External calibration of GOCE data using regional terrestrial gravity data

This paper reports on a study of the methodology of external calibration of GOCE data, using regional terrestrial-gravity data. Three regions around the world are selected in the numerical experiments. The result indicates that this calibration method is feasible. The effect is best with an accuracy of scale factor at 10 -2 level, in Australia, where the area is smooth and the gravity data points are dense. The accuracy is one order of magnitude lower in both Canada, where the area is smooth but the data points are sparse, and Norway, where the area is rather tough and the data points are sparse.

Validation and Comparison of Two Calibration Methods for the Measurement of Stable Iodine in the Urinary Matrix by ICP-MS:Standard Addition vs.External Calibration

Background: In the context of a nuclear reactor accident, thyroid is the main target organ of radioactive iodines. To avoid as much as possible thyroid disorders or even cancer development, it is recommended to administer a single dose of potassium iodide to people at risk of exposure. Nevertheless, the Fukushima Dai-ichi disaster has pointed out many questions about the conditions of stable iodine prophylaxis implementation highlighting the need for reflection further revision of the actual “iodine doctrine”. Therefore, providing useful data is required notably through the implementation of animal experiments to strengthen current knowledge and to edit new recommendations. Methods: Urinary iodine constitutes a very good indicator to investigate the function of thyroid, its interpretation demands reliable analyses. Prior to perform animal experiments, two calibration methods were designed by our lab and compared together (standard addition and external calibration) to assess the urinary concentration of stable iodine in urine by ICP-MS. They were validated based on several key parameters especially linearity, accuracy and limits of detection (LOD) and quantification (LOQ). Results: The results were nicely satisfying. Indeed, both calibration methods have indicated very good coefficients of correlations, accuracies with low expanded relative uncertainties were obtained. The estimated LOD in the sample for standard addition method and external calibration were fully acceptable, 0.39 μg·L-1 and 0.35 μg·L-1, respectively. All performance criteria have been thus fulfilled successfully. The established methods were proven to be accurate, robust and sensitive. Once validated, both calibration methods were applied to rat urine samples and the results of z-score and Wilcoxon W test concluded that there were no statistically significant differences between both methods.

Improved Analytical Methods for Determination of Residues of Nitrapyrin and 6-Chloropicolinic Acid in Different Crop Matrices by Liquid Chromatography-Tandem Mass Spectrometry

Novel analytical methods were developed for the determination of nitrapyrin and 6-chloropicolinic acid (6-CPA) residues in agricultural products. Nitrapyrin was extracted with hexane: toluene (1:1, v/v) and 6-CPA with 0.1 N sodium hydroxide (NaOH). For nitrapyrin, samples were cleaned with silica solid phase extraction (SPE) and for 6-CPA with C18 or carbon SPE. Analysis was performed by liquid chromatography-tandem mass spectroscopy (LC-MS/MS) with external calibration (0.010 to 0.0010 µg∙mL−1 for nitrapyrin and 0.0050 to 0.00025 µg∙mL−1 for 6-CPA). Recoveries for nitrapyrin and 6-CPA were 68% - 102% and 66% - 90%, respectively. Nitrapyrin was detected in celery and onion (−1) and 6-CPA in onion, mustard greens and lettuce (−1). Lower level method validation (LLMV) for nitrapyrin and 6-CPA was 0.020 µg∙g−1 and 0.050 µg∙g−1, respectively. The methods presented in this study are robust and were utilized for the registration of nitrapyrin on agricultural commodities in the United States.

Quantitative Analysis of Fe Content in Iron Ore via External Calibration in Conjunction with Internal Standardization Method Coupled with LIBS

The external calibration in conjunction with internal standardization（ECIS） coupled with laser-induced breakdown spectroscopic（LIBS） technique was proposed to perform the quantitative analysis of Fe content in iron ore The plasma temperature and the electron number density were calculated to prove that the plasma was under local thermodynamic equilibrium（LTE） conditions and to ensure that the integral intensities of Fe I lines were reasonable. In addition, the result of the quantitative analysis shows a content of （20.26±0.59）% by mass of Fe in the iron ore. It was determined by four calibration curves, drawn for four emission lines of Fe I（373.48, 373.71,404.58 and 438.35 nm） normalized by Mn I line, base on the ECIS method which can eliminate the influence of matrix effect and improve the accuracy of quantitative analysis, compared with the standard addition method. Both the results of these two analytical methods were compared with that listed in the Standard Substance Certificate. The percentage content of Fe in the same sample of iron ore by the ECIS method was （20.17±0.08）% by mass, which shows a good performance to analyze the Fe content of iron ore in combination with LIBS.