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Results for “NITRIC ACID”

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At least 577 records · Page 32Linked to original sources

PubMed1989

Micro-quantity tissue digestion for metal measurements by use of a microwave acid-digestion bomb.

We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.

Aluminum↗

PubMedDate not supplied

Analysis of submicrogramme levels of cadmium in whole blood, urine and hair by graphite furnace atomic absorption spectroscopy.

Toxicological studies require the analysis of heavy metals in many widely differing samples. In this paper, a simple and accurate method is described for the determination of cadmium in whole blood, urine, and hair. The blood and urine samples were digested in nitric acid at 70 degrees C, and the hair was digested in a 1:1 mixture of nitric and sulphuric acid. Although a low temperature necessitated longer digestion, the operation was conveniently carried out overnight. The digestion and any subsequent extraction or dilution was carried out in the same tube. The methods used optimised digestion efficiency and minimised sample contamination. The method was also found to be precise and highly reproducible with relative standard deviation (RSD) values within 5%.

Cadmium↗

PubMed1999

Selected ion flow tube mass spectrometry of urine headspace.

We describe the use of our selected ion flow tube mass spectrometric technique (SIFT-MS) for the analysis of the headspace above urine. Ammonia, nitric oxide, acetone, ethanol and methanol are identified as the dominant species. As expected, the ammonia is increased in the headspace by making the urine alkaline and the nitric oxide is increased by making the urine acidic. Nitric oxide is abnormally high in the headspace of acidified bacterially infected urine and nitrous acid is also detected. The potential clinical implications of analyses of urine by SIFT-MS are alluded to.

Acetone↗

PubMed2006

Uptake of HNO3 on hexane and aviation kerosene soots.

The uptake of HNO(3) on aviation kerosene (TC-1) soot was measured as a function of temperature (253-295 K) and the partial pressure of HNO(3), and the uptake of HNO(3) on hexane soot was studied at 295 K and over a limited partial pressure of HNO(3). The HNO(3) uptake was mostly reversible and did not release measurable amounts of gas-phase products such as HONO, NO(3), NO(2) or N(2)O(5). The heat of adsorption of HNO(3) on soot was dependent on the surface coverage. The isosteric heats of adsorption, Delta(0)H(isosteric), were determined as a function of coverage. Delta(0)H(isosteric) values were in the range -16 to -13 kcal mol(-1). The heats of adsorption decrease with increasing coverage. The adsorption data were fit to Freundlich and to Langmuir-Freundlich isotherms. The heterogeneity parameter values were close to 0.5, which suggested that a HNO(3) molecule can occupy two sites on the surface with or without being dissociated and that the soot surface could be nonuniform. Surface FTIR studies on the interaction of soot with HNO(3) did not reveal formation of any minor product such as organic nitrate or nitro compound on the soot surface. Using our measured coverage, we calculate that the partitioning of gas-phase nitric acid to black carbon aerosol is not a significant loss process of HNO(3) in the atmosphere.

Aviation↗

PubMedDate not supplied

Fast determination of lead and copper in dairy products by graphite furnace atomic absorption spectrometry.

A rapid and direct procedure for determining lead and copper in dairy products by electrothermal atomic absorption spectrometry (ETAAS) is described. Samples are slurried in a medium containing 50% v/v hydrogen peroxide, 1% v/v nitric acid, 0.5% w/v dihydrogen phosphate, and 20% v/v ethanol and directly injected into the furnace with no previous mineralization. Calibration is performed with aqueous standards. Limits of determination were 0.4 and 2.4 ng/mL for copper and lead, respectively. The reliability of the procedure was checked by comparison with the acid mineralization procedure and by analyzing 3 certified reference milk samples.

Calibration↗

PubMedDate not supplied

Effect of ultrasound agitation on the release of heavy elements in Certified Reference Material of human hair (CRM BCR 397).

An ultrasonic-assisted leaching procedure was developed for the determination of heavy elements (As, Cu, Cd, Pb, and Zn) in Certified Reference Material of human hair (CRM 397) provided from the Community Bureau of Reference (BCR) of the Commission of the European Community. Concentrated nitric acid-30% hydrogen peroxide (2 + 1) was used for the leaching method. The effects of different factors on acid leaching of elements, such as presonication time (without ultrasonic stirring), sonication or exposure time to ultrasound, and temperature of the ultrasonic bath have been investigated. Optimum values of these parameters were selected for the maximum extraction of heavy metals from CRM BCR 397 and human scalp hair samples of normal healthy males. To check the validity of the proposed method, a wet acid digestion method was used to obtain the total elemental concentration in CRM BCR 397 and scalp hair samples. Cu and Zn in leachate and digests were measured by flame atomic absorption spectrometry using a conventional air/acetylene flame, while As, Cd, and Pd were determined by electrothermal atomic absorption spectrometry. Under optimized conditions, the recovery for Zn, Cd, Pd, As, and Cu was 98, 98.5, 97.5, 98.2, and 95%, respectively, of those obtained with the wet acid digestion method.

European Union↗

PubMed2005

Evaluation of oxidation stability of lignite humic substances by DSC induction period measurement.

The stability of lignite humic acids and four regenerated humic acids was estimated by employing differential scanning calorimetry. Induction period for the oxidative decomposition of humic matter was calculated from non-isothermal measurements at six different rates of heating. To simulate the gradual evolution history of humic acids, different intensities of oxidation attack by nitric acid on the original lignite was used. Experimental data showed higher stability of natural humic acids in the temperature range where the decomposition step occurred. On the other hand, extrapolation to lower temperatures and calculated kinetic parameters did not correspond to the order observed at higher temperatures. An oscillating trend of calculated parameters of the two proposed parts of stability was observed, which agreed with data concerning regenerated humic acids production. The approach applied in this work represents a rapid and useful method for evaluation of organic matter stability.

Calorimetry, Differential Scanning↗

PubMed2006

Preparation of a water-soluble fullerene [C70] under ultrasonic irradiation.

A water-soluble fullerene [C(70)] is prepared with fullerene [C(70)] and a mixture of concd. sulfuric acid (H(2)SO(4)) and concd. nitric acid (HNO(3)) at the ratio (v/v) of 3:1 under ultrasonic irradiation at 25-43 degrees C. The MALDI-TOF-MS spectra confirmed that the product of a water-soluble fullerene compound was C(70).

Computer Simulation↗

PubMed2003

Effects of acidic deposition on forest and aquatic ecosystems in New York State.

Acidic deposition is comprised of sulfuric and nitric acids and ammonium derived from atmospheric emissions of sulfur dioxide, nitrogen oxides, and ammonia, respectively. Acidic deposition has altered soil through depletion of labile pools of nutrient cations (i.e. calcium, magnesium), accumulation of sulfur and nitrogen, and the mobilization of elevated concentrations of inorganic monomeric aluminum to soil solutions in acid-sensitive areas. Acidic deposition leaches essential calcium from needles of red spruce, making this species more susceptible to freezing injury. Mortality among sugar maples appears to result from deficiencies of nutrient cations, coupled with other stresses such as insect defoliation or drought. Acidic deposition has impaired surface water quality in the Adirondack and Catskill regions of New York by lowering pH levels, decreasing acid-neutralizing capacity, and increasing aluminum concentrations. Acidification has reduced the diversity and abundance of aquatic species in lakes and streams. There are also linkages between acidic deposition and fish mercury contamination and eutrophication of estuaries.

Acid Rain↗

PubMed2001

Novel silicate anion: Si(8)O(22)(12-). Hydrothermal synthesis and X-ray powder structure of three new niobium silicates.

A sodium niobium(V) tetrasilicate, Na(2)H(NbO)Si(4)O(11).1.25H(2)O (1), was synthesized hydrothermally at 190 degrees C from a mixture of silicic acid, NaOH, NbCl(5), and H(2)O(2) and added hydrochloric acid. The successive treatment of 1 with nitric acid yielded HNb(H(2)O)Si(4)O(11).H(2)O (2). Contact of 2 with cesium hydroxide solutions converted it to the partially exchanged Cs(+) phase Cs(0.66)H(0.33)Nb(H(2)O)Si(4)O(11) (3). The three structures were solved from X-ray powder diffraction data. All compounds crystallize in the monoclinic space group P2(1)/m with Z = 2, containing the Si(8)O(22)(12-) anion. This new silicate anion type is related to the Si(4)O(11)(6-) unit, which is present in the amphibole series. The difference between both anion types lies in the chain periodicity: two for amphiboles or four for the new niobium silicates. These niobium silicates have framework structures enclosing tunnels in which the alkali cations reside.

Journal Article↗

PubMed2004

Oxidation of alkylarenes by nitrate catalyzed by polyoxophosphomolybdates: synthetic applications and mechanistic insights.

Alkylarenes were catalytically and selectively oxidized to the corresponding benzylic acetates and carbonyl products by nitrate salts in acetic acid in the presence of Keggin type molybdenum-based heteropolyacids, H(3+)(x)()PV(x)()Mo(12)(-)(x)()O(40) (x = 0-2). H(5)PV(2)Mo(10)O(40) was especially effective. For methylarenes there was no over-oxidation to the carboxylic acid contrary to what was observed for nitric acid as oxidant. The conversion to the aldehyde/ketone could be increased by the addition of water to the reaction mixture. As evidenced by IR and (15)N NMR spectroscopy, initially the nitrate salt reacted with H(5)PV(2)Mo(10)O(40) to yield a N(V)O(2)(+)[H(4)PV(2)Mo(10)O(40)] intermediate. In an electron-transfer reaction, the proposed N(V)O(2)(+)[H(4)PV(2)Mo(10)O(40)] complex reacts with the alkylarene substrate to yield a radical-cation-based donor-acceptor intermediate, N(IV)O(2)[H(4)PV(2)Mo(10)O(40)]-ArCH(2)R(+)(*). Concurrent proton transfer yields an alkylarene radical, ArCHR(*), and NO(2). Alternatively, it is possible that the N(V)O(2)(+)[H(4)PV(2)Mo(10)O(40)] complex abstracts a hydrogen atom from alkylarene substrate to directly yield ArCHR(*) and NO(2). The electron transfer-proton transfer and hydrogen abstraction scenarios are supported by the correlation of the reaction rate with the ionization potential and the bond dissociation energy at the benzylic positions of the alkylarene, respectively, the high kinetic isotope effect determined for substrates deuterated at the benzylic position, and the reaction order in the catalyst. Product selectivity in the oxidation of phenylcyclopropane tends to support the electron transfer-proton transfer pathway. The ArCHR(*) and NO(2) radical species undergo heterocoupling to yield a benzylic nitrite, which undergoes hydrolysis or acetolysis and subsequent reactions to yield benzylic acetates and corresponding aldehydes or ketones as final products.

Acetates↗

PubMedDate not supplied

Determination of levels of lead contamination in food and feed crops.

A rapid, precise procedure is described for the determination of lead in food and feed products with electrothermal atomic absorption spectrophotometry. Samples were mineralized in a microwave acid digestion bomb in the presence of nitric acid and vanadium pentoxide. Lead concentrations were determined directly from digested samples. The detection limit was 0.04 ng/mL. Accuracy and precision were checked against National Institute of Standards and Technology standard reference material. The analytical method was tested with 51 food and feed crops from Mediterranean zones in Spain and found to be suitable for these products. Lead concentrations in samples ranged from not detectable to 2.695 micrograms/g (fresh weight).

Animal Feed↗

PubMed2000

A novel high-temperature (360 degrees C)/high-pressure (30 MPa) flow system for online sample digestion applied to ICP spectrometry.

A flow injection sample digestion system has been developed comprising an indirectly electrically heated Pt/Ir capillary. Such a capillary allows reaction temperatures of up to 360 degrees C and pressures of up to 30 MPa (300 bar) and withstands concentrated acids. This temperature is 130 degrees C to 160 degrees C higher compared to the operating temperatures of microwave heated flow systems. A combination of an ultrasonic nebulizer and membrane desolvator serves as an interface between the flow digestion system and an ICP/AES spectrometer. The membrane desolvator removes interfering gaseous digestion products so effectively before the sample stream enters the plasma that the measured residual carbon concentration falls in the region of the detection limit of ICP/OES measurements. Sewage sludge samples were digested using nitric acid and the elemental traces online determined. The detection limits related to the original dry substances amount to the lower microg/g range.

Chromatography, High Pressure Liquid↗

PubMed2005

Biosorption of Cr3+, Cd2+ and Cu2+ ions by blue-green algae Spirulina sp.: kinetics, equilibrium and the mechanism of the process.

The process of biosorption of heavy metal ions (Cr3+, Cd2+, Cu2+) by blue-green algae Spirulina sp. is discussed in this paper. Spirulina sp. was found to be a very efficient biosorbent. The aim of the present study was to investigate quantitatively the potential binding sites present at the surface of Spirulina sp., using both potentiometric titrations and adsorption isotherms. The kinetic experiments showed that the process equilibrium was reached quickly, in less than 5-10 min. It was found that the equilibrium dependence between biosorption capacity and bulk metal ion concentration could be described with Langmuir equation. This suggests that the mechanism of biosorption is rather chemisorption than physical adsorption and was further confirmed by the low surface area associated with physical adsorption and by the presence of cations that appeared in the solution after biosorption. The maximum contribution of physical adsorption in the overall biosorption process was evaluated as 3.7%. It was proposed that functional groups on the cell surface contributed to the binding of metal ions by a biosorbent via equilibrium reaction. Three functional groups capable of cation exchange were identified on the cell surface. The biomass was described as weakly acidic ion exchanger. Since deprotonation of each functional group depends on pH, the process of biosorption is strongly pH-dependent. This was confirmed in the biosorption experiments carried out at different pH. The contribution of functional groups in the biosorption process was confirmed by chemical modification of the groups. Chemically blocked groups did not show neither biosorption nor ion-exchange capabilities. It has been shown that growth conditions can affect the metal adsorption properties of microalgae. The paper also discusses desorption characteristics of the biosorbent. The criteria for desorption were high elution efficiency and preservation of biosorptive properties. Desorbent that possessed these characteristics was nitric acid.

Adsorption↗

PubMed1989

FIA determination of chlorhexidine by means of the precipitation with Cu(II).

The determination of chlorhexidine in pharmaceutical formulations is carried out using flow injection analysis (FIA) with measurement by atomic absorption spectrometry (AAS). The method is based on the formation of a copper-biguanide complex precipitate when the sample is injected into an ammoniacal copper solution. The precipitate is retained on a plastic or paper filtering device. A nitric acid stream dissolves the precipitate and carried the Cu(II) to the AAS detector. The chlorhexidine is determined over the range 5-20 ppm. The influence of interfering substances is investigated.

Biguanides↗

PubMed2005

A simple spectrophotometric method for determination of sodium diclofenac in pharmaceutical formulations.

A new, simple, rapid and accurate spectrophotometric method is proposed for determination of sodium diclofenac (SD) in pharmaceutical preparations based on its reaction with concentrated nitric acid (63% w/v). The reaction product is a yellowish compound with maximum absorbance at 380 nm. The corresponding calibration curve is linear over the range of 1-30 mg l(-1), while the limit of detection is 0.46 mg l(-1).

Diclofenac↗

PubMed1997

Development and validation of a general non-digestive method for the determination of palladium in bulk pharmaceutical chemicals and their synthetic intermediates by graphite furnace atomic absorption spectroscopy.

A simple, selective, sensitive, accurate and relatively inexpensive method for the determination of palladium in bulk pharmaceutical chemicals (BPC) and their synthetic intermediates by graphite furnace atomic absorption spectroscopy has been developed and validated. Sample preparation by direct dissolution of sample in 70% nitric acid is simple and effective without adverse effects. The limit of detection and the limit of quantitation of the method were determined to be 0.7 ppm and 2 ppm respectively in BPC.

Acetates↗

PubMed2005

Distribution of copper, lead, cadmium and zinc concentrations in soils around Kabwe town in Zambia.

The extent of pollution of the environment as a result of mining activities in Kabwe, the provincial capital of Central province in Zambia has not yet been evaluated. Mining of lead and zinc were the core activities of Kabwe mine while cadmium and silver were produced as by-products. The smelting processes produced a significant amount of copper. The spatial distribution of four heavy metals in soils in the northern, eastern, southern and western directions of the mine was analyzed using atomic absorption spectrometry (AAS). Samples were collected up to 20 km in each direction from the mine. Results were consistent with the wind flow patterns in the town. Results ranged between 0.08 and 28 mg kg(-1) (Cd); 0.20 and 0.61 mg kg(-1) (Cu); 0.10 and 758 mg kg(-1) (Pb) and 0.40 and 234 mg kg(-1) (Zn) suggesting high precipitation of metals from the core mining activities. These concentrations were for only the fractions of metals extractable by 0.5M nitric acid and that could be available for plant uptake in the environment. The distribution of metals indicated a decrease of metal concentrations with distance from the mine, which confirmed that precipitation due to mining activities was the main cause of soil contamination.

Environmental Monitoring↗