HJ 594-2010_English: PDF (HJ594-2010)
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Water quality. Determination of the total amount of the developing agent and their oxides. Iodine-starch spectrophotometry
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HJ 594-2010
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Standards related to: HJ 594-2010
| Standard ID | HJ 594-2010 (HJ594-2010) | | Description (Translated English) | Water quality. Determination of the total amount of the developing agent and their oxides. Iodine-starch spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060.01 | | Word Count Estimation | 10,120 | | 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 wastewater developer and oxides of iodine starch spectrophotometry. This standard applies to both color and black and white washing their oxides emissions from wastewater Determination of total developer. | HJ 594-2010
Water quality.Determination of the total amount of the developing agent and their oxides.Iodine-starch spectrophotometry
National Environmental Protection Standard of the People's Republic
Determination of the total amount of water-based developer and its oxides
Iodine-starch spectrophotometry
(temporary)
Water quality-Determination of the total amount of the developing agent
And their oxides-Iodine-starch 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);
6. Determination of the total amount of water color developing agent 169 Coupler spectrophotometry (provisional) (HJ 595-2010).
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 interference and elimination. 2
6 reagents and materials. 2
7 instruments and equipment.3
8 samples.3
9 Analysis steps..3
10 result calculation 4
11 Notes 4
Appendix A (informative) The types and chemical structures of commonly used black and white and color developers..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 developed for the monitoring of health and the total amount of developer and its oxides in wastewater.
This standard specifies the iodine-starch spectrophotometric method for determining the total amount of developer and its oxide 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.
Water quality - Determination of total oxidizers and their oxides - iodine-starch spectrophotometric method
1 Scope of application
This standard specifies the iodine-starch spectrophotometric method for determining the total amount of developer and its oxide in wastewater.
This standard applies to the determination of the total amount of developer and its oxides in waste water discharged from color and black-and-white sheets.
When using a 20 mm cuvette with a sample volume of 20.0 ml, the minimum detection limit is 1 × 10−6 mol/L, which is equivalent to hydroquinone.
0.11 mg/L; the lower limit of determination is 4×10−6 mol/L, which is equivalent to 0.44 mg/L of hydroquinone; the upper limit of determination is 2.50×10−5 mol/L, which is equivalent.
In the case of hydroquinone 2.75 mg/L.
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.
Developer. A drug that causes a latent image produced by exposure of a photosensitive material to appear as a visible image. Commonly used black and white developer
Phenol sulfate (Mitol), hydroquinone (hydroquinone), etc.; commonly used color developers are p-aminodiethylaniline hydrochloride (TSS), 2-ammonia
Benz-5-diethylaminotoluene hydrochloride (CD-2), 4-amino-N-ethyl-N-(β-methanesulfonamideethyl) m-toluidine sulfate (CD-3)
And 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
Most commonly used developers have the chemical structure of hydroquinone, para-aminophenol or p-phenylenediamine, which can be produced by oxidative hydrolysis.
Paired benzoquinone. Using bromine as an oxidant, the developer is oxidized to a quinone compound. In an acidic medium, hydrazine is a strong oxygen.
The agent, with the action of potassium iodide, precipitates elemental iodine. The iodine reacts with starch and turns blue. It has maximum absorption at 570 nm, and its absorbance and
The concentration of the developer substance is in accordance with Lambert-Beier's law, and the result is expressed in hydroquinone (mg/L) (other main developers may also be present)
Said).
In the case of Mitur, the chemical reaction of oxidation to hydrazine is.
NHCH3
OH
H2O Br2
CH3NH2 2H
2Br−
5 interference and elimination
Fe3 and Cu2 below 20 μg do not interfere with the method. Cr6 has a large interference with this method. When the water sample contains Cr6, it affects the measurement.
Timing, you can use NaNO2 to reduce Cr6 to Cr3, and use excess urea to remove excess NaNO2 to interfere with this experiment.
In addition to the purpose of chromium ion interference.
6 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.
6.1 Phosphoric acid solution. 1 1.
6.2 Hydrochloric acid (HCl). ρ = 1.19 g/ml, excellent grade pure.
6.3 Hydrochloric acid solution. c (HCl) = 6 mol/L.
6.4 Potassium bromate-potassium bromide solution. c (1/6KBrO3-KBr) = 0.1 mol/L.
Weigh 2.8 g potassium bromate and 4.0 g potassium bromide dissolved in water, dissolve and transfer to a 1 000 ml volumetric flask, dilute with water to the mark, store
In a brown reagent bottle.
6.5 Saturated sodium chloride solution. w (NaCl) = 40%.
Weigh 40 g of sodium chloride and dissolve in 100 ml of distilled water.
6.6 Potassium bromide solution. w (KBr) = 20%.
Weigh 20 g of potassium bromide, dissolve in water, and dilute to 100 ml.
6.7 Phenol solution. w (C6H6O) = 5%.
Weigh 5 g of colorless phenol, dissolve in water, dilute to 100 ml, and store in the refrigerator.
6.8 Potassium iodide solution. w(KI) = 5%.
Weigh 5 g of potassium iodide, dissolve in water, dilute to 100 ml, store in a brown reagent bottle, use it immediately, and store in a dark place.
6.9 Starch solution. w[(C6H10O5)n] = 0.2%.
Weigh 1 g of soluble starch, add a small amount of water and mix well, inject into boiling 500 ml of water, continue to boil for 5 min, cool, and then set the refrigerator
Save inside. Salicylic acid 0.2 g can be added in summer.
6.10 Sodium nitrite solution. w (NaNO2) = 10%.
Weigh 10 g of sodium nitrite, dissolve in water, and dilute to 100 ml.
6.11 Urea solution. w[(NH2)2CO]=20%.
Weigh 20 g of urea, dissolve in water, and dilute to 100 ml.
6.12 Standard stock solution. c = 0.010 0 mol/L.
Accurately weigh hydroquinone (molecular weight 110.11) 0.276 0 g, if it is photographic grade Mitol (molecular weight 344.40) can be weighed
0.861 0 g, photographic grade TSS (molecular weight 262.33) can be weighed 0.656 0 g (or calculated according to the molecular weight and purity of the drug used)
Dissolve in 25 ml of 6 mol/L hydrochloric acid solution (6.3), transfer to a 250 ml volumetric flask, dilute with water to the mark, and store in brown reagent bottle.
The concentration of the hydroquinone solution was 0.010 0 mol/L.
6.13 Standard intermediate. c = 0.25 mmol/L.
Take standard stock solution (6.12) 25.00 ml in a 1 000 ml volumetric flask, dilute with water to the mark, and store in a brown reagent bottle.
The concentration of hydroquinone solution was 0.25 mmol/L.
6.14 Standard use solution. c=0.025 mmol/L.
Take 25.00 ml of standard intermediate solution (6.13) in a 250 ml volumetric flask, dilute to the mark with water, and store in a brown reagent bottle.
The concentration of the diphenol solution was 0.025 mmol/L.
7 Instruments and equipment
7.1 Visible spectrophotometer. equipped with a cuvette with an optical path of 20 mm.
7.2 Constant temperature water bath.
7.3 with colorimetric tube. 50 ml.
8 samples
8.1 Sample collection
The developer is unstable and is easily oxidized to a terpenoid. Sampling filled with brown ground glass or polyethylene plastic bottles and avoiding light,
Heat and violent vibration.
8.2 Preservation of samples
It should be analyzed immediately after sampling, otherwise the sodium thiosulfate protective agent should be added in a ratio of 0.1 g of sodium thiosulfate to the sample of 1 000 ml.
Block the automatic oxidation of the developer and delay the oxidation of air. Store at 0~4 °C, no more than 48 h.
9 Analysis steps
9.1 Drawing of the calibration curve
9.1.1 Take 6 50 ml plug colorimetric tubes and prepare a calibration series according to Table 1.
Table 1 Developer Calibration Series
Pipe number 0 1 2 3 4 5
Developer Hydroquinone Standard Use Solution /ml 0.00 4.00 8.00 12.0 16.00 20.00
Color developer hydroquinone/μmol 0.00 0.10 0.20 0.30 0.40 0.50
Add an appropriate amount of water to make approximately 20 ml of solution in each colorimetric tube.
9.1.2 Add 2.0 ml of phosphoric acid solution (6.1) to each tube, and 5.0 ml of saturated sodium chloride solution (6.5).
9.1.3 Add 2.0 mg of potassium bromate-potassium bromide solution (6.4) to the fume hood. Do not stick to the pipe wall as much as possible. Rinse with a very small amount of water.
Tube wall, cover, and shake. The solution should be light yellow. Place in a constant temperature water bath at 35 ° C ± 1 ° C for 15 min.
9.1.4 Add 2.0 ml of potassium bromide solution (6.6) to each tube, add it to the colorimetric tube around the tube wall, cover it, shake it and place it at (35±1) °C.
5 to 10 minutes in the water bath.
9.1.5 Quickly add 1.0 ml of phenol solution (6.7) and shake immediately to remove the color of bromine. Allow to cool in tap water for 3 min.
Note. If added slowly, it will easily produce a white precipitate, which cannot be compared.
9.1.6 Add 2.0 ml of freshly prepared potassium iodide solution (6.8) to each tube, rinse the wall and place it in the dark cabinet for 5 min.
9.1.7 Pipette 10.0 ml of starch solution (6.9), add it to the colorimetric tube, dilute to the mark with water, cover it and shake it, then put it in the dark cabinet for 20 min.
Note. The bath temperature and reaction time per step should be accurately controlled.
9.1.8 Place the chromonic test solution in a 20 mm cuvette at a wavelength of 570 nm and use water as a reference to measure the absorbance to absorb light.
A calibration curve was prepared for the hydroquinone content (μmol).
9.2 Sample determination
9.2.1 Determination of no Cr6 water sample
9.2.1.1 Sample determination
Take an appropriate amount of water (less than 20.0 ml) into a 50 ml colorimetric tube, add water to 20.0 ml, and add phosphoric acid solution to the tube (6.1)
2.0 ml, saturated sodium chloride solution (6.5) 5.0 ml, the following steps are taken to draw the calibration curve, and the absorbance of the sample is measured, and the blank is subtracted.
After the absorbance of the test (9.2.1.2), the micromolar amount of the total amount of the developer and its oxide contained in the 50 ml colorimetric tube was found on the calibration curve.
9.2.1.2 Blank test
Add 20.0 ml of water to a 50 ml colorimetric tube instead of the water sample and measure according to the same procedure as in 9.2.1.1.
9.2.2 Determination of water samples containing chromium ions
9.2.2.1 Sample determination
Accurately take an appropriate amount of water sample containing Cr6 (1.00 ~ 20.0 ml), put it into a 50 ml colorimetric tube, add water to 20.0 ml, add phosphorus to the tube
Acid solution (6.1) 2.0 ml, add 3 drops of sodium nitrite solution (6.10), shake well, put in a (35 ± 1) °C constant temperature water bath for 15 min,
Then add 2.0 ml of urea solution (6.11), shake well, and put in a water bath at (35 ± 1) °C for 10 min. The following operations are drawn by calibration
The line step is performed, the absorbance is measured, and after subtracting the absorbance of the blank test (9.2.2.2), the 50 ml colorimetric tube is detected on the calibration curve.
The micromoles of the total amount of the developer and its oxide.
9.2.2.2 Blank test
Add 20.0 ml of water to a 50 ml colorimetric tube instead of the water sample and measure according to the same procedure as in 9.2.2.1.
10 result calculation
The total amount of the developer and its oxide ρ (calculated as hydroquinone) in the water sample is calculated according to the formula (1).
ρ= 110m
× (1)
Where. ρ - the total amount of developer and its oxide in the sample, mg/L;
M--calculate the total amount of developer and its oxide in a 50 ml colorimetric tube according to the calibration curve, μmol;
V--sample volume, ml;
110--the molar mass of hydroquinone, g/mol.
11 Precautions
11.1 The film and the printing department process color and black and white films. The main components of the discharged wastewater are developers and their oxides, mainly Phenylene.
Phenol (hydroquinone), metol (p-aminophenol sulfate), CD-2 (2-amino-5-diethylaminotoluene hydrochloride), CD-3 [4-amino-N-
Ethyl-N-(β-methanesulfonamideethyl) m-toluidine sulfate], CD-4 [4-amino-N-ethyl-N(β-hydroxyethyl) m-toluidine sulfate],
TSS (p-aminodiethylaniline hydrochloride), etc., is an aniline and phenylenediamine derivative with moderate toxicity.
11.2 The developer-based substances measured by the iodometric method include a class of organic substances with chromophores and chromophores, including phenols, anilines and
Its oxide benzoquinones.
11.3 Due to the interference of hexavalent chromium, the sampling container and glassware should be avoided by washing with sulfuric acid-chromic acid.
11.4 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.
11.5 After adding potassium bromate-potassium bromide, rinse the volume bottle wall with distilled water. Otherwise, residual potassium bromate and potassium iodide will form iodine to make it suck.
The luminosity increases.
11.6 Since the material to be tested is unstable due to light, all operating procedures should be protected from light.
Appendix A
(informative appendix)
Common types of black and white and color developers and chemical structure
The types and chemical structural formulas of commonly used black and white and color developing agents are shown in Table A.1.
Table A.1 List of common types of black and white and color developers and chemical structure
Developer name alias molecular formula relative molecular mass chemical structure
p-Methylaminophenol Sulfate Methylol C7H11NO5S 221.23
OH
NH
H3C
OH
NH
H3C
S OH
HO
Hydroquinone hydroquinone C6H6O2 110.11 OH
OH
p-Aminodiethylaniline hydrochloride TSS C10H16N2·HCl 262.33 H2N N
Cl H
2-amino-5-diethylaminotoluene
Hydrochloride CD-2 C11H18N2·HCl 214.74 N
NH2
HCl
4-amino-N-ethyl-N-(β-methane
Amidoethyl)m-toluidine sulfate
CD-3
2(C12H21N3O2S)·
3(H2SO4)·2(H2O)
873.01
NH2
OHS OH
HO
NH2
S OH
HO
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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