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HJ 489-2009Water quality. Determination of silver. Spectrophotometric method with 3, 5-Br2-PADAP (English PDF)

水质银的测定 3,5-Br2-PADAP分光光度法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

September 27, 2009

Implementation date

November 1, 2009

Scope

HJ 489-2009 is the English-translated version of 水质银的测定 3,5-Br2-PADAP分光光度法.

HJ 489-2009 — 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.

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Document preview — HJ 489-2009

National Standard of the People's Republic of China

ICS: 13.060
Classification: Z 16
Replacing: GB 11909-1989

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Principle of the method
3 Reagents and materials
3.10 EDTA-2Na solution, rho (EDTA-2Na)=0.1 mol/L. dissolve 37.24 g EDTA-2Na (C10H14N2O3Na2·2H2O)
4 Instruments and equipment
5 Interference and elimination
6 Samples
6.1 Acquisition and preservation
6.2 Preparation of samples
7 Analysis steps
7.1 Calibration curve
7.2 Sample determination
9 Precision and accuracy
9.1 Repeatability
9.2 Reproducibility

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.

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). rho = 1.40 g/ml.

3.2 Sulfuric acid (H2SO4). rho = 1.84 g/ml.

3.3 Perchloric acid (HClO4). rho = 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, rho (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, rho (NaOH) = 1 mol/L. Weigh 40 g of sodium hydroxide dissolved in water and dilute to 1 L.

3.9 Hydrogen peroxide solution (H2O2), rho (H2O2) = 3% (volume fraction). Take 10 ml of hydrogen peroxide (3.4) and dilute to 100 ml with water.

3.10 EDTA-2Na solution, rho (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, rho = 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, rho = 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, rho (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, rho (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, rho (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, rho (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 8 results the silver content in the water sample is calculated as follows.

rho = m

Where. rho - 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%.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

Referenced standards

Cited by

GB 18598-2019Standard for pollution control on the hazardous waste landfill

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