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HJ 781-2016: Solid waste. Determination of 22 metal elements. Inductively coupled plasma optical emission spectrometry
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Solid waste. Determination of 22 metal elements. Inductively coupled plasma optical emission spectrometry
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Standard similar to HJ 781-2016 HJ 799 | HJ 662 | HJ/T 298 | HJ 783 | HJ 784 | HJ 782 | Basic data | Standard ID | HJ 781-2016 (HJ781-2016) | | Description (Translated English) | Solid waste. Determination of 22 metal elements. Inductively coupled plasma optical emission spectrometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z13 | | Word Count Estimation | 27,239 | | Date of Issue | 2016-02-01 | | Date of Implementation | 2016-03-01 | | Quoted Standard | GB 5086.1; HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300; HJ 557 | | Regulation (derived from) | ?Ministry of Environment Protection Bulletin 2016 No.10 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of solid waste and solid waste leaching solution 22 kinds of metal elements in inductively coupled plasma atomic emission spectrometry. This standard applies to the solid waste and solid waste leaching solution of silver (Ag), aluminum (Al), barium (Ba), beryllium (Be), calcium (Ca), cadmium (Cd), cobalt (Co), chromium, Copper, copper, iron, potassium, magnesium, manganese, sodium, lead, strontium, titanium, , Vanadium (CV), zinc (Zn), thallium (Ti) and antimony (Sb) were measured. If verified, this standard can also be applied to the determination of other trace metals. | HJ 781-2016: Solid waste. Determination of 22 metal elements. Inductively coupled plasma optical emission spectrometry
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Solid waste.Determination of 22 metal elements.Inductively coupled plasma optical emission spectrometry
National Environmental Protection Standard of the People 's Republic of China
Determination of 22 Kinds of Metal Elements in Solid Waste
Inductively Coupled Plasma Atomic Emission Spectrometry
Solid waste - Determination of 22 metal elements -
Inductively coupled plasma optical emission spectrometry
2016-02-01 release
2016-03-01 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
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 (normative appendix) Element method detection limit and lower limit of determination
Appendix B (informative) method of precision
Appendix C (informative) method of accuracy
Appendix D (informative) Elemental determination of wavelength and inter-element interference
Appendix E (informative) Standard Addition Method 22
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 of 22 kinds of metal elements of the determination method, the development of this standard.
This standard specifies the inductively coupled plasma emission of 22 metal elements in the determination of solid waste and solid waste leachate
Spectroscopy.
This standard is the first release.
Appendix A to this standard is a normative appendix, Appendix B, Appendix C, Appendix D and Appendix E 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
Station, Changzhou City Environmental Monitoring Center Station, Ma On Shan City Environmental Monitoring Center Station, Lianyungang City Environmental Monitoring Center Station.
This standard is approved by the Ministry of Environmental Protection on February 1,.2016.
This standard has been implemented since March 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Determination of 22 Kinds of Metal Elements in Solid Waste
Inductively Coupled Plasma Atomic Emission Spectrometry
Warning. The use of perchloric acid, nitric acid, hydrogen peroxide in the experiment is highly oxidizing and corrosive, hydrochloric acid, hydrofluoric acid
Strong volatile and corrosive, the operation should be required to wear protective equipment, solution preparation and sample pretreatment process should be in the process
Do not operate in a fume hood.
1 Scope of application
This standard specifies the determination of 22 kinds of metal elements in solid waste and solid waste leachate inductive coupling plasma emission
Spectroscopy.
This standard applies to the solid waste and solid waste leaching solution of silver (Ag), aluminum (Al), barium (Ba), beryllium (Be),
Calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg)
Manganese (Mn), sodium (Na), nickel (Ni), lead (Pb), strontium (Sr), titanium (Ti), vanadium (V), zinc (Zn)
Thallium (Tl), antimony (Sb) and other 22 kinds of metal elements. If verified, this standard may also apply to other trace amounts of gold
Determination of elements.
The amount of solid waste sample is 0.25 g. When the volume of the fixed volume is 25.0 ml, the detection limit of 22 kinds of metal elements is
0.04 mg/kg ~ 8.9 mg/kg, the determination of the lower limit of 0.16 mg/kg ~ 35.6 mg/kg. 22 kinds of metal elements in solid waste leaching solution
The detection limit of the method was 0.004 mg/L ~ 0.35 mg/L, and the lower limit was 0.016 mg/L ~ 1.40 mg/L. See Appendix A. for details.
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.
Solid waste leaching toxicity leaching method
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 leaching solution after acid digestion, into the plasma emission spectrometer atomizer was atomized,
From the argon carrier gas into the plasma torch, the target element in the plasma torch is gasified, ionized, excited and radiated
Sign line. The intensity of the characteristic spectrum is proportional to the content of the element to be measured in the sample within a certain range.
4 interference and elimination
4.1 spectral interference
Spectral disturbances mainly include continuous background and overlapping lines. The usual method of correcting spectral interference is the background subtraction method (root
According to single element test to determine the location and manner of subtracting the background) and the interference coefficient method. The base may also be used in a mixed standard solution
Body matching method to eliminate its effects.
When there is a single element interference, the interference coefficient can be obtained according to equation (1).
T Q
QQK) '(- = (1)
Where. tK - interference coefficient;
'Q - the content measured at the wavelength of the element;
Q - analysis of the content of elements;
TQ - the content of interfering elements.
By preparing a series of known interfering element content solutions, the 'Q is determined at the position of the elemental wavelengths,
(1) to find tK, and then artificial deduction or computer automatic deduction. Under normal circumstances, solid waste and solid waste leaching
The concentration of each element in the liquid sample is low, and the interference between the spectrum and the matrix element can be neglected. When the concentration of each element is high,
The target element determines the wavelength spectral interference and the relevant interference coefficient. Note that the interference factor for different instruments will be measured
do not.
4.2 Non-spectral interference
Non-spectral interference mainly includes chemical interference, ionization interference, physical interference and solvent interference, etc., in the actual analysis
It is difficult to separate the various types of interference. Whether it is compensated and corrected, and the concentration of interfering elements in the sample. In addition,
Physical disturbances are generally caused by changes in the degree of stickiness and surface tension of the sample, especially when the sample contains a large amount of soluble salts or
Acid is too high, will interfere with the determination. The most common way to eliminate such interference is dilution and standard addition.
The standard addition method is described in Appendix E.
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 concentrated sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
5.2 concentrated nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure.
5.3 concentrated 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) = 1.76 g/ml, excellent grade pure.
5.6 Hydrogen peroxide. φ (H2O2) = 30%, excellent grade pure.
5.7 nitric acid solution. 1 1 (v/v), prepared with concentrated nitric acid (5.2).
5.8 nitric acid solution. 1 99 (v/v), prepared with concentrated nitric acid (5.2).
5.9 Hydrochloric acid solution. 1 1 (v/v), prepared with concentrated hydrochloric acid (5.3).
5.10 single element standard stock solution. ρ = 1000 mg/L.
Can be made of high purity metal (purity greater than 99.99%) or metal salts (reference or high purity reagent) prepared into 1000 mg/L
Standard stock solution containing 1% nitric acid (5.8). You can also purchase commercially available standard solutions.
5.11 single element standard use of liquid.
Remove the single element standard stock solution (5.10) dilution preparation separately. Diluted with a certain amount of nitric acid (5.7), so that the standard
The nitric acid content of the quasi-use solution was 1%.
5.12 multi-element mixed standard solution.
According to the interference between the elements of the situation and the nature of the standard solution of the preparation, the concentration should be based on the sample and the test
Element, the viscosity of the standard solution as far as possible with the sample to be consistent with the acidity, are 1% nitric acid. Multi - element mixed standard dissolved
The liquid grouping is shown in Table 1.
Table 1 Multi-element mixed standard solution grouping table
Grouping elements
1 Ag, Be
2 V, Ti
3 Al, Ba, Fe, Mn, Ca, Mg, K, Na
4 Sr, Sb
5 Co, Cr, Cu, Ni, Pb, Zn
6 Cd, Tl
5.13 argon. purity not less than 99.99%.
6 instruments and equipment
6.1 Inductively Coupled Plasma Atomic Emission Spectrometer.
6.2 Microwave digestion. with program temperature control function, the maximum power range of 600 W ~ 1500 W.
6.3 temperature control heating plate. control accuracy ± 2.5 ℃.
6.4 Analytical balance. Accuracy ± 0.0001 g.
6.5 Teflon crucible. 50 ml.
6.6 Polytetrafluoroethylene crucible. 100 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 or dry semi-solid samples,
(M1, accurate to 0.01 g) sample, natural dry or freeze-dried, weighing again (m2, accurate to 0.01 g)
Grinding, all over 100 mesh sieve (6.7) spare.
7.2.2 Solid waste leachate
The preparation of solid waste leachate was carried out in accordance with the relevant provisions of HJ 557, HJ/T 299, HJ/T 300 or GB 5086.1.
Leaching solution if not timely analysis, should be concentrated nitric acid (5.2) acidification (1 L leaching solution by adding 10 ml nitric acid (5.2)),
And as soon as possible to digest, not more than 24 h.
7.3 Sample preparation
7.3.1 Solid waste samples
7.3.1.1 Microwave digestion method
For solid or dry semi-solid samples, weigh 0.1 g to 0.5 g (m3, accurate to 0.0001 g) sieve samples (7.2.1);
For semi-solid samples of liquid or no drying, 0.5 g (m3, accurate to 0.0001 g) samples (oil-containing solids
Waste should be less appropriate). Placed in a microwave digestion tank, with a small amount of water wet after adding 9 ml of concentrated nitric acid (5.2), 2 ml of concentrated salt
Acid (5.3), 3 ml hydrofluoric acid (5.4) and 1 ml hydrogen peroxide (5.6), and digested according to the warming procedure of Table 2. micro-
After the digestion of the sample, the sample should be cooled for at least 15 minutes and removed with a small amount of experimental water to transfer the entire contents of the microwave digestion tank
To 50 ml of polytetrafluoroethylene crucible (6.5), add 2 ml of perchloric acid (5.5), placed on a hot plate and heated to 160 ° C ~
180 ℃, driven to white smoke exhausted, and the contents were viscous. Remove the crucible slightly cold, add 2 ml of nitric acid solution (5.8),
Warm dissolution of the residue. After cooling, transfer to a 25 ml volumetric flask, rinse the crucible with the appropriate amount of nitric acid solution (5.8), the eluent
All transferred to the 25 ml volumetric flask, with nitric acid solution (5.8) constant volume to the mark, mix, to be measured.
Table 2 Solid Waste Microwave Digestion Refer to the temperature rise procedure
Heating time (min) Digestion temperature (℃) Holding time (min)
5 room temperature ~ 120 3
3 120 ~ 160 3
3 160 ~ 180 10
Note 1. After the final digestion is still particulate matter precipitation, you need to centrifuge or 0.45 μm film after the volume capacity.
Note 2. samples with high organic matter content, need to add 5 ml of concentrated nitric acid (5.2) soak overnight.
7.3.1.2 Electrothermal plate digestion method
For solid or dry semi-solid samples, weigh 0.1 g to 0.5 g (m3, accurate to 0.0001 g) sieve samples (7.2.1);
For semi-solid samples of liquid or no drying, 0.5 g (m3, accurate to 0.0001 g) samples (oil-containing solids
Waste should be less appropriate). Placed in a polytetrafluoroethylene crucible (6.5), in the fume hood, add 1 ml to the crucible
Water wet sample, add 5 ml of concentrated hydrochloric acid (5.3) placed on the hot plate to 180 ℃ ~.200 ℃ heated to near dry, remove the slightly cold.
Add 5 ml of concentrated nitric acid (5.2), 5 ml of hydrofluoric acid (5.4), 3 ml of perchloric acid (5.5), after capping on the hot plate at 180 ℃
Heat to 2 ml of excess liquid, continue heating and shake the crucible. When heated to smoke thick white smoke, stamped with black organic carbide
break down. After the black organic matter on the wall of the crucible disappears, open the lid, drive the white smoke and steam to the contents of the sticky. Depending on the situation
(5.2), 3 ml hydrofluoric acid (5.4), 1 ml perchloric acid (5.5), repeat the above digestion
Process Remove the crucible slightly cold, add 2 ml of nitric acid solution (5.8), dissolve the soluble residue in warm. After cooling, transfer to 25 ml
In the volumetric flask, the crucible was rinsed with the appropriate amount of nitric acid solution (5.8), and the eluent was transferred to the volumetric flask. The solution was washed with nitric acid solution (5.8)
Constant volume to the marking, mixing, to be measured.
Note 3. samples with higher organic matter content, need to add 5 ml of concentrated nitric acid (5.2) soak overnight.
7.3.2 Solid waste leachate sample
7.3.2.1 Microwave digestion method
Measure the solid waste leaching solution (7.2.2) 25.0 ml into the microwave digestion tank, add 5 ml of concentrated nitric acid (5.2), press
Microwave digestion instrument instructions installed with digestion tank, according to Table 3 of the temperature program to digest. After the digestion process, digestion tank should be
In the microwave digestion machine to cool to room temperature. Put into the fume hood carefully open the digestion tank cover, with a small amount of experimental water will be microwave
The contents of the digestion tank were transferred to a 100 ml polytetrafluoroethylene crucible (6.6) and heated on a hot plate at 180 ° C
1 hour, remove the crucible slightly cold. Transferred to 25 ml volumetric flask, rinse the crucible with the appropriate amount of nitric acid solution (5.8), the eluent
All transferred to the 25 ml volumetric flask, with nitric acid solution (5.8) constant volume to the mark, mix, to be measured.
Table 3 Solid Waste Leach Solution Microwave Digestion Refer to the temperature rise procedure
Heating time (min) Digestion temperature (℃) Holding time (min)
10 room temperature ~ 150 5
5 150 ~ 180 5
Note 4. more types of solid waste, organic matter contained in a large difference, the amount of acid digestion can be digested as appropriate circumstances increase or decrease;
The degree should not be too high to prevent the deformation of PTFE crucible; sample digestion, to prevent dry, so as not to be measured element loss.
Note 5. The sum of the volume of the sample and the addition acid should not exceed 1/3 of the volume of the digestion tank.
7.3.2.2 Heater digestion method
Measure the solid waste leachate sample (7.2.2) 25.0 ml In a 100 ml polytetrafluoroethylene crucible (6.6), add 5 ml
Concentrated nitric acid (5.2), and heated and digested on a hot plate at 180 ° C for 1 to 2 hours. If there are particles or precipitation, need to drop concentrated nitric acid
(5.2) 2 ml Continue to heat digestion until the solution is clear. Rinse the crucible with the appropriate amount of nitric acid solution (5.8), the eluent all
Transferred to 25 ml volumetric flask, with nitric acid solution (5.8) constant volume to the mark, mix, to be measured.
7.3.3 Preparation of blank samples
7.3.3.1 Solid waste blank
The solid waste blank sample was prepared by adding the same procedure as the sample preparation procedure (7.3.1).
7.3.3.2 Solid waste leachate blank
Prepare the extract as an experimental water using the same procedure as in the preparation of solid waste leachate (7.2.2)
The preparation of the solid waste leachate blank is carried out according to the same procedure as for the preparation of the solid waste leaching solution (7.3.2).
8 Analysis steps
8.1 Instrument reference measurement conditions
Different models of the best test conditions of different instruments, according to the instrument specification requirements to optimize the test conditions. Instrument reference measurement
The conditions are shown in Table 4.
Table 4 Instrument reference measurement conditions
High-frequency power (kW) Reflective power (W) Carrier gas flow (L/min) Peristaltic pump speed (rpm) Flow rate (ml/min) Measuring time (s)
1.0 to 1.6 < 5 1.0 to 1.5 100 to 120 0.2 to 2.5 1 to 20
Ignite the plasma, according to the manufacturers to provide the operating parameters set, until the instrument preheat to the indicators after the stability of the open
Start the measurement.
8.2 Drawing of calibration curves
Followed by the preparation of a series of standard elements to be tested, according to the actual sample to be measured in the concentration of elements to adjust the calibration curve
Line concentration range. Respectively, to remove a certain volume of multi-element mixed standard solution (5.12), with nitric acid solution (5.8) preparation
Series of standard curve, the reference concentration in Table 5. The standard solution is introduced from the low concentration to the high concentration into the inductively coupled plasma
The spectrometer measures the emission intensity according to the instrument reference measurement conditions (8.1). To the target element series of mass concentration for the abscissa,
The emission intensity is the ordinate and the calibration curve of the target element is established.
Table 5 Standard Series Solution Reference Concentration Unit. mg/L
Element Concentration 1 Concentration 2 Concentration 3 Concentration 4 Concentration 5 Concentration 6
Silver (Ag), beryllium (Be), thallium (Tl), cadmium (Cd) 0.00 0.20 0.40 0.60 0.80 1.00
Cobalt (Co), chromium (Cr), copper (Cu), nickel (Ni),
Lead (Pb), strontium (Sr), titanium (Ti), vanadium (V),
Zinc (Zn), antimony (Sb)
0.00 1.00 2.00 3.00 4.00 5.00
Aluminum (Al), barium (Ba), iron (Fe), manganese (Mn),
Calcium (Ca), magnesium (Mg), potassium (K), sodium (Na)
0.00 5.00 10.0 15.0 20.0 25.0
8.3 Determination
8.3.1 Specimen determination
Before the analysis, rinse the system with nitric acid solution (5.8) until the blank intensity value is minimized, and after the analysis signal is stabilized,
The sample was analyzed under the same conditions as the calibration curve (7.3). During sample determination, if the measured element concentration exceeds the calibration
Curve range, the sample to be diluted after re-determination.
8.3.2 Determination of blank samples
The blank sample (7.3.3) was measured according to the same procedure as for the sample measurement.
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 metal elements in solid waste (mg/kg) is calculated according to formula (2)
()
001ω
V ×× - = ρρ (2)
Where. ω - the content of metal elements in solid waste, mg/kg;
1 - The calibration curve was used to determine the concentration of metal elements in the sample, mg/L;
0ρ - the measured concentration of the blank sample, mg/L;
0V - volume of the sample after digestion, ml;
1m - the amount of solid waste sample weighed, g;
2m - weight of solid waste sample after air drying or freeze drying, g;
3m - the amount of solid waste sample after grinding and sieving, g.
9.1.1.2 Semi-solid solid waste with or without drying
The content of metal elements in solid waste (mg/kg) is calculated according to formula (3)
()
001ω
V × - = ρρ (3)
Where. ω - the content of metal elements in solid waste, mg/kg;
1 - The calibration curve was used to determine the concentration of metal elements in the sample, mg/L;
0ρ - the measured concentration of the blank sample, mg/L;
0V - volume of the sample after digestion, ml;
3m - the amount of sample weighed, g.
9.1.2 Solid waste leachate
The concentration of metal elements in the solid waste leaching solution ρ (mg/L) is calculated according to the formula (4)
V 001) (× - = ρρρ (4)
Where. ρ - solid waste leaching solution concentration of metal elements, mg/L;
1 - The calibration curve was used to determine the concentration of metal elements in the ...
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