Boron determination in steels by inductively coupled plasma atomic emission spectrometry. Comparative study of spark ablation and pneumatic nebulization sampling systems

An experimental study for the determination of boron in steels by inductively coupled plasma atomic emission spectrometry is presented. A comparison is made of spark ablation and pneumatic nebulization (after microwave digestion) sampling systems. A one-step microwave digestion procedure for total b...

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Detalles Bibliográficos
Autores: Gómez Coedo, Aurora, Dorado López, María Teresa, Gutiérrez Cobo, Isabel
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:1993
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/221626
Acceso en línea:http://hdl.handle.net/10261/221626
Access Level:acceso abierto
Palabra clave:Spark ablation
Microwave digestion
Inductively coupled plasma atomic emission spectrometry
Boron determination
Steel
Descripción
Sumario:An experimental study for the determination of boron in steels by inductively coupled plasma atomic emission spectrometry is presented. A comparison is made of spark ablation and pneumatic nebulization (after microwave digestion) sampling systems. A one-step microwave digestion procedure for total boron content using diluted aqua regia (HCl+HNO3, 3+1) and high pressure vessels was developed. The influence of microwave power and time on the dissolution of boron compounds is discussed. The strongest available conditions (0 ?, 600 V, 600 Hz) were required for spark ablation sampling. The stability of spark sampling during the spark ablation-ICP process was tested by plotting iron and boron emission versus sparking time. The iron content of collected and dissolved spark-produced particles was analysed and showed that the amounts of aerosol from different boron steels samples during 90 s sparking processes were fairly similar. The analytical performance of both systems was evaluated. Using pneumatic nebulization, after microwave digestion of the sample, a detection limit for boron of 2.6 ?g g-1 and overall relative standard deviation (RSD) values of 1-3.5% were found. For spark ablation the detection limit for boron was 0.65 ?g g-1, the overall RSD ranging from 0.5 to 1.5%. A comparison of the data for British Chemical Standards (BCS) Certified Reference Materials (CRMs) Carbon Steel Residual Series (Group B) and Spectroscopic Standard (SS) 456/1 to 460/1, indicated that the accuracy of both methods was satisfactory.