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HJ 680-2013: Soil and sediment. Determination of mercury, arsenic, selenium, bismuth, antimony. Microwave dissolution/Atomic Fluorescence Spectrometry
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 ...