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HJ 702-2014: Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony. MicrowaveDissolution/AtomicFluorescence Spectrometry
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Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony. MicrowaveDissolution/AtomicFluorescence Spectrometry
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HJ 702-2014
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Basic data | Standard ID | HJ 702-2014 (HJ702-2014) | | Description (Translated English) | Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony. MicrowaveDissolution/AtomicFluorescence Spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z27 | | Word Count Estimation | 14,139 | | Date of Issue | 9/2/2014 | | Date of Implementation | 11/1/2014 | | Quoted Standard | GB/T 21191; HJ/T 20; HJ/T298; HJ/T 299; HJ/T300; HJ/T 557 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard provides the solid waste and solid waste leachate of mercury, arsenic, selenium, Ming, antimony microwave digestion/atomic fluorescence spectrometry. This standard applies to solid waste mercury, arsenic, selenium, buttons, and the determina | HJ 702-2014: Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony. MicrowaveDissolution/AtomicFluorescence Spectrometry
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Solid Waste-Determination of Mercury, Arsenic, Selenium, Bismuth, Antimony.MicrowaveDissolution/AtomicFluorescence Spectrometry
People's Republic of China National Environmental Protection Standards
Solid waste mercury, arsenic, selenium, bismuth, antimony determination
Microwave Digestion/Atomic Fluorescence Spectrometry
Solid Waste- Determination of Mercury, Arsenic, Selenium,
Bismuth, Antimony- Microwave Dissolution/Atomic Fluorescence
Spectrometry
(Release)
Issued on.2014-09-03
2014-11-01 implementation
release
Ministry of Environmental Protection
Table of Contents
Preface ..I
1. Scope .1
2 Normative references .1
3 .1 The principle of the method
4 Reagents and materials 1
5 Apparatus and equipment 3
Sample 4 6
7 Procedure .5
8 Results Calculation and representation .6
9 precision and accuracy .7
Quality Assurance and Quality Control 10 .8
11 waste disposal 8
12 Note ..8
Precision and accuracy in Appendix A (informative) Method 9
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, 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. ρ (HCl) = 1.19 g/ml.
Nitrate 4.2. ρ (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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference sample or weighed 0.1320g dried 105 ℃ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 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. = ρ 100.0mg/L.
Purchase a commercially available certified reference materials/certified reference sample or weighed 0.1197g after 105 ℃ 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. = ρ 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. = ρ 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 ℃.
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 (℃) 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 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 (℃) 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 ℃
When placed in 30 ℃ 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 ℃
When placed in 30 ℃ 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
(MA)
Negative high voltage
(V)
Atomizer temperature
(℃)
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 ℃, placed in 30 ℃ 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 ℃, 30 ℃ 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 ℃, placed in 30 ℃ 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 ω (μg/g) according to the equation (1) is calculated.
200 10) (- ×××
×× - = m
Vm
VVρρω (1)
Where. ω - content of the solid waste elements, μg/g;
ρ - the calibration curve Richard measuring the concentration of elements in the sample solution, μg/L;
ρ 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 ω (μg/g) according to the equation (2) is calculated.
200 10) (- ××
×× - = Vm
VVρρω (2)
Where. ω - content of the solid waste elements, μg/g;
ρ - the calibration curve Richard measuring the concentration of elements in the sample solution, μg/L;
ρ 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 ρ (μg/L) according to formula (3) Calculated.
()
V ×× - = ρρρ (3)
Where. ρ - Solid waste leachate elements (mercury, arsenic, selenium, bismuth, antimony) concentration, μg/L;
ρ 1-- from the calibration curve Richard measuring the concentration of elements in the sample solution, μg/L;
ρ 0-- laboratory blank solution determine the concentration, μg/L;
Pipette volume of leachate...
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