Solid state 13C NMR spectroscopy

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.

XPS is a semi-quantitative technique used to measure the elemental composition of material surfaces. In addition, it can also determine the binding state of the atoms. XPS is a surface-sensitive technique. Typical probing depth is 3-9 nm, and detection limits range roughly between 0.1 and 1 atomic %. XPS can measure elements from Li to U. The elemental composition is reported in at.% and measured on 1 area of a few 100 µm. Upon request, we can measure smaller areas or depth profiles, and a binding state determination can also be provided. Measurements are typically performed using one of the following instruments: PHI Genesis, Thermo Fisher ESCALAB 250Xi, PHI Quantum 2000. Synchrotron XPS is also available. Contact us for more information and a quote for your project.

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.

Determination of the biomass fraction of CO₂ emissions generated from mixed fuel incineration, as required by the EU Emissions Trading System (ETS). CO₂ originating from non-fossil sources like biomass has an emission factor of zero under EU ETS and is therefore not counted towards carbon emissions. This means that the biomass fraction of mixed fuels, such as municipal waste or solid recovered fuel (SRF), must be determined to calculate reportable emissions accurately. In this analysis, the proportion of biogenic carbon dioxide in total emitted CO₂ from the incineration process is measured using the radiocarbon (¹⁴C) method. The measurement is based on the ASTM D6866 standard. This standard is equally rigorous and based on the same methodology as EN ISO 13833, which is mentioned in Commission Implementing Regulation (EU) 2018/2066 on the monitoring and reporting of greenhouse gas emissions. Testing is relevant for industrial plants that use mixed fuels and participate in emissions trading, as well as for municipal waste incineration (MWI) plants, which have been required to monitor and report emissions according to EU ETS since the beginning of 2024.

Determination of total fluorine (F) content in plastic according to the EN 15408 mod. method. The fluorine content of the sample is obtained using oxygen bomb combustion treatment followed by ion chromatography (IC). Possible sample preparation, such as grinding into smaller particles, is available at an extra cost. This method can also be used to determine the total content of S, Cl, and Br. The results will be reported in mg/kg.

The biobased carbon content is either reported as a fraction of the total organic carbon (TOC) or total carbon (TC). The price is for non-volatile samples. If your sample is volatile, please discuss the suitability of your sample type with our experts. Please also note that we cannot accept samples that contain artificial carbon-12, carbon-13, or carbon-14 isotopes because they will cause damage to the equipment.

GC-MS analysis of 16 PAH compounds, which are listed as high-priority pollutants by the U.S. Environmental Protection Agency (EPA). The analyzed PAH compounds are: naphthalene [CAS: 91-20-3], acenaphthylene [CAS: 208-96-8], acenaphthene [CAS: 83-32-9], fluorene [CAS: 86-73-7], phenanthrene [CAS: 85-01-8], anthracene [CAS: 120-12-7], fluoranthene [CAS: 206-44-0], pyrene [CAS: 129-00-0], benz(a)anthracene [CAS: 56-55-3], chrysene [CAS: 218-01-9], benzo(b)fluoranthene [CAS: 205-99-2], benzo(k)fluoranthene [CAS: 207-08-9], benzo (a) pyrene [CAS: 50-32-8], dibenzo(ah)anthracene [CAS: 53-70-3], benzo (ghi) perylene [CAS: 191-24-2], indeno (123cd) pyrene [CAS: 193-39-5].

Carbon-13 NMR spectroscopy measurement for samples that can be dissolved in deuterated solvents. The price includes sample preparation, deuterated solvent (D₂O, DMSO-d, or CDCl₃), NMR tube, measurement, and basic data processing. The results are delivered as an image file containing the NMR spectrum. Additional information and raw data can be provided upon request. Please contact our experts if your samples require the use of other than the above-mentioned deuterated solvents or atypical measurement conditions, such as very high temperatures and/or long measurement times.

Use of 13C-NMR to identify the type and relative quantity of short-chain branching in high-density polyethylene (HDPE) samples. The prevalence of short-chain branching can have major effects on the properties of HDPE materials such as their crystallinity, melting point, density, and mechanical properties. The branching density and relative distribution of different length side chains can be determined by NMR using the Randall method. The processed spectrum is delivered as an image file. Additional interpretation and raw data can be provided upon request. Please contact Measurlabs' NMR experts to receive a testing plan tailored to your material and analysis needs. This analysis is only relevant to HDPE materials.