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Determination of Copper in Graphite Powder – Flame Atomic Absorption Spectrometry

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 名前 Technical Requirements アクセサリー
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 名前 Technical Requirements アクセサリー
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 名前 Technical Requirements 備考
1 Nitric Acid MOS grade
2 Hydrochloric Acid Guaranteed reagent

2.2.2 Prepared Reagents

Serial Number 名前 Preparation Method 備考
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 番号 名前 Technical Requirements 備考
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

  1. 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

  1. Test Conditions Reference Conditions for Flame Atomic Absorption Spectrophotometer Detection

 

エレメント
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

 

  1. 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

 

どこ:
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);

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