Biomedical subjects

K H Grobecker

Publications and source records attributed to K H Grobecker.

3 recordsLinked to original sources

PubMed2001

Water as a source of errors in reference materials.

In the field of reference materials, long-term stability is of highest importance. Particularly for biological matrices, any kind of deterioration must be avoided during shelf-life. In the production precautions are taken to prevent these, but possible alterations caused by intensive drying have been underestimated until today. This presentation discusses several mechanisms of deterioration related to water activity and water content. Comparison of the results for water and moisture for six reference materials and their water sorption isotherms serve as a base to discuss the importance of accurate dry mass corrections for certified values. It is shown that the method chosen for dry mass correction influences certified contents significantly and a method description must be given. Furthermore, it is confirmed that for biological matrices optimal ranges of water activity and water content exist, where hygroscopicity is low without significant danger of product deterioration. Additionally, handling is facilitated in the optimised ranges.

Adsorption↗

PubMed2001

Analyte transport efficiencies in electrothermal vaporization for inductively coupled plasma mass spectrometry.

A modified graphite furnace for solid-sampling atomic absorption spectrometry as an electrothermal vaporizer (ETV) was coupled to a Perkin-Elmer/Sciex ELAN 6000 ICP mass spectrometer. The integrals obtained from electrothermal vaporization of aliquots containing As, Cd, Cu, Co, Fe, Mn, Pb, Se, and Zn were compared with those obtained from pneumatic nebulization of the same aqueous standard solution. The pneumatic nebulizer was calibrated by weighing the mass of aqueous aerosol trapped on a filter. With "wet plasma" conditions maintained also for measurements with the ETV and reference signals for analyte signals obtained with the calibrated pneumatic nebulization, the transport efficiency of the ETV system, e.g. the ratio of the analyte amount introduced into the plasma to that amount dosed into the vaporizer, was determined. The transport efficiency of two different tube and interface designs has been evaluated. Investigations with and without the use of trifluoromethane as reactive gas, with different furnace heating rates, and with varying gas flows were performed. In general, the tube equipped with a nozzle led to generally higher transport efficiency than the standard tube. Without trifluoromethane transport efficiencies ranged from 10% to 35% with the standard tube and from 15% to 50% with the nozzle-type tube. With addition of 2 mL min(-1) trifluoromethane to the argon flow of 400 mL min(-1) through the tube, transport efficiencies from 20% to 70% and from 70% to 100% were achieved with the standard and nozzle-type tubes, respectively.

Journal Article↗

PubMed2001

Development of an electrothermal vaporization ICP-MS method and assessment of its applicability to studies of the homogeneity of reference materials.

A method has been developed for measurement of the homogeneity of analyte distribution in powdered materials by use of electrothermal vaporization with inductively coupled plasma mass spectrometric (ETV-ICP-MS) detection. The method enabled the simultaneous determination of As, Cd, Cu, Fe, Mn, Pb, and Zn in milligram amounts of samples of biological origin. The optimized conditions comprised a high plasma power of 1,500 W, reduced aerosol transport flow, and heating ramps below 300 degrees C s(-1). A temperature ramp to 550 degrees C ensured effective pyrolysis of approximately 70% of the organic compounds without losses of analyte. An additional hold stage at 700 degrees C led to separation of most of the analyte signals from the evaporation of carbonaceous matrix compounds. The effect of time resolution of signal acquisition on the precision of the ETV measurements was investigated. An increase in the number of masses monitored up to 20 is possible with not more than 1% additional relative standard deviation of results caused by limited temporal resolution of the transient signals. Recording of signals from the nebulization of aqueous standards in each sample run enabled correction for drift of the sensitivity of the ETV-ICP-MS instrument. The applicability of the developed method to homogeneity studies was assessed by use of four certified reference materials. According to the best repeatability observed in these sample runs, the maximum contribution of the method to the standard deviation is approximately 5% to 6% for all the elements investigated.

Arsenic↗