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HJ 601-2011 English PDF

HJ 601-2011_English: PDF (HJ601-2011)
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HJ 601-2011English269 Add to Cart 3 days [Need to translate] Water quality. Determination of formaldehyde. Acetylacetone spectrophotometric method Valid HJ 601-2011


BASIC DATA
Standard ID HJ 601-2011 (HJ601-2011)
Description (Translated English) Water quality. Determination of formaldehyde. Acetylacetone spectrophotometric method
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Classification of International Standard 13.060
Word Count Estimation 10,196
Date of Issue 2011-02-10
Date of Implementation 2011-06-01
Older Standard (superseded by this standard) GB/T 13197-1991
Drafting Organization China Shipbuilding Industry Corporation, 718th Research Institute
Administrative Organization Ministry of Environment Protection
Regulation (derived from) Department of Environmental Protection Notice No. 9 of 2011
Summary This standard specifies the determination of formaldehyde acetylacetone spectrophotometry. This standard applies to surface water, groundwater and industrial wastewater Determination of formaldehyde, this standard does not apply to dyeing wastewater.

Standards related to: HJ 601-2011

HJ 601-2011
Water quality.Determination of formaldehyde.Acetylacetone spectrophotometric method
National Environmental Protection Standard of the People's Republic
Replace GB 13197-91
Water quality - Determination of formaldehyde - Acetylacetone spectrophotometric method
Water quality-Determination of formaldehyde
-Acetylacetone spectrophotometric method
Published on.2011-02-10
2011-06-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 9 of.2011
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and standardize environmental monitoring, the water is now approved.
The determination of total mercury is determined by the Cold Atomic Absorption Spectrophotometry and other nine standards for national environmental protection standards.
The standard name and number are as follows.
I. Determination of total mercury in water - Cold atomic absorption spectrophotometric method (HJ 597-2011);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (HJ 598-2011);
3. Determination of water quality ladders N-chlorohexadecylpyridine-sodium sulfite spectrophotometry (HJ 599-2011);
4. Gas chromatographic method (HJ 600-2011) for the determination of water quality ladders, black ropes, and dien ladders;
6. Determination of water quality 石墨 Graphite furnace atomic absorption spectrophotometry (HJ 602-2011);
VII. Determination of water quality 火焰 Flame atomic absorption spectrophotometry (HJ 603-2011);
VIII. Determination of total hydrocarbons in ambient air - Gas chromatography (HJ 604-2011);
IX. Determination of Volatile Organic Compounds in Soils and Sediments Purge and Trap/Gas Chromatography-Mass Spectrometry (HJ 605-2011).
The above standards have been implemented since June 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 seven 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 total mercury in water quality by cold atomic absorption spectrophotometry (GB 7468-87);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (GB/T 13905-92);
3. Determination of water quality ladders by spectrophotometry (GB/T 13903-92);
4. Determination of water quality TNT, Hessian and Dien, gas chromatography (GB/T 13904-92);
V. Determination of water quality formaldehyde acetylacetone spectrophotometry (GB 13197-91);
6. Determination of water quality 原子 Atomic absorption spectrophotometry (GB/T 15506-1995);
VII. Determination of total hydrocarbons in ambient air Gas chromatography (GB/T 15263-94).
Special announcement.
February 10,.2011
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 interference and elimination.1
4 Reagents and materials.1
5 instruments and equipment.3
6 samples.3
7 Analysis steps..3
8 result calculation..4
9 precision and accuracy..4
10 Quality Assurance and Quality Control.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
To develop and standardize the monitoring methods for formaldehyde in water.
The method for determining formaldehyde in surface water, groundwater and industrial wastewater is specified in this standard.
This standard is a revision of the "Method for the determination of formaldehyde in water quality by acetylacetone spectrophotometry" (GB 13197-91).
This standard was first published in.1991, and the original standard drafting unit was the Beijing Environmental Protection Monitoring Center. This is the first revision. the Lord
The content to be revised is as follows.
- the scope of application increases groundwater;
-- Revise the color development conditions;
-- Revise the calculation formula;
-- Increase quality assurance and quality control.
The national environmental protection standard “Water quality approved and issued by the former National Environmental Protection Agency on August 31,.1991 since the implementation of this standard.
Determination of formaldehyde acetylacetone spectrophotometry (GB 13197-91) 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 Shipbuilding Industry Corporation, the 718th Research Institute.
This standard was approved by the Ministry of Environmental Protection on February 10,.2011.
This standard has been implemented since June 1,.2011.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of formaldehyde - Acetylacetone spectrophotometric method
1 Scope of application
This standard specifies the acetylacetone spectrophotometric method for the determination of formaldehyde in water.
This standard applies to the determination of formaldehyde in surface water, groundwater and industrial wastewater. This standard does not apply to printing and dyeing wastewater.
When the sample volume is 25 ml and the cuvette has an optical path length of 10 mm, the method detection limit is 0.05 mg/L, and the measurement range is 0.20 to 3.20 mg/L.
2 Principle of the method
Formaldehyde forms a yellow compound with acetylacetone in the presence of an excess of ammonium salt, which has maximum absorption at 414 nm.
The absorbance of the colored substance was basically unchanged within 3 h.
The chemical reaction formula is.
HC
H NH3 2 (CH3 C
C CH2
CH3)
CCH3 CH2
HH
CH2 C
CH3 3H2O
3 interference and elimination
The concentration of acetaldehyde in the water sample is less than 3 mg/L, and the propionaldehyde, butyraldehyde, acrolein, etc. are less than 5 mg/L, respectively, and do not interfere with the determination. Also when
Methanol was 20 mg/L, phenol was 50 mg/L, and no interference was observed when free cyanide was 1 mg/L.
4 reagents and materials
Unless otherwise stated in this standard, the reagents used should be analytically pure reagents that meet national or professional standards. The experimental water is distilled water.
Or water of the same purity.
4.1 Sulfuric acid. ρ(H2SO4) = 1.84 g/ml.
4.2 Sodium hydroxide. c (NaOH) = 1 mol/L.
Weigh 110 g of sodium hydroxide, dissolve in 100 ml of water, shake well, transfer to a polyethylene container, and place in a sealed container until the solution is clear. Measure
54 ml of the supernatant, diluted to 1 000 ml with water, and mixed.
4.3 Sulfuric acid solution. c(1/2 H2SO4) = 1 mol/L.
Measure 30 ml of sulfuric acid (4.1), slowly inject into 1000 ml of water, cool and mix.
4.4 Sulfuric acid solution. c (1/2 H2SO4) = 6 mol/L.
Measure 180 ml of sulfuric acid (4.1), slowly inject into 850 ml of water, cool and mix.
4.5 Iodine solution. c (1/2I2) ≈ 0.05 mol/L.
Weigh 6.35 g of pure iodine and 20 g of potassium iodide, first dissolve in a small amount of water, then dilute to 1 000 ml with water. Iodine solution should be stored in the stopper
The brown bottle is placed in the dark.
4.6 Acetylacetone solution.
Dissolve 50 g of ammonium acetate (CH3COONH4), 6 ml of glacial acetic acid (CH3COOH) and 0.5 ml of acetylacetone (C5H8O2)
In 100 ml of water. This solution was stored at 4 ° C for stable storage for one month.
Note. The purity of acetylacetone has an effect on the absorbance of the blank test. Acetylacetone should be colorless and transparent, and if necessary, it should be refined by distillation.
4.7 Potassium dichromate reference solution. c (1/6K2Cr2O7) = 0.050 0 mol/L.
Accurately weigh 2.451 6 g of reference potassium dichromate baked at 110-130 ° C for 2 h and cooled to room temperature. Dissolve in water and transfer to 1 000 ml.
In a volumetric flask, dilute to the mark with water and shake well.
4.8 Starch indicator. ρ = 10 g/L.
Weigh 1 g of starch, add 5 ml of water to make a paste, add the paste to 90 ml of boiling water with stirring, and boil for 1 to 2 minutes.
Cool and dilute to 100 ml. Available now.
4.9 Sodium thiosulfate standard solution. c (Na2S2O3 · 5H2O) ≈ 0.05 mol/L.
Weigh 12.5 g of sodium thiosulfate dissolved in boiled and cooled water and dilute to 1 000 ml. Add 0.4 g of sodium hydroxide and store in brown
The inside of the color bottle was placed for 2 weeks, filtered, and calibrated with a potassium dichromate reference solution (4.7) before use. The calibration method is as follows.
Add about 1 g of potassium iodide (KI) and 50 ml of water to a 250 ml iodine bottle, and add 20.00 ml of potassium dichromate reference solution (4.7).
Add 5 ml of sulfuric acid solution (4.4), mix and place in the dark for 5 min. Titrate with sodium thiosulfate solution, until titrated until the solution is light yellow
At the time, add 1 ml of starch indicator (4.8), continue titration until the blue color just fades, and record the amount (V1).
The concentration of sodium thiosulfate standard solution is calculated by formula (1).
C1 = 2 2
c V
× (1)
Where. c1--sodium thiosulfate standard solution concentration, mol/L;
C2--potassium dichromate reference solution concentration, mol/L;
V1--titration consumption volume of sodium thiosulfate solution, ml;
V2--take the potassium dichromate reference solution volume, ml.
4.10 Formaldehyde standard stock solution. (HCHO)ρ ≈1 mg/ml.
Preparation. Pipette 2.8 ml of formaldehyde reagent (formaldehyde content 36% ~ 38%), dilute with water to 1 000 ml, shake. Prepared solution
Store at 4 ° C for half a year. Pre-calibration before use.
Calibration. Pipette 20.00 ml of formaldehyde standard stock solution into 250 ml iodine flask, add 50.0 ml iodine solution (4.5), add 15 ml
Mix the sodium hydroxide solution (4.2) and let stand for 15 min. Add 20 ml of sulfuric acid solution (4.3), mix and let stand for 15 min. Thiosulfuric acid
Sodium standard solution (4.9) is titrated. When the solution is light yellow, add 1 ml of starch indicator (4.8) and continue to titrate to blue.
Faded, write down the amount (V).
At the same time, accurately remove 20.00 ml of water instead of formaldehyde standard stock solution. Carry out the blank test in the same way, and record the sodium thiosulfate standard.
Quasi-solution dosage (V0).
The mass concentration of formaldehyde standard stock solution is calculated by formula (2).
(HCHO)ρ = 0 1( ) 15.02 1 000
20.00
VV c− × × ×
(2)
Where. (HCHO)ρ-formaldehyde standard stock solution concentration, mg/ml;
V0--blank test consumption of sodium thiosulfate standard solution volume, ml;
V--calibration of formaldehyde storage liquid consumption of sodium thiosulfate standard solution volume, ml;
C1--sodium thiosulfate standard solution concentration, mol/L;
15.02--molar mass of formaldehyde (1/2HCHO), g/mol;
1 000--1 g is equal to 1 000 mg;
20.00--Move the volume of formaldehyde standard stock solution, ml.
Note 1. The starch solution should be added at the near end of the titration.
Note 2. The titration should be carried out in an iodometric flask and should be protected from sunlight. The titration should not be excessively shaken.
4.11 Formaldehyde standard use solution
The standard stock solution of formaldehyde (4.10) was diluted with water in a volumetric flask to a standard use solution containing 10 μg of formaldehyde per ml. Temporary
When prepared.
5 Instruments and equipment
Unless otherwise indicated, the gauges used in this standard shall be Class A glass gauges in accordance with national standards.
5.1 Full glass distiller 500 ml.
5.2 25 ml with a colorimetric tube.
5.3 Constant temperature water bath.
5.4 Spectrophotometer.
5.5 Common instruments used in general laboratories.
6 samples
6.1 Acquisition and preservation
The sample is collected in a hard glass bottle or a polyethylene bottle. The sample should be collected and the bottle should be stoppered after overflowing from the mouth of the bottle. Per liter after sampling
Add 1 ml of concentrated sulfuric acid (4.1) to the sample to make the sample pH ≤ 2 and analyze it within 24 h.
6.2 Preparation of samples
6.2.1 After the colorless, non-turbid, clean surface water and groundwater are adjusted to neutral, they can be directly measured.
6.2.2 Contaminated surface water, groundwater and industrial wastewater are distilled as follows.
Pipette 100.0 ml of the sample into a distillation flask (5.1), add 15 ml of water, add 3 to 5 ml of concentrated sulfuric acid (4.1) and several glass beads.
The 100 ml volumetric flask receives the distillate. When about 95 ml of distillate is distilled off, adjust the heating temperature and reduce the distillation speed until the distillate is close.
When 100 ml, stop the distillation, remove the receiving bottle, dilute to the mark with water, shake and set aside.
Note 1. When pre-distilling the sample, add 15 ml of water to the sample to prevent the organic matter from being in the sulfuric acid medium when the water sample with high organic content is steamed to the end.
The phenomenon of carbonization affects the determination of formaldehyde.
Note 2. For some special water samples that are not suitable for distillation under acidic conditions, such as wastewater containing high cyanide or dye wastewater, paint wastewater, etc., sodium hydroxide can be used.
The solution (4.2) is first adjusted to a weak alkaline (pH = 8 or so) and distilled.
7 Analysis steps
7.1 Drawing of the calibration curve
7.1.1 Take a 25 ml plug colorimetric tube and add 0, 0.50, 1.00, 3.00, 5.00, 8.00 ml formaldehyde standard solution (4.11).
Add water to 25 ml.
7.1.2 Add 2.50 ml of acetylacetone solution (4.6) to the above colorimetric tube and shake well. Heated in a (60 ± 2) ° C water bath for 15 min,
Take out the cooling.
7.1.3 Measure the absorbance with a 10 mm cuvette at a wavelength of 414 nm with water as a reference.
7.1.4 The absorbance As value measured by the series calibration liquid is deducted from the absorbance Ab value of the blank test to obtain the corrected absorbance Ar to correct the absorbance.
Degree Ar is the ordinate, and the calibration amount is plotted on the abscissa with the amount of formaldehyde W contained in the 25 ml calibration solution, or calculated by the least squares method.
Return to the equation, get.
rA bW a= (3)
Where. Ar--corrected absorbance;
W--formaldehyde amount, μg;
A--the intercept of the regression equation;
b--The slope of the regression equation.
7.2 Determination
Accurately remove appropriate amount of sample (containing formaldehyde within 80 μg, volume not exceeding 25 ml) in a 25 ml plug colorimetric tube, diluted with water
To the scale. Determine according to 7.1.2, 7.1.3, subtract the absorbance measured by the blank test, and find the sample from the calibration curve (7.1.4).
The amount of formaldehyde or the regression equation is used to calculate the amount of formaldehyde.
7.3 Blank test
Replace the sample with 25.00 ml of water and follow the same procedure as in 7.2 for parallel operation.
8 Calculation of results
The formaldehyde mass concentration ρ in the sample is calculated according to formula (4).
ρ = (4)
Where. ρ--the mass concentration of formaldehyde in the sample, mg/L;
W--the amount of formaldehyde calculated from the calibration curve (7.1.4) or calculated using equation (3), μg;
V--the volume of the sample, ml.
9 Precision and accuracy
Seven laboratories measured three uniform water samples at different levels of concentration, with formaldehyde levels of 0.35, 1.15, and 11.4 mg/L, respectively.
9.1 Repeatability
The relative standard deviations in the experimental room were 3.7%, 1.3%, and 5.4%, respectively.
9.2 Reproducibility
The relative standard deviations between laboratories were 11%, 6.9%, and 7.9%, respectively.
9.3 Accuracy
The average recovery rates of formaldehyde in each laboratory were 98.5%, 92.3%, and 101%, respectively.
10 Quality Assurance and Quality Control
10.1 Blank test
At least one full program blank test shall be performed for each batch of sample analysis, and the blank value shall not exceed the method detection limit.
When conditions permit, the blank sample on site is collected as the quality control sample of the site sample to evaluate the impact of the sampling process environment and transportation on the water sample.
10.2 Calibration
10.2.1 The correlation coefficient of the calibration curve regression equation γ ≥ 0.999.
10.2.2 Each batch of samples shall be provided with an intermediate check point. The relative deviation between the measured value of the intermediate check point and the corresponding point of the calibration curve shall not exceed
10%.
10.3 Parallel analysis
Parallel sample analysis should be performed at least once for each batch of samples, and the relative allowable difference of parallel sample analysis results is less than 20%.
10.4 Sample Plus Recycling
The spiked concentration is 0.5 to 2 times the concentration of the original sample, and the total concentration after the spiked does not exceed the upper limit concentration of the method.
Should be between 80% and 120%.
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