HJ 488-2009 (HJ488-2009) & related versions
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Water quality. Determination of fluoride. Fluorine reagents spectrophotometry
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HJ 488-2009
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HJ 488-2009
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HJ 488-2009: PDF in English
HJ 488-2009
Water quality.Determination of fluoride.Fluorine reagents spectrophotometry
HJ
National Environmental Protection Standard of the People's Republic
Replace GB 7483-87
Determination of fluoride in water quality
Fluorine reagent spectrophotometry
Water quality-Determination of fluoride
-Fluorine reagents spectrophotometry
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);
X. Determination of Fluoride in Water Quality by Spectrophotometric Method of Zirconium Sulfate Sulfate (HJ 487-2009);
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 and equipment. 2
5 interference and elimination. 2
6 samples. 2
7 Analysis steps..2
8 result calculation..2
9 precision and accuracy..2
Appendix A (Normative) Determination of fluoride in water quality Pretreatment with interfering ion samples..3
Foreword
In order to implement the "Environmental Protection Law of the People's Republic of China" and the "Water Pollution Prevention and Control Law of the People's Republic of China"
Body health, standardize monitoring methods for fluoride in water, and develop this standard.
This standard specifies methods for the determination of fluoride in surface water, groundwater and industrial wastewater.
This standard amends the "Fluorine Spectrophotometric Method for the Determination of Fluoride in Water Quality" (GB 7483-87), the original standard drafting list
The location is the Baotou City Environmental Monitoring Station. This is the first revision.
The main revisions are as follows.
- Broaden the linear range of the method by adjusting the cuvette;
-- Adjust and revise some text and sentence structure.
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 Fluorescence Spectrophotometry (GB 7483-87) is 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 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 - Fluorescent reagent spectrophotometric method
1 Scope of application
This standard specifies the fluorine reagent spectrophotometric method for the determination of fluoride in surface water, groundwater and industrial wastewater.
This standard applies to the determination of fluoride in surface water, groundwater and industrial wastewater.
The detection limit of this method is 0.02 mg/L, and the lower limit of determination is 0.08 mg/L.
2 Principle of the method
The fluoride ion reacts with the fluorine reagent and cerium nitrate in an acetate buffer medium with a pH of 4.1 to form a blue ternary complex.
The absorbance at 620 nm is proportional to the fluoride ion concentration and the fluoride (F−) is quantified.
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 fluoride-free distilled water.
3.1 Hydrochloric acid solution. c = 1 mol/L.
Take 8.4 ml of hydrochloric acid dissolved in 100 ml of deionized water.
3.2 Sodium hydroxide solution. c = 1 mol/L.
Weigh 4 g of sodium hydroxide in 100 ml of deionized water.
3.3 Acetone (CH3COCH3).
3.4 Sulfuric acid (H2SO4). ρ20 = 1.84 g/ml.
Take 300 ml of sulfuric acid into a 500 ml beaker, place it on a hot plate for 1 h, cool it, and put it into a bottle for later use.
3.5 Glacial acetic acid (CH3COOH).
3.6 Fluoride standard stock solution. Weigh the pure sodium fluoride (NaF) 0.221 0 g which has been dried at 105 °C for 2 h, dissolved in deionized water.
Transfer to a 1 000 ml volumetric flask, dilute to the mark, mix and store in a polyethylene bottle, and use 100 μg of fluoride per ml.
3.7 Fluoride standard use solution. Pipette 20.00 ml of sodium fluoride standard stock solution (3.6), transfer to 1 000 ml volumetric flask, use deionized water
Dilute to the mark and store in a polyethylene bottle. This solution contains 2.00 μg of fluoride per ml.
3.8 Fluorine reagent solution. c = 0.001 mol/L.
Weigh 0.193 g of fluoro reagent [3 - methylamine - alizarin - diacetic acid, referred to as ALC, C14H7O4 · CH2N (CH2COOH) 2], add 5 ml
Wet in deionized water, add sodium hydroxide solution (3.2) to dissolve it, add 0.125 g of sodium acetate (CH3COONa·3H2O), use salt
The acid solution (3.1) was adjusted to pH 5.0, diluted to 500 ml with deionized water, and stored in a brown bottle.
3.9 cerium nitrate solution. c = 0.001 mol/L.
Weigh 0.443 g of lanthanum nitrate [La(NO3)3·6H2O], dissolve it with a small amount of hydrochloric acid solution (3.1), and adjust with 1 mol/L sodium acetate solution.
The pH was 4.1 and diluted to 1 000 ml with deionized water.
3.10 Buffer solution. pH = 4.1.
Weigh 35 g of anhydrous sodium acetate (CH3COONa) dissolved in 800 ml of deionized water and add 75 ml of glacial acetic acid (CH3COOH) (3.5).
Dilute to 1 000 ml with deionized water and adjust the pH to 4.1 on a pH meter with acetic acid or sodium hydroxide solution.
3.11 Mix the developer.
Take the fluorine reagent solution (3.8), buffer solution (3.10), acetone (3.3) and cerium nitrate solution (3.9) at a volume ratio of 3.1.3.3
Mix it. Formulated when ready to use.
4 Instruments and equipment
4.1 Spectrophotometer. A cuvette with an optical path of 30 mm or 10 mm.
4.2 pH meter.
5 interference and elimination
In 25 ml of color developing solution containing 5 μg of fluoride, the following ions are present in excess of the following contents, which may interfere with the measurement and should be pre-steamed first.
Distillation. Cl− 30 mg; SO42− 5.0 mg; NO3− 3.0 mg; B4O72− 2.0 mg; Mg2 2.0 mg; NH4 1.0 mg; Ca2 0.5 mg.
6 samples
6.1 Acquisition and preservation
The fluoride sample was measured and collected and stored in a polyethylene bottle.
6.2 Preparation of samples
Unless it is proved that the pretreatment of the sample is unnecessary, the sample may be directly prepared for colorimetry, otherwise it shall be pre-distilled according to Appendix A.
7 Analysis steps
7.1 Calibration curve
Add fluoride standard solution (3.7) 0.00, 1.00, 2.00, 4.00, 6.00, 8.00 ml to 6 25.0 ml volumetric flasks.
Add deionized water to 10 ml, accurately add 10.0 ml of mixed developer (3.11), dilute to the mark with deionized water, shake and place for 30 min.
Absorbance was measured using a 30 mm or 10 mm cuvette at 620 nm with pure water as a reference. Deducting reagent blank (zero concentration)
The absorbance is plotted against the absorbance of the fluoride content, which is the calibration curve.
7.2 Determination
Accurately draw 1.00 ~ 10.00 ml of sample (depending on fluoride content in water) in a 25.0 ml volumetric flask, add deionized water to
10 ml, accurately add 10.0 ml of mixed developer (3.11), dilute to the mark with deionized water, and shake well. The following is done according to 7.1. Blank
After calibration, the fluoride (F−) content was found on the calibration curve from the absorbance value.
7.3 Blank test
The sample was replaced with water and measured according to the procedure of measuring the sample.
8 Calculation of results
The fluoride (F−) mass concentration in the sample is calculated as follows.
ρ =
Where. ρ--the concentration of fluoride (F−) in the sample, mg/L;
M--calibration curve of the sample fluorine content, μg;
V--take the sample volume, ml.
The result is accurate to two decimal places.
9 Precision and accuracy
Three laboratories analyzed a uniform distribution standard solution of fluoride containing 0.5 mg/L with a relative standard deviation of 1.2% in the laboratory.
The relative standard deviation is 1.2% and the relative error is −0.8%.
Appendix A
(normative appendix)
Determination of fluoride in water quality with pretreatment of interfering ion samples
A.1 For water samples with strong acidity and alkalinity, adjust to neutral after 1 mol/L sodium hydroxide solution or 1 mol/L hydrochloric acid solution before measurement.
Line measurement.
A.2 Pre-distillation
A.2.1 Distillation unit is shown in Figure A.1.
1-1 000 ml three-necked flask; 2-500 ml three-necked flask; 3-safety tube; 4-250 °C thermometer;
5-condensation tube; 6-receiver bottle; 7-universal electric furnace; 8-water vapor conduit; 9-bolt water
Figure A.1 Distillation unit diagram
A.2.2 Take 20 ml of the test solution and place it in a 500 ml three-necked flask (A.2.1). Add 20 ml of sulfuric acid (3.4) and mix slowly while shaking.
Connect the device according to Figure A.1 and heat up to introduce water vapor at a temperature of 145 °C. Collect the distillate at a distillation rate of 6 to 7 ml per minute to
200 ml, reserved for color development.
Note. The distillation temperature should be strictly controlled at (145 ± 5) °C, otherwise the sulfuric acid will be distilled out, affecting the measurement results.
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| Standard ID | HJ 488-2009 (HJ488-2009) | | Description (Translated English) | Water quality. Determination of fluoride. Fluorine reagents spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 9,967 | | Date of Issue | 2009-09-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | GB/T 7483-1987 | | 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 determination of surface water, groundwater and industrial effluent fluoride fluoride reagent spectrophotometry. This standard applies to surface water, groundwater and industrial wastewater Determination of fluoride. The method detection limit is 0. 02 mg/L, detection limit of 0. 08 mg/L. |
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