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HJ 680-2013 PDF in English


HJ 680-2013 (HJ680-2013) PDF English
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HJ 680-2013: PDF in English

HJ 680-2013
HJ
NATIONAL ENVIRONMENTAL PROTECTION STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Soil and sediment - Determination of mercury, arsenic,
selenium, bismuth, antimony - Microwave
dissolution/Atomic Fluorescence Spectrometry
ISSUED ON: NOVEMBER 21, 2013
IMPLEMENTED ON: FEBRUARY 01, 2014
Issued by: Ministry of Environmental Protection
Table of Contents
Foreword ... 5
1 Scope of application ... 6
2 Normative references ... 6
3 Principle of the method ... 6
4 Reagents and materials ... 7
5 Instruments and devices ... 10
6 Samples ... 10
7 Analysis steps ... 12
8 Calculation and presentation of results ... 14
9 Precision and accuracy ... 15
10 Quality assurance and quality control ... 16
11 Waste disposal ... 16
12 Precautions ... 16
Appendix A (informative) Summary data of precision and accuracy ... 18
Soil and sediment - Determination of mercury, arsenic,
selenium, bismuth, antimony - Microwave
dissolution/Atomic Fluorescence Spectrometry
1 Scope of application
This Standard specifies the microwave dissolution/atomic fluorescence spectrometry
for the determination of mercury, arsenic, selenium, bismuth, and antimony in soil and
sediment.
This Standard applies to the determination of mercury, arsenic, selenium, bismuth, and
antimony in soil and sediment.
When the sample size is 0.5 g, for mercury, the detection limit of this method is 0.002
mg/kg, and the lower limit of determination is 0.008 mg/kg; for arsenic, selenium,
bismuth, and antimony, the detection limit is 0.01 mg/kg, and the lower limit of
determination is 0.04 mg/kg.
2 Normative references
This Standard refers to the following documents or their clauses. For undated references,
the latest edition applies to this Standard.
GB 17378.3 The specification for marine monitoring - Part 3: Sample collection
storage and transportation
GB 17378.5 The specification for marine monitoring - Part 5: Sediment analysis
GB/T 21191 Atomic fluorescence spectrometer
HJ/T 166 Technical specification for soil environmental monitoring
HJ 613 Soil - Determination of dry matter and water content - Gravimetric method
3 Principle of the method
After the sample is dissolved by microwave, the test solution enters the atomic
fluorescence spectrometer; under the reducing action of potassium borohydride solution,
arsine, bismuth hydrogen, antimony hydrogen and hydrogen selenide gas are generated,
and mercury is reduced to atomic state. Ground-state atoms are formed in the hydrogen-
hydrogen flame, and atomic fluorescence is generated under the excitation of light
emitted by element lamps (mercury, arsenic, selenium, bismuth, antimony). The atomic
fluorescence intensity is proportional to the element content in the test solution.
4 Reagents and materials
Unless otherwise specified, the analysis is performed using guarantee reagents that
comply with national standards, and the experimental water is freshly prepared distilled
water.
4.1 Hydrochloric acid (HCl), ρ = 1.19 g/ml.
4.2 Nitric acid (CHNO3), ρ = 1.42 g/ml.
4.3 Potassium hydroxide (KOH).
4.4 Potassium borohydride (KBH4).
4.5 Hydrochloric acid solution: 5 + 95.
PIPETTE 25 ml of hydrochloric acid (4.1) and DILUTE to 500 ml with experimental
water.
4.6 Hydrochloric acid solution: 1 + 1.
PIPETTE 500 ml of hydrochloric acid (4.1) and DILUTE to 1000 ml with experimental
water.
4.7 Thiourea (CH4N2S): analytical reagent.
4.8 Ascorbic acid (C6H8O6): analytical reagent.
4.9 Reducing agents:
4.9.1 Potassium borohydride solution A: ρ = 10 g/L.
WEIGH 0.5 g of potassium hydroxide (4.3); PUT it in a beaker containing 100 ml of
experimental water; STIR with a glass rod until completely dissolved; ADD 1.0 g of
potassium borohydride (4.4); STIR to dissolve. This solution is prepared on the day of
use for the determination of mercury.
4.9.2 Potassium borohydride solution B: ρ = 20 g/L.
WEIGH 0.5 g of potassium hydroxide (4.3); PUT it in a beaker containing 100 ml of
experimental water; STIR with a glass rod until completely dissolved; ADD 2.0 g of
potassium borohydride (4.4); STIR to dissolve. This solution is prepared on the day of
use for the determination of arsenic, selenium, bismuth, and antimony.
4.13.3 Arsenic standard use solution: ρ = 100.0 μg/L.
PIPETTE 10.00 ml of arsenic standard intermediate solution (4.13.2); PLACE it in a
100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to
the marked line with experimental water; MIX well. Prepare before use.
4.14 Selenium (Se) standard solution.
4.14.1 Selenium standard stock solution: ρ = 100.0 mg/L.
PURCHASE commercially available certified reference materials/certified reference
samples, or WEIGH 0.1000 g of high-purity selenium powder; PLACE it in a 100 ml
beaker; ADD 20 ml of nitric acid (4.2); HEAT at low temperature until dissolved;
COOL to room temperature; TRANSFER to a 1000 ml volumetric flask; DILUTE to
the marked line with experimental water; MIX well.
4.14.2 Selenium standard intermediate solution: ρ = 1.00 mg/L.
PIPETTE 5.00 ml of selenium standard stock solution (4.14.1); PLACE it in a 500 ml
volumetric flask; DILUTE to the marked line with experimental water; MIX well.
4.14.3 Selenium standard use solution: ρ = 100.0 μg/L.
PIPETTE 10.00 ml of selenium standard intermediate solution (4.14.2); PLACE it in a
100 ml volumetric flask; DILUTE to the marked line with experimental water; MIX
well. Prepare before use.
4.15 Bismuth (Bi) standard solution.
4.15.1 Bismuth standard stock solution: ρ = 100.0 mg/L.
PURCHASE commercially available certified reference materials/certified reference
samples, or WEIGH 0.100 0 g of high-purity metal bismuth; PLACE it in a 100 ml
beaker; ADD 20 ml of nitric acid (4.2); HEAT at low temperature until completely
dissolved; COOL; TRANSFER to a 1000 ml volumetric flask; DILUTE to the marked
line with experimental water; MIX well.
4.15.2 Bismuth standard intermediate solution: ρ = l.00 mg/L.
PIPETTE 5.00 ml of bismuth standard stock solution (4.15.1); PLACE it in a 500 ml
volumetric flask; ADD 100 ml of hydrochloric acid solution (4.6); DILUTE to the mark
line with experimental water; MIX well.
4.15.3 Bismuth standard use solution: ρ = 100.0 μg/L.
PIPETTE 10.00 ml of bismuth standard intermediate solution (4.15.2); PLACE it in a
100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to
the marked line with experimental water; MIX well. Prepare before use.
4.16 Antimony (Sb) standard solution.
4.16.1 Antimony standard stock solution: ρ = 100.0 mg/L.
PURCHASE commercially available certified reference materials/certified reference
samples, or WEIGH 0.1197 g of antimony trioxide (Sb2O3) that has been dried at 105 °C
for 2 h; DISSOLVE it in 80 ml of hydrochloric acid (4.1); TRANSFER to a 1 000 ml
volumetric flask; ADD 120 ml of hydrochloric acid (4.1); DILUTE to the marked line
with experimental water; MIX well.
4.16.2 Antimony standard intermediate solution: ρ = 1.00 mg/L.
PIPETTE 5.00 ml of antimony standard stock solution (4.16.1); PLACE it in a 500 ml
volumetric flask; ADD 100 ml of hydrochloric acid solution (4.6); DILUTE to the
marked line with experimental water; MIX well.
4.16.3 Antimony standard use solution: ρ = 100.0 μg/L.
PIPETTE 10.00 ml of antimony standard intermediate solution (4.16.2); PLACE it in a
100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to
the marked line with experimental water; MIX well. Prepare before use.
4.17 Carrier gas and shielding gas: argon (purity ≥ 99.99 %).
4.18 Slow quantitative filter paper.
5 Instruments and devices
5.1 Microwave dissolution instrument with temperature control and temperature
programming functions, and the temperature accuracy can reach ±2.5 °C.
5.2 The atomic fluorescence spectrometer shall comply with the provisions of GB/T
21191, with elemental lamps of mercury, arsenic, selenium, bismuth, and antimony.
5.3 Constant temperature water bath apparatus.
5.4 Analytical balance: the accuracy is 0.000 1 g.
5.5 Common laboratory equipment.
6 Samples
6.1 Collection of samples
Collect soil samples according to the relevant provisions of HJ/T 166; collect sediment
samples according to the relevant provisions of GB 17378.3.
Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of arsenic standard
solution (4.13.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml
of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution
(4.10); PLACE at room temperature for 30 min (when the room temperature is lower
than 15 °C, place in a 30 °C water bath for 20 min); DILUTE to the marked line with
experimental water; MIX well.
(3) Calibration series for selenium
Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of selenium standard
solution (4.14.3); PLACE them in 50 ml volumetric flasks; respectively ADD 10.0
ml of hydrochloric acid (4.1); PLACE at room temperature for 30 min (when the
room temperature is lower than 15 °C, place in a 30 °C water bath for 20 min);
DILUTE to the marked line with experimental water; MIX well.
(4) Calibration series for bismuth
Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of bismuth standard
solution (4.15.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml
of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution
(4.10); DILUTE to the marked line with experimental water; MIX well.
(5) Calibration series for antimony
Respectively PIPETTE 0, 0.50, 1,00, 2.00, 3.00, 4.00, 5.00 ml of antimony standard
solution (4.16.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml
of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution
(4.10); PLACE at room temperature for 30 min (when the room temperature is lower
than 15 °C, place in a 30 °C water bath for 20 min); DILUTE to the marked line with
experimental water; MIX well.
See Table 4 for the concentrations of the calibration series solutions of mercury, arsenic,
selenium, bismuth, and antimony.
7.3 Plotting of calibration curve
Using potassium hydride solution (4.9.1 or 4.9.2) as the reducing agent and 5 + 95
hydrochloric acid solution (4.5) as the carrier, determine the atomic fluorescence
m - the mass of the sample to be weighed, g;
wdm - the dry matter content of the sample, %.
8.1.2 Calculation of results for sediment samples
The element (mercury, arsenic, selenium, bismuth, antimony) content w2 (mg/kg) in the
sediment is calculated according to formula (2):
where:
w2 - the element content in the sediment, mg/kg;
ρ - the mass concentration of the element in the test solution, obtained from the
calibration curve, μg/L;
ρ0 - the determined mass concentration of the element in the blank solution, μg/L;
V0 - the constant volume of the test solution after microwave dissolution, ml;
V1 - the volume of the divided test solution, ml;
V2 - the constant volume of the test solution determined after being divided, ml;
m - the mass of the sample to be weighed, g;
f - the moisture content of the sample, %.
8.2 Result presentation
When the determination result is less than 1 mg/kg, the number after the decimal point
shall be reserved up to three digits; when the determination result is greater than 1
mg/kg, three significant figures shall be reserved.
9 Precision and accuracy
9.1 Precision
Determined the reference samples of mercury, arsenic, selenium, bismuth, and
antimony by six laboratories, and the inner-laboratory relative standard deviations are
1.44 % ~ 11.7 % for mercury, 0.67 % ~ 8.91 % for arsenic, 0.79 % ~ 23.1 % for selenium,
1.47 % ~ 19.4 % for bismuth, and 1.83 % ~ 11.7 % for antimony; inter-laboratory
relative standard deviations are 3.42 % ~ 11.2 % for mercury, 3.14 % ~ 4.44 % for
arsenic, 3.92 % ~ 9.46 % for selenium, 4.92 % ~ 7.59 % for bismuth, and 3.35 % ~
9.95 % for antimony; repeatability limits are 0.003 ~ 0.006 mg/kg for mercury, 0.298 ~
3.03 mg/kg for arsenic, 0.013 ~ 0.025 mg/kg for selenium, 0.019 ~ 0.299 mg/kg for
bismuth, and 0.049 ~ 0.363 mg/kg for antimony; reproducibility limits are 0.003 ~
0.007 mg/kg for mercury, 0.320 ~ 3.55 mg/kg for arsenic, 0.017 ~ 0.029 mg/kg for
selenium, 0.019 ~ 0.485 mg/kg for bismuth, and 0.068 ~ 0.655 mg/kg for antimony.
The summary results of precision tests are detailed in Appendix A.
9.2 Accuracy
Determined the reference samples of mercury, arsenic, selenium, bismuth, and
antimony by six laboratories, and the relative errors are -12.5 % ~ 12.5 % for mercury,
-7.5 % ~ 4.7 % for arsenic, -25.0 % ~ 8.6 % for selenium, -12.7 % ~ 8.8 % for bismuth,
and -15.8 % ~ 11.1 % for antimony. The summary results of accuracy tests are detailed
in Appendix A.
10 Quality assurance and quality control
10.1 Measure at least 2 whole-process blanks for each batch of samples. The blank
samples shall use the same dissolution procedure as the samples, and the determination
results shall be lower than the lower limit of the method.
10.2 According to the batch size, for each batch of samples, it shall determine 1 ~ 2
reference material(s) containing target elements, and the determination results shall be
within the controllable range.
10.3 In each batch (less than 10) or every 10 samples, at least 10 % of the samples shall
be repeatedly dissolved.
10.4 If the sample dissolution process produces excessive pressure and causes pressure
release and destroys its closed system, the data of this sample shall not be used.
10.5 This Standard specifies that the correlation coefficient of the calibration curve shall
not be less than 0.999.
11 Waste disposal
The waste liquid generated during the experiment cannot be dumped at will, and shall
be entrusted to a qualified organization for disposal according to the provisions.
12 Precautions
12.1 Nitric acid and hydrochloric acid are highly corrosive, so the sample dissolution
process shall be carried out in a fume hood, and experimenters shall wear protective
devices.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.