Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.     

Neutron activation analysis of 35 elements in Chinese standard rocks (GSR) and soils (GSS) using the SLOWPOKE reactor

Concentrations of 35 elements in Chinese Standard Rocks (GSR-1 to GSR-3) and Soils (GSS-1 to GSS-8) have been measured with INAA using the SLOWPOKE reactor. At the same time, the U. S. NBS reference standards: SRM-1632a (Bituminous Coal), SRM-1633a (Coal Fly Ash) and SRM-1646 (Estuarine Sediment) were also analyzed in order to cross-check the accuracy of this method. The results obtained indicate that the reproducibility of the method is satisfactory for most of the elements, namely the precision in general, is better than ±10%. Comparison of our values for NBS SRM-1632a, 1633a and 1646 with the certified values of NBS or with values cited in the literature indicates good agreement. The results were found to be accurate within ±10% error of the established results.     

Surface treatment of borosilicate glass beakers for prevention of sodium contamination

Pyrex glass beakers are treated with molten Ca(NO₃)₂-KNO₃ (20:80 mol %) mixture at 500°C for 3 h. Treated beakers can be used successfully in wet oxidation of SRM-1571 Orchard Leaves for sodium determination; at least 10 oxidations can be done without sodium contamination. Mass spectrometry is used to investigate the depth profiles of glass components within 60 nm of the glass surfaces and to clarify the mechanism of the sodium contamination.     

The preparation of thick-film glass capillary columns

A detailed method for the routine preparation of glass capillary columns is presented. The method consists of coating a glass tube with quartz powder prior to pulling the tube into a capillary. The inner surface of the capillary consists of an even distribution of quartz particles fused to the walls. This surface has been found readily deactivated by standard procedures and ideal for the preparation of thick-film glass capillary columns. The method has been thoroughly tested in two independent laboratories to ensure that the procedures described are reproducible.     

Simultaneous determination of sixteen major and minor elements in river sediments by energy-dispersive x-ray fluorescence spectrometry after fusion in lithium tetraborate glass

Fluvial sediments, including the NBS SRM-1645 Standard River Sediment, were fused in lithium tetraborate to form glass discs on which determinations of 16 elements (K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr, Y, Zr and Pb) were obtained simultaneously at a single set of x-ray conditions by energy-dispersive x-ray fluorescence spectrometry (e.d.x.r.f.). Relatively high sample-to-flux ratios of 1:3 were employed to obtained determinations of several minor as well as major elements on a single disc. Lower sample concentrations 1:6 and 1:10 were also used with the NBS SRM-1645. Inter-element corrections for absorption by iron were significant for detectable elements heavier than iron. In the NBS SRM-1645 samples, corrections were made for the fluorescence of chromium by the Fe K lines as well as the absorption of the Fe K lines by chromium. A background correction was also necessary for manganese in NBS SRM-1645. At the lowest sample-to-flux ratio (1:10) good agreement was obtained between the e.d.x.r.f. determinations and the NBS values for all quantifiable elements except zinc. At higher sample-to-flux ratios, agreement with the NBS values was generally poorer with increasing sample concentration. The relative standard deviation (RSD) of the eight quantifiable major and minor elements (K, Ca, Ti, Mn, Fe, Zn, Sr and Zr) determined under a single set of x-ray conditions ranged from 2 to 9% (RSD) with a mean RSD of 4.4% for a set of replica discs fused with Lake Pueblo/Arkansas River sediment samples.     

Analytical control of silica glass production. Voltammetric determination of titanium and iron in raw materials and silica glass samples

Adsorptive stripping voltammetric (AdSV) methods are presented for the determination of titanium and iron in quartz and silica glass samples obtained after pressure decomposition. Mandelic acid and catechol were used as complexing agents for titanium and iron, respectively. The method for titanium determination is based on the catalytic effect of chlorate ions. An insoluble residue remaining after decomposition of quartz and silica glass samples in HF+H2SO4 mixture was checked by energy-dispersive X-ray analyses. ET-AAS was applied as a reference method to AdSV measurements.     

Analytical control of silica glass production. Voltammetric determination of titanium and iron in raw materials and silica glass samples

Adsorptive stripping voltammetric (AdSV) methods are presented for the determination of titanium and iron in quartz and silica glass samples obtained after pressure decomposition. Mandelic acid and catechol were used as complexing agents for titanium and iron, respectively. The method for titanium determination is based on the catalytic effect of chlorate ions. An insoluble residue remaining after decomposition of quartz and silica glass samples in HF+H₂SO₄ mixture was checked by energy-dispersive X-ray analyses. ET-AAS was applied as a reference method to AdSV measurements.     

Characterization and traceability of two generations of standard reference material for the measurement of vitamin K1(phylloquinone) at endogenous concentrations in human plasma and serum

Vitamin K is an essential micronutrient required for blood coagulation, regulation of vascular calcification and bone mineralization. Plasma and serum measurements of vitamin K₁(phylloquinone, K₁) made using high-performance liquid chromatography with fluorescence detection, or tandem mass spectrometry are used clinically and in population studies to assess vitamin K status. Standard reference materials provide a validation tool for laboratories, helping assure clinical diagnosis and the comparability of data from different populations. We manufactured two K₁ standard reference materials, in 2009 (KEQAS SRM-001) and in 2019 (KEQAS SRM-002). The target concentrations of K₁ were assigned to each SRM using the All Laboratory Trimmed Mean of results reported by selected laboratories enrolled in the Vitamin K External Quality Assurance Scheme (KEQAS). The assigned concentrations of K₁ for KEQAS SRM-001 and SRM-002 were 0.25 and 0.36 μg/L respectively. In 2019 KEQAS SRM-001 was re-analysed simultaneously with KEQAS SRM-002 to provide traceability between the two standards, therefore aiding comparability of analysis performed using these materials. Both standards were stored as aliquots at −80°C in the dark; annual re-analysis of the materials indicated that K₁ is stable for at least 12 years in these conditions.     

Determination of Essential Elements in Ayurvedic Medicinal Leaves by k0 Standardized Instrumental Neutron Activation Analysis

Elemental concentrations of a few medicinal leaves are determined by instrumental neutron activation analysis using the single comparator (k ₀) method. Data obtained for neem leaves, collected from two different places, have been used to see the effect of soil condition. The applicability of the method particularly for the simultaneous determination of Ca, Mg, V and Al in biological matrices has been evaluated in terms of the detection limit, precision and accuracy. The method was validated by analysing the NIST Standard Reference Material (SRM-1571) and it was found that the elemental concentrations measured in SRM-1571 are within ±10% of the reported values.     

Application of laser-excited atomic fluorescence spectrometry to the determination of iron

A frequency-doubled, flashlamp-pumped tunable dye laser is used to excite the Stokes direct-line atomic fluorescence transition of iron (296.7 nm/373.5 nm). Limits of detection are determined with single (0.6 ng/ml) and multipass (0.2 ng/ml) and with a l s time constant (a 0.06 ng/ml limit detection is obtained with an 8 s time constant). Noise sources limiting precision at both low (background flame emission shot and flicker noise) and high concentrations (laser pulse to pulse variability) concentrations are investigated and the technique is used for the determination of iron in simulated fresh water NBS SRM-1643), unalloyed copper (NBS SRM-394) and fly ash (NBS SRM-1633).     

Determination of Titanium In Quartz and Silica Glass Samples By Adsorptive Stripping voltammetry

ABSTRACT

This article presents a method for determination of titanium in quartz and silica glass samples based on adsorptive stripping voltammetry (AdSV) with mandelic acid. Hanging mercury drop electrode as a working electrode was used. The optimized conditions include: pH 3.3, accumulation potential –0.15 V, accumulation time 90 s, scan rate 10 mV/s, pulse amplitude 25 mV. In case of 5 min accumulation time the obtained detection limit was 6.5×10^-9 mol/L Ti. ET-AAS was applied as a reference method to AdSV measurements. The procedure for decomposition of quartz and silica glass samples applying small amount of acids is described.     

Influence of cetyltrimethylammonium bromide aqueous solutions on the surface strength of quartz glass under conditions of pH variation

A mechanism of the combined influence of solutions of electrolytes with various pHs (in 10^?3 N KCl solution) and cetyltrimethylammonium bromide (CTAB) cationic surfactant on the surface strength of quartz glass in a mechanical contact is studied. A similar cation-active medium is shown to embrittle quartz glass in neutral and alkaline pH ranges. The brittle strength of a near-surface layer of a material decreases owing to adsorption and electrocapillary reduction of its surface energy. The surface strength of the glass decreases to the largest extent at the CTAB critical micellization concentration. At low concentrations (10^?6M), a protective effect of forming chemisorbed CTAB layers prevails that is manifested in the hydrophobization of the surface of quartz glass by CTAB molecules and its screening from direct contact with an electrolyte solution. At the CTAB concentrations that are higher than the CMC, a formed micellar structure of CTAB has a lubricating effect, leading to softer boundary conditions of a frictional contact and a decreased probability of the damage of the near-surface layer of quartz glass. In acidic electrolyte solutions, CTAB cations or molecules did not affect the surface strength of quartz glass.     

采用石英玻璃作为离子减薄制样仪离子枪高压绝缘体的应用

针对离子减薄制样仪的离子枪高电压绝缘体（环）污染失效、再生变型等问题，提出了以石英玻璃环替代陶瓷环为绝缘体的方案，设计实施方法并进行实践验证.结果表明：使用高光洁度石英玻璃绝缘体显著提高了抗金属粉尘污染的能力，寿命长且经济耐用，还能经热处理清洁后再生重复使用，大大延长了更换绝缘体的时间，具有重要的应用价值.     

A portable total reflection X-ray fluorescence spectrometer with a diamond-like carbon coated X-ray reflector

A diamond-like carbon (DLC) coated quartz glass sample holder is used in a portable total reflection X-ray fluorescence (TXRF) spectrometer. A spot area of a water sample on the DLC sample holder becomes smaller than that on a quartz glass sample holder usually used in TXRF analysis because DLC is more hydrophobic. Therefore, the use of the DLC sample holder enhances fluorescent X-rays reaching a detector compared with the use of a quartz glass sample holder, leading to improvement in detection sensitivity. A detection limit of 28 pg is achieved for Cr in a river water sample when using the DLC sample holder.     

Anti-Reflective Coatings of Flowerlike Alumina on Various Glass Substrates by the Sol–Gel Process with the Hot Water Treatment

Anti-reflective (AR) properties of flowerlike alumina thin films with a small roughness of less than 100 nm have been studied on substrates such as soda-lime silica glass, non-alkali glass, and quartz glass. The highest AR effects were obtained on quartz glass substrate, which has the lowest refractive index of the three substrates. The reflectance of quartz glass substrates coated with flowerlike Al₂O₃ was less than 0.5% in the wavelength region from 300 to 720 nm.     

Multielement analysis of Chinese Biological Standard Reference Material by monostandard instrumental neutron activation analysis

A procedure for monostandard INAA of 21 elements (Hg, As, Br, Cr, Sb, Se, Ba, Zn, Ca, Ce, Co, Cs, Eu, Fe, Hf, K, La, Rb, Sc, Sr, Ta) in Chinese Biological Standard Reference Material (peach leaves) is described. The accuracy of the procedure was checked by analyzing the U.S. NBS Standard Reference Materials SRM-1571 and SRM-1632a.     

Substoichiometric determination of phosphorus

Phosphorus in orchard leaves (NBS SRM-1571) and spinach (SRM-1570) was determined by various substoichiometric analytical methods such as the direct method, GRASHCHENKO's method and the method of carrier amount variation. All samples were labelled with³²P radioisotope. The data obtained by the method of carrier amount variation were also treated by the method of least squares instead of De VOE's method. Phosphorus concentration in orchard leaves was 0.206±0.011% by the direct method, 0.219±0.011% by GRASHCHENKO's method, 0.211±0.011% by the method of carrier amount variation and 0.207±0.007% by the method of least squares, respectively. These values agree with the value reported by NBS (0.21±0.01%). Furthermore, these concentrations obtained by various substoichiometric methods were compared with those by radioactivation reported in a prevoius paper.     

Studies of LA-ICP-MS on quartz glasses at different wavelengths of a Nd:YAG laser

The capability of LA-ICP-MS for determination of trace impurities in transparent quartz glasses was investigated. Due to low or completely lacking absorption of laser radiation, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) proves difficult on transparent solids, and in particular the quantification of measurement results is problematic in these circumstances. Quartz glass reference materials of various compositions were studied by using a Nd:YAG laser system with focused laser radiation of wavelengths of 1064 nm, 532 nm and 266 nm, and an ICP-QMS (Elan 6000, Perkin Elmer). The influence of ICP and laser ablation conditions in the analysis of quartz glasses of different compositions was investigated, with the laser power density in the region of interaction between laser radiation and solid surface determining the ablation process. The trace element concentration was determined via calibration curves recorded with the aid of quartz glass reference materials. Under optimized measuring conditions the correlation coefficients of the calibration curves are in the range of 0.9–1. The relative sensitivity factors of the trace elements determined in the quartz glass matrix are 0.1–10 for most of the trace elements studied by LA-ICP-MS. The detection limits of the trace elements in quartz glass are in the low ng/g to pg/g range.