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HJ 767-2015: Solid waste. Determination of total barium. Graphite furnace atomic absorption spectrophotometry
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Solid waste. Determination of total barium. Graphite furnace atomic absorption spectrophotometry
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HJ 767-2015
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Standard similar to HJ 767-2015 HJ 511 HJ 945.3 HJ 943 Basic data | Standard ID | HJ 767-2015 (HJ767-2015) | | Description (Translated English) | Solid waste. Determination of total barium. Graphite furnace atomic absorption spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Word Count Estimation | 13,187 | | Date of Issue | 2015-11-20 | | Date of Implementation | 2015-12-15 | | Quoted Standard | HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557 | | Regulation (derived from) | Ministry of Environment Announcement 2015 No.73 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the determination of solid waste and solid waste leaching solution of barium graphite furnace atomic absorption spectrophotometry. This Standard applies to the determination of solid waste and solid waste leaching solution of barium. | HJ 767-2015: Solid waste. Determination of total barium. Graphite furnace atomic absorption spectrophotometry
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Solid waste.Determination of total barium.Graphite furnace atomic absorption spectrophotometry
National Environmental Protection Standard of the People 's Republic of China
Determination of barium in solid waste
Graphite Furnace Atomic Absorption Spectrophotometry
Solid waste-Determination of total barium-Graphite atomic atomic
Absorption spectrophotometry
2015-11-20 release
2015-12-15 implementation
Ministry of Environmental Protection
Directory
Preface ..ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials 2
6 instruments and equipment 3
7 Sample 3
8 Analysis steps
9 Results calculation and presentation
10 precision and accuracy
11 Quality assurance and quality control
12 Waste treatment .9
13 Precautions .9
Appendix A (informative) Standard Addition Method .10
Appendix B (informative appendix) Appraisal of the applicability of the standard addition method
Foreword
In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Environmental Pollution by Solid Wastes,
Protect the environment, protect human health, regulate the solid waste and solid waste leaching solution of barium determination method, the development of this standard.
This standard specifies the graphite furnace atomic absorption spectrophotometric method for the determination of barium in solid waste and solid waste leachate.
This standard is the first release.
Appendix A and Appendix B of this standard are informative.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. China Environmental Monitoring Station, Guangdong Province Environmental Monitoring Center.
The standard verification unit. Sichuan Province Environmental Monitoring Station, Chongqing Environmental Monitoring Center, Liaoning Province, environmental monitoring experiment
Xin, Henan Province Environmental Monitoring Center, Guangdong Province Environmental Monitoring Center, Guangzhou Environmental Monitoring Center Station, Nanchang Environmental Monitoring
station.
The Environmental Protection Department of this standard approves on November 20,.2015.
This standard is implemented as of December 15,.2015.
This standard is explained by the Ministry of Environmental Protection.
Determination of barium in solid waste - Graphite furnace atomic absorption spectrophotometric method
WARNING. The barium standard solution used in the experiment is toxic. Nitric acid, perchloric acid with strong oxidizing and corrosive, salt
Acid, hydrofluoric acid with strong volatile and corrosive, the operation should wear protective equipment, solution preparation and sample pretreatment process should be
In the fume hood operation.
1 Scope of application
This standard specifies the determination of barium in solid waste and solid waste leachate by graphite furnace atomic absorption spectrophotometry.
This standard applies to the determination of barium in solid waste and solid waste leachate.
When the amount of solid waste is 0.1 g, the limit of detection is 6.3 mg/kg and the lower limit is determined.
For 25.2 mg/kg. When the sample volume of solid waste leaching solution is 25 ml, the volume is set to 50 ml and the injection volume is 20 μl.
The detection limit was 2.5 μg/L and the lower limit was 10.0 μg/L.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Any unspecified date of the reference file, the effective version of the appropriate
For this standard.
Technical specification for SJ sample preparation for industrial solid waste
Technical Specification for Hazardous Waste Identification
HJ/T 299 Solid waste leaching toxicity leaching method sulfuric acid nitric acid method
HJ/T 300 solid waste leaching toxicity leaching method acetic acid buffer solution method
HJ 557 Solid waste leaching toxicity leaching method Horizontal oscillation method
3 Principle of the method
Solid waste or solid waste leachate after digestion, into the graphite furnace atomizer, after drying, ashing and atomic
And the barium-based atoms formed by the barium compound are absorbed by the 553.6 nm characteristic line, and the absorption intensity is within a certain range
The mass concentration of barium in the test solution is proportional.
4 interference and elimination
4.1 The total concentration of potassium, sodium and magnesium in the sample is 500 mg/L, the chromium is 10 mg/L, the manganese is 25 mg/L, the total concentration of iron and zinc
2.5 mg/L, 2 mg/L aluminum, and 5% nitric acid, there was no effect on the determination of barium. When the concentration of these substances is over
When the mass concentration is used, the sample dilution method or the standard addition method can be used to eliminate the interference.
4.2 Calcium concentration in the sample is greater than 5 mg/L, the barium determination of positive interference. When injecting the concentration of calcium in the atomizer
100 mg/L ~ 300 mg/L, the interference of calcium to barium does not change with the change of calcium concentration. According to the interference characteristics of calcium, join the base
Body modifier calcium nitrate, can eliminate the memory effect can improve the sensitivity of the determination. If the concentration of calcium in the sample exceeds 300
Mg/L, the sample should be properly diluted and determined.
4.3 When the sample matrix composition is complex or unknown, the sample dilution method or standard addition method should be used to examine whether the sample
It is appropriate to use the calibration curve method to quantify directly. See Appendix A for the standard addition method curve. See Appendix B for the applicability of the standard addition method.
5 reagents and materials
Unless otherwise stated, analytical analytical reagents conforming to national standards are used in the analysis, and the test water is a newly prepared deionized
water.
5.1 nitric acid (HNO3). ρ = 1.42 g/ml, excellent grade pure.
5.2 hydrochloric acid (HCl). ρ = 1.19 g/ml, excellent grade pure.
5.3 hydrofluoric acid (HF). ρ = 1.49 g/ml, excellent grade pure.
5.4 perchloric acid (HClO4). ρ = 1.68 g/ml, excellent grade pure.
5.5 barium nitrate [Ba (NO3) 2]. pure spectrum.
5.6 calcium nitrate [Ca (NO3) 2 · 4H2O]. excellent grade pure.
5.7 argon. purity ≥99.999%.
5.8 nitric acid solution. 1 1 (v/v), prepared with (5.1).
5.9 Nitric acid solution. 1 9 (v/v), prepared with (5.1).
5.10 nitric acid solution. 1 99 (v/v), prepared with (5.1).
5.11 hydrochloric acid solution. 1 1 (v/v), prepared with (5.2).
5.12 barium standard stock solution. ρ (Ba) = 1 000 mg/L.
Use a commercially available standard solution or weigh 0.190 3 g barium nitrate (5.5) (accurate to 0.000 1 g), add 1 ml
Nitric acid (5.1) dissolved, if necessary, can be heated. Into the 100 ml volumetric flask, with nitric acid solution (5.10) constant volume to the marking,
Mix well.
5.13 barium standard intermediate liquid. ρ (Ba) = 10.00 mg/L.
Accurate removal of barium standard stock solution (5.12) 10.00 ml in 1 000 ml volumetric flask, with nitric acid solution (5.10) constant volume
To mark, mix well. Can be stored at 4 ℃ for 30 days.
5.14 barium standard use of liquid. ρ (Ba) = 1.00 mg/L.
Accurate removal of barium standard intermediate (5.13) 10.00 ml in 100 ml volumetric flask, with nitric acid solution (5.10)
Marking, mixing. Pro is now available.
5.15 Calcium nitrate solution. ρ (Ca) = 500 mg/L.
Accurately weighed 0.295 g calcium nitrate (5.6), dissolved in nitric acid solution (5.10) and diluted volume to 100 ml, mix.
6 instruments and equipment
6.1 Graphite Furnace Atomic Absorption Spectrophotometer (with background correction function).
6.2 Pyrolytic coated graphite tube.
6.3 hot plate or graphite digestion. a temperature control function (temperature stability ± 5 ℃), the maximum temperature can be set to 180 ℃.
6.4 Microwave digestion. Output power 1 000 W ~ 1 600 W. With programmable control function, can be temperature, pressure and time
(Heating time and holding time) to carry out the whole process of monitoring; with security features.
6.5 Digestion tank. closed tank made of fluorocarbon (soluble polytetrafluoroethylene PFA or modified polytetrafluoroethylene TFM)
Body, can be compressive (170 psi ~.200 psi), acid and corrosion resistance, with automatic pressure relief function.
6.6 Balance. Accuracy 0.01 g.
6.7 Analytical Balance. Accuracy 0.0001 g.
6.8 Triangle bottle. 150 ml.
6.9 glass small funnel. can be placed in the triangle bottle.
6.10 Teflon crucible. 50 ml.
6.11 volumetric flask. 25 ml, 50 ml, 100 ml, 250 ml.
6.12 Suction device. with a pore size of 0.45 μm acetate fiber or polyethylene filter.
6.13 Screen. non-metallic sieve, 100 mesh.
7 samples
7.1 Sample collection and storage
The collection and storage of solid waste samples are carried out in accordance with the relevant provisions of HJ/T 20 and HJ/T 298.
7.2 Sample preparation
7.2.1 Solid waste
The preparation of solid waste samples was carried out in accordance with the relevant provisions of HJ/T 20. For solid or dry semi-solid samples, weighed
10 g sample (m1, accurate to 0.01 g), naturally air-dried or freeze-dried, weighed again (m2, accurate to 0.01 g), ground,
All over 100 mesh sieve (6.13) spare.
7.2.2 Solid waste leachate
Prepare leachate according to the relevant regulations of HJ/T 299 or HJ/T 300 or HJ 557. Leaching solution can not be carried out soon
Treatment analysis, should be added nitric acid (5.1) acidification (1 L leaching solution by adding 10 ml nitric acid (5.1)), and digestion as soon as possible, do not exceed
24 h.
7.3 Sample preparation
7.3.1 Solid waste samples
7.3.1.1 Electric plate digestion method
Weigh 0.1 g of the sieved sample (m3, accurate to 0.000 1 g) in a 50 ml polytetrafluoroethylene crucible (6.10). use
After a small amount of water, add 10 ml of hydrochloric acid (5.2), in the fume hood on the hot plate at low temperature (95 ± 5 ℃ ℃) heating, so that
Product preliminary decomposition (higher organic matter content of the sample, need to be added in advance hydrochloric acid (5.2) soaked overnight). To be evaporated to about 3 ml
When removed slightly cold. Add 5 ml of nitric acid (5.1), 5 ml of hydrofluoric acid (5.3), 3 ml of perchloric acid (5.4), after capping
On the temperature (120 ± 5 ℃ ℃) heating 1 h. Open lid, heating plate temperature control (140 ± 5 ℃ ℃), continue to heat, and by
Often shake the crucible. When heated to smoke thick smoke, capped to black organic carbon carbide decomposition. The black organic matter on the wall of the crucible
After disappearing, open the lid, drive away the white smoke and steamed into the contents of the sticky. Depending on the situation, can add 3 ml of nitric acid (5.1), 3 ml
Hydrofluoric acid (5.3), 1 ml perchloric acid (5.4), repeat the above digestion process. Remove the crucible slightly cold, add 2 ml of nitric acid solution (5.8),
Soluble dissolved residue. After cooling, transfer to 250 ml volumetric flask, rinse the crucible with experimental water, the eluent all
Transferred to the volumetric flask, with the experimental water volume to the mark, mix, to be measured.
If the graphite digestion instrument is used instead of the hot plate to digest the sample, refer to the above steps.
7.3.1.2 Microwave digestion method
Weigh 0.1 g of the sieved sample (m3, accurate to 0.0001 g) in a microwave digestion tank. Moist with a small amount of water after adding
6 ml of nitric acid (5.1), 2 ml of hydrofluoric acid (5.3) (higher organic matter content, need to be added in advance nitric acid (5.1) soaked
night). Set the microwave digestion of the working procedures (Table 1), start the instrument. After cooling, microwave digestion with a small amount of experimental water
The entire contents of the tank were transferred to a 50 ml polytetrafluoroethylene crucible, 2 ml of perchloric acid (5.4) was added, and the hot plate temperature was controlled
150 ° C, drive away the white smoke and the contents are viscous. Remove the crucible slightly cold, add 2 ml of nitric acid solution (5.8), warm dissolved
Soluble residue. After cooling, transfer to 250 ml volumetric flask, rinse the crucible with experimental water, all the eluent transferred to the capacity
Measuring bottles, with the experimental water volume to the marking, mixing, to be measured.
Table 1 Solid Waste Microwave Digestion Method
Heating time (min) Digestion temperature (℃) Holding time (min)
7.3.2 Solid waste leachate sample
7.3.2.1 Electric plate digestion method
Measure 50.0 ml of leachate in 150 ml Erlenmeyer flask, add 2 ml nitric acid (5.1) and mix well. Insert small in the triangle bottle
After the funnel placed on the hot plate at low temperature (95 ℃ ± 5 ℃) heating, less than 20 ml when the removal of cooling. Wash with a small amount of experimental water
Small funnel and the inner wall of the flask, such as the digestion solution contains more impurities, you need to filter, pumping device using nitric acid solution (5.9)
Rinse. The amount of digestion solution transferred to 50 ml volumetric flask, with experimental water elution Erjiao bottle, the eluent transferred to the volumetric flask,
With the experimental water volume to the mark, mix, to be measured.
7.3.2.2 Microwave digestion method
Measure 25.0 ml leaching solution into the digestion tank (according to the digestion tank volume and sample concentration to determine the amount of leaching solution volume,
The final solution volume shall not exceed the limits specified by the instrument). Add 2 ml nitric acid (5.1) to the digestion tank and tighten the tank. will
Digestion tank on the microwave oven. Set the microwave digestion procedures (Table 2), start the instrument.
Table 2 Solid Waste Leach Solution Microwave Digestion Method
Heating time (min) Digestion temperature (℃) Holding time (min)
At the end of the digestion procedure, the digestion tank should be removed in the microwave digestion for at least 5 min. Carefully open in the fume hood
Digest the lid of the tank and release the gas. If the digestion solution contains more impurities, you need to filter. Pumping device required
Nitric acid solution (5.9) rinse. The digestion solution into the 50 ml volumetric flask, with experimental water rinse digestion tank, the eluent turn
Moved to the volumetric flask, with the experimental water volume to the marking, mixing, to be measured. Microwave digestion can also be done with a hot plate or a graphite digestion
After the digestion in the sub-boiling state (to maintain the solution temperature 95 ℃ ± 5 ℃) heated and concentrated, with the experimental water leaching digestion tank, the leaching
Wash the lotion to 25 ml volumetric flask, with the experimental water volume to the mark.
7.3.3 Preparation of blank samples
7.3.3.1 Solid waste blank
Use empty containers to prepare solid waste blank samples according to the procedure in 7.3.1.
7.3.3.2 Solid waste leachate blank
The use of experimental water prepared as a leaching agent, according to 7.2.2 preparation of solid waste leachate blank, according to 7.3.2 digestion.
8 Analysis steps
8.1 Instrument reference measurement conditions
According to the instrument specification requirements to optimize the test conditions. The instrument reference measurement conditions are shown in Table 3.
Table 3 Instrument reference measurement conditions
Elemental barium (Ba)
Light source barium hollow cathode lamp
Determination of wavelength (nm) 553.6
Passband width (nm) 0.5
Drying temperature/time/(℃/s) 85 ~ 120/55
Ashing temperature/time/(° C/s) 1 000/8
Atomic temperature/time/(° C/s) 2 600/2.8
Clear the temperature/time/(℃/s) 2 650/2
Whether the atomic phase is stopped
Argon flow rate (L/min) 3.0
Injection volume (μl) 20
8.2 Calibration curve
Respectively, the use of barium standard use of liquid (5.14) 0.00 ml, 1.00 ml, 2.00 ml, 4.00 ml, 6.00 ml, 8.00 ml,
10.00 ml in 100 ml volumetric flask, with nitric acid solution (5.10) constant volume to the mark, mix. This standard series contains barium respectively
0 μg/L, 10.0 μg/L, 20.0 μg/L, 40.0 μg/L, 60.0 μg/L, 80.0 μg/L, 100.0 μg/L. Or in accordance with the above concentrated
The degree is automatically formulated by the instrument. From low concentration to high concentration in turn to the graphite tube by adding 20 μl standard solution, according to the instrument measuring strip
(8.1) Measure the absorbance. With the corresponding absorbance as the ordinate, barium standard series of mass concentration for the abscissa, the establishment of barium
Calibration curve.
8.3 blank sample determination
Prepare a blank sample (7.3.3) and perform the same conditions as the calibration curve.
8.4 Sample determination
Prepare the sample (7.3.1 or 7.3.2) and make the same conditions as the calibration curve.
Note 1. Determine whether 10% by volume of the matrix modifier calcium nitrate solution (5.15) is required, depending on background interference during sample analysis. If so
Add the matrix modifier, the use of the calibration curve should also be prepared in proportion to the preparation.
9 Results calculation and representation
9.1 Results calculation
9.1.1 Solid waste
9.1.1.1 Solid or dry semi-solid solid waste
The content of barium in solid waste is calculated according to formula (1)
001 10) f (- ××× - × =
Vw ρρ
(1)
Where. w - the content of barium in solid waste, mg/kg;
1 - The calibration curve was used to determine the mass concentration of barium in the sample, μg/L;
F - sample dilution factor;
0ρ - mass concentration of barium in laboratory blank samples, μg/L;
0V - volume of the sample after digestion, ml;
1m - the amount of solid waste sample weighed, g;
2m - the quality of solid waste samples after air drying or freeze drying, g;
3m - the amount of sample to be sintered after grinding, g.
9.1.1.2 Semi-solid solid waste with or without drying
The content of barium in solid waste is calculated according to formula (2)
001 10) f (- ×× - × =
Vw ρρ
(2)
Where. w - the content of barium in solid waste, mg/kg;
1 - The calibration curve was used to determine the mass concentration of barium in the sample, μg/L;
F - sample dilution factor;
0ρ - mass concentration of barium in laboratory blank samples, μg/L;
0V - volume of the sample after digestion, ml;
1m - the amount of solid waste sample weighed, g.
9.1.2 Solid waste leachate
The mass concentration of barium in the leachate of solid waste is calculated according to formula (3)
101) f (
V × - × = ρρρ (3)
Where. ρ - solid waste leachate concentration of barium, μg/L;
1 - The calibration curve was used to determine the mass concentration of barium in the sample, μg/L;
F - sample dilution factor;
0ρ - mass concentration of barium in laboratory blank samples, μg/L;
1V - the volume of the decoction after decoction, ml;
2V - the volume of leach solution when digested, ml.
9.2 The result is shown
For solid waste, when the result is less than 10 mg/kg, one after the decimal point is retained; when the result is greater than or equal
At 10 mg/kg, three valid digits are retained.
For solid waste leachate, when the determination is less than 10 μg/L, one after the decimal point is retained; when the result is greater than
Or equal to 10 μg/L, retain three significant digits.
10 precision and accuracy
10.1 Precision
Seven laboratories carried out six replicates of solid samples with a solid sample of 110 mg/kg of solid waste. the hot plate method
The relative standard deviation of the laboratory was 1.5% ~ 8.6%; the relative standard deviation between the laboratory was 3.3%, the repeatability limit was 17 mg/kg,
The reproducibility limit was 19 mg/kg. The relative standard deviation of the laboratory was 2.9% ~ 8.4%. The relative standard deviation
Was 5.4%, the repeatability was 19 mg/kg, and the reproducibility was 24 mg/kg.
Seven laboratories carried out six replicates of the solid sample of solid waste leachate at a concentration of 480 μg/L for six times.
The relative standard deviation of the laboratory was 0.87% ~ 13%. The relative standard deviation was 14% between the laboratory and the repeatability limit was
90 μg/L, reproducibility limit of 210 μg/L. The relative standard deviation of the laboratory was 1.6% ~ 7.0%
The standard deviation was 8.0%, the repeatability was 60 μg/L, and the reproducibility was 114 μg/L.
10.2 Accuracy
Seven laboratories carried out standard samples of solid waste barium content of 213 ± 20 mg/kg and 296 ± 26 mg/kg, respectively
The relative error of the thermo-plate method was -8.0% ~ 1.9%, 5.4 ~ 1.0%, and the relative error was
-2.4% ± 6.2%, - 2.8% ± 4.6%. The relative error of microwave method is -6.6% ~ 2.3%, - 5.4% ~ 1.7%, respectively
The final values were -1.5% ± 6.8%, - 0.95% ± 5.8%, respectively.
Seven laboratories for the solid waste barium content of 110 mg/kg of the unified actual sample digestion after the spike recovery rate of 6 times the weight
The recoveries were 82.7% ~ 109%, and the final recoveries were 93.7% ± 19.0%. Microwave method
The recoveries were 82.0% ~ 107%. The final recoveries were 95.3% ± 20.2%.
Seven laboratories were digested with a uniform sample of solid waste leachate at a mass concentration of 480 μg/L.
Yield was repeated by repeating the determination. the recoveries were 78.0% ~ 110% by the hot plate method. The final recoveries were 95.5%
19.6%. The recoveries were 79.0% ~ 101%, and the final recoveries were 95.0% ± 16.4%.
11 quality assurance and quality control
11.1 each bat...
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