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HJ 490-2009: Water quality. Determination of silver. Spectrophotometry with cation 2B
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Water quality. Determination of silver. Spectrophotometry with cation 2B
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HJ 490-2009
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Basic data | Standard ID | HJ 490-2009 (HJ490-2009) | | Description (Translated English) | Water quality. Determination of silver. Spectrophotometry with cation 2B | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 9,954 | | Date of Issue | 2009-09-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | GB/T 11908-1989 | | Regulation (derived from) | Department of Environmental Protection Notice No. 47 of 2009 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard provides water and wastewater 2B silver cadmium reagent spectrophotometric method. 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. Sample volume is 25ml, using the optical path is 10mm cuvette, the method detection limit of 0. 01mg/L, detection limit of 0. 04mg/L, measured a maximum of 0. 8mg/L. | HJ 490-2009: Water quality. Determination of silver. Spectrophotometry with cation 2B---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Water quality.Determination of silver.Spectrophotometry with cation 2B
HJ
National Environmental Protection Standard of the People's Republic
Replace GB 11908-89
Determination of water quality silver
Cadmium reagent 2B spectrophotometry
Water quality-Determination of silver
-Spectrophotometry with cation 2B
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);
XII. Determination of Silver in Water Quality 3,5-Br2-PADAP Spectrophotometry (HJ 489-2009);
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 representation of the result. 3
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 "Measurement of mercury in water, cadmium reagent 2B spectrophotometry" (GB 11908-89), drafted the original standard
The unit is China Environmental Monitoring Station, first published in 1989, 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
Determination of steric silver cadmium reagent 2B spectrophotometry (GB 11908-89) 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 mercury in water quality - Cadmium reagent 2B spectrophotometric method
1 Scope of application
This standard specifies the gamma reagent 2B spectrophotometric method for the determination of silver in water and wastewater.
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 0.01 mg/L, and the lower limit of determination is 0.04 mg/L.
The upper limit of determination is 0.8 mg/L.
2 Principle of the method
In the sodium tetraborate buffer medium in the presence of Triton X-100, the complex ratio of cadmium reagent 2B to silver ions is
a 4.1 stable magenta complex that is stable for at least 24 h and the color intensity is proportional to the concentration of silver, the complex
The maximum absorption wavelength is 554 nm; cadmium reagent 2B is a brown solid powder, which exists in molecular form in a weak acid or alkaline medium.
The agent is yellow with a maximum absorption wavelength of 445 nm.
3 reagents and materials
The reagents used in this standard are analyzed using analytical analytical reagents in accordance with national standards, unless otherwise stated.
Deionized 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 Ethanol (C2H5OH). 95%.
3.6 Nitric acid (HNO3) 1 1 Solution. Add 50 ml of nitric acid (3.1) to 50 ml of water and mix.
3.7 Sodium hydroxide (NaOH) solution, ρ (NaOH) = 1 mol/L. Weigh 40 g of sodium hydroxide dissolved in water and dilute to 1 L.
3.8 EDTA-2Na solution, ρ (EDTA-2Na)=0.05 mol/L. dissolve 1.86 g EDTA-2Na (C10H14N2O3Na2·2H2O)
In water, and dilute to 100 ml.
3.9 Sodium tetraborate solution, ρ (Na2B4O7)=50 g/L. Dissolve 10 g of sodium tetraborate (Na2B4O7·10H2O) in water and dilute to
200 ml.
3.10 Qu Li Tong X-100 solution, ρ (Qu Li Tong X-100) = 5% (volume fraction). 5 ml Qu Li Tong X-100 [Triton X-100,
(CH3)3CCH2C(CH3)2-C6H4(OCH2CH2)nOHn~10] is dissolved in 95 ml of water and allowed to dissolve by heating.
3.11 Cadmium reagent 2B Ethanol solution, ρ (cadmium reagent 2B) = 0.4 g/L. dissolve 0.080 g cadmium reagent 2B (4-nitronaphthyldiazoaminoazo)
Benzene, O2NC10H6N. NNHC6H4N. NC6H5) In.200 ml of ethanol (3.5), add 2 drops of sodium hydroxide solution (3.7), use 4
The sand core funnel was filtered to remove insolubles.
3.12 Silver standard stock solution, ρ (Ag)=1.00 mg/ml. accurately weigh 0.157 5 g silver nitrate (AgNO3), dissolve in appropriate amount of water, add
2 ml nitric acid solution (3.6). After dissolving, transfer to a 100 ml volumetric flask and dilute to the mark with water. Store in a brown glass bottle, protected from light,
At least one month stable.
3.13 Silver standard solution, ρ (Ag)=0.100 mg/ml. Transfer 10.00 ml of silver standard stock solution (3.12) to a 100 ml volumetric flask.
Add 2 ml of nitric acid solution (3.6) and dilute to the mark with water. Store in a brown glass bottle protected from light.
3.14 Silver standard solution, ρ (Ag)=4.0 μg/ml. Transfer 20.00 ml silver standard solution (3.13) to a 500 ml volumetric flask for use
Dilute the water to the mark and prepare it before use.
3.15 methyl orange solution, w (methyl orange) = 10%. Dissolve 0.010 g of methyl orange in water and dilute to 100 ml.
4 Instruments and equipment
4.1 Spectrophotometer and 10 mm quartz cuvette.
4.2 pH meter.
4.3 Volumetric flasks. 50, 100, 500, 1 000 ml.
5 interference and elimination
Without the masking agent EDTA, under these conditions, Na, B4O72−, PO3− each 100 mg, K, Ca2, Mg2, NH4, NO3−,
SO42−, PO43−, citrate 10 mg each, As3, WO42−, MoO42−, ClO4−, BrO3−, IO3−, S2O82− each 1.0 mg and
0.1 mg of Be2, Cr6, SeO32−, TeO32−, VO3− does not interfere with the determination of 10 μg Ag, a small amount of Cd2, Hg2, Zn2, Ni2,
There is positive interference in Cu2, etc., but adding 0.5 ml of 0.05 mol/L EDTA-2Na solution can at least mask Cd2, Cu2, Ni2, Zn2, Pb2,
1.0 mg of Mn2, Fe3, Fe2, and La3, and 100 μg of each of Co2, Hg2, Al3, Cr3, Pd2, and Y3. 10 μg Ag
Impact.
6 samples
6.1 Acquisition and preservation
The water sample of silver was measured, collected and stored in a polyethylene bottle, and the water sample was acidified to pH 1-2 with concentrated nitric acid and analyzed as soon as possible.
Wastewater from the production of photosensitive materials, film processing, silver plating, etc., no acid is added after sample collection, and analysis is performed immediately.
Water samples collected should be protected 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 the homogeneous sample in a 100 ml beaker. If the concentration of silver exceeds 0.8 mg/L, the sample may be appropriately reduced and diluted with water until
25 ml. In the sample, 4 ml of nitric acid (3.1), 1 ml of sulfuric acid (3.2) and 0.5 ml of hydrogen peroxide (3.4) were added in sequence. On the hot plate
Heat slowly to white smoke. After removing the cooling, add 1 ml of perchloric acid, cover the watch glass, and continue to heat until near dry. After cooling, add 0.5 ml
Nitric acid (3.6), rinse the cup wall with a little water and dissolve the residue slightly. Then, carefully wash into a 25 ml volumetric flask, the volume of the solution should not exceed
Over 15 ml.
Samples with precipitates or suspended solids, such as photosensitive materials, printing waste water, etc., should be sampled as evenly as possible.
The sample is complex, contains more organic matter, or precipitates, and can be repeatedly digested with nitric acid. Compared with clean samples, nitric acid and perchloric acid are eliminated.
Just solve it. In the digestion process, it is not suitable to evaporate. Otherwise, silver has a loss.
That is, the water sample is acidified to pH 1-2 using concentrated nitric acid, which is not suitable for storage, and should be analyzed as soon as possible. Especially for printing wastewater, after sample collection,
Samples should be prepared for analysis without acid.
7 Analysis steps
7.1 Calibration curve
7.1.1 Add 0.00, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml silver standard solution (3.14) to each of the 7 25 ml volumetric flasks.
7.1.2 Add 0.5 ml of EDTA-2Na solution (3.8) to the above volumetric flask, add 1 drop of methyl orange indicator (3.15), and use hydrogen and oxygen.
The sodium solution (3.7) was adjusted until the indicator just turned yellow. Add 2 ml of sodium tetraborate solution (3.9), 1.0 ml of Triton X-100 solution
(3.10) and 1.5 ml cadmium reagent 2B ethanol solution (3.11). Dilute to the mark with water and shake well. After 10 min, use 10 mm colorimetric
The dish was measured at 554 nm and the absorbance was measured. The absorbance of the reagent blank (zero concentration) was measured with water as a reference. To subtract the reagent empty
The absorbance after white (zero concentration) is plotted against the silver content (μg).
7.2 Sample determination
Accurately pipette 1 to 15 ml of the test sample (depending on the silver content in the water) in a 25 ml volumetric flask, as described below in 7.1.2. From the calibration curve
The amount of silver in the sample is determined online or calculated using a regression equation.
8 representation of the result
The silver mass concentration is calculated as follows.
ρ = m
Where. ρ - the mass concentration of silver in the sample, mg/L;
m -- the silver content of the sample obtained by the calibration curve or calculated by the regression equation, μg;
V--sample volume taken, ml.
9 Precision and accuracy
Four 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 2.2%.
9.2 Reproducibility
The relative standard deviation of reproducibility was 4.0%.
9.3 Accuracy
The relative error is −0.2%.
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