Synchrotron powder XRD measurement - Quantitative analysis

Qualitative or comparative analysis of crystalline powders using X-ray diffraction (XRD). The analysis is only suitable for materials with at least one crystalline phase.

This metal screening analysis includes the semi-quantitative determination of 70 elements. The method can be used, for example, to determine the background concentrations of metals in environmental samples or to study the elemental distribution of unknown samples. Screening is also often performed to assess which metals should be analyzed by a quantitative method. The measurement is performed using a high-resolution ICP-MS technique (ICP-SFMS), which can identify very low elemental concentrations. A semi-quantitative determination of the following elements is included: Ag, Al, As, Au, B, Ba, Be, Bi, Br, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, I, Ir, K, La, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Rb, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Te, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn and Zr. However, please note that some elements may not be determinable due to matrix interference. During this semi-quantitative analysis, the instrument is calibrated for about 30 elements and the rest of the analytes are quantified using sensitivity factors for calibrated elements with similar mass and first ionization potential considering isotope abundances. Quantitative analysis is also available at an additional price. During this analysis, all elements are calibrated (excluding halogens and Os). Please ask for an offer for this service.

Phase identification and quantification (Rietveld analysis) of a crystalline powder material using X-ray diffraction (XRD). The analysis can also provide unit cell dimensions. The analysis is only suitable for materials with at least one crystalline phase. The quantification accuracy is roughly 0.1 %, depending on the sample matrix and the phase in question. The available temperature range for XRD measurements is 25-1100 °C and the crystallinity can be studied as a function of temperatures. The measurements can be done under a normal atmosphere, inert gas, or vacuum. Please contact our experts to discuss the available temperature and atmosphere combinations. Please mention which crystalline phases your material contains and which ones are you interested in quantifying when requesting testing. However, the method can be applied to unknown phases as well. Either a tabletop or a synchrotron XRD can be used to perform the measurements.

Imaging of the sample using scanning electron microscopy (SEM). Typically, several images are taken with varying magnifications to get a good overview of the sample. Non-conductive samples can be prepared with a metallic coating to allow imaging. For cross-section measurement, additional preparation might be needed: FIB, BIB or freeze fracturing. If compositional analysis is also needed, please see the SEM-EDX measurement.

BET (Brunauer–Emmett–Teller) analysis to determine the specific surface area of solid materials.

Qualitative identification of chemical groups in solid samples by Attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR). Results will be delivered as an FTIR spectrum. In addition, a comparison to an FTIR library will be provided. The method is not quantitative, but it can be used to identify the main chemical components of the sample.

Determination of carbon, hydrogen, nitrogen, sulfur, and oxygen content of an organic sample. CHNS analysis (”LECO analysis”) is performed using a flash combustion method, where the sample is combusted under 25 kPa of O2 at an elevated temperature (1000 °C), followed by gas chromatography separation and detection using a thermal conductivity detector. Oxygen is analyzed by reduction on granulated carbon at 1480 °C, utilizing high-temperature thermal decomposition and conversion of oxygen into carbon monoxide before gas chromatography separation and detection with a thermal conductivity detector. The sample can be either solid or liquid, but water in the sample affects the results. In the case of aqueous samples, it is possible to dry the sample before analysis. The price includes two parallel measurements. The results are reported as wt-% of the initial sample. The ash, drying and dry loss measurements will increase the minimum required sample material need to 300 mg. The analysis gives the total carbon, hydrogen, nitrogen, sulfur, and oxygen content of the material, but it does not identify any chemical structures. The measurement can be combined with other methods, such as GC-MS, 1H, and 13C NMR, to perform substance structure identification. Possible element packages: O, CHNS, and CHNOS.

Analysis of gaseous samples using Raman spectroscopy.

Pyrolysis gas chromatography-mass spectrometry (py-GC-MS) analysis to determine the identity of an unknown polymer sample. During the measurement, the sample is instantaneously heated in an inert atmosphere or vacuum. This causes the sample to decompose into smaller molecular fragments which are then analyzed with GC-MS. Different types of polymers can be identified by their unique decomposition products. This includes, but is not limited to: PE, PP, PS, ABS, PMMA, PET, PC, PVC, polyamides, natural & synthetic rubbers, and more. The price includes the basic preparation and analysis of the sample. More extensive sample preparation is subject to additional costs.

Classic stable isotope analysis of carbon (13C) with isotope-ratio mass spectrometry (IRMS). The results are reported in the unit VPDB, ‰. The analysis is suitable for various sample materials. Please contact the Measurlabs expert for more detailed information on the analysis.