Coating properties of a novel water stationary phase in capillary supercritical fluid chromatography

The coating properties of a novel water stationary phase used in capillary supercritical fluid chromatography were investigated. The findings confirm that increasing the length or internal diameter of the type 316 stainless‐steel column used provides a linear increase in the volume of stationary phase present. Under normal operating conditions, results indicate that about 4.9 ± 0.5 μL/m of water phase is deposited uniformly inside of a typical 250 μm internal diameter 316 stainless‐steel column, which translates to an area coverage of about 6.3 ± 0.5 nL/mm² regardless of dimension. Efforts to increase the stationary phase volume present showed that etching the stainless‐steel capillary wall using hydrofluoric acid was very effective for this. For instance, after five etching cycles, this volume doubled inside of both the type 304 and the type 316 stainless‐steel columns examined. This in turn doubled analyte retention, while maintaining good peak shape and column efficiency. Overall, 316 stainless‐steel columns were more resistant to etching than 304 stainless‐steel columns. Results indicate that this approach could be useful to employ as a means of controlling the volume of water stationary phase that can be established inside of the stainless‐steel columns used with this supercritical fluid chromatography technique.     

Co3O4 Decorated Ti/TiO2 Nanotubes for Photogenerated Cathodic Protection of 304 Stainless Steel

The Co₃O₄ decorated TiO₂ nanotube arrays(NTAs) coatings are fabricated by the combination of anodization and impregna-ting methods. It is found that the introduction of Co₃O₄ can reduce the diffraction intensity of (101) plane of the TiO₂ and accelerate the separation of photogenerated electron/hole pairs. In addition, the open circuit potential(OCP) and the corrosion potential of 304 stainless steel(304SS) with or without Co₃O₄ decorated TiO₂ NTAs were measured under visible light, which indicated the 304SS coupled with Co₃O₄ decorated TiO₂ NTAs had better anticorrosion performance than that of the 304SS or the 304SS coupled with pure TiO₂ NTAs. The enhancement of the cathodic protection performance of the Co₃O₄ decorated TiO₂ NTAs can be ascribed to the matched energy levels and strong interaction between Co₃O₄ and TiO₂ NTAs, and the improvement of light absorption.     

Growth of cedar-like Au nanoparticles coating on an etched stainless steel wire and its application for selective solid-phase microextraction

A novel cedar-like Au nanoparticles (AuNPs) coating was fabricated on an etched stainless steel (SS) wire by direct chemical deposition and used as an efficient and unbreakable solid phase microextraction (SPME) fiber. The etched SS wire offers a rough surface structure for subsequent growth of AuNPs in chloroauric acid solution. As a result, the uniform cedar-like AuNPs coating with larger surface area was tightly attached to the etched SS wire substrate. The AuNPs coated etched SS fiber (AuNPs/SS) was examined for SPME of ultraviolet (UV) filters, phthalate esters and aromatic hydrocarbons coupled to high-performance liquid chromatography with UV detection. The fabricated fiber exclusively exhibited excellent extraction efficiency and selectivity for some aromatic hydrocarbons. Influential parameters of extraction and desorption time, temperature, stirring rate and ionic strength were investigated and optimized. The limits of detection ranged from 0.008 μg L⁻¹ to 0.037 μg L⁻¹. The single fiber repeatability varied from 3.90% to 4.50% and the fiber-to-fiber reproducibility ranged from 5.15% to 6.87%. The recovery of aromatic hydrocarbons in real water samples spiked at 2.0 μg L⁻¹ and 20 μg L⁻¹ ranged from 94.38% to 106.2% with the relative standard deviations below 6.44%. Furthermore the growth of the cedar-like AuNPs coating can be performed in a highly reproducible manner. This fabricated fiber exhibits good stability and withstands at least 200 extraction and desorption replicates.     

Electrochemical Characterization of Stainless Steel as a New Electrode Material in a Medical Device for the Diagnosis of Sudomotor Dysfunction

An electrochemical sensor detects the risk of diabetes and prediabetes; low potentials are applied to nickel electrodes and electrical responses are measured. Although the contact of nickel with skin is short, the risk of allergical reactions cannot be discarded. SS 304L, with lower Ni content, was tested in carbonate buffer solutions containing chloride, lactate and urea to investigate its sensitivity to different parameters in sweat and compare it to nickel. The results show that SS 304L is a suitable material for the assessment of sudomotor dysfunction due to its high capacity to detect the deviation in Cl^? concentration. Sensitivity of SS 304L to Cl^? is much higher than for nickel.     

Die Isolierung radioaktiv markierter nichtmetallischer Einschlüsse aus Hochlegierten Stählen

Zur Isolierung von Einshlüssen aus hochlegierten Stählen werden die Hauptkomponenten Fe, Ni, Cr und weitere Metalle durch mehrstufig ausgeführte Flüssig-Flüssig-Extraktionen mit verschiedenen Extraktionsmitteln abgetrennt. Die im Eindampfrückstand der wäβrigen Phase nach der Extraktion verbleibenden Einschlüsse können für die meisten Radionuklide ohne nennenswerte Selbstabsorption mit einem Groβflächenzählrohr oder anderen geeignetenZählvorrichtungen ausgemessen werden.     

Influence of modification time and high frequency ultrasound irradiation on self-assembling of alkylphosphonic acids on stainless steel: Electrochemical and spectroscopic studies

Self-assembly of alkylphosphonic acids on stainless steel was investigated under different conditions. Four different alkylphosphonic acids exhibiting alkyl chain of various size were synthesized and studied: butylphosphonic acid (C4P), octylphosphonic acid (C8P), decylphosphonic acid (C10P), and hexadecylphosphonic acid (C16P). Electrochemistry experiments were extensively carried out in order to determine electrochemical surface blocking of adsorbed layers in function of grafting time. In term of surface blocking, an 8 h modification time was optimal for all alkylphosphonic acids. Longer immersion times lead to degradation of adsorbed layers. For the first time, grafting of C16P was studied under high frequency ultrasound irradiation. Interestingly, grafting process is highly accelerated under sonication and well-covering C16P modified substrates are obtained after 1 h of immersion under ultrasound irradiation. This would allow to elaborate high-quality alkylphosphonic acids modified samples within much shorter times. Water contact angles measurements and X-ray Photoelectrons Spectroscopy (XPS) confirmed presence of adsorbed alkylphosphonic acids on stainless steel surface. A very tight link between electrochemical blocking, surface hydrophobicity and species chemical grafting was established.     

Investigation on Semi-conductive Properties of Hot Growth Film on 316L Austenitic Stainless Steel

The semi-conductive performances of hot growth film on 316L stainless steel were studied by means of electrochemical impedance spectroscopy(EIS) and Mott-Schottky analysis.The chemical compositions of the hot growth films were detected by X-ray photoelectron spectroscopy(XPS).The results show that the transfer resistance and film resistance increase with increasing temperature to 400℃,then they decrease sharply with further continuously increasing temperature.Formation time plays an important role in determ...     

氢化物发生-原子荧光光谱法测定低合金钢中微量砷

采用氢化物发生-原子荧光光谱法测定低合金钢中砷的含量。样品经盐酸-硝酸混合酸消解,以盐酸(5+95)溶液为反应介质,15g·L~(-1)硼氢化钾-2g·L~(-1)氢氧化钾的混合溶液为还原剂,采用柠檬酸作为掩蔽剂。砷的质量浓度在60.0μg·L~(-1)以内与荧光强度呈线性关系,方法的检出限(3s/k)为0.023μg·L~(-1)。应用此法对标准钢样进行了分析,测定结果与认定值相符合,可满足钢铁中微量砷(质量分数0.001%～0.04%)的测定要求。     

XPS study of Cr segregation in a martensitic stainless steel

Cr martensitic steels are promising materials for structural applications in future nuclear fusion reactors. Because the embrittlement after tempering treatments can be a serious problem, the fracture mode of a steel with 10.5 wt% of Cr treated at 700°C for 18 h has been investigated through Charpy tests in the temperature range from −100°C to +150°C. X-ray photoelectron spectroscopy (XPS) analyses carried out on the fracture surfaces evidenced the segregation of Cr in both ductile and brittle (quasicleavage) fields. The unexpected result indicates that Cr segregation weakens the atomic bonds; thus, the fracture path in both the cases corresponds to the zones with higher Cr content.