Indirect atomic absorption spectrometric method for the determination of silicon

Summary An indirect atomic absorption Spectrometric method for the determination of silicon is proposed which is based on the precipitation of an equivalent amount of lead molybdate from solutions treated with a known excess of lead ion and subsequent measurement of the lead ion remaining in solution. A typical calibration graph is linear for samples containing 0.5–7g silicon.

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Zusammenfassung Eine indirekte Siliciumbestimmungsmethode durch Atomarabsorption wurde vorgeschlagen. Sie beruht auf der Fällung einer äquivalenten Menge Bleimolybdat aus Lösungen mit einem bekannten Überschuß von Bleiionen und nachfolgender Messung des Bleis im Filtrat. Die Eichkurve für Proben mit 0,5 bis 7g Silicium ist linear.

     

Indirect amplification method for determining formaldehyde and chloralhydrate by differential pulse polarography

An indirect differential pulse polarographic method for the determination of formaldehyde and chloralhydrate is described; it is based on the oxidation of the alkaline sample solutions of formaldehyde and chloralhydrate with a chloroform solution of iodine and removal of its excess. The resulting iodide is oxidized with bromine water and measured polarographically as iodate (at pH 9.3) with sixfold amplification.     

国家监测网方法测定地表水中总磷与国标法差异及改进

比较了国家地表水环境质量监测网总磷测定方法与国标法的差异。浊度补偿与过滤两种去除浊度方法测定结果的绝对偏差为-0.02~0.07 mg/L,其中含细颗粒物较多的样品绝对偏差较大,为0.04~0.07 mg/L,因此采用过滤法时,需对含较多细颗粒物的水样进行浊度补偿。对国家地表水环境质量监测网方法进行了改进,将原来的过滤后定容改为定容摇匀后过滤。方法改进前后,样品测定值的相对偏差不大于3.4%,绝对偏差为-0.01~0.02 mg/L。改进后的方法与原方法测定结果没有显著差异,但改进后方法浊度贡献减少,试剂用量减半,而且可操作性强,更加简便和环境友好。     

A radioreagent method for determination of traces of phosphorus in high-purity silicon

The present study explores the feasibility of the determination of phosphorus at the extreme trace levels in high-purity silicon by radioreagent method. After silicon dissolution with hydrofluoric and nitric acids and matrix volatilization, 12-molybdophosphoric acid (12-MPA) is formed by the addition of the radioreagent,⁹⁹MoO ₄ ^2– , in nitric acid medium and then extracted into isobutyl acetate. By plotting the phosphorus content against the radioactivity of⁹⁹Mo in the organic phase, a linear relationship persisting down to 5 ng is obtained. Special effort has been made to the elimination of the unreacted⁹⁹MoO ₄ ^2– reagent and the optimal control of phosphorus blank introduced through the multistage analytical procedure in order to ensure reliable determination of phosphorus at the ppb level.     

Simultaneous determination of arsenic,phosphorus, and silicon

Summary A simple, rapid, accurate and reliable method for the simultaneous determination of arsenic, phosphorus and silicon in the presence of each other is reported. The method involves the selective solvent extraction of phosphomolybdic acid by isobutyl acetate, the differential formation of phospho and arsenomolybdic acid when perchloric acid is added before the addition of ammonium molybdate, and the selective destruction of phospho and arsenomolybdic acid complexes in the presence of silicomolybdic acid. Silicon, phosphorus and arsenic were determined as their heteropoly blues.

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Zusammenfassung Eine einfache, rasche und verläßliche Methode zur gleichzeitigen Bestimmung von Arsen, Phosphor und Silicium nebeneinander wurde beschrieben. Phosphormolybdänsäure wird selektiv mit Isobutylacetat extrahiert. Setzt man vor der Zugabe von Ammoniummolybdat Perchlorsäure zu, so erfolgt die Bildung von Phospho- bzw. Arsenomolybdänsäure in differenter Weise. Diese beiden Säuren sind in Gegenwart von Silicomolybdänsäure selektiv zerstörbar. Silicium, Phosphor und Arsen werden auf der Grundlage der blauen Farbreaktion ihrer Heteropolysäure bestimmt.

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Résumé On communique une méthode simple, rapide, précise et sûre pour le dosage simultané de l'arsenic, du phosphore et du silicium en présence les uns des autres. La méthode met en jeu l'extraction par solvant sélectif de l'acide phosphomolybdique par l'acétate d'isobutyle, la formation différentielle de l'acide phospho et arsénomolybdique quand l'addition de l'acide perchlorique précède celle du molybdate d'ammonium, et la destruction sélective des complexes acides phospho et arsénomolybdiques en présence d'acide silicomolybdique. On a dosé le silicium, le phosphore et l'arsenic sous forme d'hétéropolycomplexes bleus.

     

A semi-automated and manual method for determining the total phospholipid phosphorus in amniotic fluid

A rapid method for estimating the total phospholipid content of amniotic fluid has been described that requires 1 ml of sample. Perchloric acid containing a trace of molybdate is the acid digestant for inorganic phosphate release. After digestion at 225 °C for 30 min, dilution with water yields a solution with a hydrogen ion concentration of about 2.5 mol/liter that allows the use of stannous chloride-hydrazine sulfate as the reducing agent for phosphate color development. The color development and measurement may be carried out manually or with use of the AutoAnalyzer at an analysis rate of 40/hr. A coefficient of variation of about 7% and a standard deviation of 0.02 will be obtained with either the manual or semi-automated procedure.     

Indirect amplification method for determining mercury by direct-current polarography. Application to organomercury compounds

An amplification method for the determination of 0.5–70 ppm (2.5 × 10⁻⁶ to 3.5 × 10⁻⁴ M) of Hg(II) is described. Hg(II) is reacted with a slight excess of KI, and the excess iodide is oxidized by bromine water and measured polarographically as iodate with sixfold amplification. Alternatively, the iodate formed is reacted to liberate iodine which is then reduced to iodide, and again oxidized to yield six iodate ions for every iodide ion originally present;

2. Microdetermination of Mercury in Organomercurial Compounds

polarographic reduction requires 36 electrons. Oxidation of the excess iodide with periodate yields four iodate ions for every iodide ion and therefore allows 24-fold amplification.Microdetermination of mercury in organomercurials is achieved using the sixfold method following closed flask combustion: the average percentage error for 10 determinations is ±0.40 and the time required for one sample run is 45 min.     

Determination of silicon,phosphorus and sulfur in alloy steel by neutron activation analysis

Silicon, phosphorus, and sulfur in alloy steel were determined by neutron activation analysis involving rapid radiochemical separation procedures. The standard deviations for silicon, phosphorus, and sulfur were 1.6%, 2.3%, and 2.4% respectively; the sensitivity limits were 3.2, 0.20, and 2.50 p.p.m., respectively. The three constituents could be determined in alloy steel within 2 h of the irradiation.     

Indirect flame-photometric determination of silicon

An indirect flame-photometric method for the determination of silicon in terms of the potassium in precipitated K(2)SiF(6) has been developed. Optimum conditions have been found for the precipitation and the washing of the precipitate with aqueous ethanol. Satisfactory results have been obtained for silicon contents > 1 % in ores and alloys.     

Helium-4 and neutron activation analysis for phosphorus in aluminium—silicon alloys

An instrumental determination of phosphorus in aluminium-silicon alloys by activation with 20-MeV helium-4 particles can be based on the ³¹P(α , n)^34m Cl reaction. A mixture of aluminium powder and disodium hydrogenphosphate is used as a standard. For concentrations ranging from 1.7 to 25 μg g^-1, the experimental standard deviation ranges from 1 to 24% with an average of 8%. The method was compared with thermal neutron activation analysis based on the ³¹P(n, γ)³²P reaction. ³²P was chemically separated by precipitation as ammonium molybdophosphate. This technique yielded results with a standard deviation between 0.3 and 7.5% with an average of 2%. The agreement between the two methods was satisfactory. The results were also compared with photometry and atomic absorption spectrometry.     

Application of total selective solvent extraction of germanium,phosphorus and silicon to the simultaneous determination of arsenic,germanium, phosphorus and silicon

A simple rapid, accurate, and reliable method of simultaneous determination of arsenic, germanium, phosphorus, and silicon is reported. The method involves first, the determination of germanium as its phenlfluorone complex and its selective extraction with isoamyl alcohol. Phosphorus is next determined as its heteropoly blue after selective extraction of phosphomolybdic acid by isobutyl acetate at pH 1.0-0.8 and its direct reduction in this solvent. Silicon is then determined after its extraction as silicomolybdic acid by isooctyl alcohol at pH < 0.4 and direct reduction in the solvent phase. Finally, arsenic is determined in the remaining aqueous phase after reduction to its heteropoly blue.     

Synthesis, characterization and thermal properties of novel epoxy containing silicon and phosphorus nanocomposites by sol-gel method

Organic-inorganic hybrids were prepared using diglycidyl ether of bisphenol A (DGEBA) type epoxy and tetraethoxysilane via the sol-gel process. The DGEBA type epoxy was modified by a coupling agent to improve the compatibility of the organic and inorganic phases. The sol-gel technique was used successfully to incorporate silicon and phosphorus into the network of hybrids increasing flame retardance.Fourier transform infrared spectroscopy and ²⁹Si nuclear magnetic resonance spectroscopy were used to characterize the structure of the hybrids. In condensed siloxane species for TEOS, silicon atoms through mono-, di-, tri-, and tetra-substituted siloxane bonds are designated as Q¹, Q², Q³, Q⁴, respectively. For 3-isocyanatopropyltriethoxysilane and diethylphosphatoethyltriethoxysilane, mono-, di-, tri-, tetra-substituted siloxane bonds are designated as T¹, T², T³. Results revealed that Q⁴, Q³, T³ are the major environments forming a network structure. The morphology of the ceramer was examined by scanning electron microscopy and Si mapping. Particle sizes were below 100 nm. The hybrids were nanocomposites. The char yield of pure epoxy resin was 14.8 wt.% and that of modified epoxy nanocomposite was 31 wt.% at 800 °C. A higher char yield enhances the flame retardance. Values of limiting oxygen index of pure epoxy and modified epoxy nanocomposites are 24 and 32, respectively, indicating that modified epoxy nanocomposites possess better flame retardance than the pure epoxy resin.     

Elemental analysis of organic phosphorus compounds X. Schöniger-flask method for phosphorus

By use of a fused-silica hook for holding the sample packet in a Schöniger combustion flask, even difficultly combustible phosphorus compounds can be completely decomposed.     

The preparation of a phosphorus doped silicon film from phosphorus containing silicon nanoparticles

Phosphorus containing and octyl-terminated silicon nanoparticles (NPs) are generated by a solution reduction route under room temperature conditions for the first time and characterized by TEM, HRTEM, EDX, 1H/13C/31P NMR, EPR, and PL spectroscopy, then annealed to form a thin film with phosphorus doping confirmed by microprobe elemental analyses.     

Determination of phosphorus in semiconductor grade silicon by neutron activation analysis

A method of determination of phosphorus in silicon has been elaborated. The separation of phosphorus is based on the extraction of phosphomolybdic complex in the presence of hold-back carriers of Ta and Au. Contamination factors for various impurities were determined. The lower limit of determination equals 3·10^?11 g P. Types of errors in the determination of concentration profiles are discussed.