BASF - We create chemistry


BASF Global   |    E-Business   |    Deutsch    |    Sitemap   |    Contact     

  »  search

About us  |  Special Equipment  |  Test methods
Visual BASF Competence Center Analytics
 

Special Equipment


Automated nuclear magnetic resonance spectroscopy
     (NMR spectroscopy)

Cleanroom lab

Fourier Transform Mass Spectrometry (FTMS)

Fully automated heavy metal analysis

Automated nuclear magnetic resonance spectroscopy (NMR spectroscopy)

Nuclear magnetic resonance spectroscopy (NMR) is one of the main spectroscopic methods used for structure elucidation in chemical synthesis. We measure and evaluate up to 100,000 spectra every year at the Competence Center Analytics. Our NMR lab achieves this kind of high throughput through the systematic use of automation technology for repetitive operations.

Our "NMR robot" prepares a multiplicity of samples around the clock and forwards them to the spectrometer. Preparation by this method is both efficient and safe. This automated process rules out safety problems even when dealing with reactive or highly toxic agents. Our spectrometer's job is to measure spectra on its own and pass them straight on to the client. Our LIMS System knows your e-mail address and can send the results directly to your PC if you so wish.

Our spectra evaluation experts are supported by the world's largest NMR database SpecInfo and our SpecSolv structure generator.


zum Seitenanfang

Cleanroom lab

 
The air in our analytical cleanroom lab is virtually particle-free. This is where we test the purity of electronic grade chemicals. Manufacturers of electronic components in particular depend on ultrapure chemicals because even the tiniest metal impurity may destroy extremely sensitive integrated circuits. Protective clothing must be worn during analysis. Our tests detect impurities in electronic grade chemicals at concentrations below one microgram per kilogram.
 

The air in the lab is exchanged forty times an hour and contains no more than 30 particles per liter. The same volume of "normal" air contains around 30,000 particles. Positive pressure prevents impure air from penetrating into the lab. Protective garments must be worn by staff. The lab furnishings are made of plastic to protect the samples from metal impurities.

We use the highest-performance measuring and monitoring equipment (such as inorganic mass spectrometry) to identify the tiniest traces of metal impurities in electronic grade chemicals in the cleanroom lab. This equipment gives access to multi element analysis in a short space of time.

We use several different methods and analyzers in the cleanroom lab for independent confirmation of our test results. These include flameless atom absorption and emission spectrometry as well as inorganic mass spectrometry.

The test samples (e.g. hydroxylamine) must be in liquid form. We transfer them to an aerosol in the spray chamber prior to mass spectrometry analysis.

Ultrapure acid samples need to be prepared prior to analysis. Sulfuric acid is evaporated in a quartz chamber to avoid interference during measurement and to increase the analyte concentrations. Semiconductor manufacturers require these chemicals for treatment of the surfaces of silicon wafers. Maximum purity is required for the manufacture of a successful product.

We place great demands on monitoring and test methods in all areas, not only in the analytical cleanroom lab. All samples must be handled in vessels that present no sources of contamination. Suitable materials include ultrapure quartz (the material of which the quartz chamber is made) and fluorinated Teflon-like polymers.

We assay approximately 300 elements every day for our clients. Success depends to a great extent on the special know-how and long-standing experience of our staff members. Continuous internal controls, training and professional quality management produce an optimum error-free analysis process.


zum Seitenanfang

Fourier Transform Mass Spectrometry (FTMS)

In order to establish a molecular formula for an organic compound, analytical chemists need to know the compound's precise molecular mass. The number of molecular formulae than can be elucidated increases in proportion to the precision of the method used to determine molecular mass. The more precise the method used to determine mass, the more accurate the resultant molecular formulae will be. Fourier transform mass spectrometry (FTMS) is the method with the highest mass precision, allowing determination of masses at precisions of better than 0.0005 amu. This value corresponds to the mass of an electron. Hence, data evaluation with FTMS is more accurate and rapid than with other MS technologies.

Another remarkable feature of FTMS is its signal resolution. High signal resolution allows us to simultaneously measure the molecular masses of different compounds of similar molecular weight contained in the same mixture. FTMS enables us to differentiate between substances whose difference in molecular mass is so small as to begin at the third decimal place. The method allows us to investigate complex mixtures without first having to conduct time-consuming sample preparation steps.

Discover the precision of FTMS for yourself. Here's an example showing two molecules with the same nominal mass:
 

zum Seitenanfang

Fully automated heavy metal analysis

Sample preparation (digestion) is an essential, but also extremely time- and labor-consuming, step in the analysis of metals in organic samples. Ideally, the sample would be ready for immediate analysis without sample preparation steps. However, this is rarely possible (an exception being x-ray fluorescence analysis); sample "digestion" is required in most cases. This step, also known as "mineralization", removes the organic parts of the sample. Two self-developed digestion robots perform this task at the BASF Competence Center Analytics. Multistage open acid digestion was optimized for a broad spectrum of organic matrices. The samples are pretreated with sulfuric acid and then mineralized in an acid mixture. The acids are fumed off and the cooled residue is taken up with hydrochloric acid. The digestion system is linked online with the measurement instrument (ICP-OES), allowing fully automated overnight digestion of up to 400 test samples and determination of more than 30 elements in each sample. The results are transferred automatically to our lab information management system (LIMS). Consistently low blank values help to validate the method, resulting in constantly low blank values and an improved limits of quantitation.

Film example:
  View the film



top of page
Quickfinder

Service
Brochure (PDF, english)
Print this page
 
  Copyright  2024   BASF SE