HJ 487-2009 (HJ487-2009) & related versions
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Water quality. Determination of fluoride. Visual colorimetry with zirconium alizarinsulfonate
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HJ 487-2009
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HJ 487-2009
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HJ 487-2009: PDF in English
HJ 487-2009
Water quality.Determination of fluoride.Visual colorimetry with zirconium alizarinsulfonate
HJ
National Environmental Protection Standard of the People's Republic
Replace GB 7482-87
Determination of fluoride in water quality
Zirconium sulfonate visual colorimetry
Water quality-Determination of fluoride
-Visual colorimetry with zirconium alizarinsulfonate
Published on.2009-09-27
2009-11-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 47 of.2009
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 water quality polycyclic aromatic hydrocarbons.
Eighteen standards, such as fixed liquid extraction and solid phase extraction high performance liquid chromatography, are national environmental protection standards and are released.
The standard name and number are as follows.
I. Determination of Polycyclic Aromatic Hydrocarbons by Liquid-Liquid Extraction and Solid Phase Extraction High Performance Liquid Chromatography (HJ 478-2009);
2. Determination of nitrous oxides (nitrogen oxides and nitrogen dioxide) - Determination of naphthalene diamine hydrochloride spectrophotometric method (HJ 479-
2009);
III. Determination of Fluoride in Ambient Air Filtration of Fluoride Ion Selective Electrode Method (HJ 480-2009);
IV. Determination of fluoride in ambient air Determination of fluoride ion-selective electrode method for lime filter paper (HJ 481-2009);
V. Determination of Sulfur Dioxide in Ambient Air - Formaldehyde Absorption - Pararosaniline Spectrophotometry (HJ 482-2009);
6. Determination of Sulfur Dioxide in Ambient Air - Tetrachloromercury Salt Absorption - Pararosaniline Spectrophotometry (HJ 483-2009);
VII. Determination of water content cyanide volumetric method and spectrophotometry (HJ 484-2009);
VIII. Determination of copper in water quality by diethyldithiocarbamate spectrophotometry (HJ 485-2009);
IX. Determination of copper in water quality 2,9-Dimethyl-1,10 phenanthroline spectrophotometry (HJ 486-2009);
XI. Determination of Fluoride in Water Quality Fluorescence Spectrophotometry (HJ 488-2009);
XII. Determination of Silver in Water Quality 3,5-Br2-PADAP Spectrophotometry (HJ 489-2009);
XIII. Determination of Silver in Water Quality by Cadmium Reagent 2B Spectrophotometry (HJ 490-2009);
XIV. Determination of Total Chromium in Soils by Flame Atomic Absorption Spectrophotometry (HJ 491-2009);
15. Air Quality Vocabulary (HJ 492-2009);
XVI. Technical Regulations for the Preservation and Management of Water Quality Samples (HJ 493-2009);
17. Water Quality Sampling Technical Guidance (HJ 494-2009);
18. “Technical Guidance for the Design of Water Quality Sampling Plans” (HJ 495-2009).
The above standards have been implemented since November 1,.2009 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 20 national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The exact name and number are as follows.
1. "Determination of six specific polycyclic aromatic hydrocarbons in water quality by high performance liquid chromatography" (GB 13198-91);
2. Determination of nitrogen oxides in air quality - Determination of naphthylethylenediamine hydrochloride (GB 8969-88);
3. "Saltzman method for determination of nitrogen oxides in ambient air" (GB/T 15436-1995);
4. Determination of the concentration of fluoride in ambient air, filter membrane and fluoride ion selective electrode method (GB/T 15434-1995);
V. Determination of Fluoride in Ambient Air Lime Filter Paper · Fluoride Ion Selective Electrode Method (GB/T 15433-1995);
6. Determination of Sulphur Dioxide in Ambient Air - Formaldehyde Absorption - Pararosaniline Spectrophotometry (GB/T 15262-94);
VII. Determination of Air Quality, Sulfur Dioxide, Tetrachloromercury Salt - Pararosaniline Hydrochloride Colorimetric Method (GB 8970-88);
VIII. Determination of Cyanide in Water Quality Part I Determination of Total Cyanide (GB 7486-87);
IX. Determination of Cyanide in Water Quality Part 2 Determination of Cyanide (GB 7487-87);
X. Determination of copper in water quality by diethyldithiocarbamate spectrophotometry (GB 7474-87);
XI. Determination of Copper in Water Quality 2,9-Dimethyl-1,10-phenanthroline Spectrophotometric Method (GB 7473-87);
Twelve, "Determination of Fluoride in Water Quality, Zirconium Sulfonic Acid Visual Colorimetric Method" (GB 7482-87);
XIII. Determination of Fluoride in Water Quality Fluorescence Spectrophotometry (GB 7483-87);
XIV. Determination of Silver in Water Quality, 3,5-Br2-PADAP Spectrophotometry (GB 11909-89);
Fifteen, "Measurement of mercury in water, cadmium reagent 2B spectrophotometry" (GB 11908-89);
XVI. Determination of Total Chromium in Soil Quality by Flame Atomic Absorption Spectrophotometry (GB/T 17137-1997);
17. Air Quality Vocabulary (GB 6919-86);
18. Technical Regulations for the Preservation and Management of Water Samples (GB 12999-91);
Nineteen, "Water Quality Sampling Technical Guidance" (GB 12998-91);
20. Technical Regulations for the Design of Water Quality Sampling Plans (GB 12997-91).
Special announcement.
September 27,.2009
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 reagents and materials.1
4 instruments.1
5 interference and elimination. 2
6 samples. 2
7 Analysis steps..2
8 result calculation..2
9 precision and accuracy..2
10 Notes 3
Appendix A (Normative) Determination of fluoride in water quality Pretreatment with interfering ion samples..4
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 fluoride in health and water and wastewater.
This standard specifies the visual colorimetric method for the determination of fluoride in drinking water, surface water, groundwater and industrial wastewater.
This standard amends the "Determination of Fluoride in Water Quality by Zirconium Sulfonic Acid Visual Colorimetric Method" (GB 7482-87), this standard
First published in 1987, the original standard drafting unit was China Environmental Monitoring Station. This is the first revision.
The main revisions are as follows.
-- Modified the preparation method of the zirconium sulfonate solution;
- Changed the amount of zirconium sulfonate acidic solution added.
The national environmental protection standard “Water quality approved and issued by the former National Environmental Protection Agency on March 14, 1987 since the implementation of this standard.
Determination of Fluoride The Zirconium Sulfate Sulfate Visual Colorimetric Method (GB 7482-87) was abolished.
Appendix A of this standard is a normative appendix.
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, Liaoning Provincial Environmental Monitoring Center Station.
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.
Iv
Water quality - Determination of fluoride - Zirconium sulphonate
1 Scope of application
This standard specifies the visual colorimetric determination of zirconium sulfonate of fluoride in drinking water, surface water, groundwater and industrial wastewater.
This standard applies to the determination of fluoride in drinking water, surface water, groundwater and industrial wastewater.
When taking 50 ml sample and directly measuring the concentration of fluoride, the detection limit of this method is 0.1 mg/L, and the lower limit of determination is 0.4 mg/L.
The upper limit is 1.5 mg/L (high samples can be analyzed after dilution).
2 Principle of the method
In an acidic solution, sodium limonate sulfonate and zirconium salt form a red complex, which can capture zirconium in the complex when fluoride ions are present in the sample.
Ions, producing colorless zirconium fluoride ions, releasing yellow sodium bismuth sulfonate, depending on the color of the solution from red to yellow
Colorimetric quantification.
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 Perchloric acid (HClO4). 70% to 72%.
3.2 Hydrochloric acid (HCl). ρ20 = 1.19 g/ml.
3.3 Sulfuric acid (H2SO4). ρ = 1.84 g/ml.
3.4 Sodium arsenite (NaAsO2). ρ = 5 g/L, weigh 0.5 g of sodium arsenite, dissolve in a small amount of water, and dilute to 100 ml.
Note. Sodium arsenite is highly toxic and prevents entry into the mouth.
3.5 Fluoride standard stock solution. ρ = 100.0 μg/ml, take sodium fluoride at 105 ° C for 2 h, after cooling in a desiccator, accurately
Take 0.221 0 g, dissolve in water, transfer to a 1 000 ml volumetric flask, and dilute to the mark with water.
3.6 Fluoride standard solution. ρ =10.00 μg/ml, take 10.00 ml of fluoride standard solution (3.5), in a 100 ml volumetric flask, with water
Dilute to the mark.
3.7 Zirconium sulfonate acidic solution
3.7.1 Zirconium silicate sulfonate solution. Weigh 0.3 g of zirconium oxychloride (ZrOCl2·8H2O) in a 100 ml beaker and dissolve it in 50 ml of water.
Move into a 1 000 ml volumetric flask. Another 0.7 g sodium decanoate (C14H7O7SNa·H2O) is dissolved in 50 ml of water and shaken continuously.
Next, slowly inject the zirconium oxychloride solution. After shaking fully, place it for clarification.
3.7.2 Mixed acid solution. Measure 101 ml of hydrochloric acid (3.2) and dilute to 400 ml with water, and measure 33.3 ml of sulfuric acid (3.3).
With stirring, slowly add to 400 ml of water and, after cooling, combine the two acids.
3.7.3 Zirconium sulfonate acidic solution. Pour the mixed acid (3.7.2) into a volumetric flask containing zirconium sulfonate solution (3.7.1), with water
Dilute to the mark and shake well. This solution can be used from red to yellow after about 2 hours. This solution is stored in the dark and stable for 6 months.
4 instruments
4.1 50 ml with colorimetric tube.
4.2 Distillation unit, see A.5.1.
5 interference and elimination
Pre-distillation is required when the interfering ions in the sample exceed the following concentrations. total alkalinity (CaCO3) 400 mg/L, chloride 500 mg/L,
Sulfate.200 mg/L, aluminum 0.1 mg/L, phosphate 1.0 mg/L, iron 2.0 mg/L, turbidity 25 degrees, chroma 25 degrees.
6 samples
6.1 Acquisition and preservation
The water sample of the fluoride was measured, and a polyethylene bottle was used for collecting and storing the sample.
6.2 Preparation of samples
(1) If the water sample contains residual chlorine, add one drop (0.05 ml) of sodium arsenite solution per 0.1 mg of chlorine and mix to remove
It.
(2) If there are many interfering substances in water, and can not be directly measured by colorimetry, pre-distillation treatment can be carried out according to Appendix A.
7 Analysis steps
7.1 Preparation of standard colorimetric series
Pipette 0.00, 0.50, 1.00, 2.00, 2.50, 4.00, 5.00, and 7.50 ml of fluoride standard solution (3.6) into 50 ml.
In the colorimetric tube, make up to volume with pure water. The fluoride content of this standard color column is. 0.00, 5.00, 10.00, 20.00, 25.00, 40.00,
50.00 and 75.00 μg. Add 1.0 ml of zirconium sulfonate acidic solution (3.7.3) to the above standard solution and mix for 1 h or
Color development in 50 ° C water for 20 min, cool to room temperature can be visual colorimetric (in the standard solution selected, at least two lower than two and higher than the test
The concentration of fluoride in the sample is usually at 50 μg/L or 100 μg/L of fluorine. This standard color column is stable for 3 months in the dark.
7.2 Determination
Take 50 ml of sample or distillate in a colorimetric tube (4.1). When the fluorine content is higher than 2.5 mg/L, a small amount of sample or distillate can be taken.
Dilute to 50 ml with water. Add 1.0 ml of zirconium sulfonate acidic solution (3.7.3) in a colorimetric tube and place it for 1 h or in 50 ° C water.
Color 20 min, cool to room temperature for visual colorimetry with standard color bars.
7.3 Blank test
Replace the sample with 50 ml of pretreated water, using the same reagents as used in assay (7.2) and using
In the same step, a blank measurement was performed.
8 Calculation of results
The fluoride (F−) mass concentration in the water sample is calculated as follows.
twenty one
200m
VV
ρ = × (1)
Where. ρ - the mass concentration of fluoride (F−) in the water sample, mg/L;
M--the fluoride content given by the standard series, μg;
V2--the volume of the test (sample volume when colorimetric), ml;
V1--sample volume (take the original water sample distillation volume), ml.
9 Precision and accuracy
9.1 Repeatability
The standard solution with a fluoride concentration of 1.00 mg/L was prepared and tested 11 times with a relative standard deviation of 9.3% in the laboratory.
Twenty laboratories measured the results of the following water samples.
Uniform water sample with no turbidity of 830 μg/L. The relative standard deviation between chambers was 4.9% with a relative error of 3.6%.
Uniform water sample containing interfering substances with a fluorine content of 570 μg/L. The relative standard deviation between chambers was 11.1% with a relative error of zero.
9.2 Accuracy experiment
Fluoride national standard sample numbered GSB07-1194-2000.201722 was pre-steamed using zirconium sulfamate visual colorimetry
The experimental determination of the distillation-visual colorimetric method has an average value of 2.40 mg/L, which is within the uncertainty of the guaranteed value.
9.3 Method of comparison experiment
The method was compared with the fluoride ion selective electrode method, and the paired t test was used for statistical processing. The t values were all smaller than
T0.05 (5) = 2.57, there was no significant difference between the two methods.
10 Precautions
(1) Coexisting ion influence. the presence of sulfate, phosphate, iron and manganese in the sample can make the measurement result high, aluminum can be combined with fluoride ion
A stable complex [(AlF6)3−] is formed, which results in a low measurement result.
(2) The sodium bismuth sulfonate is preferably stored separately with the zirconium salt, and mixed in proportions during use to maintain the sensitivity of the reagent.
(3) The formation of color in the process of zirconium sulfonate and fluoride ion is affected by various factors, so in the analysis, control samples
The amount of reagents, blanks and standard series added reagents, reaction temperature, placement time and other conditions must be the same, between the test and the standard colorimetric series
The temperature difference does not exceed 2 °C.
Appendix A
(normative appendix)
Determination of fluoride in water quality with pretreatment of interfering ion samples
A.1 Principle of steam distillation
Fluoride in water is introduced into a solution containing perchloric acid (or sulfuric acid), and is vaporized in the form of fluorosilicic acid or hydrofluoric acid.
A.2 distillation unit
1-receiver bottle (200 ml volumetric flask); 2-condensation tube (snake or spherical); 3-distillate bottle (250 ml straight-mouth three-necked flask);
4-2 000 ml flat-bottomed flask (for steam); 5-tunable electric furnace; 6-thermometer; 7-safety tube; 8-way tube (for exhaust)
Figure 1 Steam distillation device diagram
A.3 steps
Take 50 ml of water sample (when the concentration of fluorine is higher than 2.5 mg/L, a small amount of sample can be separated and diluted to 50 ml with water) in the distillation flask (3).
Add 10 ml of perchloric acid (3.1), shake well, connect as shown in Figure 1, and turn on the reflux water in the condenser. Heat the flat bottom flask (4) and close the tee
Valve B in the valve opens the valve A to the air and causes it to boil to produce water vapor. At the same time, heat the distillation bottle (3), and dissolve the bottle (3)
When the liquid temperature rises to about 130 ° C, open the valve B in the three-way valve, close the valve A to the air, start to open the steam, and maintain the distillation bottle (3)
The temperature is between 130 and 140 ° C and the distillation rate is between 5 and 6 ml/min. Stop the distillation when the volume of the distillate in the receiving bottle (1) is about.200 ml, and
Dilute to.200 ml with water and leave for measurement.
If the content of organic matter in the water sample is high, in order to avoid explosion with perchloric acid, use sulfuric acid instead of perchloric acid (volume ratio of sulfuric acid to water sample)
Distillation was carried out for 1 1 .), and the temperature was controlled at 145 ° C ± 5 ° C. When distilling the water sample, do not let the temperature exceed 180 ° C to prevent excessive evaporation of sulfuric acid.
When several water samples are continuously distilled, the temperature of the sulfuric acid solution in the bottle can be lowered to below 120 ° C, and another water sample is added, and a fluorine is distilled.
After a high water sample, 250 ml of purified water should be added before distilling another water sample. Distillation with the same method to remove fluorine that may remain in the distiller
Compound. The sulfuric acid in the distillation flask can be used multiple times until it turns black.
......
| Standard ID | HJ 487-2009 (HJ487-2009) | | Description (Translated English) | Water quality. Determination of fluoride. Visual colorimetry with zirconium alizarinsulfonate | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 10,136 | | Date of Issue | 2009-09-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | GB/T 7482-1987 | | Drafting Organization | China Environmental Monitoring Station | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Department of Environmental Protection Notice No. 47 of 2009 | | Summary | This standard specifies the drinking water, surface water, groundwater and industrial wastewater alizarinsulfonate zirconium fluoride visual colorimetric assay. This standard applies to drinking water, surface water, groundwater and industrial wastewater Determination of fluoride. Take 50ml sample, direct determination of the concentration of fluoride, the method detection limit of 0. 1mg/L, detection limit of 0. 4mg/L, measured a maximum of 1. 5mg/L (high content of samples can be analyzed after dilution). |
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