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HJ 787-2016: Solid waste. Determination of lead and cadmium. Graphite furnace atomic absorption spectrometry
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Solid waste. Determination of lead and cadmium. Graphite furnace atomic absorption spectrometry
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HJ 787-2016
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Basic data | Standard ID | HJ 787-2016 (HJ787-2016) | | Description (Translated English) | Solid waste. Determination of lead and cadmium. Graphite furnace atomic absorption spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z13 | | Word Count Estimation | 13,175 | | Date of Issue | 2016-03-29 | | Date of Implementation | 2016-05-01 | | Quoted Standard | HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557 | | Regulation (derived from) | Ministry of Environmental Protection Announcement No | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 787-2016: Solid waste. Determination of lead and cadmium. Graphite furnace atomic absorption spectrometry
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Solid waste.Determination of lead and cadmium.Graphite furnace atomic absorption spectrometry
National Environmental Protection Standard of the People 's Republic of China
Determination of Lead and Cadmium in Solid Waste
Graphite Furnace Atomic Absorption Spectrophotometry
Solid waste-Determination of Lead and Cadmium - Graphite Furnace Atomic
Absorption Spectrometry
2016-03-29 released
2016-05-01 implementation
Ministry of Environmental Protection
Directory
Preface iii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples .3
8 Analysis steps
9 Results calculation and presentation
10 precision and accuracy
Quality assurance and quality control
12 Waste treatment
13 Precautions
Appendix A (informative appendix) Standard addition method error! Undefined bookmarks. 0
Appendix B (informative) method of precision and accuracy. Undefined bookmarks. 1
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 lead and cadmium determination method, the development of this standard
quasi.
This standard specifies the graphite furnace atomic absorption spectrophotometric method for the determination of lead and cadmium 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. Jiangsu Province Environmental Monitoring Center.
The standard verification unit. Nanjing Environmental Monitoring Center Station, Zhejiang Province Environmental Monitoring Center, Shanghai Environmental Monitoring Center,
Changzhou City Environmental Monitoring Center Station, Ma On Shan City Environmental Monitoring Center Station, Lianyungang City Environmental Monitoring Center Station.
The environmental protection department of this standard approved on March 29,.2016.
This standard has been implemented since May 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Solid waste - Determination of lead and cadmium - Graphite furnace atomic absorption spectrophotometric method
Warning. nitric acid used in the experiment, perchloric acid with strong oxidizing and corrosive, hydrochloric acid, hydrofluoric acid with strong volatile
And corrosive, the operation should be required to wear protective equipment, solution preparation and sample pretreatment process should be in the fume hood into
Line operation.
1 Scope of application
This standard specifies the graphite furnace atomic absorption spectrophotometric method for the determination of lead and cadmium in solid waste and solid waste leachate.
This standard is applicable to the determination of lead and cadmium in solid waste and solid waste leachate.
When the amount of solid waste is 0.5 g and the volume of the volume is 25 ml after digestion, the detection limits of lead and cadmium are 0.3
Mg/kg and 0.1 mg/kg, with a lower limit of 1.2 mg/kg and 0.4 mg/kg, respectively. When the solid waste leachate is sampled in volume
50 ml, digested to 50 ml, the lead and cadmium detection limit were 0.9 μg/L and 0.6 μg/L, the determination of the lower limit
Do not be 3.6 μg/L and 2.4 μg/L.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the 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 acid digestion, into the graphite furnace atomizer, after drying, ashing and the original
Sub-atomization, as the ground state of the vapor, the element of the hollow cathode lamp or electrodeless discharge lamp emission characteristics of the radiation line selectivity
absorb. In a certain concentration range, the absorption intensity and the sample to be measured in proportion to the mass concentration.
4 interference and elimination
When the mass concentration of Ca in the sample is higher than 500 mg/L, the mass concentration of Fe is higher than 50 mg/L, the mass concentration of Mn is high
At 25 mg/L, the determination of lead and cadmium interference, sample dilution method or standard addition method to eliminate its interference. solid
Waste matrix composition is more complex, adding matrix modifier ammonium dihydrogen phosphate, can eliminate the organic matter caused by matrix interference. when
When the sample matrix composition is unknown or the recoveries are more than the range of the control requirements of this method, the standard addition method should be used to measure
And calculate the results, see Appendix A.
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 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.2 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure.
5.4 hydrofluoric acid. ρ (HF) = 1.49 g/ml, excellent grade pure.
5.5 perchloric acid. ρ (HClO4) = 1.68 g/ml, excellent grade pure.
5.6 Hydrogen peroxide. φ (H2O2) = 30%, excellent grade pure.
5.7 Metal Lead. Spectrum Pure.
5.8 Metal cadmium. Spectrum pure.
5.9 Ammonium dihydrogen phosphate (NH4H2PO4). excellent grade pure.
5.10 nitric acid solution. 1 9 (v/v), prepared with nitric acid (5.2).
5.11 nitric acid solution. 1 99 (v/v), prepared with nitric acid (5.2).
5.12 hydrochloric acid solution. 1 1 (v/v), prepared with hydrochloric acid (5.3).
5.13 matrix modifier. ammonium dihydrogen phosphate solution.
Accurately weigh 13.8 g (accurate to 0.0001 g) ammonium dihydrogen phosphate (5.9), dissolved with experimental water and set to 1000 ml.
5.14 lead standard stock solution. ρ = 1000 mg/L.
Accurately weigh 1.000 g (accurate to 0.0001 g) of metal lead (5.7), add 15 ml of nitric acid (5.2) to dissolve, if necessary
Can be dissolved by heating. The whole volume into the 1000 ml volumetric flask, with nitric acid solution (5.11) constant volume to the mark, shake. Can also be used
Commercially available standard solution.
5.15 cadmium standard stock solution. ρ = 1000 mg/L.
Accurately weigh 1.000 g (accurate to 0.0001 g) of metal cadmium (5.8), add 15 ml of nitric acid (5.2) to dissolve, if necessary
Can be dissolved by heating. The whole volume into the 1000 ml volumetric flask, with nitric acid solution (5.11) constant volume to the mark, shake. Can also be used
Commercially available standard solution.
5.16 Lead Standard Intermediate. ρ = 100 mg/L.
Accurate removal of lead standard stock solution (5.14) 10.0 ml in 100 ml volumetric flask, with nitric acid solution (5.11) constant volume to standard
Line, shake well. Pro is now available.
5.17 cadmium standard intermediate liquid. ρ = 100 mg/L.
Accurate removal of cadmium standard stock solution (5.15) 10.0 ml in 100 ml volumetric flask, with nitric acid solution (5.11) constant volume to standard
Line, shake well. Pro is now available.
5.18 lead standard use of liquid. ρ = 1.00 mg/L.
Accurate removal of lead standard intermediate (5.16) 1.00 ml in 100 ml volumetric flask, with nitric acid solution (5.11) constant volume to standard
Line, shake well. Pro is now available.
5.19 cadmium standard use of liquid. ρ = 1.00 mg/L.
Accurate removal of cadmium standard intermediate (5.17) 1.00 ml in 100 ml volumetric flask, with nitric acid solution (5.11) constant volume to standard
Line, shake well. Pro is now available.
5.20 high purity argon. purity of not less than 99.999%.
6 instruments and equipment
6.1 Graphite Furnace Atomic Absorption Spectrophotometer (with background correction function).
6.2 lead hollow cathode lamp, cadmium hollow cathode lamp.
6.3 electric plate or graphite digestion. with temperature control function (temperature stability ± 5 ℃), the maximum temperature can be set to.200 ℃.
6.4 Microwave digestion. Output power 1000 W ~ 1600 W. With programmable control function, can be temperature, pressure and time
(Heating time and holding time) to monitor the whole; with security features.
6.5 Analysis of the balance. accuracy of 0.1 mg.
6.6 Teflon crucible. 50 ml.
6.7 sieve. non-metallic sieve, 100 mesh.
6.8 Common laboratory equipment and equipment.
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 waste or dry semi-solid waste
Product, accurately weighed 10 g (m1, accurate to 0.01 g) sample, naturally air-dried or freeze-dried, weighing again (m2, accurate to
0.01 g), grinding, all over 100 mesh sieve (6.7) standby.
7.2.2 Solid waste leachate
The preparation of solid waste leachate was carried out in accordance with the relevant provisions of HJ/T 299, HJ/T 300 or HJ 557. If the leaching solution does not
Can be timely analysis, should be added nitric acid (5.2) acidification to pH < 2, can be stored for 14 d.
7.3 Preparation of samples
7.3.1 Solid waste samples
7.3.1.1 Electric plate digestion method
Weigh the sample (m3, exact to 0.1 mg) after sieving 0.25 g to 1.00 g in a 50 ml polytetrafluoroethylene crucible (6.6)
in. After wetting the sample with a small amount of water, add 5 ml of hydrochloric acid (5.3) and add about 120 ° C to the hot plate (6.3) in the fume hood
Heat, so that the initial digestion of the sample, to be evaporated to about 3 ml when removed slightly cold. Add 5 ml nitric acid (5.2), 5 ml hydrofluoric acid (5.4),
3 ml perchloric acid (5.5), capped and heated at about 160 ° C for 1 h on a hot plate. Open lid, hot plate temperature control at 180 ℃ ± 5 ℃
Continue to heat, and often shake the crucible. When heated to smoke thick smoke, capped to make black organic carbide fully decomposed. To be crucible
After the black organic matter on the wall of the wall disappears, the lid is opened and the white smoke is driven and the contents are viscous. Depending on the situation, can be added 3
Ml of nitric acid (5.2), 3 ml of hydrofluoric acid (5.4) and 1 ml of perchloric acid (5.5). When the white smoke again
Exhausted and the contents were viscous, remove the crucible slightly cold, add 1 ml of nitric acid solution (5.11) warm dissolved soluble residue,
After cooling the whole transfer to 25 ml volumetric flask, with the right amount of experimental water rinse the crucible lid and the inner wall, lotion into the 25 ml volumetric flask,
With the experimental water volume to the mark, shake, to be measured. If the digestion solution contains undissolved particles, need to be filtered, centrifugal points
Or natural settlement.
Note 1. Do not expose the sample to a large number of bubbles when heating, otherwise it will cause the loss of the sample.
Note 2. If the content of lead or cadmium in solid waste is high, the volume of volume after digestion can be determined according to the actual situation.
Note 3. 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 the sample (m3, accurate to 0.1 mg) after sieving 0.25 g to 1.00 g in a microwave digestion tank. Wet with a small amount of water
After adding 5 ml of nitric acid (5.2), 5 ml of hydrochloric acid (5.3), 3 ml of hydrofluoric acid (5.4) and 1 ml of hydrogen peroxide (5.6)
According to Table 1 of the temperature program to digest. After cooling, the contents of the microwave digestion tank were transferred to 50 ml of polytetrafluoroethylene
Crucible, add 1 ml of perchloric acid (5.5), placed on the hot plate 170 ℃ ~ 180 ℃ to drive white smoke, to the contents of the sticky.
Remove the crucible slightly cold, add 1 ml of nitric acid solution (5.11), dissolve the soluble residue in warm, after cooling the total transfer to 25 ml
Capacity bottle, with the amount of experimental water rinse the crucible lid and the inner wall, lotion into the 25 ml volumetric flask, with the experimental water volume to the mark,
Shake, test. If the digestion solution contains undissolved particles, need to be filtered, centrifugal or natural sedimentation.
Table 1 Solid Waste Microwave Digestion Method
Heating time (min) Digestion power (W) Digestion temperature (℃) Holding time (min)
12 400 room temperature ~ 160 3
5 500 160 ~ 180 3
5 500 180 ~.200 10
7.3.2 Solid waste leachate sample
7.3.2.1 Electric plate digestion method
Measure 50 ml of leachate (7.2.2) in a 150 ml Erlenmeyer flask, add 5 ml nitric acid (5.2) and shake it. In the triangular bottle mouth
Insert a small funnel, placed on the hot plate at 120 ℃ heating, in the micro-boiling state of the sample heated to about 5 ml, remove the cooling. Add 3
Ml of nitric acid (5.2), add 1 ml of perchloric acid (5.5) until the digestion is complete (digestion clarification, or digestion color and transparency
The degree is no longer changed), continue at 180 ° C evaporation to near dry, remove the cooling, add 1 ml of nitric acid solution (5.11), warm dissolved
Soluble residue, after cooling with the amount of experimental water leaching small funnel and the inner wall of the flask, the amount of digestion solution to 50 ml capacity
Measuring bottles, with the experimental water volume to the mark, shake, to be measured. If the digestion solution contains more impurities, need to be filtered, away from
Heart separation or natural settlement.
7.3.2.2 Microwave digestion method
Measure 50 ml leachate (7.2.2) (according to digestion tank volume and sample concentration to determine the amount of leaching volume to take the volume, the most
The final solution volume should not exceed the limit specified by the instrument) in the microwave digestion tank, add 5 ml of nitric acid (5.2), according to the instructions
Require to tighten the digestion tank. Place the digestion tank on the microwave oven. According to Table 2 of the temperature program to digest. After digestion,
To be digested in the microwave digestion tank to cool to room temperature after the removal. Put it into the fume hood carefully to open the lid of the digestion tank and release it
In the gas. The amount of digestion solution transferred to the polytetrafluoroethylene crucible, with the amount of experimental water rinse digestion tank wall, lotion and
Into the polytetrafluoroethylene crucible, in the hot plate in the state of micro-boiling heated to near dry. With the amount of experimental water rinse crucible inner wall,
The contents of the crucible and lotion transferred to 50 ml volumetric flask, with the experimental water volume to the mark, shake, to be measured. If the consumer
The solution contains more impurities, need to be filtered, centrifugal separation or natural settlement.
Table 2 Solid Waste Leach Solution Microwave Digestion Method
Heating time (min) Digestion power (W) Digestion temperature (℃) Holding time (min)
10 400 room temperature ~ 150 5
5 500 150 ~ 180 5
Note 4. Due to the large number of solid wastes, the organic matter contained a large difference, and the amount of each acid in digestion can be increased or decreased as appropriate.
The temperature of the hot plate should not be too high to prevent the deformation of the PTFE crucible; sample digestion, to prevent the dry, so as to avoid the loss of element to be measured.
7.3.3 Preparation of blank samples
7.3.3.1 Solid waste blank
The empty waste sample was prepared using the empty container according to the procedure of 7.3.1.
7.3.3.2 Solid waste leachate blank
Using the experimental water prepared as a leaching agent, according to 7.2.2 preparation of solid waste leachate blank, according to the steps of 7.3.2 into
Line digestion.
8 Analysis steps
8.1 Instrument reference conditions
Different models of graphite furnace atomic absorption spectrophotometer the best measurement conditions are different, according to the instrument manual requirements
Optimize test conditions. The instrument reference measurement conditions are shown in Table 3.
Table 3 Instrument reference measurement conditions
Elemental lead (Pb) cadmium (Cd)
Determination of wavelength (nm) 283.3 228.8
Lamp current (mA) 8.0 6.0
Passband width (nm) 0.5 0.5
Drying temperature (℃)/time (s) 85 ~ 120/20 85 ~ 120/45
Ashing temperature (° C)/time (s) 400/5 250/5
Atomic temperature (° C)/time (s) 2100/3 1800/3
Elimination temperature (° C)/time (s) 2200/2.2000/3
Whether the atomic phase is stopped
Argon flow rate (L/min) 3.0 3.0
Injection volume (l) 20 20
Substrate modifier (l) 5 5
8.2 Standard curve drawing
8.2.1 Lead Standard Curve Series
Respectively, accurate removal of 0.00 ml, 0.50 ml, 1.00 ml, 2.00 ml, 4.00 ml and 5.00 ml lead standard use of liquid (5.18)
In a group of 100 ml volumetric flask, with nitric acid solution (5.11) constant volume to the mark, shake. This standard series lead is 0.00
Μg/L, 5.00 μg/L, 10.0 μg/L, 20.0 μg/L, 40.0 μg/L and 50.0 μg/L, respectively. According to the instrument reference conditions (8.1),
After adjusting the instrument zero with nitric acid solution (5.11), the standard series was inhaled from low concentration to high concentration, and the corresponding absorbance was measured
Degree, with the corresponding absorbance as the ordinate, lead standard series of mass concentration for the abscissa, the establishment of lead calibration curve.
8.2.2 Cadmium standard curve series
0.10 ml, 0.20 ml, 0.30 ml, 0.40 ml and 0.50 ml of cadmium standard solution (5.19), respectively,
In a group of.200 ml volumetric flask, with nitric acid solution (5.11) constant volume to the mark, shake. This standard series of cadmium were 0.00
Μg/L, 0.50 μg/L, 1.00 μg/L, 1.50 μg/L, 2.00 μg/L and 2.50 μg/L, respectively. According to the instrument reference conditions (8.1),
After adjusting the instrument zero with nitric acid solution (5.11), the standard series was inhaled from low concentration to high concentration, and the corresponding absorbance was measured
Degree, with the corresponding absorbance as the ordinate, cadmium standard series of mass concentration for the abscissa, the establishment of cadmium 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
The prepared sample (7.3.1 or 7.3.2) was subjected to the same conditions as the established calibration curve.
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 the element to be measured in solid waste (mg/kg) Calculated according to formula (1)
(1)
Where. - the content of the element to be measured in the solid waste, mg/kg;
- Check the mass concentration of the element in the sample by the calibration curve, mg/L;
0_1 - Mass concentration in the laboratory blank sample, mg/L;
0V - volume of the sample after digestion, ml;
1m - the amount of solid waste sample weighed before drying, g;
2m - the quality of solid waste samples after 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 the element to be measured in solid waste (mg/kg) Calculated according to formula (2)
V
(2)
Where. - the content of the element to be measured in the solid waste, mg/kg;
- Check the mass concentration of the element in the sample by the calibration curve, mg/L;
0_1 - Mass concentration in the laboratory blank sample, mg/L;
0V - volume of the sample after digestion, ml;
3m - the amount of solid waste sample weighed, g.
9.1.2 Solid waste leachate
Concentration of the element to be measured in the solid waste leachate (mg/L) Calculated according to equation (3).
V001) - (
(3)
Where. - mass concentration of the element to be tested in the solid waste leachate, mg/L;
1 - Check the mass concentration of the element in the sample by the calibration curve, mg/L;
0_1 - Mass concentration in the laboratory blank sample, mg/L;
V - Sampling volume when digested with solid waste leachate, ml;
0V - solid waste leachate after digestion of the sample volume, ml.
9.2 The result is shown
For solid waste, when the result is less than 100 mg/kg, one after the decimal point is retained; when the result is greater than or equal
At 100 mg/kg, three valid digits are retained.
For solid waste leachate, when the determination results less than 1.00 mg/L, the retention of two decimal places; when the determination of large
At or equal to 1.00 mg/L, retain three valid digits.
10 precision and accuracy
10.1 Precision
The ESS-1, GSS-1 and ISS-2 standard samples of lead and cadmium were tested six times in six laboratories.
The relative standard deviation...
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