption - Pararosaniline Spectrophotometry (HJ 483-2009);
VII. Determination of water content cyanide volumetric method and spectrophotometry (HJ 484-2009);
VIII. Determination of copper in water quality by diethyldithiocarbamate spectrophotometry (HJ 485-2009);
IX. Determination of copper in water quality 2,9-Dimethyl-1,10 phenanthroline spectrophotometry (HJ 486-2009);
X. Determination of Fluoride in Water Quality by Spectrophotometric Method of Zirconium Sulfate Sulfate (HJ 487-2009);
XI. Determination of Fluoride in Water Quality Fluorescence Spectrophotometry (HJ 488-2009);
XIII. Determination of Silver in Water Quality by Cadmium Reagent 2B Spectrophotometry (HJ 490-2009);
XIV. Determination of Total Chromium in Soils by Flame Atomic Absorption Spectrophotometry (HJ 491-2009);
15. Air Quality Vocabulary (HJ 492-2009);
XVI. Technical Regulations for the Preservation and Management of Water Quality Samples (HJ 493-2009);
17. Water Quality Sampling Technical Guidance (HJ 494-2009);
18. “Technical Guidance for the Design of Water Quality Sampling Plans” (HJ 495-2009).
The above standards have been implemented since November 1,.2009 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
From the date of implementation of the above standards, the following 20 national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The exact name and number are as follows.
1. "Determination of six specific polycyclic aromatic hydrocarbons in water quality by high performance liquid chromatography" (GB 13198-91);
2. Determination of nitrogen oxides in air quality - Determination of naphthylethylenediamine hydrochloride (GB 8969-88);
3. "Saltzman method for determination of nitrogen oxides in ambient air" (GB/T 15436-1995);
4. Determination of the concentration of fluoride in ambient air, filter membrane and fluoride ion selective electrode method (GB/T 15434-1995);
V. Determination of Fluoride in Ambient Air Lime Filter Paper · Fluoride Ion Selective Electrode Method (GB/T 15433-1995);
6. Determination of Sulphur Dioxide in Ambient Air - Formaldehyde Absorption - Pararosaniline Spectrophotometry (GB/T 15262-94);
VII. Determination of Air Quality, Sulfur Dioxide, Tetrachloromercury Salt - Pararosaniline Hydrochloride Colorimetric Method (GB 8970-88);
VIII. Determination of Cyanide in Water Quality Part I Determination of Total Cyanide (GB 7486-87);
IX. Determination of Cyanide in Water Quality Part 2 Determination of Cyanide (GB 7487-87);
X. Determination of copper in water quality by diethyldithiocarbamate spectrophotometry (GB 7474-87);
XI. Determination of Copper in Water Quality 2,9-Dimethyl-1,10-phenanthroline Spectrophotometric Method (GB 7473-87);
Twelve, "Determination of Fluoride in Water Quality, Zirconium Sulfonic Acid Visual Colorimetric Method" (GB 7482-87);
XIII. Determination of Fluoride in Water Quality Fluorescence Spectrophotometry (GB 7483-87);
XIV. Determination of Silver in Water Quality, 3,5-Br2-PADAP Spectrophotometry (GB 11909-89);
Fifteen, "Measurement of mercury in water, cadmium reagent 2B spectrophotometry" (GB 11908-89);
XVI. Determination of Total Chromium in Soil Quality by Flame Atomic Absorption Spectrophotometry (GB/T 17137-1997);
17. Air Quality Vocabulary (GB 6919-86);
18. Technical Regulations for the Preservation and Management of Water Samples (GB 12999-91);
Nineteen, "Water Quality Sampling Technical Guidance" (GB 12998-91);
20. Technical Regulations for the Design of Water Quality Sampling Plans (GB 12997-91).
Special announcement.
September 27,.2009
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 reagents and materials.1
4 instruments and equipment. 2
5 interference and elimination. 2
6 samples. 2
7 Analysis steps..2
8 results. 2
9 precision and accuracy..3
Foreword
To protect the environment and protect the human body 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 Water Pollution Prevention and Control
This standard is developed for the monitoring of health and the regulation of silver in water and wastewater.
This standard specifies the method for determining silver in water and wastewater.
This standard amends the determination of mercury in water, 3,5-Br2-PADAP spectrophotometry (GB 11909-89), the original standard
The drafting unit is the China National Environmental Monitoring Center. This is the first revision.
The main revisions are as follows.
-- Increase coexisting ion interference and elimination and adjust and revise the standard text.
From the date of implementation of this standard, the national environmental protection standard “Water” approved and issued by the former National Environmental Protection Agency on December 25, 1989
The determination of silver, 3,5-Br2-PADAP spectrophotometry (GB 11909-89) was abolished.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. China Environmental Monitoring Center.
This standard was approved by the Ministry of Environmental Protection on September 27,.2009.
This standard has been implemented since November 1,.2009.
This standard is explained by the Ministry of Environmental Protection.
Iv
Determination of silver in water quality 3,5-Br2-PADAP spectrophotometry
1 Scope of application
This standard specifies 3,5-Br2-PADAP([2-(3,5)-dibromo-2-pyridylazo]-5-diethylaminophenol) for the determination of silver in water and wastewater.
Photometric method.
This standard is applicable to silver in industrial wastewater from the production of surface water and photosensitive materials contaminated by silver, film printing, silver plating, smelting and other industries.
Determination.
When the test volume is 25 ml and the optical path is 10 mm cuvette, the detection limit of this method is 0.02 mg/L, and the lower limit of determination is 0.08 mg/L.
The upper limit of determination is 1.0 mg/L.
2 Principle of the method
Silver and 3,5-Br2-PADAP are stable in the presence of 1% sodium lauryl sulfate in an acetate buffer medium at pH 4.5-8.5
The 1.2 magenta complex, whose absorbance is proportional to the concentration of silver. The maximum absorption wavelength of the complex is 570 nm; the maximum absorption of the reagent
The wavelength was 470 nm; the molar absorptivity was 7.6×104 L/(mol·cm).
3 reagents and materials
The reagents used in this standard are analytically pure reagents that meet the national standards unless otherwise stated. The experimental water is newly prepared.
Ionic water or distilled water.
3.1 Nitric acid (HNO3). ρ = 1.40 g/ml.
3.2 Sulfuric acid (H2SO4). ρ = 1.84 g/ml.
3.3 Perchloric acid (HClO4). ρ = 1.68 g/ml.
3.4 Hydrogen peroxide (H2O2). 30%.
3.5 Nitric acid (HNO3) 1 1 solution. Add appropriate amount of nitric acid (3.1) to an equal volume of water and mix.
3.6 Nitric acid (HNO3) solution, ρ (HNO3) = 1 mol/L. Prepared with nitric acid (3.1).
3.7 Sulfuric acid (H2SO4) 1 1 solution. Add appropriate amount of sulfuric acid (3.2) to an equal volume of water and mix.
3.8 Sodium hydroxide (NaOH) solution, ρ (NaOH) = 1 mol/L. Weigh 40 g of sodium hydroxide dissolved in water and dilute to 1 L.
3.9 Hydrogen peroxide solution (H2O2), ρ (H2O2) = 3% (volume fraction). Take 10 ml of hydrogen peroxide (3.4) and dilute to 100 ml with water.
3.10 EDTA-2Na solution, ρ (EDTA-2Na)=0.1 mol/L. dissolve 37.24 g EDTA-2Na (C10H14N2O3Na2·2H2O)
In water, and diluted to 1 000 ml.
3.11 Sodium citrate solution, ρ = 50 g/L. Weigh 50 g of sodium citrate, dissolve in water, and dilute to 1 000 ml.
3.12 sodium lauryl sulfate (sls) solution, ρ = 10 g/L. Weigh 1 g of sodium lauryl sulfate in 100 ml of water.
3.13 Acetic acid-sodium acetate buffer solution, pH=5. Mix with 1 mol/L sodium acetate and 1 mol/L acetic acid solution under the pH meter
To the desired pH.
3.14 3,5-Br2-PADAP ethanol solution, ρ (3,5-Br2-PADAP)=0.3 g/L. dissolve 0.03 g 3,5-Br2-PADAP in 100 ml anhydrous
In ethanol.
3.15 Silver standard stock solution, ρ (Ag)=1.00 mg/ml. accurately weigh 0.157 5 g silver nitrate, add 10 ml nitric acid solution (3.6), dissolve
After dissolving, transfer to a 100 ml volumetric flask, dilute to the mark with water, shake well, and store in a brown bottle.
3.16 Silver standard use solution, ρ (Ag)=0.100 mg/ml. Transfer 10.00 ml of silver standard stock solution (3.15) to a 100 ml volumetric flask
Add 2 ml of nitric acid solution (3.5), dilute to the mark with water, store in a brown glass bottle and store in the dark.
3.17 Silver standard use solution, ρ (Ag)=5.0 μg/ml. Transfer 5.00 ml of silver standard solution (3.16) to a 100 ml volumetric flask.
Dilute to the mark with water and configure before use.
3.18 methyl orange indicator solution, w (methyl orange) = 10%. 0.1 g of methyl orange (methy orange) was dissolved in water and diluted to 100 ml.
4 Instruments and equipment
4.1 Spectrophotometer and 10 mm quartz cuvette.
4.2 pH meter.
4.3 100 ml, 1 000 ml volumetric flask.
5 interference and elimination
Add 2 ml of masking agent 0.1 mol/L EDTA-2Na solution to mask 50 μg of Co2 and Bi3, 100 μg of each of Cr3, Ba2 and Sr2.
200 μg of Cd2, Cu2, Pb2, Ni2, Mn2, VO3−, Hg2, 400 μg of Fe2, 500 μg of Fe3, Al3, Mg2, K,
The effect of 1 000 μg of Na and Ca2 on the determination of 5.0 μg Ag. Cl−, Br−, I−, S2O32−, SCN− and S2− produce negative interference and are easy to use
Strong acid is decomposed and removed when digesting the water sample.
6 samples
6.1 Acquisition and preservation
Determine the water sample of silver, collect and store it in a polyethylene bottle, acidify the water sample to pH 1-2 with concentrated nitric acid, and analyze as soon as possible.
Water samples should be stored away from light.
6.2 Preparation of samples
Unless it is proved that the pretreatment of the sample is unnecessary, the sample may be directly prepared for colorimetry, otherwise the pretreatment should be carried out as follows.
Take 25.0 ml of uniform sample in a 100 ml beaker (if the concentration of silver exceeds 1.0 mg/L, it can be taken less or diluted with water)
When the concentration is taken, it is divided again). In the sample, 5 ml of nitric acid (3.5), 1 ml of sulfuric acid (3.2) and 6.5 ml of hydrogen peroxide solution (3.9) were added in sequence.
Cover the watch glass, carefully heat it to boiling on the hot plate, remove it after 5-10 minutes, add 1~2 ml perchloric acid (3.3), in the electric heating
The plate evaporates to near dryness. After cooling, add 1 ml of nitric acid solution (3.6), rinse the cup with a little water, and transfer to a hot plate to dissolve the salt warmly.
Then carefully transfer into a 25 ml volumetric flask.
7 Analysis steps
7.1 Calibration curve
7.1.1 Adding 0.00, 0.50, 1.00, 2.00, 2.50, 3.00, 4.00, 5.00 ml silver standards to 8 25 ml volumetric flasks.
Using a liquid (3.17), wash the wall with a small amount of water.
7.1.2 Add 1 ml of sodium citrate solution (3.11) to the above volumetric flask, add 1 drop of methyl orange indicator (3.18), and use sodium hydroxide.
The solution (3.8) neutralized the solution from red to yellow, and then added 2 ml of acetic acid-sodium acetate buffer solution (3.13), 2 ml of EDTA-2Na solution (3.10).
2 ml sodium lauryl sulfate solution (3.12), 2 ml 3,5-Br2-PADAP ethanol solution (3.14) (shake well after each reagent).
Dilute to the mark with water and shake well. After standing for 20 min, the absorbance was measured at a wavelength of 570 nm using a 10 mm cuvette. Taking water as
For reference, measure the absorbance of the reagent blank (zero concentration). The absorbance after subtracting the reagent blank (zero concentration), the corresponding silver content (μg)
Draw a calibration curve.
7.2 Sample determination
Take an appropriate amount of the digested water sample (containing Ag < 35 μg) in a 25 ml volumetric flask and wash the tube wall with a small amount of water, as described below in 7.1.2.
Row. The silver content in the sample is found from the calibration curve or calculated using a regression equation.
8 results
The silver content in the water sample is calculated as follows.
ρ = m
Where. ρ - the concentration of silver in the water sample, mg/L;
M--calculated by the calibration curve or calculated by the regression equation, the amount of silver contained in the sample, μg;
V--sample volume taken, ml.
9 Precision and accuracy
Five laboratories analyzed a uniform sample containing 1.00 mg/L of silver in distilled water (sample plus ammonia and cyanogen iodide).
9.1 Repeatability
The relative standard deviation of repeatability was 1.60%.
9.2 Reproducibility
The relative standard deviation of reproducibility was 1.75%.
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