HJ 595-2010_English: PDF (HJ595-2010)
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Water quality. Determination of the total amount of the color developing agent. 169 coupler spectrophotometry
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HJ 595-2010
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Standards related to: HJ 595-2010
| Standard ID | HJ 595-2010 (HJ595-2010) | | Description (Translated English) | Water quality. Determination of the total amount of the color developing agent. 169 coupler spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060.01 | | Word Count Estimation | 10,130 | | Date of Issue | 2010-10-21 | | Date of Implementation | 2011-01-01 | | Quoted Standard | GB/T 6682 | | Drafting Organization | Beijing Municipal Environmental Monitoring Center | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 77 of 2010 | | Summary | This standard specifies the determination of the total amount of 169 color developer coupler spectrophotometry. This standard applies to photofinishing wastewater Determination of total color developer. | HJ 595-2010
Water quality.Determination of the total amount of the color developing agent.169 coupler spectrophotometry
National Environmental Protection Standard of the People's Republic
Determination of the total amount of water color developing agent
169 coupler spectrophotometry
(temporary)
Water quality-Determination of the total amount of the color developing
Agent-169 Coupler spectrophotometry
Released on.2010-10-21
2011-01-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 77 of.2010
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 ambient air ozone.
Six standards, such as the fixed ultraviolet photometry, are national environmental protection standards and are released.
The standard name and number are as follows.
1. Determination of ambient air ozone by ultraviolet photometry (HJ 590-2010);
2. Determination of water quality pentachlorophenols by gas chromatography (HJ 591-2010);
3. Determination of water quality nitrobenzene compounds by gas chromatography (HJ 592-2010);
4. Determination of water quality, elemental phosphorus, phosphorus molybdenum blue spectrophotometry (provisional) (HJ 593-2010);
5. Determination of the total amount of water-based developer and its oxides - Iodine-starch spectrophotometry (interim) (HJ 594-2010);
The above standards have been implemented since January 1,.2011 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 three national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The name and number are as follows.
1. Determination of ambient air ozone by ultraviolet spectrophotometry (GB/T 15438-1995);
2. Determination of water quality pentachlorophenols by gas chromatography (GB 8972-88);
3. Determination of Total Nitro Compounds in Industrial Wastewater Gas Chromatography (GB 4919-85).
Special announcement.
October 21,.2010
Content
Foreword..iv
1 Scope..1
2 Normative references..1
3 Terms and Definitions.1
4 method principle..1
5 reagents and materials. 2
6 instruments and equipment.2
7 samples.3
8 Analysis steps..3
9 result calculation..3
10 Notes 4
Appendix A (informative) The type and chemical structure of commonly used color developing agents..5
Iv
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-(β-methanesulfonamideethyl) m-toluidine sulfate (CD-3), 4-amino-N-ethyl-N (β- 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
NC
H2C C
C17H35
SO3H
NC
CC
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. ρ = 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
7.1 Sample collection
Color developers are unstable and are easily oxidized to terpenoids. The sample is filled with brown glass bottles and the sample should be protected from light, heat and vibration.
move.
7.2 Preservation of samples
Samples should be analyzed as soon as possible after collection. If not measured on the same day, add 0.1 g of sodium sulfite to the sample of 1 000 ml.
Sodium sulfate is used as a protective agent and stored at 0~4 °C for a period of not more than 48 h.
8 Analysis steps
8.1 Drawing of the calibration curve
Take 6 50 ml plug colorimetric tubes and prepare a calibration series according to Table 1.
Table 1 Color developer calibration series
Pipe number 0 1 2 3 4 5
Color Developer TSS Standard Solution/ml 0.00 1.00 2.00 3.00 4.00 5.00
Color developer TSS content/μg 0.00 100.200 300 400 500
Add 1.0 ml of 169 coupler solution (5.8) to each colorimetric tube, dilute with water to the mark, shake well, then add 1.0 ml respectively.
Mix the oxidizer solution (5.9) and shake well. In 5 min, at a wavelength of 550 nm, use a cuvette with an optical path of 10 mm.
Ratio, measure absorbance. A calibration curve was drawn on the color developer content (μg) by absorbance. Calibration curve intercept is a, slope is b, school
The quasi-equation is y=a bx.
Note. The absorbance of the resulting magenta dye is stable within 8 min, so it should be measured within 5 min after dye formation.
8.2 Sample determination
8.2.1 Sample determination
Take an appropriate amount of water (less than 20 ml) in a 50 ml colorimetric tube, add 1.0 ml of 169 coupler solution (5.8), dilute with water to the standard
Line, the following steps are the same as the calibration curve, and the absorbance A is measured with water as a reference.
8.2.2 Determination of sample blanks
Take the water sample volume as 8.2.1, place it in a 50 ml colorimetric tube, dilute directly to the mark with water, shake well, then add 1.0 ml of mixed oxygen.
The solution (5.9) was shaken. In 5 min, at a wavelength of 550 nm, use a cuvette with an optical path of 10 mm, using water as a reference.
The amount of absorbance A0.
9 Calculation of results
The total amount of color developing agent ρ in the water sample is calculated according to the formula (1).
0( )AA a
b V
ρ − −= × (1)
Where. ρ--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-(β-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 (β-hydroxyethyl)
Methyl)toluidine sulfate CD-4 C11H18N2O·H2SO4 292.35
NH
'H3N
OH
O−−O
OO
...
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