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HJ 737-2015: Soil and sediment. Determination of total beryllium. Graphite furnace atomic absorption spectrophotometry
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Soil and sediment. Determination of total beryllium. Graphite furnace atomic absorption spectrophotometry
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HJ 737-2015
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Basic data | Standard ID | HJ 737-2015 (HJ737-2015) | | Description (Translated English) | Soil and sediment. Determination of total beryllium. Graphite furnace atomic absorption spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Classification of International Standard | 13.080 | | Word Count Estimation | 8,877 | | Date of Issue | 2015-02-07 | | Date of Implementation | 2015-04-01 | | Quoted Standard | GB 17378.3; GB 17378.5; HJ 613; HJ/T 91; HJ/T 166 | | Regulation (derived from) | Ministry of Environmental Protection Announcement 2015 No. 7 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the determination of beryllium in soil and sediments by graphite furnace atomic absorption spectrophotometry. This Standard applies to the determination of beryllium in soil and sediments. When weighed 0.2g sample digestion, the volume to 50ml, the detection limit of this method is 0.03mg/kg, detection limit of 0.12mg/kg. | HJ 737-2015: Soil and sediment. Determination of total beryllium. Graphite furnace atomic absorption spectrophotometry
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Soil and sediment. Determining of total beryllium.Graphite furnace atomic absorption spectrophotometry
National Environmental Protection Standard of the People 's Republic of China
Determination of beryllium in soil and sediments
Graphite Furnace Atomic Absorption Spectrophotometry
Soil and sediment-Determination of total beryllium-Graphite furnace
Atomic absorption spectrophotometry
Released in.2015-02-07
2015-04-01 implementation
Issued by the Ministry of Environmental Protection
I directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples .2
8 Analysis steps
The results are calculated and expressed
10 Precision and Accuracy 4
11 Quality assurance and quality control
12 Waste treatment 5
13 Precautions 5
Foreword
To implement the "Environmental Protection Law of the People's Republic of China" to protect the environment, protect human health, regulate soil, sediment
Beryllium determination method, the development of this standard.
This standard specifies the determination of beryllium in soil and sediments by graphite furnace atomic absorption spectrophotometry.
This standard is the first release.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. China Environmental Monitoring Station, Nanjing Environmental Monitoring Center Station.
The standard verification unit. Tianjin Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Center, Henan Province Environmental Monitoring Center,
Guangdong Province Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Changzhou Environmental Monitoring Center, Jiangsu Province Physical and Chemical Analysis and Testing
center.
This standard is approved by the Ministry of Environmental Protection on February 7,.2015.
This standard is implemented as of April 1,.2015.
This standard is explained by the Ministry of Environmental Protection.
Determination of beryllium in soil and sediments - Graphite furnace atomic absorption spectrophotometric method
Warning. The beryllium standard solution used in the experiment is highly toxic chemicals, perchloric acid, nitric acid with corrosive and strong oxidizing properties,
Hydrochloric acid, hydrofluoric acid with strong volatile and corrosive, the operation should be required to wear protective equipment, solution preparation and sample preparation
The process should be carried out in a fume hood.
1 Scope of application
This standard specifies the determination of beryllium in soil and sediments by graphite furnace atomic absorption spectrophotometry.
This standard applies to the determination of beryllium in soil and sediments. When weigh 0.2 g sample digestion, constant volume to 50 ml when this method
The detection limit was 0.03 mg/kg and the lower limit was 0.12 mg/kg.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version is applicable
In this standard.
Specification for ocean monitoring - Part 3. Sample collection, storage and transport
Specification for marine monitoring - Part 5. Sediment analysis
Determination of Dry Matter and Moisture in Soil
Technical specification for surface water and wastewater monitoring
Technical specification for soil environmental monitoring
3 Principle of the method
Soil or sediment is digested and injected into a graphite furnace atomizer, dried, ashed and atomized, beryllium compound
The absorption intensity of 234.9 nm characteristic lines is proportional to the concentration of beryllium in a certain range.
4 interference and elimination
20 mg/L of iron had a negative effect on the determination of beryllium; 75 mg/L of magnesium had a positive effect on the determination of beryllium. Adding palladium chloride
Body modifier that eliminates interference.
5 reagents and materials
Unless otherwise stated, analytical analytical reagents conforming to national standards are used for the analysis of freshly prepared deionized water
Or the same purity of water.
5.1 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.2 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 hydrofluoric acid. ρ (HF) = 1.49 g/ml, excellent grade pure.
5.4 perchloric acid. ρ (HClO4) = 1.68 g/ml, excellent grade pure.
5.5 Nitric acid solution. 1 1, prepared with (5.2).
5.6 Nitric acid solution. 5 95, prepared with (5.2).
5.7 Nitric acid solution. 1 99, prepared with (5.2).
5.8 beryllium standard Huaihu liquid. ρ (Be) = 100 mg/L.
2 using a commercially available standard solution or accurately weighing 1.9660 g of beryllium sulfate (BeSO4 · 4H2O), with a small amount of water dissolved after the full amount
Into the 1000 ml volumetric flask, add 10 ml nitric acid (5.2), water volume to the mark, shake.
5.9 Beryllium Standard Intermediate. ρ (Be) = 1.00 mg/L.
Accurate to learn 1.00ml beryllium standard stock solution (5.8) in 100 ml volumetric flask, with nitric acid solution (5.7) constant volume to the mark, shake.
5.10 beryllium standard use of liquid. ρ (Be) = 10.0 μg/L.
Accurately absorb 1.00 ml of standard intermediate (5.9) in 100 ml volumetric flask, with nitric acid solution (5.7) constant volume to the mark, shake.
Pro is now available.
5.11 palladium chloride solution, ρ (PdCl2) = 17.0 g/L.
Weigh 1.70 g of palladium chloride, dissolved in nitric acid solution (5.6) at low temperature and fixed to 100 ml.
5.12 argon. purity ≥99.99%.
6 instruments and equipment
6.1 graphite furnace atomic absorption spectrophotometer, with background correction function.
6.2 beryllium hollow cathode lamp.
6.3 Graphite tube. Pyrolytic coated graphite tube (commercially available).
6.4 microwave digestion device.
6.5 Electric plate. with temperature control function.
6.6 Teflon crucible.
6.7 Common laboratory equipment and equipment.
7 samples
7.1 Sample collection and storage
According to the relevant provisions of HJ/T 166 collection and preservation of soil samples; in accordance with GB 17378.3 and HJ/T 91 of the relevant provisions of mining
Set and store sediment samples.
7.2 Sample preparation
According to the requirements of HJ/T 166 and GB 17378.3, the collected samples were air-dried, coarsely and finely ground in the laboratory
Pore size 0.15 mm (100 mesh) sieve. Sample collection, transport, preparation and preservation should avoid contamination and loss of element to be measured.
7.3 Sample preparation
7.3.1 Electric plate digestion method
Weigh the sample 0.1 ~ 0.3 g (accurate to 0.1 mg) in 50 ml polytetrafluoroethylene crucible, wet with water and add l0 ml
Hydrochloric acid (5.1), in the fume hood on the hot plate at low temperature (95 ± 5 ℃) heating, so that the initial decomposition of the sample, to be evaporated to about 3 ml
(5.2), 5 ml of hydrofluoric acid (5.3), capped on the hot plate at the temperature (120 ± 5 ℃) heating 0.5 ~ 1 h,
After cooling, add 2 ml of perchloric acid (5.4), capped at medium temperature for 1 h, open the cover fly silicon (in order to achieve good flying silicon effect, should
Often shake the crucible), when heated to take a thick perchloric acid white smoke, stamped, so that the black organic carbide decomposition. To be on the wall of the crucible
Black organic matter disappeared, open the lid, drive white smoke (temperature control at 140 ± 5 ℃) and steamed to near dry (hot observation of the content was
Non-flowing liquid beads). As the digestion, can add 3 ml of nitric acid (5.2), 3 ml of hydrofluoric acid (5.3), 1 ml
Perchloric acid (5.4), repeat the above digestion process. Remove the crucible slightly cold, add 1 ml of nitric acid solution (5.5), warm dissolved can be
Soluble residue, transferred to 50 ml volumetric flask, the water volume to the mark, shake, stored in the polyethylene bottle.
Some soil and sediment organic matter content is high, should increase the amount of nitric acid; in the digestion process, should pay attention to observe, the
3 kinds of acid dosage and digestion time visualization of the situation as appropriate increase or decrease; hot plate temperature should not be too high to prevent the polytetrafluoroethylene crucible change
Shape and sample evaporated.
7.3.2 Microwave digestion method
Weigh the sample 0.1 ~ 0.3 g (accurate to 0.1 mg) in the microwave digestion tank, with a small amount of water wet after adding 6 ml of nitric acid (5.2)
2 ml hydrochloric acid (5.1), 2 to 5 ml hydrofluoric acid (5.3), digested according to a certain warming procedure (see Table 1), after cooling (or
Transfer the solution to 50 ml of polytetrafluoroethylene crucible) Add 1.0 ml of perchloric acid (5.4), heat on a hot plate,
System at 150 ° C, heated to take a thick perchloric acid white smoke and the contents were not flow state, remove the crucible slightly cold, add 1 ml of nitrate
Acid solution (5.5), dissolve the soluble residue in warm, transfer to 50 ml volumetric flask, water volume to the mark, shake, save in
Polyethylene bottle.
Table 1 Microwave digestion temperature program reference table
Heating time (min) Digestion temperature (℃) Holding time (min)
7 room temperature ~ 120 3
5 120 ~ 160 3
5 160 ~ 190 25
7.4 Preparation of laboratory blanks
Instead of the sample with deionized water, the same procedure and reagents were prepared using the sample to prepare a laboratory blank.
7.5 Determination of dry matter content and moisture content of samples
The dry matter content of soil samples was determined according to HJ 613. The moisture content of the sediment samples was determined according to GB 17378.5.
8 Analysis steps
8.1 Instrument reference measurement conditions
According to the instrument specification requirements to select the measurement conditions, the instrument reference measurement conditions in Table 2.
Table 2 Instrument reference measurement conditions
Element Be
Determination of wavelength (nm) 234.9
Passband width (nm) 0.5
Drying temperature (℃)/time (s) 85 ~ 120/55
Ashing temperature (℃)/time (s) 1200 ~ 1400/10 ~ 15
Atomization temperature (℃)/time (s) 2600/2.9
Clear temperature (℃)/time (s) 2650/2
Whether the atomic phase is stopped
Argon flow rate (ml/min) 300
Injection volume (μl) 20 (autosampler or manual injection)
Substrate modifier addition (μl) 2
8.2 Calibration curve
Accurate removal of beryllium standard use of liquid (5.10) 0.00,0.50,1.00,2.00,3.00,4.00 ml in 10 ml volumetric flask,
4 with nitric acid solution (5.7) constant volume shake. The concentration of beryllium in this standard series is 0,0.50,1.00,2.00,3.00,4.00 μg/L.
According to the instrument measurement conditions (8.1), from the low concentration to high concentration followed by adding 20 μl of the standard solution to the graphite tube and 2 μl of the base solution
Addition (5.11), measuring absorbance. With the corresponding absorbance as the ordinate to beryllium standard series of mass concentration for the abscissa, drawing beryllium
Of the calibration curve.
8.3 Determination
The laboratory blank and the absorbance of the sample were measured under the same conditions as the calibration curve. By the absorbance value in the calibration song
Check the beryllium content online. If the sample is diluted before the measurement, the measurement result should be multiplied by the corresponding dilution factor.
9 Results calculation and representation
9.1 Results calculation
9.1.1 Calculation of soil samples
The content of beryllium in the soil ω1 (mg/kg) calculated according to formula (1).
) (
Dmwm
V (1)
Where. 1 - the content of beryllium in the soil, mg/kg;
- Check the calibration curve to determine the mass concentration of beryllium in the test solution, μg/L;
0 - mass concentration of beryllium in blank solution, μg/L;
V - the volume of the sample volume, ml;
M - the quality of the sample, g;
Dmw - dry matter content of soil samples,%.
9.1.2 Calculation of the results of sediment samples
Sediment beryllium content ω2 (mg/kg) calculated according to formula (2).
2 10) 1 (
) (
Fm
V (2)
Where. 2 - the content of beryllium in the sediment, mg/kg;
- Mass concentration of beryllium in the test solution from the calibration curve, μg/L;
0 - mass concentration of beryllium in blank solution, μg/L;
V - the volume of the sample volume, ml;
M - the quality of the sample, g;
F - sediment sample moisture,%.
9.2 The result is shown
When the determination result is less than 1.00 mg/kg, two digits after the decimal point are retained; when the result is greater than or equal to 1.00 mg/kg,
Keep three valid digits.
10 precision and accuracy
10.1 Precision
5 laboratory tests were carried out on the actual soil samples (chernozem) and sediment samples (Songhua River sediments)
(N = 6), the results show that.
The relative standard deviations in the laboratory range from 2.8% to 12% and 1.2% to 9.1%, respectively;
The relative standard deviations were 7.3% and 8.4%, respectively.
The reproducibility limits (r) were 0.465 mg/kg and 0.419 mg/kg, respectively;
Reproducibility limits (R) were 0.665 mg/kg and 0.736 mg/kg, respectively.
10.2 Accuracy
Seven samples of soil were tested for soil standard samples with a concentration of 2.0 ± 0.4 mg/kg and a concentration of 1.8 ± 0.3 mg/kg
The relative error of the standard samples is -18% ~ 9.2% and -13% ~ 13% respectively. The mean values of the relative errors are
(-5.7% ± 22%) and (0.8% ± 17.6%).
11 quality assurance and quality control
11.1 each batch of samples at least two laboratory blanks, the determination of the results should be lower than the lower limit of determination.
11.2 Each batch of samples need to be calibrated curve, with a linear fitting curve calibration, the correlation coefficient should be greater than 0.995.
11.3 each batch of samples at least 10% of the proportion of parallel parallel sample determination, the number of samples less than 10, should be measured at least one level
Line, the relative deviation of the measured results is generally not more than 20%.
11.4 After measuring 10 samples and after analysis, the calibration blank and a standard point in the middle of the calibration curve should be determined to ensure that the standard
The change of the measured value is not more than 10%.
11.5 Each batch of samples is randomly inserted at least 10% of the proportion of soil or sediment samples were measured, the number of samples less than 10
, A standard sample should be measured at least to control the accuracy of the sample assay.
12 Waste treatment
The waste solution produced in the experiment should be collected and commissioned by qualified units for processing.
13 Precautions
13.1 The glassware used in the experiment shall be washed with detergent and then soaked with (14) nitric acid solution for 24 h before use
Tap water, deionized water washed. For new containers, the corresponding blank check should be used before use.
13.2 Preparation of standard solution and preparation of samples should use the same batch of reagents.
13.3 In order to extend the life of the graphite tube, the amount of nitric acid added after digestion, depending on the requirements of different instruments may be appropriate to adjust.
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