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HJ 491-2009 English PDF

HJ 491-2009_English: PDF (HJ491-2009)
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HJ 491-2009English399 Add to Cart 3 days [Need to translate] Soil quality. Determination of total chromium. Flame atomic absorption pectrometry Obsolete HJ 491-2009
HJ 491-2019English275 Add to Cart 0--9 seconds. Auto-delivery Soil and sediment - Determination of copper, zinc, lead, nickel and chromium - Flame atomic absorption spectrophotometry Valid HJ 491-2019


BASIC DATA
Standard ID HJ 491-2009 (HJ491-2009)
Description (Translated English) Soil quality. Determination of total chromium. Flame atomic absorption pectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Classification of International Standard 13.080
Word Count Estimation 10,179
Date of Issue 2009-09-27
Date of Implementation 2009-11-01
Older Standard (superseded by this standard) GB/T 17137-1997
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 total chromium in soil by flame atomic absorption spectrophotometry. This standard applies to the determination of total chromium in soil. Weigh 0. 5g sample digestion volume to 50ml, the method detection limit of 5mg/kg, detection limit is 20. 0mg/kg.

Standards related to: HJ 491-2009

HJ 491-2009
Soil quality.Determination of total chromium.Flame atomic absorption pectrometry
HJ
National Environmental Protection Standard of the People's Republic
Replace GB/T 17137-1997
Determination of total chromium in soil
Flame atomic absorption spectrophotometry
Soil quality-Determination of total chromium
-Flame atomic absorption spectrometry
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);
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);
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.1
5 interference and elimination. 2
6 samples. 2
7 Analysis steps..3
8 result calculation..3
9 precision and accuracy..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 the monitoring method of total chromium in soil, and develop this standard.
This standard specifies the flame atomic absorption spectrophotometry for the determination of total chromium in soil.
This standard is a revision of the Determination of Total Chromium in Soil Quality by Flame Atomic Absorption Spectrophotometry (GB/T 17137-1997).
The original standard drafting unit was the China National Environmental Monitoring Center, which was first published on December 8,.1997. This is the first revision.
The main revisions are as follows.
- a method of total decomposition using hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid;
- Added pretreatment method for microwave digestion;
- Simplify soil pretreatment steps;
-- Added method of preparation of chromium stock solution.
From the date of implementation of this standard, the national environmental protection standard “Soil” approved and issued by the former National Environmental Protection Agency on December 8,.1997
Determination of total chromium content by flame atomic absorption spectrophotometry (GB/T 17137-1997) 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
Soils - Determination of total chromium - Flame atomic absorption spectrophotometric method
1 Scope of application
This standard specifies the flame atomic absorption spectrophotometry for the determination of total chromium in soil.
This standard applies to the determination of total chromium in soil.
When weigh 0.5 g of sample and dilute to 50 ml, the detection limit of this method is 5 mg/kg, and the lower limit of determination is 20.0 mg/kg.
2 Principle of the method
Using the method of total decomposition of hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid, the mineral lattice of the soil is destroyed, and all the elements to be tested in the sample are entered.
The test solution, and, during the digestion process, all chromium is oxidized to Cr2O72−. The digestion solution is then sprayed into a rich air-acetylene flame.
At the high temperature of the flame, a chromium ground state atom is formed, and selective absorption of the characteristic line emitted by the chromium hollow cathode lamp is 357.9 nm. in
The absorbance of chromium is determined under the optimal measurement conditions selected.
3 reagents and materials
The reagents used in this standard are applicable to the analytical purification reagents in accordance with national standards unless otherwise specified. The experimental water is newly prepared.
Deionized water or distilled water. The glassware used in the experiment should be washed first with detergent and then soaked with 1 1 nitric acid solution for 24 h (not allowed)
Wash with potassium dichromate), wash with tap water and deionized water before use.
3.1 Hydrochloric acid (HCl). ρ = 1.19 g/ml, excellent grade pure.
3.2 Hydrochloric acid solution, 1. 1. Prepared with (3.1).
3.3 Nitric acid (HNO3). ρ = 1.42 g/ml, excellent grade pure.
3.4 Hydrofluoric acid (HF). ρ = 1.49 g/ml.
3.5 10% ammonium chloride aqueous solution. accurately weigh 10 g ammonium chloride (NH4Cl), dissolve it with a small amount of water and transfer it into a 100 ml volumetric flask.
Make up to the mark with water and shake well.
3.6 Chromium standard stock solution, ρ =1.000 mg/ml. accurately weigh 0.282 9 g of reference potassium dichromate (K2Cr2O7) and dissolve it with a small amount of water.
Transfer the whole amount into a 100 ml volumetric flask, dilute to the mark with water, shake well, and store at 2-8 °C in the refrigerator for 6 months.
3.7 Chromium standard use solution, ρ = 50 mg/L. remove chromium standard stock solution (3.6) 5.00 ml in a 100 ml volumetric flask, add water to volume
Line, shake evenly, ready to use.
3.8 Perchloric acid (HClO4). ρ = 1.68 g/ml, excellent grade.
4 Instruments and equipment
4.1 Instrumentation
Atomic absorption spectrophotometer, chrome hollow cathode lamp, microwave digestion instrument, agate grinding machine, etc.
4.2 Instrument parameters
The best measurement conditions for different types of instruments are different and can be selected according to the instruction manual of the instrument. Usually this standard uses the test in Table 1.
The amount of conditions, the microwave digestion instrument uses the temperature rise program in Table 2.
Table 1 Instrument measurement conditions
Element Cr
Determination wavelength/nm 357.9
Passband width/nm 0.7
Flame property reduction
Sub-sensitive line/nm 359.0; 360.5; 425.4
The burner height is 8 mm (the hollow cathode light spot is passed through the bright blue part of the flame)
Table 2 Microwave digestion device heating program
Heating time/min digestion temperature/°C retention time/min
5.0 120 1.0
3.0 150 5.0
4.0 180 10.0
6.0 210 30.0
5 interference and elimination
5.1 Chromium is easy to form high temperature resistant oxide, its atomization efficiency is greatly affected by flame state and burner height, and it is necessary to use rich combustion.
(reducing) flame.
5.2 Addition of ammonium chloride can inhibit the interference of coexisting ions such as iron, cobalt, nickel, vanadium, aluminum, magnesium and lead.
6 samples
6.1 Acquisition and preservation
The collected soil samples (generally not less than 500 g) are mixed and divided by a quarter method to about 100 g. The soil sample after shrinking is air dried (since
After air drying or freeze-drying, remove foreign matter such as stones and animal and plant residues in the soil sample, and grind with a wooden rod (or agate stick) through 2 mm.
Nylon sieve (remove more than 2 mm of gravel) and mix. Grind the soil sample through a 2 mm nylon sieve to a total of 100 with an agate mortar
A mesh (pore size 0.149 mm) nylon mesh was mixed and ready for use.
6.2 Preparation of samples
6.2.1 Total digestion method
Accurately weigh 0.2 to 0.5 g (accurate to 0.000 2 g) of the sample in 50 ml of Teflon, wet with water and add 10 ml.
Hydrochloric acid (3.1) is heated at a low temperature on a hot plate in a fume hood to preliminarily decompose the sample. When it is evaporated to about 3 ml, it is slightly cold.
Then add 5 ml of nitric acid (3.3), 5 ml of hydrofluoric acid (3.4), 3 ml of perchloric acid (3.8), cover and heat at medium temperature on the hot plate for 1 h.
Left and right, then open the cover, the temperature of the hot plate is controlled at 150 °C, continue to heat the silicon removal, in order to achieve a good flying silicon effect, it should be shaken frequently
crucible. When heated to a thick white smoke of perchloric acid, it is capped to decompose the black organic carbide. After the black organic matter on the wall disappears,
Open the lid, drive away the white smoke and steam until the contents are sticky. According to the digestion, 3 ml of nitric acid (3.3) and 3 ml of hydrofluoric acid (3.4) can be added.
1 ml perchloric acid (3.8), repeat the above digestion process. Remove the sputum and let it cool slightly. Add 3 ml of hydrochloric acid solution (3.2) to dissolve the soluble residue.
Transfer the slag to the 50 ml volumetric flask and add 5 ml of ammonium chloride solution (3.5). After cooling, dilute to the mark with water and shake well.
6.2.2 Microwave digestion
Accurately weigh 0.2 g (accurate to 0.000 2 g) of the sample in a microwave digestion tank, wet with a small amount of water and add 6 ml of nitric acid (3.3), 2
Ml hydrofluoric acid (3.4), digested according to a certain heating procedure, after cooling, transfer the solution to 50 ml of polytetrafluoroethylene hydrazine, add 2
Ml Perchloric acid (3.8), the temperature of the hot plate is controlled at 150 ° C, the white smoke is driven away and steamed until the contents are viscous. Remove the cockroach and add a little salt
Acid solution (3.2) 3 ml, dissolve the soluble residue warmly, transfer the whole amount to a 50 ml volumetric flask, and add 5 ml of NH4Cl solution (3.5).
After cooling, make up to the mark and shake well.
Due to the variety of soils, the organic matter contained in the machine has a large difference. When dissolving, it should be observed. The amount of various acids can be visualized.
Increase or decrease of the situation; the temperature of the hot plate should not be too high, otherwise the Teflon will be deformed; when the sample is digested, it needs special during the steaming to near dry process.
Be careful to prevent evaporation, otherwise the elements to be tested will be lost.
7 Analysis steps
7.1 Calibration curve
Accurately remove the chromium standard solution (3.7) 0.00, 0.50, 1.00, 2.00, 3.00, 4.00 ml in a 50 ml volumetric flask, then
Add 5 ml NH4C1 solution (3.5), 3 ml hydrochloric acid solution (3.2), dilute to the mark with water, shake well, and the mass concentration of chromium
Do not be 0.50, 1.00, 2.00, 3.00, 4.00 mg/L. This mass concentration range should include the mass concentration of chromium in the test solution. Press the instrument in 4.2
The measurement conditions were determined by the absorbance of the standard solution from low to high quality concentration.
A calibration curve is drawn by subtracting the absorbance of the blank from the corresponding mass concentration of chromium (mg/L).
7.2 Blank test
Deionized water is used instead of the sample, and the same procedure and reagents as in the test solution are prepared to prepare a full-program blank solution, which is the same as 7.1.
The conditions were measured. Prepare at least 2 blank solutions for each batch of samples.
7.3 Determination
Take an appropriate amount of test solution and measure the absorbance of the test solution under the same conditions as in 7.1. The chromium mass concentration was found on the calibration curve from the absorbance value.
Perform an instrument zero calibration for every 10 samples measured and inhale 1.00 mg/L of standard solution to check if sensitivity has occurred.
Variety.
8 Calculation of results
The chromium content of the soil sample w (mg/kg) is calculated by the following formula.
w =
(1 )
Mf
ρ ×
× −
Where. ρ - absorbance of the test solution minus the absorbance of the blank solution, and then find the mass concentration of chromium on the calibration curve, mg/L;
V--the volume of the test solution to a constant volume, ml;
M--weigh the weight of the sample, g;
F--the content of moisture in the sample, %.
9 Precision and accuracy
9.1 The results of this method for the analysis of the precision of chromium in the ESS series of soil standards are shown in Table 3.
Table 3 Precision test results of the method
Soil standard digestion method guaranteed value/(mg/kg)
average value/
(mg/kg) standard deviation
The relative standard deviation/
ESS-4 Total Resolution 66.3 1.99 3.0
ESS-4 microwave digestion
70.4±4.9
65.4 3.01 4.6
GSD-4 total digestion method 75.8 1.82 2.4
GSD-4 microwave digestion
81.0±6.0
75.2 2.56 3.4
9.2 Multiple laboratories This method is used to analyze the precision and accuracy of chromium in ESS series soil standards. The experimental results are shown in Table 4.
Table 4 Precision and Accuracy of the Method Experimental Results
Soil standard laboratory number guaranteed value/total mean/indoor relative standard deviation/inter-room relative standard deviation/relative error /
(mg/kg) (mg/kg) % % %
ESS-1 16 57.2±4.2 56.1 2.0 9.8 −1.9
ESS-3 18 98.0±7.1 93.2 2.3 8.3 −4.9
9.3 In the case of total digestion (hydrochloric acid hydrofluoric acid perchloric acid), the standard soil sample recovery rate is 88% to 94%, microwave plus electric heating plate elimination
In the case of solution (hydrofluoric acid perchloric acid), the recovery rate of standard soil samples is 90% to 100%.
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