Application of Sample-Specific Preparation Artifact Microwave Oxygen Combustion System in Elemental Analysis

Application of Sample-Specific Preparation Artifact Microwave Oxygen Combustion System in Elemental Analysis

Make a hundred gods! Microwave oxygen combustion system

Anton Paar Multiwave Pro sample preparation specificity

For samples that are difficult to disintegrate, such as graphite, coal, and complex drugs, Anton Paar Multiwave PRO offers a new type of pretreatment: Microwave-Induced combustion (MIC). The combustion method is a commonly used method in the pretreatment of halogen element analysis, and the MIC combines the combustion method and the closed digestion into one system, and the combustion of the sample is initiated by the microwave. In a subsequent reflux step, microwave irradiation can help digest the residue and reduce the analyte in the absorbing solution.
The MIC's analysis of elements has the following characteristics:
• Closed sample preparation reduces analyte loss;
• The residual quartz tube is lower than the PTFE or metal alloy reaction tube;
• The high temperature reflow step ensures complete elution of the analyte from the inner surface;
• Acid/alkaline solution can be used as reflux absorbent for subsequent elemental analysis (ICP-MS/AAS/IC, etc.);
• No dilution after digestion;
• The combustion process reduces the matrix effect of subsequent analyses;
• The combustion and reflow process can be completed in 15 minutes;
Application Case 1: Determination of Cl in Coal
Experimental overview:
 sample: coal GBW11120 (chlorine content: 1100ug / g)
Element to be tested: Cl
Nickname sample quantity: 0.1g
 reagent: ammonium nitrate, ammonium carbonate
包裹 Wrap the weighed sample in ashless filter paper and carefully place it in the quartz sample holder.
Set as follows:
Table 1: Multiwave PRO Microwave Oxygen Combustion Program Settings
Power [ W a t t] Power ramp [minutes] Power remains [minutes] Fan grade
1 900 0:00 1:30 1
2 900 0:00 10:00 1
Experimental results:
The solution was clear and transparent after oxycombustion and analyzed by ion chromatography (TOSOH). Column: TSKgel SuperIC-AZ (4.6mm ID* 15cm), mobile phase: 6.3mmol/L NaHCO3+1.7mmol/L Na2CO3, flow rate: 0.8 ml/ Min, detection: Conductivity, temperature: 40 ° C. The chlorine content is shown in the following table:
Table 2: Experimental results
sample name content
coal standard value Actual value
0.11% 0.12%
Application Case 2: Determination of Metal Elements in Active Components of Pharmaceutical Products

Experimental overview:
 sample: amitriptyline hydrochloride, carbamazepine, imipramine hydrochloride
 Elements to be tested: As (arsenic), Hg (mercury), Pb (lead), Cr (chromium)
Nickname sample quantity: 0.5g
Hydrazine reagent: different concentrations of nitric acid solution, ammonium nitrate
包裹 Wrap the weighed sample in ashless filter paper and carefully place it in the quartz sample holder.
Set as follows:
Table 3 Multiwave PRO Microwave Oxygen Burning Program Settings
Power [ watt ] Power ramp [minutes] Power remains [minutes] Fan grade
1 900 0:00 1:30 1
2 900 0:00 10:00 1
Experimental results:
This experiment compares the recovery rates of four elements at different concentrations of the absorbing solution, from left to right, respectively, the recovery of each element at concentrations of 1, 7, and 14.5 mol/L HNO3 solution. It can be seen that when nitric acid is used At a concentration of 7 mol/L, the absorption is best.

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