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LY/T 3129-2019: Determination of the total copper, zinc, iron and manganese in forest soils by Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES)
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Determination of the total copper, zinc, iron and manganese in forest soils by Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES)
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LY/T 3129-2019
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Basic data | Standard ID | LY/T 3129-2019 (LY/T3129-2019) | | Description (Translated English) | Determination of the total copper, zinc, iron and manganese in forest soils by Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES) | | Sector / Industry | Forestry Industry Standard (Recommended) | | Classification of Chinese Standard | B10 | | Classification of International Standard | 13.080.10 | | Word Count Estimation | 14,147 | | Date of Issue | 2019-10-23 | | Date of Implementation | 2020-04-01 | | Regulation (derived from) | Announcement of the State Forestry and Grassland Administration No. 17 of 2019 | | Issuing agency(ies) | State Forestry and Grassland Administration | LY/T 3129-2019: Determination of the total copper, zinc, iron and manganese in forest soils by Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES)
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(Determination of total copper, zinc, iron and manganese in forest soils-Inductively coupled plasma emission spectrometry)
ICS 13.080.10
B 10
LY
People's Republic of China Forestry Industry Standard
Determination of total copper, zinc, iron, and manganese in forest soils
Coupled plasma emission spectrometry
Determination of the total copper, zinc, iron and manganese in forest soils by
Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES)
2019-10-23 released
2020-04-01 implementation
Published by the National Forestry and Grassland Administration
Contents
Foreword ... II
1 Scope ... 1
2 Normative references ... 1
3 Notes ... 1
4 Method summary ... 1
5 Reagents and materials ... 2
6 Instruments and equipment ... 2
7 Analysis steps ... 3
8 Quality Assurance and Quality Control ... 5
Appendix A (informative) Mass concentration of standard solution series ... 6
Appendix B (informative) Reference conditions for instrument operation ... 7
References ... 8
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard is proposed and managed by the State Forestry and Grassland Administration.
This standard was drafted. Forestry Research Institute of Chinese Academy of Forestry, Beijing Forestry University, Chinese Academy of Forestry Subtropical Forest
Industry Research Institute, Beijing Huaxue North Testing Technology Co., Ltd.
The main drafters of this standard. Jiao Ruzhen, Dong Yuhong, Hou Lingyu, Sun Qiwu, Geng Yuqing, Qu Minghua, Tian Yan, Zhang Ying, Ni Zhang Lin,
Yue Zhiyi, Wen Zhaocheng, Xu Zhicheng.
Determination of total copper, zinc, iron and manganese in forest soils-Inductively coupled plasma emission spectrometry
1 Scope
This standard specifies the determination of the total amount of copper (Cu), zinc (Zn), iron (Fe), and manganese (Mn) in forest soils by inductively coupled plasma.
Emission Spectroscopy (ICP-OES).
This standard applies to the determination of copper, zinc, iron, and manganese in forest soils.
2 Normative references
The following documents are essential for the application of this document. For dated references, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
Preparation of preparations and products used in GB/T 603 chemical reagent test method
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 4842 Argon
LY/T 1210 Collection and preparation of forest soil samples
3 matters needing attention
Some of the reagents used in the experiment are toxic or corrosive. The operation of adding acid, digestion, and acid drive should be performed in a fume hood.
Protective equipment should be worn in accordance with regulations to avoid contact with skin and clothing. If accidentally splashed on the skin, immediately use spray facilities or clean water.
Contamination should be prevented during sampling and sample preparation. The vessel used in the sample analysis process should be soaked with 10 90 nitric acid solution for 24 h.
Then rinse with tap water and experimental water in order, and dry in a clean environment for later use.
The main source of errors in the determination of copper, zinc, iron, and manganese is whether the sample is completely digested. During the actual measurement, it can be based on the difference in soil organic matter.
Adjust the amount of nitric acid, hydrochloric acid and hydrofluoric acid appropriately.
During the digestion using a microwave digester, attention should be paid to the requirements of the corresponding instrument and the temperature and pressure limitations of the digestion tank to avoid
Bursting can cause personal and instrument damage.
ICP-OES cannot open the rectangular chamber door or rectangular tube chamber after igniting the plasma to prevent high frequency radiation from causing harm to personnel.
Due to the differences in the manufacturer and model of the instrument used in each laboratory, the instrument safety and operating instructions are different. List all relevant
The recommendations are beyond the scope of this method. You can refer to the relevant instrument manual, consult the manufacturer, or consult the literature on safe operation.
4 Method summary
Soil samples are mixed with acid, digested by electric hot plate, graphite digestion furnace, microwave digestion instrument or automatic digestion instrument, and then inductively coupled to plasma
The daughter emission spectrometer (ICP-OES) was used for detection.
The digested sample enters the atomizer of the plasma emission spectrometer to be atomized, and is carried into the plasma torch by the argon carrier gas.
The element is vaporized, ionized, excited and radiates characteristic lines in the plasma torch. The intensity of the characteristic spectral line and the content of the test element in the sample
It is proportional to a certain concentration range.
5 Reagents and materials
5.1 Reagents
5.1.1 Water.
The deionized or distilled water used should meet the specifications for secondary water in GB/T 6682. It is recommended to use the same batch of water in the same batch.
5.1.2 Hydrofluoric acid. excellent grade pure, concentration ω (HF) = 40%...
5.1.3 Nitric acid. excellent grade pure, ω (HNO3) = 65%.
5.1.4 Perchloric acid. excellent grade pure, ω (HClO4) = 70%.
5.1.5 Hydrochloric acid. excellent grade, ω (HCl) = 36%.
5.1.6 Hydrogen peroxide. super pure, ω (H2O2) = 30%.
5.1.7 Argon. purity ≥99.99%.
5.2 Reagent preparation
5.2.1 Nitric acid solution (1 99).
Take 10 mL of nitric acid, slowly add to 990 mL of water, and mix.
5.2.2 Nitric acid solution (10 90).
Take 100 mL of nitric acid, slowly add it to 900 mL of water, and mix well.
5.3 Standard solution
5.3.1 Element Standard Stock Solution
Use high-purity metals (purity greater than 99.99%) or metal salts (reference or high-purity reagents), configured to 100 mg/L or 1000 mg/L
Standard solution of copper, zinc, iron, and manganese containing nitric acid solution, the acidity of the solution should be kept above 1% (v/v) Or use national certification and award
Standard solution for quasi-substance certificates.
5.3.2 Preparation of standard series solutions
Accurately absorb the appropriate amount of element standard stock solution, and dilute with nitric acid solution (1 99) to prepare a mixed standard solution series, each element
See Appendix A.1 for mass concentration. According to the element concentration in the sample solution, the element concentration range of the standard series can be adjusted appropriately.
6 Instruments and equipment
6.1 Inductively coupled plasma emission spectrometer.
6.2 Electric heating plate. The temperature control accuracy is ± 2.5 ℃.
6.3 Graphite digestion furnace. equipped with Teflon digestion tank.
6.4 Microwave Digestion Apparatus. The temperature accuracy is ± 2.5 ° C, equipped with a polytetrafluoroethylene digestion tank.
6.5 Acid drive. acid drive equipment for microwave digestion.
6.6 Automatic digestion instrument. equipped with PTFE digestion tank.
6.7 Balance. Accuracy is 0.0001 g.
6.8 PTFE crucible. 50 mL.
6.9 Soil sieve. non-metal sieve, 0.149 mm (100 mesh).
6.10 Platinum crucible tongs.
6.11 Protective gloves.
6.12 Common laboratory equipment.
7 Analysis steps
7.1 Sample preparation
Prepare laboratory samples according to LY/T 1210.
7.2 Determination of moisture content
Determine the moisture conversion factor of the sample according to LY/T 1210.
7.3 Sample preparation
7.3.1 Total resolution
Weigh 0.1 ~ 0.5 g (accurate to 0.0001g) of air-dried soil that passed through a 0.149 mm sieve in a 50 mL polytetrafluoroethylene crucible or graphite digestion furnace.
Inside a polytetrafluoroethylene digestion tank, wet with a small amount of water, add 5 mL of hydrofluoric acid, 3 mL of nitric acid and 3 mL of perchloric acid in order, and gently shake to make
The sample is thoroughly mixed with the digestive acid, and the air bubbles are exhausted, and the cap is capped.
Put the crucible or digestion tank on a hot plate or graphite digestion furnace, first digest at low temperature of 130 ° C for 1 h, then gradually increase to high temperature of.200 ° C for digestion.
When starting to emit white smoke, wear protective gloves or remove the lid with crucible pliers, and gently shake the crucible or digestion tank to fully react the liquid and soil mixing.
When the perchloric acid has exhausted white smoke and the sample is pasty, continue to heat until it is nearly dry, and the residue is colorless and transparent or bright yellow, which means that the digestion is complete. in case
The residue appears gray, indicating incomplete digestion. Add 1 mL of perchloric acid and 3 mL of hydrofluoric acid, and continue to cook until digestion is complete.
Remove the crucible or digestion tank and cool to room temperature, add 5 mL of nitric acid solution (10 90), heat to dissolve the residue, and after cooling, transfer completely
Into a 50 mL volumetric flask, wash the crucible or Teflon digestion tank with water, transfer all the washing liquid to the volumetric flask, and finally make up the volume with water
Shake well and let it stand.
7.3.2 Microwave Digestion
Accurately weigh 0.1 ~ 0.5 g of air-dried soil passing through a 0.149 mm sieve (accurate to 0.0001 g) in a polytetrafluoroethylene digester supporting a microwave digester
Untie the jar, moisten it with a small amount of water, and add 2 mL of hydrochloric acid, 3 mL of hydrofluoric acid, and 6 mL of nitric acid (8 mL < total solution volume < 30 mL) in this order.
Gently shake to fully mix the sample with the digestive acid. After the air bubbles are exhausted, cover. Weigh each digestion tank.
Put the digestion tank into the digestion tank holder and place it in the microwave digester oven cavity. Use the working procedure recommended by the instrument manufacturer to set the temperature range
Refer to Appendix B.1 for the reference heating procedure. After digestion, cool to room temperature. Take out the digestion tank, weigh each tank, before and after digestion
The weight difference should be less than 10% ~ 15%. If the weight after digestion exceeds the weight before digestion by more than this value, discard the sample and find
the reason.
Slowly open the inner lid of the digestion tank for venting, and wash the inner lid of the digestion tank with water. Transfer the washing liquid to the digestion tank and continue to the digestion tank.
Add 1 mL of perchloric acid or 1 mL of hydrogen peroxide and use an acid analyzer to catch the acid. If no acid drive is available, transfer the solution from the digestion tank to Teflon
In the ethylene crucible, after washing the inside of the digestion tank and the digestion tank with a little water, the washing liquid was completely transferred into the crucible, and the crucible was placed on a hot plate on the
The acid is removed in a slightly boiling state.
When the digestion solution is viscous, colorless and transparent or bright yellow, cool, dissolve in 5 mL nitric acid solution (10 90), and transfer into a 50 mL container.
In a measuring flask, wash the crucible or Teflon digestion tank with water, combine all the washing liquid into the volumetric flask, and finally shake with water to make it stand still for testing.
7.3.3 Fully automatic digestion
Accurately weigh 0.1 ~ 0.5 g of air-dried soil with 0.149 mm sieve opening (accurate to 0.0001g) in the polytetrafluoroethylene supporting the automatic digester.
Inside the digestion tank, moisten with a small amount of water, place the digestion tank in the digestion tank hole of the automatic digester, and set it in the control software of the automatic digester
Sample position, refer to the instrument list, set the work program, start the edited work program (Table 1), and the sample digestion process will be completed automatically
to make.
Table 1 Working procedure of automatic digestion instrument
Program setting step method content
1 Add 10 mL of nitric acid and 4 mL of hydrofluoric acid
2 Shock at 60% intensity for 1 min
3 Heat to 140 ℃ for 60 min
4 Add 2 mL of perchloric acid
5 Heat to 160 ℃ for 60 min
6 Heat to 180 ℃ for 30 min
7 Cool 30 minutes
8 Add 0.5 mL nitric acid
9 Add 20 mL of water and make up to 50 mL with water
7.4 Preparation of blank sample
The blank solution was prepared in the same manner as in 7.3 except that no soil sample was added.
7.5 Instrument reference conditions
The best test conditions for different models of instruments are different. Optimize the measurement conditions according to the requirements of the instrument manual. And choose according to the sample matrix
Appropriate analytical spectrum. Refer to Appendix B.2, B.3 for the reference measurement conditions and recommended wavelength of the instrument. After the instrument warms up until the indicators are stable,
Line measurement.
7.6 Drawing calibration curve
The standard series of solutions were sequentially extracted from the low concentration to the high concentration by a peristaltic pump and introduced into the inductively coupled plasma emission spectrometer.
Measure the intensity signal response value of the analytical spectral line of the element to be measured, with the mass concentration of the element to be measured as the abscissa, and the signal response value of the element to be measured
Ordinate, draw the standard curve.
7.7 Determination
The blank solution and the sample solution were respectively extracted into the inductively coupled plasma emission spectrometer by an equal amount of the peristaltic pump, and the elements to be measured were measured.
The signal response value of the element was obtained according to the standard curve. In the process of sample measurement, if the concentration of the element to be measured
Beyond the range of the calibration curve, the sample needs to be re-measured after dilution.
7.8 Calculation
The content ω (mg/kg) of each metal element in the soil sample is calculated according to formula (1).
km
tV s
)-(
ω 0Mn) Fe, Zn, (Cu,
...(1)
ts ... (2)
In the formula.
ω- soil total element mass fraction, mg/kg;
ρ- mass concentration of measured element in test sample, mg/L;
ρ0- mass concentration of measured element in blank sample, mg/L;
V- constant volume of sample, mL;
ts-divided multiples;
V1-Separate the volume of test solution, mL;
V2-Determine the volume of the test solution after fractionation, mL;
m-weigh the mass of the air-dried sample after screening, g;
k-Moisture conversion factor for air-dried sample mass converted to dry sample mass.
7.9 Representation of results
The calculation result retains three significant figures and is expressed in scientific notation.
7.10 Allowable deviation
Table 3 Control of the maximum allowable relative deviation of parallel double samples
Content range
(mg/kg)
Allowable maximum relative deviation
(%)
> 100 5
10 ~ 100 10
< 10 20
8 Quality assurance and quality control
8.1 Blank experiment
The result of the blank test should be less than the detection limit of the method.
8.2 Calibration
A calibration curve must be drawn for each batch of sample analysis, and the correlation coefficient of the calibration curve should be greater than or equal to 0.999.
Every 20 samples must be calibrated and checked with a standard solution at the middle point of the calibration curve.
The relative deviation of concentration at this point of the quasi-curve should be ≤10%, otherwise the calibration curve should be redrawn.
8.3 Accuracy Control
Every 20 samples should be tested for a certified soil standard sample or certified reference material, and the measured value should be within the guaranteed value range.
AA
Appendix A
(Informative appendix)
Standard solution series mass concentration
See Table A.1 for the mass concentration of element standard solutions in the ICP-OES method.
Table A.1 Mass concentration of standard solution series
Ordinal element
Standard series mass concentration (mg/L)
Series 1 Series 2 Series 3 Series 4 Series 5 Series 6
1 Cu 0 0.05 0.50 1.00 5.00 10.0
2 Zn 0 0.05 0.50 1.00 5.00 10.0
3 Fe 0 0.50 5.00 10.0 50.0 100
4 Mn 0 0.05 0.50 1.00 5.00 10.0
Appendix B
(Informative appendix)
Reference conditions for instrument operation
B.1 Reference conditions for operation of microwave digestion apparatus
Table B.1 Reference heating program of microwave digestion instrument
B.2 Instrument parameters of inductively coupled plasma emission spectrometer
Table B.2 Reference conditions for ICP operation
power
(kW)
Observation method
Plasma
air flow volume
(L/min)
Auxiliary
air flow volume
(L/min)
rinse
Pump speed
(rpm/min)
analysis
Pump speed
(rpm/min)
Nebulizer pressure
(kPa)
Clean
time
(s)
1.15
Copper, zinc and manganese levels
Survey, iron vertical observation
12 0.5 100 50.200 28
B.3 Recommended wavelength for elemental determination and interfering elements
Table B.3 Recommended wavelengths for elemental determination and interfering elements
No. Determination Element Recommended Wavelength (nm) Interfering Element
1 Cu 324.752/327.393 Fe, Al, Ti, Mo
2 Zn
202.548
206.200
213.856
Co, Mg
Ni, La, Bi
Ni, Cu, Fe, Ti
3 Fe
238.204
239.924
240.488
259.940
261.762
Cr, W
Mo, Co, Ni
Mo, W
Mg, Cu, Be, Mn
4 Mn
257.610
259.372
293.306
Fe, Mg, Al, Ce
Fe
Al, Fe
Step temperature (℃) Heating time (min) Holding time (min)
4.200 5 5
references
EPA 3052 Microwave assisted acid digestion of siliceous and organically based matrices.
ISO 14869-2017 Soil quality-dissolution for the determination of total element content-Part 3.
Dissolution with hydrofluoric, hydrochloric and nitric acids using pressurised microwave technique.
GB 5009.268-2016 National Food Safety Standard Determination of Multi-Elements in Foods.
HJ 777-2015 Determination of metal elements in air and waste particles. Inductively coupled plasma emission spectrometry.
HJ 781-2016 Determination of 22 metal elements in solid waste by inductively coupled plasma emission spectrometry.
HJ 803-2016 Determination of 12 metal elements in soil and sediments Aqua regia extraction-inductively coupled plasma mass spectrometry.
HJ 832-2017 Microwave digestion method for total metal elements in soil and sediment.
Lu Rukun. Chemical analysis method of soil agriculture. Beijing. China Agricultural Science and Technology Press..1999.
Yang Hua, Zhang Yonggang. Determination of six heavy metal elements in aqueous sediments by inductively coupled plasma atomic emission spectrometry (ICP-OES).
Chinese Inorganic Analytical Chemistry,.2014, 4 (1). 22-24.
Zheng Hongyan, Guo Xueqin, Zhu Zhixun, et al. Comparison of different pretreatment and analysis methods for determination of heavy metals in soil and sediment. Guangdong Chemical
Engineering,.2017, (16). 242-245.
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