1 Method Overview
After the sample is digested with aqua regia, the determination is carried out using an air-acetylene flame at a wavelength of 324.7 nm with the instrument.
2 Instruments and Reagents
2.1 Instruments and Equipment
2.1.1 Detection Instruments
Serial Number | Nombre | Cantidad | Technical Requirements | Accesorios |
---|---|---|---|---|
1 | Flame Atomic Absorption Spectrophotometer | 1 set | Copper hollow cathode lamp | |
2 | Acetylene | 1 cylinder | Purity ≥ 99.99% | |
3 | Air Compressor | 1 set | Rated exhaust pressure: 0.3 MPa |
2.1.2 Pretreatment Equipment
Serial Number | Nombre | Cantidad | Technical Requirements | Accesorios |
---|---|---|---|---|
1 | Temperature-controlled Hot Plate | 1 set | Rated temperature: room temperature ~ 300℃ | |
2 | Electronic Balance | 1 set | Sensitivity 0.1 mg | |
3 | Ultrapure Water Device | 1 set | ||
4 | Micropipette | 1 each | 20μL ~ 200μL; 100μL ~ 1000μL | |
5 | Volumetric Flask | Several | 100 mL | |
6 | Test Tube | Several | 25 mL |
2.2 Reagents
2.2.1 Reagents
Serial Number | Nombre | Technical Requirements | Observaciones |
---|---|---|---|
1 | Nitric Acid | MOS grade | |
2 | Hydrochloric Acid | Guaranteed reagent |
2.2.2 Prepared Reagents
Serial Number | Nombre | Preparation Method | Observaciones |
---|---|---|---|
1 | (1+99) Nitric Acid Solution | Measure 10 mL of nitric acid, slowly add to 990 mL of deionized water, and mix well |
2.3 Standards
2.3.1 Stock Solutions
Serial Number | Número | Nombre | Technical Requirements | Observaciones |
---|---|---|---|---|
1 | GBW08615 | Copper Single Element Solution Standard Substance | 1000μg/mL | National Institute of Metrology, China |
3 Operation Process
3.1 Sample Processing
3.1.1 Preparation of Test Solution
Weigh 0.25 g of the sample, accurate to 0.00001 g, into a digestion tank. Add 3 mL of concentrated nitric acid and 9 mL of concentrated hydrochloric acid, cover and tighten the digestion tank, and put it into a microwave digestion instrument for digestion. Prepare a blank in the same way. After cooling, filter and dilute to volume in a 25 mL volumetric flask, and put it on the machine for testing.
Microwave Heating Program
Step | Temperature/℃ | Holding Time/min |
---|---|---|
1 | 100 | 3 |
2 | 120 | 3 |
3 | 140 | 3 |
4 | 160 | 3 |
5 | 180 | 30 |
3.1.2 Preparation of Standard Solution
- Preparation of copper standard series: Accurately pipette 0.0, 0.025, 0.05, 0.1, and 0.2 mL of copper standard solution (1000μg/mL) into 100 mL volumetric flasks respectively, dilute to the mark with (1+99) nitric acid, and mix well. The mass concentrations of this standard series solution are 0.0, 0.25, 0.5, 1.0, and 2.0 μg/mL respectively.
3.2 Sample Testing
- Test Conditions Reference Conditions for Flame Atomic Absorption Spectrophotometer Detection
Elemento | Cobre |
---|---|
Wavelength (nm) | 324.7 |
Spectral Bandwidth (nm) | 0.4 |
Element Lamp Current (mA) | 3.0 |
Fuel Gas Height (mm) | 6 |
Fuel Gas Flow Rate (mL/min) | 1400 |
Air Compressor Pressure (MPa) | 0.22 |
Background Correction Method | None |
- Sample Testing Adjust the instrument to the best working state, ignite the flame, adjust the fuel gas flow rate, test the standard and sample solutions in sequence, read the data, input the sample weight, and check and record the results.
3.3 Result Calculation
Dónde:
X — Copper content in the sample, unit is milligram per kilogram (mg/kg);
ρ — Mass concentration of copper in the sample solution to be tested, microgram per milliliter (μg/mL);
ρ₀– Mass concentration of copper in the blank solution, microgram per milliliter (μg/mL);
f — Dilution factor of the sample digestion solution;
V — Total volume of the sample digestion solution, unit is milliliter (mL);
m — Mass of the sample, unit is gram (g);