HJ 595-2010Water quality. Determination of the total amount of the color developing agent. 169 coupler spectrophotometry (English PDF)

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 formulated for the health and regulation of the total amount of color developing agents in wastewater.

This standard specifies the 169 coupler spectrophotometric method for determining the total amount of color developing agent in wastewater.

Appendix A of this standard is an informative annex.

This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.

This standard was drafted. 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.

Determination of the total amount of water-based color developing agents 169 Coupler spectrophotometric method

1 Scope of application

This standard specifies the 169 coupler spectrophotometric method for determining the total amount of color developing agent in water.

This standard applies to the determination of the total amount of color developing agent in the printing wastewater.

When using a 20 mm cuvette with a sample volume of 20.0 ml, the method detection limit is 1.03 × 10-6 mol/L, which is equivalent to p-aminodiethyl Aniline hydrochloride (TSS) 0.27 mg/L; the lower limit of determination is 4.12 × 10-6 mol/L, equivalent to p-aminodiethylaniline hydrochloride (TSS) 1.08 Mg/L; the upper limit of determination is 8.55×10-5 mol/L, which is equivalent to 25.0 mg/L of p-aminodiethylaniline hydrochloride (TSS).

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard.

GB/T 6682 Analytical laboratory water specifications and test methods

3 Terms and definitions

The following terms and definitions apply to this standard.

Color developer. the latent image produced by exposure of the photosensitive material appears as a visible image, and interacts with the coupler of the emulsion layer to form an organic Dyeing agent. Commonly used color developing agents include p-aminodiethylaniline hydrochloride (TSS), 2-amino-5-diethylaminotoluene hydrochloride (CD-2), 4-amino-N-ethyl-N-(beta-methanesulfonamideethyl) m-toluidine sulfate (CD-3), 4-amino-N-ethyl-N (beta- Hydroxyethyl) M-toluidine sulfate (CD-4), etc., the structural formula is shown in Appendix A.

4 Principle of the method

The color developing agent in the printing wastewater can be oxidized by the oxidizing agent, and the oxide is immediately coupled when it encounters the water-soluble color forming agent in the alkaline solution.

Form a dye. Maximum absorption of different structures of developer (TSS, CD-2, CD-3, CD-4) and 169 coupler couples the spectral wavelengths are all at 550 nm, and the absorbance and color developer content are in accordance with Lambert-Beer law.

This method does not include a black and white developer.

Taking TSS as an example, the chemical reaction formula is as follows.

C2H5H5C2

NH2

SO3H

H2C C

C17H35

SO3H

C17H35NN

H5C2

H5C2

Cu2

(TSS) (169 coupler) (magenta dye)

5 Reagents and materials

Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. The experimental water is in accordance with GB/T 6682, Level 3.

5.1 Sodium hydroxide (NaOH). excellent grade pure.

5.2 Copper sulfate (CuSO4·5H2O). analytically pure.

5.3 anhydrous sodium carbonate (Na2CO3). analytically pure.

5.4 Sodium nitrite (NaNO2). analytically pure.

5.5 Ammonium chloride (NH4Cl). analytically pure.

5.6 sodium sulfite (Na2SO3). analytically pure.

5.7 169 coupler.

5.8 169 coupler solution. w = 0.5%.

Weigh 0.5 g of 169 coupler (5.7) into a beaker with 100 ml of distilled water, and add 1 or 2 sodium hydroxide with stirring.

(5.1), completely dissolve, shake, and transfer to a brown reagent bottle.

5.9 Mix the oxidizer solution.

0.5 g of copper sulfate (5.2), 5.0 g of anhydrous sodium carbonate (5.3), 5.0 g of sodium nitrite (5.4) and 5.0 g of ammonium chloride (5.5) Dissolve in water, dilute to 100 ml, shake well, and store in brown reagent bottle.

5.10 Color developer TSS standard solution. rho = 0.10 mg/ml.

Accurately weigh 0.100 g photographic grade color developer TSS, dissolved in a small amount of distilled water, pre-dissolved into 0.1 g Na2SO3 (5.6) as a protective agent, transfer it to a 1 000 ml volumetric flask, dilute it to the mark with water, shake it, and store in a polyethylene bottle. This standard solution contains per ml 0.10 mg color developer TSS, ready for use.

Note. TSS is recommended for the developer standard solution. TSS is the most used in production, and the relative molecular mass (262.33) is moderate and stable.

6 Instruments and equipment

6.1 Visible spectrophotometer. equipped with a cuvette with an optical path of 10 mm.

6.2 with colorimetric tube. 50 ml.

7 Samples

8 Analysis steps

9 Calculation of results

The total amount of color developing agent rho in the water sample is calculated according to the formula (1).

0( )AA a

rho - -= × (1)

Where. rho--the total amount of color developing agent in the water sample, mg/L;

A--the absorbance value of the water sample;

A0--the absorbance value of the sample blank;

V--water sample volume, ml;

A--standard curve intercept;

b--Standard curve slope.

10 Precautions

10.1 Due to the interference of hexavalent chromium, the sampling container and glassware should be avoided by washing with sulfuric acid-chromic acid.

10.2 Used cuvettes and colorimetric tubes should be washed with acid in time, otherwise the blue color is difficult to wash. Wash with a colorimetric tube (1 1) hydrochloric acid solution the polyester and cuvettes were washed with a mixture of (1 4) hydrochloric acid solution and 1/3 volume of ethanol.

Appendix A

(informative appendix) Common types of color developing agents and chemical structure the types and chemical structural formulas of commonly used color developing agents are shown in Table A.1.

Table A.1 List of commonly used color developers and chemical structure formula

Name alias molecular formula relative molecular mass chemical structure p-Aminodiethylaniline hydrochloride TSS C10H16N2·HCl 262.33 H2N N Cl H 2-amino-5-diethylamino Toluene hydrochloride CD-2 C11H18N2·HCl 214.74 N NH2 HCl 4-amino-N-ethyl-N-(beta-甲 Sulfonamide ethyl) m-toluidine sulfur Acid salt CD-3 2(C12H21N3O2S)· 3(H2SO4)·2(H2O) 873.01 NH2 OHS OH HO S OH HO NH2 S OH HO H2O H2O 4-amino-N-ethyl-N (beta-hydroxyethyl) Methyl)toluidine sulfate CD-4 C11H18N2O·H2SO4 292.35 NH 'H3N OH O--O OO