HJ 702-2014Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony. MicrowaveDissolution/AtomicFluorescence Spectrometry (English PDF)
固体废物 汞、砷、硒、铋、锑的测定 微波消解原子荧光法
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Issued by
Ministry of Ecology and Environment
Level / Type
National · Mandatory
Issue date
September 2, 2014
Implementation date
November 1, 2014
Scope
HJ 702-2014 is the English-translated version of 固体废物 汞、砷、硒、铋、锑的测定 微波消解原子荧光法.
HJ 702-2014 — This standard specifies the microwave solid waste and solid waste leaching solution of mercury, arsenic, selenium, bismuth, antimony digestion/atomic fluorescence measurement Setting Method.
This standard applies to solid waste mercury, arsenic, selenium, bismuth, antimony and determination of solid waste leaching solution.
When the solid waste taken the sample size is 0.5g, the present method of mercury detection limit of 0.002µg/g, detection limit 0.008µg/g; arsenic, selenium, bismuth and antimony inspection the limit was 0.010µg/g, detection limit 0.040µg/g.
When the solid waste leachate sampling volume of 40ml, the mercury detection limit it was 0.02µg/L, detection limit 0.08µg/L; arsenic, selenium, bismuth, antimony detection limit is 0.10µg/L, detection limit 0.40µg/L.
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Document preview — HJ 702-2014
National Standard of the People's Republic of China
- Classification
- Z 27
Issued by: Ministry of Ecology and Environment
Contents
- Preface
- 1. Scope .1
- 2 Normative references .1
- 3 .1 The principle of the method
- 4 Reagents and materials
- 5 Apparatus and equipment
- Sample 4
- 7 Procedure .5
- 8 Results Calculation and representation .6
- 9 Precision and accuracy .7
Foreword
To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Solid Waste Pollution Prevention Law" Protecting the environment, safeguarding human health, regulate solid waste and solid waste leaching solution of mercury, arsenic, selenium, bismuth, antimony monitoring methods, Development of this standard.
This standard provides solid waste and solid waste leaching solution of mercury, arsenic, selenium, bismuth, antimony microwave digestion/Atomic Fluorescence Spectrometry test methods.
This standard is the first release.
Appendix A of this standard is an informative catalog.
This standard is developed by the Ministry of Environmental Protection Science, Technology organization.
This standard was drafted. Ningbo Municipal Environmental Monitoring Center.
The standard verification. Zhejiang Zhoushan Marine Ecological Environmental Monitoring Station, Jiaxing Municipal Environmental Protection Monitoring Station, Huzhou City Environment Conservation Monitoring Centre Station, Jinhua Municipal Environmental Monitoring Center, Taizhou City Environmental Monitoring Center, Ningbo Beilun District Environmental Protection supervisor ST.
This standard MEP September 3, 2014 for approval.
This standard since November 1, 2014 implementation.
The standard explanation by the Ministry of Environmental Protection.
Solid waste mercury, arsenic, selenium, bismuth, antimony determination Microwave Digestion/Atomic Fluorescence Spectrometry Warning. nitric acid used in the experiments, volatile and corrosive hydrochloric acid, the operation should be required to required to wear protective equipment, Solution preparation and sample pre-treatment process should be performed in a fume hood.
1 Scope
This standard specifies the microwave solid waste and solid waste leaching solution of mercury, arsenic, selenium, bismuth, antimony digestion/atomic fluorescence measurement Setting Method.
This standard applies to solid waste mercury, arsenic, selenium, bismuth, antimony and determination of solid waste leaching solution. When the solid waste taken the sample size is 0.5g, the present method of mercury detection limit of 0.002µg/g, detection limit 0.008µg/g; arsenic, selenium, bismuth and antimony inspection the limit was 0.010µg/g, detection limit 0.040µg/g. When the solid waste leachate sampling volume of 40ml, the mercury detection limit it was 0.02µg/L, detection limit 0.08µg/L; arsenic, selenium, bismuth, antimony detection limit is 0.10µg/L, detection limit 0.40µg/L.
2 Normative references
This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable for this standard.
GB/T 21191 atomic fluorescence spectrometer HJ/T 20 industrial solid waste sampling sample preparation Technical Specifications HJ/T 298 Identification of Hazardous Waste Technical Specifications HJ/T 299 methods for leaching toxicity of solid waste sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity Acetic acid buffer solution method HJ 557 solid waste leaching toxicity level oscillation method
3 PRINCIPLE OF THE METHOD
Solid waste and leachate samples after microwave digestion, atomic fluorescence into the instrument, wherein the arsenic, bismuth, antimony, selenium and mercury Element in the solution of potassium borohydride reduction to produce arsine, hydrogen bismuth, antimony, hydrogen, selenide and mercury vapor atoms.
These gases are excited by the formation of ground-state atoms in an argon hydrogen flame, the light elements (mercury, arsenic, selenium, bismuth, antimony) emitting light production Health atomic fluorescence spectrometry, atomic fluorescence intensity is proportional to the elements in the sample.
4 Reagents and materials
Unless otherwise indicated, the use of line with national standards for gifted class pure reagents analysis, test water is distilled water.
4.1 HCl. rho (HCl) = 1.19 g/ml.
Nitrate 4.2. rho (HNO3) = 1.42 g/ml.
4.3 Potassium hydroxide (KOH).
4.4 potassium borohydride (KBH4).
4.5 hydrochloric acid solution. 5 95 (v/v).
Measure 25ml of hydrochloric acid (4.1) diluted to 500ml with distilled water.
Hydrochloric acid solution was 4.6. 1 1 (v/v).
Measure 500ml of hydrochloric acid (4.1) diluted to 1000ml with distilled water.
4.7 thiourea (CH4N2S). AR.
4.8 ascorbic acid (C6H8O6). AR.
4.9 reductant.
4.9.1 potassium borohydride (KBH4) Solution A. = rho 10g/L.
Weigh 0.5g of potassium hydroxide (4.3) containing 100 ml of distilled water into a beaker, stirring until completely dissolved and then the glass rod Join the weighed 1.0g potassium borohydride (4.4), stirring to dissolve. This solution preparation day, for the determination of mercury.
4.9.2 potassium borohydride (KBH4) solution B. = rho 20g/L.
Weigh 0.5g of potassium hydroxide (4.3) containing 100 ml of distilled water into a beaker, stirring until completely dissolved and then the glass rod Join the weighed 2.0g potassium borohydride (4.4), stirring to dissolve. This solution preparation day, for the determination of arsenic, selenium, bismuth, antimony.
1 Note. You can also use sodium hydroxide, sodium borohydride, sodium borohydride solution configuration.
4.10 thiourea and ascorbic acid mixed solution.
Weigh thiourea (4.7), ascorbic acid (4.8) each 10g, with 100ml distilled water, mix, formulated the day.
4.11 mercury (Hg) standard solution.
4.11.1 the mercury standard fixative (fixative for short).
0.5g of potassium dichromate was dissolved in 950ml of distilled water, then add 50ml of nitric acid (4.2) and mix.
4.11.2 the mercury standard stock solution. = rho 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference materials, or weighed on a silica gel dryer stand overnight mercuric chloride (HgCl2) 0.1354g, with the amount of dissolved in distilled water to move 1000ml volumetric flask, and finally with fixative (4.11.1) volume to the mark, Mix well.
4.11.3 mercury intermediate standard solution. = rho 1.00mg/L.
Pipette mercury stock standard solution (4.11.2) 5.00ml, placed in 500ml volumetric flask, add 50ml hydrochloric acid solution (4.6), with fixative (4.11.1) volume to the mark, and mix.
4.11.4 mercury standard solution. = rho 10.0µg/L.
Pipette mercury intermediate standard solution (4.11.3) 5.00ml, placed 500ml volumetric flask, add 50ml hydrochloric acid solution (4.6), with fixative (4.11.1) volume to the mark, and mix. The time is now equipped with.
4.12 Arsenic (As) standard solution.
4.12.1 arsenic standard stock solution. = rho 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference sample or weighed 0.1320g dried 105 °C 2h of pure class distinctions trioxide of arsenic (As2O3) was dissolved in 5ml 1mol/L sodium hydroxide solution, with 1mol L hydrochloric acid solution/neutralized to phenolphthalein red fade Go, moved 1000ml volumetric flask, constant volume with distilled water to the mark, and mix.
4.12.2 arsenic intermediate standard solution. = rho 1.00mg/L.
Pipette arsenic standard stock solution (4.12.1) 5.00ml, placed in 500ml volumetric flask, add 100ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix.
4.12.3 arsenic standard solution. = rho 100.0µg/L.
Pipette arsenic intermediate standard solution (4.12.2) 10.00ml, a 100ml volumetric flask, add 20ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix. The time is now equipped with.
4.13 selenium (Se) standard solution.
4.13.1 selenium standard stock solution. = rho 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference sample or weighed 0.1000g of high purity selenium powder, placed in 100ml beaker, Add 20ml nitric acid (4.2) over low heat to dissolve cooled to a greenhouse and transferred to 1000ml volumetric flask, dilute to mark with distilled water Line, and mix.
4.13.2 selenium intermediate standard solution. = rho 1.00mg/L.
Pipette stock selenium standard solution (4.13.1) 5.00ml, placed in 500ml volumetric flask, add 200ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix.
4.13.3 selenium standard solution. = rho 100.0µg/L.
Pipette selenium intermediate standard solution (4.13.2) 10.00ml, a 100ml volumetric flask, add 40ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix. The time is now equipped with.
4.14 bismuth (Bi) standard solution.
4.14.1 bismuth standard stock solution. = rho 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference materials, or high-purity bismuth weighed 0.1000g, placed in 100ml beaker, Plus 20ml of nitric acid (4.2), low heat to dissolve completely cooled and transferred to 1000ml volumetric flask, dilute to mark with distilled water Line, and mix.
4.14.2 bismuth intermediate standard solution. = rho 1.00mg/L.
Pipette bismuth stock standard solution (4.14.1) 5.00ml, placed in 500ml volumetric flask, add 100ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix.
4.14.3 bismuth standard solution. = rho 100.0µg/L.
Pipette bismuth intermediate standard solution (4.14.2) 10.00ml, a 100ml volumetric flask, add 20ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix. The time is now equipped with.
4.15 antimony (Sb) standard solution.
4.15.1 Antimony standard stock solution. = rho 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference sample or weighed 0.1197g after 105 °C drying 2h antimony trioxide (Sb2O3) was dissolved in 80ml hydrochloric acid (4.1), and transferred to 1000ml volumetric flask, supplemented with 120ml of hydrochloric acid (4.1), with steam Distilled water volume to the mark, and mix.
4.15.2 antimony intermediate standard solution. = rho 1.00mg/L.
Pipette antimony stock standard solution (4.15.1) 5.00ml, placed in 500ml volumetric flask, add 100ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix.
4.15.3 Antimony standard solution. = rho 100.0µg/L.
Pipette 10.00ml antimony intermediate standard solution (4.15.2), a 100ml volumetric flask, add 20ml of hydrochloric acid solution (4.6), Volume with distilled water to the mark, and mix. The time is now equipped with.
4.16 carrier gas and shield gas. argon (purity >=99.99%).
4.17 slow quantitative filter paper.
5 Apparatus
5.1 atomic fluorescence spectrometer. Instrument performance indicators should be consistent with the provisions of GB/T 21191 of.
5.2 light elements (mercury, arsenic, selenium, bismuth, antimony).
5.3 Microwave Digestion System. a temperature control and temperature-programmed functions, temperature accuracy up to ± 2.5 °C.
5.4 Balance. accuracy of 0.01g.
5.5 Analytical balance. accuracy of 0.0001g.
5.6 General Commonly used laboratory instruments and equipment.
6 Samples
6.1 Acquisition and Preservation
Solid waste collection and preservation of samples in accordance with HJ/T 20 and HJ/T 298 of the relevant provisions.
6.2 Sample Preparation
6.2.1 Solid Waste
Preparation of solid waste samples were carried out according to HJ/T relevant provisions 20. For solid waste or sludge samples viscous, Accurately weigh 10g sample (m1, accurate to 0.01g), natural air-dried or freeze-dried, weighed (m2, accurate to 0.01g) again, Grinding, all through a 100 mesh sieve spare.
6.2.2 Solid waste leachate
Preparation of leachate follow HJ 557, HJ/T 299, HJ/T 300 of the relevant provisions.
6.3 Preparation of the sample
6.3.1 Solid waste samples
For solid samples, using the analytical balance (5.5) accurately weighed sample were sieved (6.2.1) 0.5g (m3), the liquid or semi-solid samples directly sample weighed 0.5g (m3), accurate to 0.0001g. Place the specimen sample dissolution cup, with a small amount of steam Distilled water wetting. In the hood, to join 6ml hydrochloric acid (4.1), and then slowly add 2ml of nitric acid (4.2), and the sample digestion Liquid contact. If serious chemical reaction, after the end of the reaction solution sample cup was placed in the digestion tank seal. The digestion tank After loading the stent into the digestion vessel microwave digestion apparatus, according to Table 1 Recommended temperature program microwave digestion. Digestion end, to be After the tank temperature to room temperature, taken out in a fume hood, deflated, open. Judgment is fully digested, whether the solution clarified If you need further clarification digestion.
Table 1 solid waste microwave digestion temperature program
Step heating time (min) Target Temperature (°C) retention time (min) After digestion solution was slow quantitative filter paper (4.17) will be filtered into 50ml volumetric flask, rinse with distilled water to dissolve the sample cup and precipitation Less three times. All eluent incorporated into the flask, constant volume with distilled water to the mark, and mix.
6.3.2 Solid waste leachate sample
Pipette 40.0 ml of solid waste leachate into 100ml Dissolving cup, add 3ml of hydrochloric acid in a fume cupboard (4.1) and 1ml of nitric acid (4.2) and mix. If severe reactions, or a large number of bubbles overflow, after the end of the reaction solution sample cup was placed digestion tank Seal. The digestion tank after filling into the stent into a microwave digestion apparatus, as shown in Table 2 Recommended temperature program microwave extinction solution. After the end of digestion, in accordance with 6.3.1 out, deflated, open the digestion tank.
Table 2 microwave digestion of solid waste leachate temperature program
Step heating time (min) Target Temperature (°C) retention time (min) the test solution was transferred to a 50ml volumetric flask, rinse with distilled water sample dissolution cups, lids (at least three), will be incorporated into the eluent Flask, constant volume with distilled water to the mark, and mix.
6.4 Preparation of the sample
6.4.1 Solid waste sample
Dispensing 10.0ml test solution (6.3.1) into 50ml volumetric flask, the amounts of different elements in Table 3 was added hydrochloric acid (4.1), sulfur Urea and ascorbic acid solution (4.10), constant volume with distilled water to the mark, and mix at room temperature for 30min (room temperature below 15 °C when placed in 30 °C water bath for 30min), to be tested.
Reagent was added per unit Table 3 constant volume 50ml. ml Name mercury arsenic, bismuth, antimony, selenium Hydrochloric acid (4.1) 2.5 5.0 10.0 Thiourea and ascorbic acid solution (4.10) - 10.0 -
6.4.2 Solid waste leachate sample
Dispensing 10.0ml test solution (6.3.2) into 50ml volumetric flask, the amounts of different elements in Table 3 was added hydrochloric acid (4.1), sulfur Urea and ascorbic acid solution (4.10), constant volume with distilled water to the mark, and mix at room temperature for 30min (room temperature below 15 °C when placed in 30 °C water bath for 30min), to be tested.
7 Procedure
7.1 Instrument Reference conditions
Warmed up the instrument is stable, according to the instruction manual atomic fluorescence set lamp current, negative pressure, carrier gas flow rate, Shielding gas flow rate and other operating parameters, the parameters shown in Table 4 generally employed.
TABLE 4 instrument parameters
element
name
Lamp current
Negative high voltage (V) Atomizer temperature (°C) Carrier gas flow (Ml/min) Shielding gas flow (Ml/min) Mercury 15 ~ 40230 ~ ~ 300 200 400 800 1000 Arsenic 40 ~ 80 230 ~ 400 800 ~ 300 200 300 Se ~ 40 ~ 80230 ~ 400 600 300 200 350 1000 -Bismuth 40 ~ 80230 ~ ~ 400 800 300 200 300 1000 -Antimony 40 ~ 80230 ~ 300 200 200 ~ 400 400 ~ 700
7.2 Calibration
7.2.1 Preparation of the calibration series
7.2.1.1 Mercury calibration series
Pipette 0,0.50,1.00,2.00,3.00,4.00,5.00ml were using mercury standard solution (4.11.4) to a set of 50ml Flask were added 2.5ml of hydrochloric acid (4.1), constant volume with distilled water to the mark, and mix.
7.2.1.2 Arsenic calibration series
Pipette 0,0.50,1.00,2.00,3.00,4.00,5.00ml were using arsenic standard solution (4.12.3) to a set of 50ml Flask were added 5.0ml of hydrochloric acid (4.1), 10ml thiourea and ascorbic acid solution (4.10), at room temperature for 30min (At room temperature below 15 °C, placed in 30 °C water bath for 30min), constant volume with distilled water to the mark, and mix.
7.2.1.3 Selenium calibration series
Pipette 0,0.50,1.00,2.00,3.00,4.00,5.00ml selenium respectively using standard solution (4.13.3) to a set of 50ml when the flask were added 10ml of hydrochloric acid (4.1), at room temperature for 30min (room temperature below 15 °C, 30 °C placed in a water bath Insulation 30min), constant volume with distilled water to the mark, and mix.
7.2.1.4 Calibration bismuth series
Pipette 0,0.50,1.00,2.00,3.00,4.00,5.00ml are using bismuth standard solution (4.14.3) to a set of 50ml Flask were added 5.0ml of hydrochloric acid (4.1), 10ml thiourea and ascorbic acid solution (4.10), with distilled water Container to the mark, and mix.
7.2.1.5 Calibration antimony series
Pipette 0,0.50,1.00,2.00,3.00,4.00,5.00ml are using antimony standard solution (4.15.3) to a set of 50ml Flask were added 5.0ml of hydrochloric acid (4.1), 10ml thiourea and ascorbic acid solution (4.10), at room temperature for 30min (At room temperature below 15 °C, placed in 30 °C water bath for 30min), constant volume with distilled water to the mark, and mix.
Mercury, arsenic, selenium, bismuth, antimony concentration calibration solution series are shown in Table 5, the series is suitable for measuring the concentration of the general sample.
Table 5 series element calibration solution concentration units. µg/L
Element Standards Series Mercury 0.00 0.10 0.20 0.40 0.60 0.80 1.00 Arsenic 0.00 1.00 2.00 4.00 6.00 8.00 10.00 Selenium 0.00 1.00 2.00 4.00 6.00 8.00 10.00 0.00 1.00 2.00 4.00 6.00 Bi 8.00 10.00 0.00 1.00 2.00 4.00 6.00 Sb 8.00 10.00
7.2.2 Calibration curve
With potassium borohydride solution (4.9.1 or 4.9.2) as a reducing agent, a hydrochloric acid solution (4.5) as the carrier concentration from low to high
Table 5 Determination of the elements in the calibration solution series. By deducting the blank zero concentration calibration series atomic fluorescence intensity ordinate dissolved
Liquid element corresponding to the concentration (µg/L) as the abscissa, the calibration curve.
7.3 Blank test
Step by step from 6.3 to 6.4 prepared blank samples, were measured according to 7.4.
7.4 Determination
The prepared sample with the same instrument calibration curve analysis conditions were determined.
8 Results Calculation and representation
Test results 8.1 Calculation of solid waste
8.1.1 Solid and viscous sludge solid waste
Solid waste elements (mercury, arsenic, selenium, bismuth, antimony) content of omega (µg/g) according to the equation (1) is calculated.
200 10) (- ×××
VVrhorhoomega (1)
Where. omega - content of the solid waste elements, µg/g;
rho - the calibration curve Richard measuring the concentration of elements in the sample solution, µg/L;
rho 0-- laboratory blank solution determine the concentration, µg/L;
After microwave digestion V0-- constant volume of test solution volume;
V1-- points to take the test solution volume, ml;
The test solution was measured after V2-- dispensing volume by volume, ml;
Quality m1-- solid sample, g;
M2-- quality solid sample after drying, g;
After grinding quality m3-- sieved sample, g;
8.1.2 Liquid and semi-solid (except viscous sludge) Solid waste
Solid waste elements (mercury, arsenic, selenium, bismuth, antimony) content of omega (µg/g) according to the equation (2) is calculated.
200 10) (- ××
VVrhorhoomega (2)
Where. omega - content of the solid waste elements, µg/g;
rho - the calibration curve Richard measuring the concentration of elements in the sample solution, µg/L;
rho 0-- laboratory blank solution determine the concentration, µg/L;
After microwave digestion V0-- constant volume of test solution volume;
V1-- points to take the test solution volume, ml;
The test solution was measured after V2-- dispensing volume by volume, ml;
m3-- saying that the quality of the samples taken, g;
8.2 Solid waste leachate test results calculated
Solid waste leachate elements (mercury, arsenic, selenium, bismuth, antimony) concentration rho (µg/L) according to formula (3) Calculated.
V ×× - = rhorhorho (3) where. rho - Solid waste leachate elements (mercury, arsenic, selenium, bismuth, antimony) concentration, µg/L;
rho 1-- from the calibration curve Richard measuring the concentration of elements in the sample solution, µg/L;
rho 0-- laboratory blank solution determine the concentration, µg/L;
Pipette volume of leachate...
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 9 pages — is available in the English PDF.
Referenced standards
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