Microanalysis Service

 
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Presentation

Protocol

 

 

 

The IQAC’s Microanalysis Service provides determination of carbon, hydrogen, nitrogen and sulphur (C, H, N, S) and halogens present in a wide range of organic and inorganic compounds.

Since in March 1999, Microanalysis Service has been accredited by ENAC, under regulation EN 45001. This was the first accredited Elemental Microanalysis laboratory in Spain and the first to be accredited of the CSIC.

As of November 2001, this Service has been accredited under regulation UNE-EN ISO/IEC 17025 for analysis of CHNS until at the end of November 2012.

 

Quality

The Microanalysis Service has a Quality Manual avaible for customers, where the Quality policy of the laboratory is outlined. Client satisfaction and analysis confidenciality are guaranteed.

Equipment

This facility has the appropriate instruments for accurate sample analysis. The use of all primary and accessory equipment is restricted to laboratory personnel.

Primary Instruments:

- 1 Elemental Microanalyzer (A5) model Flash 1112, for C, H, N determination.

- 1 Elemental Microanalyzer (A7) model Flash 2000, for C, H, N, S determination.

- 2 Mettler Microscale (B3 and B4) models MT5 and MX5.

- 1 Metrohm Titrando model 808 for Cl, Br, I and F determination.

Principle of Method

C, H, N and S elemental analysis is performed by the modified Pregl-Dumas technique (dynamic flash combustion), using helium as carrier gas.
Instruments are calibrated according to the standards methods (Working Standardized Procedures).

Analyses are always carried out in duplicate. All results for elemental analysis are given as a percent of weight of each element, based on a known value of a standard by using the k value factors calculation.

Halogen determination is carried out according to the Schöniger procedure (flask full of oxigen), followed by potentiometric titration with AgNO3 for Cl, Br and I, and La(NO3)3 for F.

Requirements for submitting samples

Due to the small amount of sample (1mg) used in CHNS analysis, the requirements for sample submission are:

Dry samples, without water or solvent residues.
Solid or liquid materials combustible at 2000ºC or lower.
Homogeneous samples or able to be homogenized.
In the case of halogen determinations (Cl, Br and I), samples containing Hg can not be analyzed.

Application forms

For analysis forms or other questions contact:

Servei de Microanàlisi IQAC (CSIC)
Jordi Girona 18-26
08034 - BARCELONA
Tel. 93 400 61 00 ext. 1315
Fax 93 204 59 04
Email: micro@cid.csic.es

Analyses will be done according to submission forms (protocol) supplying all required information. Each sample must be accompanied by a submission form.

The minimum amount of sample required is:

Optionmg sample
CHN10duplicate analysis
CHNS10duplicate analysis
Cl, Br, I7if > 50%
Cl, Br, I40if < 10%
F50if < 10%

A copy of the results completed and signed by the Technical Director will be sent to the client by mail, and a copy will be released by email within ten to fifteen days of sample reception.

Sample reception is from 8 to 15 h (Monday through Friday) in the Service Laboratory and from 8 to 22 h in the IQAC reception.

For the price list, please contact the laboratory Service.