Inductively Coupled Plasma Optical Emission Spectrometry Measurements Research Articles

Correction for partial volume averaging in the quantification of radiopaque nanomaterial-embedded resorbable polymers

Resorbable inferior vena cava (IVC) filters require embedded contrast for image-guided placement and integrity monitoring. We calculated correction factors to account for partial volume averaging of thin nanoparticle (NP)-embedded materials, accounting for object and slice thicknesses, background signal, and nanoparticle concentration. We used phantoms containing polycaprolactone disks embedded with bismuth (Bi) or ytterbium (Yb): 0.4- to 1.2-mm-thick disks of 20 mg ml−1 NPs (thickness phantom), 0.4-mm-thick disks of 0–20 mg ml−1 NPs in 2 mg ml−1 iodine (concentration phantom), and 20 mg ml−1 NPs in 0.4-mm-thick disks in 0–10 mg ml−1 iodine (background phantom). Phantoms were scanned on a dual-source CT with 80, 90, 100, and 150 kVp with tin filtration and reconstructed at 1.0- to 1.5-mm slice thickness with a 0.1-mm interval. Following scanning, disks were processed for inductively coupled plasma optical emission spectrometry (ICP-OES) to determine NP concentration. Mean and maximum CT numbers (HU) of all disks were measured over a 0.5-cm2 area for each kVp. HU was converted to concentration using previously measured calibrations. Concentration measurements were corrected for partial volume averaging by subtracting residual slice background and extrapolating disk thickness to both nominal and measured slice sensitivity profiles (SSP, mm). Slice thickness to agreement (STTA, mm) was calculated by replacing the CT-derived concentrations with ICP-OES measurements and solving for thickness. Slice thickness correction factors improved agreement with ICP-OES for all measured data. Yb corrections resulted in lower STTA than Bi corrections in the concentration phantom (1.01 versus 1.31 STTA/SSP, where 1.0 is perfect agreement), phantoms with varying thickness (1.30 versus 1.87 STTA/SSP), and similar ratio in phantoms with varying background iodine concentration (1.34 versus 1.35 STTA/SSP). All measured concentrations correlated strongly with ICP-OES and all corrections for partial volume averaging increased agreement with ICP-OES concentration, demonstrating potential for monitoring the integrity of thin IVC resorbable filters with CT.

Evaluation of Analytical Methods for Boron Determination in Maize Shoots

ABSTRACTFor the comparison of the digestion and spectroscopic determination methods used to measure boron (B) concentrations in maize shoots, increasing doses of boron (0, 2.5, 5, and 10 mg kg−1 B) were applied to soil and maize plants (Zea mays L.) cultivar “Euralis Es Armandi” (FAO 640). The plants were grown under greenhouse conditions. Dried and ground maize shoots were digested according to two digestion procedures of microwave and dry ashing. Boron concentrations were determined using spectrophotometer and inductively coupled plasma-optical emission spectrometry (ICP-OES). The concentrations of boron influenced statistically (p < 0.01) due to the B applications and analysis methods. Spectrophotometric measurement of B amounts of the samples prepared with microwave digestion method was found irrelevant with other indicated methods. However, the ICP-OES measurements were found compatible with the dry ashing also with microwave digestion and suggested as a suitable method to determine boron contents of the maize shoots.

A Combined Spectroscopic/Molecular Dynamic Study for Investigating a Methyl-Carboxylated PEI as a Potential Uranium Decorporation Agent.

Natural uranium has a very limited radioactive dose impact, but its chemical toxicity due to chronic exposure is still a matter of debate. Once inside the human body, the soluble uranium, under its uranyl form (U(VI)), is quickly removed from the blood system, partially excreted from the body, and partially retained in targeted organs, that is, the kidneys and bone matrix essentially. It is then crucial to remove or prevent the incorporation of uranium in these organs to limit the long-term chronic exposure. A lot of small chelating agents such as aminocarboxylates, catecholamides, and hydroxypyridonates have been developed so far. However, they suffer from poor selectivity and targeting abilities. Macromolecules and polymers are known to present a passive accumulation (size related), that is, the so-called enhanced permeability and retention effect, toward the main organs, which can be used as indirect targeting. Very interestingly, the methyl carboxylated polyethylenimine (PEI-MC) derivative has been described as a potent sequestering agent for heavy metals. It would be therefore an interesting candidate to evaluate as a new class of decorporation agents with passive targeting capabilities matching uranium preferential sequestering sites. In the present work, we explored the ability of a highly functionalized (89% rate) PEI-MC to uptake U(VI) close to physiological pH using a combination of analytical and spectroscopic techniques (inductively coupled plasma optical emission spectrometry (ICP-OES); extended X-ray absorption fine structure (EXAFS); and Fourier transformed infrared (FT-IR)) together with molecular dynamics (MD) simulation. A maximum loading of 0.47 mg U(VI) per milligram of PEI-MC was determined by ICP-OES measurements. From FT-IR data, a majority of monodentate coordination of the carboxylate functions of the PEI-MC seems to occur. From EXAFS and MD, a mix of mono and bidentate coordination mode was observed. Note that agreement between the EXAFS metrical parameters and MD radial distribution functions is remarkable. To the best of our knowledge, this is the first comprehensive structural study of a macromolecular PEI-based agent considered for uranium decorporation purposes.

Elemental analysis of burnt human bone for classifying sex and age at death by logistic regression

This study aims to develop a protocol for classifying sex and age groups of deceased persons by using the chemical information in burnt bone fragments. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) has been employed to assess the chemical compositions of the burnt bones from the deceased, all of Thai nationality. By performing three ICP-OES measurements on burnt bone samples from 75 individuals, 43 males and 32 females, with an accurate record of their age at death, only six elements i.e. Al, Ca, K, Mg, P, S, were observed in the fragments above the instrumental detection limit of ICP-OES. Fifteen concentration ratios of these particular elements were examined for their significant difference with respect to sex and age group by Mann–Whitney U and Kruskal–Wallis tests, respectively. Subsequently, the significantly different ratios were employed to assess the relationship between bone chemical compositions and sex/age groups of the deceased using logistic regression analysis. Binary and multinomial logistic regressions were required to classify sex and age group at death, respectively. Regression analyses indicated that the input variables representing sex should be included for classifying the age group of the deceased. The chemical information in burnt bone fragments could be employed to assess the sex and age groups of the deceased with 79.60% and 75.10% accuracy, respectively. Chemical measurements were performed on burnt bone samples from two additional individuals to verify the developed logistic equations and classification protocol. More fractions of bones from an individual give a higher percentage of correction for classifying sex and age at death of the deceased.

Separation of lead from high matrix electroless nickel plating waste solution using an ion-selective immobilized macrocycle system

Separation of trace levels of lead from concentrated-matrix electroless nickel plating (ENP) waste solutions is required to meet the increasingly stringent environmental regulations. A solid phase extraction (SPE) system using a molecular recognition technology (MRT) gel was used for the selective separation of trace levels of lead (Pb) from the waste discharge of ENP operations, followed by subsequent analysis with inductively coupled plasma optical emission spectrometry (ICP-OES). Two SPE–MRTs, AnaLig® Pb-01 and AnaLig® Pb-02, packed in 3mL polypropylene cartridges were used to treat the synthetic metal-waste solutions that were used to simulate the typical metal mixture in ENP bath waste. The fortified solutions contained 100–1000μgL−1 of Pb in an HNO3 matrix with pre-added Ni, Cu and other interfering elements (1000mgL−1). After the sample treatment, the SPE–MRT cartridges were washed with water and 0.1M nitric acid, followed by elution with 0.03M EDTA. The matrix elements (e.g., Ni, Cu) were completely removed at the washing step, while the ‘captured’ Pb was quantitatively eluted, as determined by ICP-OES measurements. The detection limit of the proposed method was 2.6μgL−1. ‘Real’ samples from commercial ENP operations were used to assess the validity of this method, and almost quantitative Pb recovery was observed. The excellent Pb selectivity of the SPE–MRT system indicates the potential of the proposed technique for trace-level Pb separation from the Pb-containing high matrix aqueous waste discharge.

Multi-element determination in raft mussels by fast microwave-assisted acid leaching and inductively coupled plasma-optical emission spectrometry

Studies on the application of a short microwave irradiation cycle and the use of diluted acids to extract trace elements from raft mussel samples were developed. Multi-element determinations (Al, Ba, Cd, Cr, Cu, Fe, Mn, Pb, Sn, V and Zn) were carried out by inductively coupled plasma-optical emission spectrometry (ICP-OES). Parameters such as acid/oxidizing reagents (diluted nitric acid, hydrochloric acid and hydrogen peroxide) concentrations, acid/oxidizing solution volume, temperature, ramp time and hold time for the microwave heating were simultaneously studied by using an experimental design approach. The optimum conditions have showed the sample pre-treatment of 10 mussel samples to less than 3.0 min when a microwave power of 600 W and a controlled temperature of 65 °C were used. This time (hold time plus ramp time) is quite shorter than those reported for conventional microwave-assisted acid digestion procedures. Since temperature inside the reactor is not high, the venting time can be shorted to 15 min. In addition, the concentration of acid/oxidizing reagents needed to complete the acid leaching (2.5 M, 3.0 M and 0.5 % (m/v) for nitric acid, hydrochloric acid and hydrogen peroxide, respectively) is lower than the required concentration for a conventional microwave-assisted acid digestion (concentrated acids). The proposed method has showed a good repeatability of the overall method, and relative standard deviations between 11 and 2% were reached for 12 replicate microwave-assisted acid leaching and ICP-OES measurements. The method was finally validated by analyzing TORT-1 and GBW-08571 certified reference materials and it was successfully applied to fast multi-element determinations in several raft mussel samples.