Identification and quantification of sources of variation in the analysis of steel

In steel industries a need exists for the reduction of variation in the element concentrations. This need is triggered by an increasing demand for high quality steel products by clients. The results of a large-scale experiment concerning the identification and quantification of sources of variation in the production, sampling and analysis of steel are presented. The results are obtained by means of a strategic approach that consists of six steps. By means of this strategic approach, insight is obtained in the build-up of the total variation. This knowledge can be used to reduce the influence of those factors that have a major impact on the total variation. Attention is focused on estimating the magnitude of sources of variation apparent in sampling of certain stages of the steel making process and in analysis of steel samples by means of spark emission spectrometry. Received: 6 November 1999 / Revised: 10 February 2000 / Accepted: 19 March 2000     

Identification of nitride inclusions in steel using differential thermal analysis and evolved gas analysis

A preliminary study has been made of the feasibility of applying differential thermal analysis/evolved gas analysis (DTA/EGA) to the identification and estimation of nitrides in residues extracted from iron base alloys. A set of commercially available nitride powders have also been examined.The results showed that EGA traces are more informative than the DTA observations and, additionally, provide an estimate of the total nitrogen present. Residues from steels often contain elemental carbon and this complicates the interpretation of the DTA and EGA traces. It is generally concluded that the DTA/EGA technique is useful in identifying nitrides but should be ancilliary to other techniques such as X-ray diffraction.

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Zusammenfassung Eine Vorstudie wurde durchgeführt um die Einsatzmöglichkeit der Differentialthermoanalyse/Emittierte Gasanalyse (DTA/EGA) zur Identifizierung und Abschätzung der Nitride in aus Eisenbasenlegierungen extrahierten Rückständen zu prüfen. Eine Reihe handelsüblicher Nitridpulver wurde ebenfalls untersucht.Die Ergebnisse zeigten, daß EGA-Spuren informativer sind als die DTA-Beobachtungen und überdies eine Schätzung des Gesamtstickstoffgehaltes gestatten. Rückstände aus Stählen enthalten oft Kohlstoff und dies erschwert die Deutung der DTA- und EGA-Spuren. Im Allgemeinen kann gefolgert werden, daß die DTA/EGA-Technik bei der Identifizierung von Nitriden nützlich ist, doch nur als Ergänzung anderer Techniken, wie z. B. die Röntgendiffraktion, eingesetzt werden sollte.

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Résumé On a effectué une étude préliminaire pour rechercher si l'emploi conjugué de l'analyse thermique différentielle et de l'analyse des gaz émis (ATD/AGE) pouvait servir à l'identification et à l'estimation de la teneur des nitrures présents dans les résidus d'extraction des alliages à base fer. On a également examiné une série de nitrures en poudre disponibles commercialement.Les résultats ont montré que les enregistrements d'AGE fournissent davantage de renseignements que les courbes ATD car ils donnent en plus la valeur de l'azote total présent. Les résidus d'extraction des aciers contiennent souvent du carbone élémentaire, ce qui complique l'interprétation des enregistrements d'ATD et d'AGE. L'étude permet de conclure qu'en général la technique d'ATD/AGE est utile pour identifier les nitrures, mais qu'elle devrait être utilisée comme méthode auxiliaire vis-à-vis d'autres techniques, par ex. la diffraction des rayons X.

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The authors would like to express their thanks to the Directors of the British Steel Corporation, Tubes Division for permission to publish this paper.     

Identification and quantification of p-chlorobenzenesulfonic acid in groundwater

Infrared spectra of various extracts were used to identify p-chlorobenzenesulfonic acid in groundwater, and several derivatives were prepared for confirmation. A reversed-phase ion-pair liquid chromatographic method was developed to quantify the compound. Groundwater from the Stringfellow Superfund site was used as a test sample, p-Chlorobenzenesulfonic acid was determined to be the predominant organic species in the water, comprising as much as 50% of the organic carbon.     

Identification and quantification of N-methylepinephrine in human urine

N-Methylepinephrine was analysed in human urine using a high-performance liquid chromatographic catecholamine assay. The identity of the compound was confirmed by gas chromatography-mass spectrometry. The excretion of N-methylepinephrine is slightly less than that of epinephrine: excretion values were in the range 2-65 nmol per 24 h (0.4-13 micrograms per 24 h) in 150 hypertensive patients. In addition to increased epinephrine excretion, increased urinary excretion of N-methylepinephrine was found in three out of five patients with histologically proven pheochromocytoma.     

Identification of atmospheric trace-element sources by passive biomonitoring employing PCA and variogram analysis

The epiphyte plant Tillandsia capillaris was used as a passive biomonitor to study the relationship between elemental accumulation and emission sources in the province of Córdoba, Argentina. The concentrations of As, Ba, Br, Ca, Ce, Co, Cr, Cs, Eu, Fe, Gd, Hf, K, La, Lu, Na, Nd, Rb, Sb, Sc, Se, Sm, Ta, Tb, Th, U, Yb, and Zn were determined in T. capillaris leaves by Instrumental Neutron Activation Analysis. A variogram analysis was performed to identify the emission sources of these elements in the study area, obtaining different patterns for each element analysed. A principal-component analysis was subsequently performed to further confirm the different contaminant emission sources and it coincided with the results of the variogram analysis. We observed that the enrichment of most elements was associated with natural sources (soil) and that only some elements showed evidence of enrichement related to sources such as traffic (K, Sb and Zn), industries (Br), and mining activity (Ca).     

Identification and quantification of major species of arsenic in rice

A study was undertaken to develop a method for the chemical speciation of As in rice on the basis of current knowledge in this field for use in preparing a certified reference material (CRM). Samples of the Arborio rice variety were ground to a fine powder, which was extracted under sonication with a water-methanol mixture (1 + 1, v/v). The resulting solutions were injected into a high-performance liquid chromatograph combined on-line with a quadrupole inductively coupled plasma-mass spectrometer. This hyphenated system allowed for the quantification of As species in one analytical step. Four forms of As were detected: inorganic As (III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA), and inorganic As (V) at concentrations of 88.2 +/- 7.1, 50.8 +/- 5.0, 15.2 +/- 1.7, and 51.2 +/- 3.5 ng/g, respectively. The concentration of total As was 211 +/- 7 ng/g. The limits of detection (3sigma criterion) and the quantitation (10sigma criterion) were, respectively, as follows (in ng/g): As (III), 0.095 and 0.320; As (V), 0.082 and 0.273; MMA, 0.110 and 0.367; and DMA, 0.145 and 0.480. Ten hours were needed for the extraction procedure, 6 h for the evaporation, and 30 min for quantification of the analytes. This investigation was performed in the frame of a European Commission Project on the feasibility of CRMs for As and Se species.     

Identification and quantification of apolipoprotein D in normal human urine

Apolipoprotein D has been identified in normal human urine, using sodium dodecyl sulfate-polyacrylamide gel electrophoresis, followed by immunoblotting with monospecific antibodies. Urinary apolipoprotein D appeared as a main 33,000 u protein together with a minor fraction corresponding to its partially deglycosylated species of lower molecular mass. No high molecular mass forms of apolipoprotein D naturally occurring in plasma could be detected. The apolipoprotein D mean +/- SD concentration assayed with rocket immunoelectrophoresis, in urine samples from nine apparently healthy normal men, was 1.4 +/- 1.0 mg/L (range: 0.2-3.0 mg/L). Among the plasma apolipoproteins, apolipoprotein D behaves uniquely as regards its excretion in urine; the other apolipoproteins belonging to the A, B, D and E groups, although of low molecular masses, are present, at most, in trace amounts in normal urine.     

Identification of steel by X-ray fluorescence analysis with a pyroelectric X-ray generator

An application of X-ray fluorescence analysis with a pyroelectric X-ray generator is presented. Steel standard samples were identified by X-ray fluorescence analysis with this novel X-ray generator to check its capability for performing qualitative and quantitative analysis as an X-ray source for X-ray fluorescence spectrometers. Cr, Ni, V, Co, and W were detected in steel standard samples. V and Cr can be detected even when the content is below 1%. Although it is difficult to detect minor elements because of the low power of the excitation X-rays, it is possible to identify the analyzed samples on the basis of major elements at the percentage level. The pyroelectric X-ray generator is very suitable for portable X-ray fluorescence spectrometers.     

Identification and quantification of polynuclear aromatic compounds in synthoil by room-temperature phosphorimetry

Room-temperature phosphorimetry (r.t.p.) is used to identify and quantify polynuclear aromatic compounds in a synthetic fuel (Synthoil). Several trace and major components, benzo[a]pyrene, chrysene, fluorenes, fluoranthene, phenanthrene, and pyrene, have been identified and determined at concentrations ranging from tens to thousands of parts-per-million. The selectivity of the r.t.p. analysis is greatly improved by using selective heavy-atom perturbation and synchronous excitation scanning.     

Identification and relative quantification of specific glycation sites in human serum albumin

Glycation (or non-enzymatic glycosylation) is a common non-enzymatic covalent modification of human proteins. Glucose, the highest concentrated monosaccharide in blood, can reversibly react with amino groups of proteins to form Schiff bases that can rearrange to form relatively stable Amadori products. These can be further oxidized to advanced glycation end products (AGEs). Here, we analyzed the glycation patterns of human serum albumin (HSA) in plasma samples obtained from five patients with type 2 diabetes mellitus. Therefore, glycated peptides from a tryptic digest of plasma were enriched with m-aminophenylboronic acid (mAPBA) affinity chromatography. The glycated peptides were then further separated in the second dimension by RP-HPLC coupled on-line to an electrospray ionization (ESI) tandem mass spectrometer (MS/MS). Altogether, 18 Amadori peptides, encompassing 40% of the HSA sequence, were identified. The majority of the peptides were detected and relatively quantified in all five samples with a high reproducibility among the replicas. Eleven Lys-residues were glycated at similar quantities in all samples, with glycation site Lys₅₄₉ (K_Am(Glc)QTALVELVK) being the most abundant. In conclusion, the established mAPBA/nanoRP-HPLC-ESI-MS/MS approach could reproducibly identify and quantify glycation sites in plasma samples, potentially useful in diagnosis and therapeutic control.     

Identification and quantification of the antimicrobial components of a citrus essential oil vapor

The anti-bacterial components of a citrus essential oil vapor were identified as linalool, citral and beta-pinene using a bioautography method and quantified by GC-MS. Essential oil vapor release, monitored in real-time with Atmospheric Pressure Chemical Ionization - MS (APCI-MS), showed differences in the vapor release profile oflimonene, beta-pinene and linalool over 24 hours, while Solid Phase Micro-extraction (SPME) GC-MS demonstrated changes in composition of the vapor at 35 degrees C. Fourteen isolates were tested in vitro for their susceptibility to the EO vapor and to linalool, citral and beta-pinene vapors, both separately and in a mixture containing the three components in the amounts at which they occur in the EO vapor. All eleven Gram-positive strains tested were susceptible to the EO vapor, linalool, citral and beta-pinene vapors separately and the mixture with zones of inhibition of 4.34 cm, 5.32 cm, 5.58 cm, 4.86 cm and 4.68 cm, respectively. Of the three Gram-negative strains tested, Pseudomonas aeruginosa 10145 was resistant to all the vapors. When bacteria inoculated onto stainless steel surfaces were exposed to either the EO vapor or a linalool/citral/beta-pinene vapor mixture there was no significant difference in reduction for the Gram-positive isolates, while the Gram-negative isolates were resistant to both EO vapor and the linalool/citral/beta-pinene mixture.     

Identification and quantification of main flavonoids in the leaves of Bambusa multiplex cv. Fernleaf

Abstract

The chemical profile of Bambusa multiplex cv. Fernleaf (B. multiplex) leaves was analysed by UPLC-DAD-Q-TOF-MS. Twelve compounds were identified and C-glycosyl flavonoids, including vitexin, isovitexin, isoorientin and its derivatives, are the main constitutes of the plant. Besides, a HPLC method for isoorientin quantification was developed. The RSD of retention time and peak area were 0.05% and 2.04% for six times analysis of isoorientin with concentration of 20?μg/mL. The recovery of isoorientin in real sample was 99.2%. The general trend of isoorientin content in B. multiplex leaves was that it steady increased from Jan. to May, and then quickly decreased. The maximum was found on May with value of 4.7?mg/g. The lowest level of isoorientin was found during Aug. to Nov. with value of about 1.66?mg/g. In different seasons, isoorientin is always the most dominant flavonoid which was accounted for about 50% of total flavonoids in the sample.     

Identification and quantification of anticarcinogens in garlic extract and licorice root extract powder

Nine organosulfur compounds present in an aged garlic extract and two isoflavonoids and one triterpenoid present in a licorice root extract powder have been identified and quantified. Quantification involved solvent extraction and gas chromatographic – mass spectrometric analysis (garlic extract) or hydrolysis, solvent extraction, and liquid chromatographic analysis (licorice root extract powder). Although the garlic extract proved to be unstable and the concentration of the organosulfur compounds varied with time, one analysis of the extract gave the following results: methyl disulfide (0.607 μg/g), methyl trisulfide (0.181 μg/g), allyl sulfide (2.02 μg/g), allyl disulfide (0.784 μg/g), allyl trisulfide (0.795 μg/g), allyl methyl sulfide (1.64 μg/g), allyl methyl disulfide (0.411 μg/g), allyl methyl trisulfide (0.695 μg/g), and ethyl 2-propenesulfinate (11.4 μg/g). The analysis of the licorice root extract powder gave the following results: formononetin (1.92 mg/g), isoliquiritigenin (9.61 mg/g), and 18β-glycyrrhetinic acid (43.9 mg/g). Methods were successfully developed to quantify the same compounds in the serum of test animals which had consumed feed spiked with garlic extract or licorice root extract powder. Only the 18β-glycyrrhetinic acid could be detected in the sera of such animals, however. An effort was also made to determine serum levels of prostaglandin E2 to correlate its inhibition with levels of the dietary components, but the prostaglandin E2 levels were too low to measure.     

Detection, distribution, and quantification of carbon in steel microstructures by PEELS.

This work concerns the use of parallel electron energy loss spectroscopy (PEELS) to investigate the detection, distribution, and quantification of carbon in various steel microstructures generated by rapid cooling rates or by isothermal transformation. The feasibility of detecting C in steels containing very small amounts of carbon was first examined by calculating the minimum detectable mass fraction for a variety of binary Fe-C alloy specimen thicknesses and microscope conditions. These theoretical studies indicated that the detection of carbon in steel microconstituents containing about 0.01 wt.% (or even less) was easily possible with an analytical transmission electron microscope equipped with a LaB6 emitter and a PEEL spectrometer. These theoretical calculations seemed to be reasonable, as it proved possible to make a quantitative PEELS study of the partitioning between the microconstituents ferrite, retained austenite, and martensite found in an ultralow carbon (0.03 wt.%) steel weld metal provided care was taken to avoid hydrocarbon contamination. Studies of both carbon and molybdenum segregation to ferrite/martensite interfaces in an isothermally transformed Fe-C-Mo alloy were also carried out in order to investigate the nature of the "solute drag" effect in this alloy system.     

Identification and quantification of nucleosides and nucleobases in Geosaurus and Leech by hydrophilic-interaction chromatography

A simple hydrophilic-interaction chromatography (HILIC) method was developed for the identification and quantification of 14 nucleosides and nucleobases, namely cytosine, uracil, cytidine, guanine, hypoxanthine, xanthine, uridine, thymine, inosine, guanosine, thymidine, 2′-deoxyadenosine, 2′-deoxyinosine and 2′-deoxyuridine in two traditional Chinese medicines, Geosaurus and Leech. The separation was achieved on a TSKgel Amide-80 column (150 mm × 2.0 mm, 3.0 μm) with a mixture of acetonitrile and 10 mM aqueous ammonium acetate as the mobile phase at a flow rate of 0.2 mL/min. The temperature was set at 30 °C and UV detection wavelength was set at 260 nm. All calibration curves showed good linearity (R² > 0.9957) within the test ranges. The overall intra- and inter-day RSD ranged from 0.4 to 3.4% and from 0.7 to 3.3%, respectively. The LOD and LOQ were in the range of 0.07-30.49 ng/mL and 0.26-60.98 ng/mL, respectively. The repeatability of the method was in the range of 2.2-5.8% for Geosaurus and 1.4-5.5% for Leech. The recoveries of the samples were in the range of 91.4-100.9% for Geosaurus, and 91.9-99.3% for Leech. The established method was applied successfully for the analysis of nucleosides and nucleobases in 22 commercially available samples collected from different regions in China and Japan. Our data showed that HILIC had advantages as a useful tool for the study of the bioactive components in Geosaurus and Leech as well as their quality control, and could therefore be used for the determination of the analytes in pharmaceutical products and biological fluids.     

Identification and quantification of lignans in wheat bran by gas chromatography-electron capture detection

Whole grain cereals are an important source of bioavailable lignans, the group of compounds with potential anti-cancerogenic, antioxidant, anti-proliferative, pro-apoptotic, and antiangiogenic properties. The aim of this work was to develop a sensitive method for determination of wheat bran lignans. The analysis of lignans secoisolariciresinol, hydroxymatairesinol, lariciresinol, matairesinol, pinoresinol, syringaresinol is based on derivatization with pentafluoropropionic anhydride (PFPA) and gas chromatography-electron capture detection (GC-ECD), using styrene glycol as internal standard. To our knowledge, this is the first time that EC detection has been used for lignan analysis. The results show that the technique is reproducible and sensitive enough for detecting lignans in wheat at parts-per-billion (ppb) levels, except for hydroxymatairesinol. The method developed showed good recovery (85-105%) and precision (4-20%) for five types of lignans and thus represents a simpler and more affordable alternative to state-of-the-art wheat lignan liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis.     

Identification and quantification of major bovine milk proteins by liquid chromatography

In the field of food quality, bovine milk products are of particular interest due to the social and economic importance of the dairy products market. However, the risk of fraudulent manipulation is high in this area, for instance, replacing milk powder by whey is very interesting from an economic point of view. Therefore, there is a need to have suitable analytical methods available for the determination of all milk components, which is currently not the case, especially for the main proteins. The detection of potential manipulations requires then a clear analytical characterisation of each type of bovine milk, what constitutes the goal of this work. The separation of the major milk proteinic components has been carried out by ion-pair reversed-phase HPLC with photodiode array detection, using a C4 column. The overall optimisation has been achieved using a statistical experimental design procedure. The identification of each protein was ascertained using retention times, peak area ratios and second derivative UV spectra. Quantification was based on calibration curves drawn using purified proteins. Major sources of uncertainty were identified and the full uncertainty budget was established. The procedure was initially developed using the skimmed milk powder certified reference material CRM 063R and then applied to various types of commercial milks as well as to raw milk. The method is able to separate and quantify the seven major proteins (K-casein, alphas2-casein, alphas1-casein, beta-casein, alpha-lactalbumin, beta-lactoglobulin B and beta-lactoglobulin A) in one run and also to provide precise determinations of the total protein concentration. These are important results towards the further development of a reference method for major proteins in milk. In addition, the use of a certified material reference is suggested in order to make comparisons of method performances possible.     

Force variation of chlorinated butyl-rubber peeling from steel in the process of vulcanization

Vulcanization of an adhered layer with the use of low-temperature vulcanizing agents with different adhesion activities was carried out to increase the heat resistance and resistance to displacement of the adhesive tapes with different adhesive activity. It is shown that the force variation of the vulcanized adherent layer based on the chlorobutyl rubber and polymeric petroleum resin for peeling from steel depends on the measurement temperature: at 25°C, the peeling force decreases, while at 80°C it increases as compared with nonvulcanized adhesive. The observed changes are conditioned both by the increase of the cohesion strength of the adhered layer and by decrease of the elastic component in the layer peeling energy.     

Identification and quantification of valuable plant substances by IR and Raman spectroscopy

This review presents various infrared and Raman spectroscopic methods applied to the analysis of valuable plant substances or quality parameters in horticultural and agricultural crops. In most cases, vibrational measurements can be performed directly on plant tissues as well as on fractions isolated from the plant material by hydro-distillation or solvent extraction. Generally, both spectroscopy techniques allow to obtain spectra which present some characteristic key bands of individual components. These bands provide information about the chemical composition, including both primary and secondary metabolites, of the investigated samples. Furthermore, based on such markers related to individual plant substances, spectroscopic analyses in principle allow the discrimination of different species, and even chemotypes among the same species. Combination of vibrational spectroscopy and hierarchical cluster analysis provides a fast, easy and reliable method for chemotaxonomy characterization. In most presented cases, determination of main plant components applying the PLS algorithm results in comparatively high R² and low SECV values. The ability to rapidly monitor various plant components makes it possible to efficiently select high-quality single plants from wild populations as well as progenies of crossing experiments. Furthermore, the vibrational spectroscopy methods can also be used by the processing industry in order to perform fast quality checks of incoming raw materials as well as continuous controlling of the production.