By Institute for Advanced Chemistry of Catalonia (IQAC-CSIC)
The Microanalysis Service performs carbon, hydrogen, nitrogen and sulfur (C, H, N, S) analyses and halogen analyses in organic and inorganic compounds. This Service provides services and support to CSIC research groups, universities and private companies. It has a Quality Manual and Standard Operating Procedures (SOPs) through which the laboratory achieves its quality objectives and the qualification and reliability of its tests. Contact: micro@cid.csic.es Sample requirements for analysis: Due to the small amount of sample used for CHNS analyses (1 mg), the general and specific conditions required are: - Dry samples, with no traces of moisture or solvents - Solid or liquid materials combustible at 2000°C or at a lower temperature - Homogeneous or able to be homogenised - In the case of halogens (Cl, Br and I), samples containing mercury cannot be analysed. The minimum amount of sample required is: - CHN: 10 mg sample, Test in duplicate - CHNS: 10 mg sample, Test in duplicate - Cl, Br, I: 7 mg sample, If it is > 50% - Cl, Br, I: 40 mg sample, If it is < 10% - F: 50 mg sample, If it is < 10% Analysis methods: Elemental analysis of C, H, N and S is carried out using the modified Pregl-Dumas method (dynamic flash combustion), using helium as the carrier gas. To calibrate the equipment, standards of known composition are used in accordance with the Standard Operating Procedures. Analyses are always performed in duplicate. Test results are expressed as weight percent for each element, compared with the value of a known standard and using the k-factor method to perform the calculations. Halogen determination is carried out using the Schöniger method (oxygen-filled flask) and subsequent potentiometric titration with AgNO3 for Cl, Br and I; with La(NO3)3 for F. Sample request form: To request analyses or for any questions, please contact: IQAC Microanalysis Service (CSIC), Jordi Girona 18-26. 08034 Barcelona, Tel. +34 93 255 77 10 / +34 93 255 76 19, Email: micro@cid.csic.es. Analysis requests must be accompanied by a protocol with the information duly completed, one protocol per sample. Result reports are sent by email within 7–10 days of receipt of the sample. Sample delivery hours are from 8:00 to 15:00 (Monday to Friday) in the laboratory, and from 8:00 to 22:00 at the IQAC reception desk. To request the price list, you can contact the laboratory staff. EQUIPMENT: The Microanalysis Service has the equipment required to carry out the tests. Use of this equipment is restricted to laboratory staff. Main equipment: - 1 Elemental Microanalyser (A8), Flash Smart model, for the determination of C, H, N, S - 1 Elemental Microanalyser (A7), Flash 2000 model, for the determination of C, H, N, S. - 2 Mettler microbalances (B3 and B4), MT5 and MX5 models. - 1 Metrohm titroprocessor, model 808, for the determination of Cl, Br, I and F.
