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HJ 1080-2019: Soil and sediment--Determination of thallium--Graphite furnace atomic absorption spectrophotometry
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Soil and sediment--Determination of thallium--Graphite furnace atomic absorption spectrophotometry
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HJ 1080-2019
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Basic data | Standard ID | HJ 1080-2019 (HJ1080-2019) | | Description (Translated English) | Soil and sediment--Determination of thallium--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 | 11,152 | | Date of Issue | 2019 | | Date of Implementation | 2020-06-30 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1080-2019: Soil and sediment--Determination of thallium--Graphite furnace atomic absorption spectrophotometry
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
5.10 Ascorbic acid solution. ρ (C6H8O6) = 30 g/L.
Weigh 3 g of ascorbic acid (5.5), dilute with water and make up to 100 ml. Provisional use.
5.11 铊 Standard stock solution. ρ (Tl) = 100 μg/ml.
Accurately weigh 0.1 g (accurate to 0.1 mg) metal rhenium (5.6) and heat to dissolve in 20 ml nitric acid solution (5.7).
After cooling, dilute to 1000 ml with water. Commercially available certified standard solutions can also be purchased directly. Keep refrigerated at 4 ℃, valid period 2
year.
5.12 铊 Standard intermediate solution. ρ (Tl) = 1.00 μg/ml.
Accurately measure 1.00 ml of standard stock solution (5.11) in a 100 ml volumetric flask and dilute it with nitric acid solution (5.8) to
Mark the line and shake well. Keep refrigerated at 4 ℃, valid for 1 year.
5.13 铊 Standard solution. ρ (Tl) = 100 μg/L.
Accurately measure 10.00 ml of 铊 standard intermediate solution (5.12) in a 100 ml volumetric flask and dilute with a nitric acid solution (5.8)
To the mark, shake well. Provisional use.
5.14 Filter. 0.45 µm water-based microporous filter.
5.15 Argon. Purity ≥99.9%.
6 Instruments and equipment
6.1 Graphite furnace atomic absorption spectrophotometer. with background correction function.
6.2 Light source. Xie Rui line light source or continuous light source.
6.3 Pyrolytic coated graphite tube.
6.4 Microwave digestion device (power above 1200 W).
6.5 Electric heating plate. with temperature control function.
6.6 Agate mortar or ball mill.
6.7 Analytical balance. Sensitivity is 0.1 mg.
6.8 Nylon screen. 0.15 mm (100 mesh).
6.9 Instruments and equipment commonly used in general laboratories.
7 samples
7.1 Sample collection and storage
Collection and preservation of soil samples in accordance with the relevant provisions of HJ/T 166 and HJ 25.2; in accordance with GB 17378.3
Collection and preservation of marine sediment samples according to relevant regulations; in accordance with relevant regulations of HJ/T 91, HJ/T 166 and HJ 494
Collection and storage of water sediment samples.
7.2 Sample preparation
According to the requirements of HJ/T 166 and GB 17378.3, the foreign matter such as sticks, leaves, stones, etc. in the sample will be removed and collected.
The samples were air-dried, coarsely ground, and finely ground to a nylon sieve (6.8) in the laboratory.
7.3 Moisture determination
Determine the dry matter content of soil samples (7.2) according to HJ 613, and determine the sediment samples (7.2) according to GB 17378.5
Moisture content.
7.4 Preparation of test specimens
7.4.1 Hot plate digestion method
Accurately weigh 0.2 g to 0.5 g (accurate to 0.1 mg) of the sample in a 50 ml PTFE crucible, add 2 to 3 drops
After wetting the sample with water, add 10 ml of nitric acid (5.1) and 3 ml of hydrofluoric acid (5.2), and cover with 160 ℃ ～ 180 ℃ until digestion is not obvious.
Black matter, if there are more black matter, add 2 ml of nitric acid (5.1) and 2 ml to 3 ml of hydrogen peroxide (5.3).
Digestion, repeat the above digestion process. Open the lid at 180 ℃ to catch the acid (to achieve a good acid catch effect, the crucible should be shaken frequently),
Steam to near dryness (contents are immobile and sticky). Remove the crucible and cool slightly, add 0.5 ml nitric acid (5.1), warm and dissolve
Dissolve the soluble residue, transfer to a 50 ml volumetric flask after cooling, make up to the mark with water, shake well, and leave the supernatant to be measured.
Or it can be tested after filtering through the filter membrane (5.14).
7.4.2 Microwave Digestion
Accurately weigh 0.2 g to 0.5 g (accurate to 0.1 mg) of the sample in a microwave digestion tank, add 5 ml of nitric acid (5.1),
3 ml hydrofluoric acid (5.2), digestion according to certain digestion conditions (Table 1), cool to room temperature after digestion
Transfer to a 50 ml PTFE crucible, wash the digestion tank and lid with a little water and pour it into the crucible. Place the crucible in
Heat the acid on a hot plate at 180 ° C (to achieve good acid resistance, shake the crucible often), and steam to dryness (contents
(Not flowing and sticky). If there is a black substance after microwave digestion, add 2 ml of nitric acid (5.1) and 2 ml to the crucible.
3 ml hydrogen peroxide (5.3), cover the reaction at 160 ℃ ~ 180 ℃ until there is no obvious black substance, open the cover at 180 ℃ to drive the acid to dryness.
Remove the crucible and cool slightly, add 0.5 ml nitric acid (5.1), dissolve the soluble residues warmly, transfer to a 50 ml capacity after cooling
In the bottle, make up to the mark with water, shake well, and leave the supernatant to be tested or filtered through the filter membrane (5.14) to be tested.
Note. The types of soil and sediment samples are complex, and the matrix is quite different. The amount of various acids, the temperature and time of digestion can be visually digested during digestion
The situation may increase or decrease as appropriate.
Table 1 Reference table for microwave digestion heating program
No. temperature/℃ heating time/min holding time/min
1 room temperature ～ 120 6 3
2 120 ～ 150 8 10
3 150 ～ 180 8 30
7.5 Preparation of blank sample
Follow the same procedure as for sample preparation (7.4) to prepare a blank sample.
8 Analysis steps
8.1 Instrument working conditions
The optimal measurement conditions for different models of instruments are different, which can be selected according to the instrument's instruction manual; refer to the measurement conditions for reference
Table 2.
Table 2 Instrument reference measurement conditions
Element Thallium (Tl)
Measurement wavelength (nm)
Lamp current (mA) 10.0
Passband width (nm) 0.5
Drying temperature (℃)/time (s) 85 ～ 120/55
Ashing temperature (℃)/time (s) 600/14
Atomization temperature (℃)/time (s) 2100/3
Elimination temperature (℃)/time (s) 2200/2
Is the gas out of phase
Argon flow rate (L/min) 3.0
Injection volume (µl) 10
Matrix improver (µl) Ascorbic acid 5 µl Palladium nitrate 5 µl
Buckle background fashion zeeman
8.2 Establishment of standard curve
Accurately take 0 ml, 2.50 ml, 5.00 ml, 10.00 ml, 15.00 ml, 20.00 ml, 25.00 ml 铊 Standard use
Solution (5.13) in a 50 ml volumetric flask, dilute with nitric acid solution (5.8) and shake well. The radon concentrations in this standard series are
The values are. 0 μg/L, 5.00 μg/L, 10.0 μg/L, 20.0 μg/L, 30.0 μg/L, 40.0 μg/L, 50.0 μg/L.
According to the instrument's reference measurement conditions (8.1), the matrix improver adopts advanced palladium nitrate solution (5.9), and then enters ascorbic acid.
The method of acid solution (5.10), from low concentration to high concentration injection and analysis. Mass concentration of radon in standard series solution
Is the abscissa, and the corresponding absorbance value is the ordinate, and a standard curve of radon is established.
Note. Standard series of other concentration levels can be prepared according to the sensitivity of the instrument or the concentration range of the sample.
8.3 Sample determination
The measurement of the sample (7.4) was performed under the same analysis conditions as the standard curve establishment (8.2). If the sample concentration exceeds
The standard curve range needs to be re-measured after dilution with nitric acid solution (5.8).
8.4 Determination of blank sample
The blank sample (7.5) was measured under the same analysis conditions as the sample measurement (8.3).
9 Calculation and representation of results
9.1 Calculation of results
9.1.1 Calculation of results for soil samples
The content of europium element w1 (mg/kg) in the soil sample was calculated according to formula (1).
1 1000dm
V Dw
mw
(1)
In the formula. w1--the content of thorium in soil samples, mg/kg;
ρ--mass concentration of thorium in the sample calculated from the standard curve, g/L;
V--constant volume of sample after digestion, ml;
D--the dilution factor of the sample;
m--weigh the mass of the soil sample, g;
wdm-dry matter content of soil sample,%.
9.1.2 Results calculation of sediment samples
The content of plutonium element w2 (mg/kg) in the sediment sample is calculated according to formula (2).
(2)
In the formula. w2-- content of thorium element in sediment sample, mg/kg;
ρ--mass concentration of thorium in the sample calculated from the standard curve, g/L;
V--constant volume of sample after digestion, ml;
D--the dilution factor of the sample;
m--weigh the mass of the sediment sample, g;
OHw 2-moisture content of sediment sample,%.
2 (1) 1000H O
V Dw
mw
9.2 Representation of results
The number of decimal places in the measurement result is consistent with the detection limit of the method, and a maximum of 3 significant digits are retained.
10 Precision and accuracy
10.1 Precision
Eight laboratories adopted microwave digestion for GSS-2, GSS-28, paddy soil (1.4 mg/kg), GSD-17,
GSD-19 and marine sediment (0.8 mg/kg) samples were tested in 6 replicates. Relative standard deviation range in the laboratory
0.06% to 12%, 0.80% to 9.2%, 2.2% to 5.9%, 2.4% to 6.6%, 1.6% to 7.9%, and 3.2% to 9.5%, respectively;
The inter-laboratory relative standard deviations were 14%, 5.7%, 17%, 4.2%, 5.5%, and 14%; the repeatability limits (r) were
0.2 mg/kg, 0.2 mg/kg, 0.1 mg/kg, 0.1 mg/kg, 0.1 mg/kg, and 0.1 mg/kg; reproducibility limit (R) points
They are 0.3 mg/kg, 0.3 mg/kg, 0.7 mg/kg, 0.2 mg/kg, 0.2 mg/kg and 0.4 mg/kg.
Eight laboratories adopted the hot plate digestion method for GSS-2, GSS-28, paddy soil (1.3 mg/kg), GSD-17,
GSD-19 and marine sediment (0.8 mg/kg) samples were tested in 6 replicates. Relative standard deviation range in the laboratory
0.06% to 14%, 2.1% to 11%, 2.3% to 7.1%, 0.04% to 8.5%, 1.6% to 7.4%, and 3.2% to 11%;
The inter-laboratory relative standard deviations were 12%, 4.9%, 11%, 4.8%, 4.2%, and 13%, respectively; the repeatability limits (r) were
0.2 mg/kg, 0.1 mg/kg, 0.2 mg/kg, 0.2 mg/kg, 0.1 mg/kg, and 0.1 mg/kg; reproducibility limit (R) points
They are 0.3 mg/kg, 0.2 mg/kg, 0.5 mg/kg, 0.3 mg/kg, 0.2 mg/kg and 0.3 mg/kg.
10.2 Accuracy
Eight laboratories conducted microwave digestion on GSS-2, GSS-28, GSD-17, and GSD-19 standard samples.
6 repeated determinations. the relative error ranges in the laboratory are -18% to 23%, -12% to 7.5%, -10% to 0.72%, and
-9.1% ~ 6.5%; the average relative errors among the laboratories were 1.4%, -2.5%, -4.1%, and -0.80%; the relative errors were final
The values were 1.4% ± 30%, -2.5% ± 11%, -4.1% ± 7.8%, and -0.80% ± 11%.
Eight laboratories used GSA-2, GSS-28, GSD-17 and GSD-19 standard samples
Six repeated determinations. The relative error ranges in the laboratory were -19% to 18%, -10% to 2.5%, -5.8% to 5.8%, and
-5.2% ～ 5.2%; the average relative errors among the laboratories are 0.43%, -3.4%, -2.4%, and 0.32%; the relative errors are finally
The values were 0.43% ± 26%, -3.4% ± 7.6%, -2.4% ± 10%, and 0.32% ± 8.6%.
Eight laboratories use microwave digestion for actual samples of soil and sediments containing radon content of 1.4 mg/kg and 0.8 mg/kg
Analysis of products with spikes. The spiked recoveries range from 85.0% to 113% and 80.0% to 122%, respectively.
The final values were 97.8% ± 17.4% and 95.9% ± 32.6%.
Eight laboratories used electric hot plate digestion for soil and sediment with thorium content of 1.3 mg/kg and 0.8 mg/kg
Samples were spiked for analysis. The spiked recoveries ranged from 90.0% to 109% and 83.0% to 122%, respectively.
The final values were 100% ± 14.3% and 100% ± 29.4%.
11 Quality Assurance and Quality Control
11.1 At least two blank samples should be made for each batch of samples, and the measurement results should not exceed the method detection limit.
11.2 A standard curve shall be established for each analysis, and the correlation coefficient of the standard curve shall be ≥0.995. Every 20 samples analyzed, one should be analyzed
The relative error between the middle concentration point of the secondary standard curve and the standard value should be within ± 10%.
11.3 Measure one parallel sample every 20 samples or batch samples (less than 20 samples/batch).
The relative deviation should be ≤25%.
11.4 Determine one soil/sediment standard sample every 20 samples or batch samples (less than 20 samples/lot)
The relative error between the determination result and the standard value should be within ± 25%. Or measure 1 matrix spiked sample, the spiked recovery should be within
70% to 140%.
12 Waste treatment
The waste generated during the experiment should be collected in a centralized manner, be labeled accordingly, and be entrusted to a qualified unit for processing.
13 Notes
The introduction of chlorine-containing substances should be avoided during the sample digestion, storage and preparation of standard solutions during the experiment.
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