1. Method Overview
Wet digestion: Dissolve the sample with hydrochloric acid, nitric acid, and hydrogen peroxide. Determine lead at a wavelength of 283.3 nm using an air-acetylene neutral flame.
2. Instruments and Reagents
2.1 Instruments and Equipment
2.1.1 Testing Instruments
Serial No. | Name | Menge | Technical Requirements | Zubehör |
---|---|---|---|---|
1 | Flame atomic absorption spectrophotometer | 1 set | Lead hollow cathode lamp | |
2 | Acetylene | 1 cylinder | Purity ≥ 99.99% | |
3 | Air compressor |
2.1.2 Pretreatment Equipment
Serial No. | Name | Menge | Technical Requirements | Zubehör |
---|---|---|---|---|
1 | Temperature-controlled electric hot plate | 1 set | Rated temperature: room temperature ~ 300℃ | |
2 | Electronic balance | 1 set | Sensitivity: 0.1 mg | |
3 | Ultrapure water system | 1 set | ||
4 | Micropipette | 1 each | 20 μL ~ 200 μL; 100 μL ~ 1000 μL | |
5 | Volumetric flask | Several | 100 mL | |
6 | Test tube | Several | 25 mL |
2.2 Reagents
2.2.1 Reagents
Serial No. | Name | Technical Requirements | Anmerkungen |
---|---|---|---|
1 | Hydrochloric acid | Guaranteed reagent | |
2 | Nitric acid | MOS grade |
3. Operational Procedures
3.1 Sample Processing
3.1.1 Preparation of Test Solution
Experimental method: Weigh 0.25 g of the sample into a beaker, add 15 mL of mixed acid (HCl: HNO₃: H₂O = 6:1:7), heat until completely dissolved, and cool. Transfer to a 100 mL volumetric flask, dilute to the mark, and mix well. Zero with the blank solution, and determine at a wavelength of 283.3 nm using an air-acetylene flame.
3.1.2 Preparation of Standard Solutions
- Preparation of lead standard series: Accurately pipette 0.0, 0.1, 0.2, 0.4, and 0.8 mL of lead standard stock solution (1000.0 μg/mL) into 100 mL volumetric flasks respectively, dilute to the mark with (1+99) hydrochloric acid, and mix well. The concentrations of this solution series are 0.0, 1.0, 2.0, 4.0, and 8.0 μg/mL.
3.2 Sample Testing
- Testing Conditions Reference conditions for flame atomic absorption spectrophotometer detection
Element | Blei |
---|---|
Wavelength (nm) | 283.3 |
Spectral bandwidth (nm) | 0.4 |
Element lamp current (mA) | 6.0 |
Fuel height (mm) | 6 |
Fuel flow rate (mL/min) | 1500 |
Air compressor pressure (MPa) | 0.22 |
Background correction method | None |
- Sample Testing Adjust the instrument to the optimal working state, ignite the flame, adjust the fuel flow rate, test the standard solutions and sample solutions in sequence, read the data, input the sample weight, and check and record the results.
3.3 Result Calculation
Wo:
X — Lead content in the sample, in milligrams per kilogram (mg/kg);
ρ — Mass concentration of lead in the sample solution to be tested, in micrograms per milliliter (μg/mL);
ρ₀ — Mass concentration of lead in the blank solution, in micrograms per milliliter (μg/mL);
f — Dilution factor of the sample digestion solution;
V — Total volume of the sample digestion solution, in milliliters (mL);
m — Mass of the sample, in grams (g).