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Ambient air. Determination of the fluoride. Filter sampling followed by fluorine ion-selective electrode method
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HJ 480-2009
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Basic data | Standard ID | HJ 480-2009 (HJ480-2009) | | Description (Translated English) | Ambient air. Determination of the fluoride. Filter sampling followed by fluorine ion-selective electrode method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Classification of International Standard | 13.040 | | Word Count Estimation | 10,193 | | Date of Issue | 2009-09-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | GB/T 15434-1995 | | Quoted Standard | GB 7484; HJ/T 194 | | Regulation (derived from) | Department of Environmental Protection Notice No. 47 of 2009 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of fluoride in ambient air filter collection, fluoride ion selective electrode method. This standard applies to fluoride -hour ambient air concentrations and daily average concentration was determined. When the sample size is 6m ^ 3, the detection limit was 0. 9��g/m ^ 3. | HJ 480-2009: Ambient air. Determination of the fluoride. Filter sampling followed by fluorine ion-selective electrode method
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Ambient air.Determination of the fluoride.Filter sampling followed by fluorine ion-selective electrode method
HJ
National Environmental Protection Standard of the People's Republic
Replace GB/T 15434-1995
Determination of ambient air fluoride
Filter membrane sampling fluoride ion selective electrode method
Ambient air-Determination of the fluoride-Filter sampling followed by
Fluorine ion-selective electrode method
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);
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);
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 Normative references..1
3 Terms and Definitions.1
4 method principle..1
5 Reagents and materials.1
6 instruments and equipment.2
7 interference and elimination. 2
8 samples.2
9 Analysis steps..3
10 results indicate 4
11 Precision and Accuracy 4
12 Notes 4
Foreword
To protect the environment and protect people 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 the Prevention and Control of Air Pollution
The body health, standardize the monitoring method of fluoride in the air, and develop this standard.
This standard specifies a membrane sampling fluoride ion selective electrode method for determining the concentration of fluoride in air.
This standard is applicable to the Determination of Fluoride Concentration of Ambient Air Fluoride and Fluoride Ion Selective Electrode Method (GB/T 15434-1995)
Make revisions.
This standard was first published in.1995. The original standard drafting unit was Baotou Environmental Monitoring Station. This is the first revision.
The main revisions are as follows.
-- modified the name of the standard;
-- Supplementary and complete the scope of application of the method;
--In the reagents and materials, the purity of the reagents used was modified, and the detailed preparation process of hydrochloric acid and sodium hydroxide was added;
a method for preparing a total ionic strength adjusting buffer; simplifying the preparation process of the standard solution;
- specifies the operating conditions of the fluoride ion selective electrode;
- increased the field blank of the sample;
-- Added electrode cleaning method to the precautions.
The national environmental protection standard “Environmental Environment” approved and issued by the former National Environmental Protection Agency on March 25,.1995, from the date of implementation of this standard.
Determination of the concentration of air fluoride, the filter membrane · fluoride ion selective electrode method (GB/T 15434-1995) abolished.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard was drafted. Shenyang 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
Determination of ambient air fluoride
Filter membrane sampling fluoride ion selective electrode method
1 Scope of application
This standard specifies the membrane collection and fluoride ion selective electrode method for the determination of fluoride in ambient air.
This standard applies to the determination of the hourly and daily average concentrations of fluoride in ambient air.
When the sampling volume is 6 m3, the lower limit of measurement is 0.9 μg/m3.
2 Normative references
The contents of this standard refer to the terms in the following documents. For undated references, the latest valid version applies to this standard.
quasi.
GB 7484 Determination of fluoride in water quality - Ion selective electrode method
HJ/T 194 Technical Specifications for Manual Air Quality Monitoring
3 Terms and definitions
The following terms and definitions apply to this standard.
Fluoride fluoride
Refers to gaseous fluoride present in the air and particulate fluoride dissolved in hydrochloric acid solution [c (HCl) = 0.25 mol/L].
4 Principle of the method
When a known volume of air passes through a filter impregnated with dipotassium hydrogen phosphate, the fluoride is fixed or retained on the filter membrane, and the fluoride on the filter membrane is used.
After the hydrochloric acid solution was immersed, it was measured by a fluoride ion selective electrode method.
5 reagents and materials
The reagents used in this standard are analyzed using analytical analytical reagents in accordance with national standards, unless otherwise stated.
Deionized water or distilled water.
5.1 hydrochloric acid solution c (HCl) = 2.5 mol/L. take 1 000 ml of water, add 20.8 ml of hydrochloric acid (excellent grade, ρ = 1.18 g/ml), stir
Evenly.
5.2 Sodium hydroxide solution c (NaOH) = 1.0 mol/L. Weigh 40.0 g of superior grade sodium hydroxide, dissolved in water, and diluted to 1 000 ml after cooling.
5.3 Sodium hydroxide solution c (NaOH) = 5.0 mol/L. Weigh 100.0 g of excellent grade pure sodium hydroxide, dissolved in water, and then diluted to 500 ml after cooling.
5.4 Dipotassium hydrogen phosphate impregnating solution. Weigh 76.0 g of dipotassium hydrogen phosphate (K2HPO4·3H2O) dissolved in water and transferred to a 1 000 ml volumetric flask.
Make up to the mark with water and shake well.
5.5 Total Ionic Strength Modulation Buffer Solution (TISAB)
5.5.1 Total ionic strength adjustment buffer solution (TISABI). Weigh 58.0 g of sodium chloride, 10.0 g of sodium citrate, and measure 50 ml of glacial acetic acid.
Add 500 ml of water. After dissolving, add 135 ml of sodium hydroxide solution (5.3), adjust the pH of the solution to 5.2, and transfer to a 1 000 ml volumetric flask.
In the middle, add water to the mark and shake well.
5.5.2 Total ionic strength adjustment buffer solution (TISABII). Weigh 142 g of hexamethylenetetramine ((CH2)6N4) and 85 g of potassium nitrate
(KNO3), 9.97 g ferrotitanium reagent (C6H4Na2O8S2·H2O), dissolved in water, adjusted to pH 5-6, transferred to 1 000 ml capacity
Dilute the bottle to the mark with water and shake well.
The preparation of the solution is not limited thereto, and the preparation method of the total ionic strength adjusting buffer solution in GB 7484 can also be referred to.
Note. When the sample composition is complex, acid (pH ≈ 2) or alkaline (pH ≈ 12), TISABII formula can be used.
5.6 Sodium fluoride standard stock solution ρ (NaF)=1 000 μg/ml. Weigh 0.221 0 g sodium fluoride (excellent grade, dry at 110 °C for 2 h)
Cool to room temperature in a desiccator, dissolve in water and transfer to a 100 ml volumetric flask. Make up to the mark with water and shake well. Stored in a polyethylene bottle,
Store in the refrigerator, remove it when it is ready, and put it at room temperature.
5.7 Standard use solution of sodium fluoride. Dilute sodium fluoride standard stock solution (5.6) with water to 2.50, 5.00, 10.0, 25.0, 50.0,
The standard solution of 100.0 μg/ml is ready for use. Stored in polyethylene plastic bottles.
5.8 Acetic acid-nitrocellulose microporous membrane. pore size 5 μm, diameter 92 mm.
5.9 Dipotassium hydrogen phosphate impregnated membrane. After the acetic acid-nitrocellulose microporous membrane (5.8) is soaked in dipotassium hydrogen phosphate impregnation solution (5.4),
Drain (use a small amount of impregnating solution each time, with no filter membrane as the standard, after immersing 4 to 5 sheets of membrane, replace with new impregnation solution). Spread out,
Fluorine-free qualitative filter paper (cannot be directly used on glass plates or enamel pans), dried below 40 ° C, packed in plastic boxes (bags), sealed
Then put it into the desiccator for use (no desiccant in the dryer).
6 Instruments and equipment
6.1 Sampler. medium flow sampling pump with a polyethylene mesh pad supporting the filter membrane. The sampling head has an effective diameter of 80 mm and can be installed.
A filter with a diameter of 92 mm.
6.2 Ion activity meter or precision acidity meter. resolution is 0.1 mV.
6.3 Fluoride ion selective electrode.
a. Measure the concentration range of fluoride ion. 10−5～10−1 mol/L.
b. Determination of the slope of the curve. at t ° C, (54 0.2 t) mV.
6.4 Calomel electrode. The salt bridge solution is saturated potassium chloride.
6.5 Magnetic stirrer. stirrer with polyethylene wrap.
6.6 Small ultrasonic cleaner.
6.7 Polyethylene plastic beaker. 100 ml.
6.8 Polyethylene plastic bottles. 100, 1 000 ml.
7 interference and elimination
When there are Si4, Fe3, and Al3 in the measurement system and the concentration does not exceed 20 mg/L, the interference generated may be added to the total ion.
The intensity adjustment buffer is eliminated.
8 samples
8.1 Sample collection and preservation
Sample collection should be in accordance with the requirements of the Technical Specifications for Manual Air Quality Monitoring (HJ/T 194). Various samplers should be in the mining
Perform air tightness check and flow calibration before sample.
During sampling, two filter plates of dipotassium hydrogen phosphate were placed in the filter holder, separated by a filter gasket of 2 to 3 mm thick (see Figure 1).
The gas is collected at a flow rate of 100 to 120 L/min (air flow rate of 0.3 to 0.4 m/s) for more than 45 minutes, and the sampling is designed according to the performance of the instrument used.
Record (should include sampling time, flow or sample volume at the beginning and end, wind direction, wind speed, air temperature, air pressure, sampling point, sample number
Etc) and record. After sampling, remove the sample film with a clean tweezers, fold it into a plastic bag (box), seal it, and bring it back to the lab.
The collected samples were stored in a laboratory desiccator (with no desiccant in the desiccator) and must be analyzed within 40 days.
Polyethylene plastic washer
First filter
Spacer filter gasket
Second filter
Support filter mesh mat
80 mm
92 mm
Figure 1 Filter sampling device
8.2 Field blank
8.2.1 Replace the sample with the blank filter after immersion, bring it to the site, store it under the same conditions as the sample, transport it, and send it to the experiment.
Room analysis, care should be taken to prevent contamination during transportation.
8.2.2 Compare the field blank with the measurement results of the laboratory blank filter. If the field blank is too different from the laboratory blank, look for it.
Reason, resampling.
8.2.3 Require at least 2 field blanks for each sample.
9 Analysis steps
9.1 Drawing of standard curve
9.1.1 Take 6 100 ml polyethylene plastic cups and prepare standard series according to Table 1. It can also be prepared according to the actual sample concentration, not less than 6
a little bit. Take 2.00 ml of six standard solutions (5.7), and add hydrochloric acid solution (5.1) 20.00 ml, sodium hydroxide solution (5.2).
5.00 ml, TISAB solution (5.5) 10.00 ml, water 3.00 ml, fluoride ion content is 5.0, 10.0, 20.0, 50.0, 100,
200 μg.
Table 1 Standard solution preparation series
Cup number 1 2 3 4 5 6
F− standard use liquid concentration (5.7)/(μg/ml) 2.5 5.0 10.0 25.0 50.0 100.0
Standard use liquid volume/ml 2.00 2.00 2.00 2.00 2.00 2.00
Hydrochloric acid solution (5.1)/ml 20.00 20.00 20.00 20.00 20.00 20.00
Sodium hydroxide solution (5.2)/ml 5.00 5.00 5.00 5.00 5.00 5.00
TISAB solution (5.5)/ml 10.00 10.00 10.00 10.00 10.00 10.00
Water/ml 3.00 3.00 3.00 3.00 3.00 3.00
F− content/μg 5.0 10 20 50 100.200
9.1.2 Turn on the ion activity meter and insert the cleaned fluoride ion selective electrode and calomel electrode into the prepared test solution as required.
Do not stir the solution before inserting the electrode to avoid air bubbles on the electrode surface and affect the accuracy of the measurement. Measure from low to high concentration one by one
get on. Stir for a few minutes on a magnetic stirrer, the magnetic stirring time should be consistent, and the stirring speed should be moderate and stable. After the reading is stable
(ie, the electrode potential change is less than 0.2 mV per minute) Stop stirring, read the millivolt value after standing, and record the temperature at the time of measurement.
Note. The temperature of the solution is controlled at 15 ~ 35 ° C to ensure that the fluoride ion selection electrode works normally.
9.1.3 Regression with the logarithm of the fluorine content and its corresponding millivolt value, the absolute value of the correlation coefficient r is required to be greater than 0.999, and the slope is consistent.
(54 0.2t) mV; or on semi-logarithmic paper, the fluorine content (μg) is expressed in logarithmic coordinates, and the millivolt value is expressed in equidistant coordinates.
Quasi-curve.
9.2 Preparation of samples
Cut the sample membrane into small pieces (approx. 5 mm × 5 mm), place in a 100 ml polyethylene plastic cup, add hydrochloric acid solution (5.1) 20.00 ml,
Extract in an ultrasonic cleaner for 30 min, take it out, wait until the temperature of the solution is cooled to room temperature, and then add 5.00 ml of sodium hydroxide solution (5.2).
TISAB solution (5.5) 10.00 ml and water 5.00 ml, total volume 40.00 ml, and then placed for 3 h, measured, the placement time should not exceed 5
h.
9.3 Blank test
The instability of the blank value will directly affect the accuracy of the measurement results, so each batch of acetic acid-nitrocellulose filter should be tested blank.
Extract 4 to 5 sheets of unsampled dipotassium hydrogen phosphate impregnated filter, cut into small pieces (about 5 mm × 5 mm), and put in 100 ml of poly
In the olefin plastic cup, add 0.50 ml of sodium fluoride standard solution (5.7) (10.0 μg/ml), and prepare the sample according to 9.2 (note that the amount of water added is
4.50 ml), read the millivolt value according to 9.1.2, calculate the fluorine content according to the regression equation or find the fluorine content from the standard curve.
The amount is the measured value (μg) minus the standard fluorine content added 5 μg, and the average value is the fluorine content of the blank filter (fluorine per blank filter)
The content should not exceed 1 μg).
9.4 Sample determination
The processed sample is measured in the same way as the calibration curve. After reading the millivolt value, calculate the fluorine content according to the regression equation or from the standard
The fluorine content was found on the curve.
The sample measurement should be performed simultaneously with the calibration curve. The difference between the temperature at which the sample is measured and the temperature at which the calibration curve is drawn should not exceed
±2 °C.
10 results indicate
The mass concentration ρ (F−) of fluoride in the air is calculated according to formula (1).
Where. ρ (F−)--the mass concentration of fluoride in the air, μg/m3;
W1 W2--the fluorine content of the two-layer filter sample measured according to 9.4, μg;
W0--the average fluorine content of laboratory blank filter, μg;
V0 - the sampling volume in the standard state, m3.
11 Precision and accuracy
11.1 Precision. Four laboratories collect atmospheric environmental samples at different locations, and each laboratory collects 4 to 5 parallel samples per batch.
A total of 25 batches of samples were obtained with a mean value ranging from 0.57 to 18.2 μg/m3 with an average coefficient of variation of 7.8% and a maximum of 22%.
11.2 Accuracy. Five laboratory samples of fluorine-containing 50.0 μg membranes were prepared with a relative error of 0.9%.
12 Precautions
Do not touch the surface of the electrode membrane with your fingers. To protect the electrode, the measured concentration of fluorine in the test solution should not exceed 40 mg/L. in case
The surface of the electrode film is contaminated with organic matter, etc., and must be cleaned before use. It can be cleaned with organic reagents such as methanol and acetone.
Detergent. For example, the electrode can be immersed in a warm, dilute detergent (1 part detergent plus 9 parts water) for 3 to 5 minutes. If necessary, can be
Put in another diluted detergent. Then rinse with water, then immerse in (1 1) hydrochloric acid for 30 s, finally rinse with water, suck with filter paper
Remove moisture.
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