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1.
Determination of trace elements in AR grade alkali salts after preconcentration by column solid-phase extraction on TiO2 (anatase) 总被引:1,自引:0,他引:1
Column solid-phase extraction using TiO2 (anatase) as a solid sorbent was applied to preconcentrate traces of Cd, Co, Cu, Fe, Mn, Ni and Pb from AR grade alkali salts
prior to their measurements by atomic absorption spectrometry (AAS). Multi-element preconcentration was achieved from NaCl, KCl,
KNO3, NaNO3, CH3COONa, NaHCO3 and Na2CO3 solutions, whereas the sorption of trace elements from phosphates and sulfates is not quantitative. Optimal conditions (recoveries
of the analytes >95%) for solid-phase co-extraction of the most common heavy metal ions are proposed. The conditions for quantitative
and reproducible elution and subsequent AAS are established. A method of determination of trace elements in different salts
is proposed. It is characterized by precision, reproducibility and a high preconcentration factor. The solid-phase extraction
by TiO2, combined with ETAAS allows the determination of 0.1 ng g-1 Cd, 2 ng g-1 Co, 1 ng g-1 Cu and Ni, 0.5 ng g-1 Mn and 0.4 ng g-1 Pb.
Received: 1 April 1996/Revised: 24 June 1996/Accepted: 9 July 1996 相似文献
2.
Waxes were separated from needles by chloroform washing, drying and dissolving the residue in tetrahydrofuran (THF). Both
a THF solution of the wax and an aqueous solution of the Pd-Mg matrix modifier were sampled directly into the graphite tube.
The reaction conditions were optimised for the wax concentration of 45 mg ml-1 in THF and the Pd:Mg ratio of 1:1 in the matrix modifier. The atomisation and charring temperatures for As, Cd and Pb were
the same as those recommended for analysis of aqueous solutions except the charring temperature of Cd takes 200 °C lower.
The characteristic masses for As (26 pg), Cd (0.5 pg) and pb (9 pg) are also comparable to published data. The parameters
of calibration curves were identical for all three elements dissolved either in clear THF or in the wax solution. Elemental
concentrations were found to range from 0.1 to 1.0 mg g-1, increasing with needle age for As, Pb but not Cd.
Received: 20 September 1996 / Revised: 14 November 1996 / Accepted: 13 December 1996 相似文献
3.
I. López-García E. Navarro P. Viñas M. Hernández-Córdoba 《Analytical and bioanalytical chemistry》1997,357(6):642-646
A method is proposed for the determination of Pb, Cd and Tl in cements by ETAAS. The samples are suspended in a medium containing
10% v/v ethanol and 1% v/v both conc. nitric and hydrofluoric acids and are directly introduced into the electrothermal atomizer.
The drying stage is performed by programming a 400 °C temperature, a ramp time of 5 s and a hold time of 30 s on the power
supply to the atomizer. No ashing step is used. Atomization is carried out at 2100, 1800 and 1700 °C for Pb, Cd and Tl, respectively.
For Cd determination, ammonium dihydrogen phosphate is added to the suspension medium. No modifier other than hydrofluoric
acid is required for the Pb and Tl determination. It is shown that the results obtained by using direct calibration with aqueous
standards for five commercial samples agree with those found by means of the standard additions method.
Received: 29 March 1996/Revised: 24 May 1996/Accepted: 30 May 1996 相似文献
4.
The hydrolysis of SbCl3 in hydrochloric acid solution (2.0 mol dm-3 HCl) at 0 °C yields an amor-phous product consisting of uniform spherical particles (d∼0.5 μm), which on continuous aging at the same temperature transform to larger crystals, indicated by XRD to be Sb4O5Cl2. In contrast, in the same solution kept at 25 °C crystalline particles of the same composition form directly after an induction
period and then grow with time. The final products, obtained at 0 °C and 25 °C consist of aggregated subunits. These powders
on calcination in nitrogen are converted to Sb2O3 and in air to Sb2O4.
Received: 23 June 1997 Accepted: 1 July 1997 相似文献
5.
Sol and Gel state properties of aqueous gelatin solutions of concentrations 4%, 6%, 8% and 10% (w/v) have been investigated
through dielectric relaxation studies done at various temperatures in the range T=20–60 °C carried out over a frequency range f=20 Hz–10 MHz and no relaxation of any nature was observed. The sharp transition observed at the gelation temperature T
gel provided an excellent matching with the same measured through differential scanning calorimetry (DSC). The capacitance (C
p) values above f=100 kHz became increasingly negative as the gel was melted to the sol state. However, in the gel state C
p was found to be almost independent of temperature for frequencies above 100 kHz. At frequencies lower than 10 kHz, C
p measured was ∼105 F, implying pronounced interfacial polarization either due to electro-chemical reaction or because of ions getting trapped
at some interface within the bulk.
Received: 10 February 1997 Accepted: 2 September 1997 相似文献
6.
A. N. Araújo José A. M. Catita José L. F. C. Lima Elias A. G. Zagatto 《Fresenius' Journal of Analytical Chemistry》1998,360(1):100-103
A monosegmented flow system (MCFA) is proposed to achieve slow enzymatic spectrophotometric determinations, here applied
to the determination of triglycerides in blood serum. The sample (4.5 μL), enzymatic reagent (150 μL) and an air plug (100 μL)
are simultaneously inserted into a carrier stream buffered to pH 7.9 (Tris ⋅ HCl). In order to avoid the cumbersome step of
air removal, a relocating detector was used. This system handles about 60 samples/h, yielding precise results (r.s.d. usually<2.5%).
Sensitivity is 56 mAU ⋅ L/mmol up to 6 mmol/L triglycerides. Accuracy was assessed by running 50 samples already analysed
by a conventional procedure yielding the equation CMCFA(mmol/L)=1.00(±0.04) CRef(mmol/L)−0.03(±0.08); r=0.990.
Received: 22 January 1997/Revised: 12 March 1997/Accepted: 28 March 1997 相似文献
7.
Amorphous spherical particles of nickel sulfide of 10 nm in diameter were synthesized by the controlled double-jet precipitation
(CDJP) technique using nickel sulfate and sodium sulfide. Cubic crystalline particles of ∼200 nm were obtained by aging dispersions
of amorphous particles at 80 °C for more than a week, as long as the pH was kept between 3 and 3.5. Electrokinetic mobilities
of these particles are reported, as well as color properties of their dispersions in liquids and in poly(vinyl alcohol) films
are described.
Received: 20 January 1997 Accepted: 21 January 1997 相似文献
8.
The association behaviour of triblock copoly(ethylene oxide/tetrahydrofuran/ethylene oxide), in particular E100T27E100, in aqueous solutions has been investigated by means of static and dynamic light scattering, nuclear magnetic reso-nance
(NMR) and surface tension techniques. On raising the polymer concentration at room temperature, the copolymer aggregates to
form micelles with an aggregation number of about 105 (R
G, mic≈15 nm and R
H, mic≈13 nm, as revealed by light scattering and FT-PGSE NMR measurements, respectively). The micelles are kinetically quite stable,
the micellar lifetime is shown to be more than 1 h. The residence time of a single unimer in a micelle is more than 140 ms.
The apparent radius of gyration R
G, mic is fairly independent of concentration, but large effects are observed on varying the temperature. Raising the temperature
initially results in an increase of the apparent micellar size, followed by a maximum at an intermediate temperature (≈45 °C).
At higher temperatures a contraction of the micelles is observed. The shape of the micelles also appear to vary in this temperature
interval. The interactions responsible for these phenomena are discussed in terms of, e.g., the temperature-dependent solubility
of the alkylene oxide segments in water and polydispersity effects.
Received: 29 January 1996 acccepted : 4 November 1996 相似文献
9.
C. Vanderdonckt M. Krumova F. J. Baltá Calleja H. G. Zachmann S. Fakirov 《Colloid and polymer science》1998,276(2):138-143
Poly(ethylene terephthalate) (PET) was annealed in vacuum at different temperatures (190–260 °C) for different times (10 min–24 h)
in order to examine the mechanical properties (microhardness) of PET samples with a wide range of molecular weights (10 000–120 000).
Short annealing times result in a twofold decrease in mol. wt. due to hydrolytic decomposition. However, long annealing times
give rise to a substantial molecular weight increase. It is found that microhardness (H) rises linearly with the degree of crystallinity obtained during up-grading of mol. wt. and its extrapolation leads to H-values of completely crystalline PET, H
PET
c=405 MPa for samples with conventional mol. wt. and of 426 MPa for samples with mol. wt. higher than 30 000. It is shown that
the increase of mol. wt. for each set of samples with a given range of degree of crystallinity also causes a slight increase
of H. The influence of mol. wt. upon hardness is discussed in the light of the changes in the physical structure (crystallinity,
crystal thickness) which is formed at given heat treatment conditions.
Received: 29 April 1997 Accepted: 23 September 1997 相似文献
10.
The electrochemical behaviour of new doped Li-M-Mn-O (M = Al, Fe, Ni) spinel oxides in liquid electrolyte lithium cells was
studied. The insertion electrode materials were obtained by heating stoichiometric amounts of thoroughly mixed LiOH and M
x
Mn1−
x
CO3 (M = Fe, Ni; x = 0.08−0.15) or Al
x
Mn1−
x
(CO3) (OH)
y
, in the case of Al, at 380 °C in air for 20 h. The transition metal-doped samples, particularly those containing Ni or obtained
at low temperatures, where the resulting spinel was cation-deficient and highly disordered, exhibited the best cycling performance
in the potential window 3.3−2.3 V. Cell capacity was retained by 80% after 200 cycles. Capacity fading was observed on increasing
the firing temperature, together with improved crystallinity and the disappearance of cation vacancies. This impaired electrochemical
behaviour is ascribed to a Jahn-Teller effect, which induces an X-ray-detectable cubic-tetragonal phase transition upon lithium
insertion. The phase transition was undetectable in the low-temperature samples. The influence of the Jahn-Teller distortion
is thus seemingly lessened by a highly disordered structure.
Received: 25 November 1997 / Accepted: 28 January 1998 相似文献
11.
Traces of uranium and thorium in barium(II), strontium(II) titanate ((Ba, Sr)TiO3) ferroelectric materials were determined by inductively coupled plasma mass spectrometry (ICP-MS). Samples were completely
dissolved by a mixture of 1.4% H2O2 and 1.0 mol⋅l-1 HNO3. For a complete separation of the analytes from the matrix elements, a two step separation technique involving leaching and
anion-exchange was applied. By the leaching step with HNO3 more than 90% of the matrix can be removed whereas the analytes completely remained in the solution. The anion-exchange step
was carried out on a BIO⋅RAD AG1-X8 column with a mixture of 1.0 mol⋅l-1 HF and 0.5 mol⋅l-1 HNO3 as eluent. The content of uranium and thorium was subsequently measured by ICP-MS. The detection limits (D.L.) obtained were
0.043 ng g-1 and 0.035 ng g-1 for U and Th, respectively. The reproducibility was satisfactory with a relative standard deviation of less than 3% (at the
1 ng g-1 level, n=5). The matrix concentrations in the final solution were reduced to the sub-μg ml-1 level which is in the range of the detection limits of USN-ICP-AES (ultrasonic nebulization-ICP-atomic emission spectroscopy).
The method was successfully applied to the determination of uranium and thorium in three synthetic (Ba, Sr)TiO3 samples spiked with the analytes at levels of 1, 5 and 10 ng g-1 and three (Ba, Sr)TiO3 ferroelectric samples containing sub-ng g-1 levels of the analytes.
Received: 26 February 1996/Revised: 28 May 1996/Accepted: 5 June 1996 相似文献
12.
Silvana V. Rodrigues Decio Nepomuceno Luci Viana Martins W. Baumann 《Fresenius' Journal of Analytical Chemistry》1998,360(1):58-61
The solubility of two related series of each three triazine compounds has been determined in supercritical CO2, at 40 °C and pressures between 80 and 220⋅105 Pa. A high pressure small volume cell with adjustable optical path and built-in circulation pump has been constructed to
be used with quartz windows in a Perkin Elmer UV-VIS spectral photometer. At 220 bar solubilities are between 0.3 and 25 g/L,
dependent on the specific triazine structure. The isothermal pressure dependence of the solubility could be modelled using
the pressure dependent dielectric constant of CO2 as the only variable.
Received: 30 October 1996/Revised: 3 April 1997/Accepted: 13 April 1997 相似文献
13.
Francisco Laborda María V. Vicente José M. Mir J. R. Castillo 《Analytical and bioanalytical chemistry》1997,357(7):837-843
Chromatographic effluents were on-line analyzed by Zeeman-ETAAS, using a flow-through cell placed in a graphite furnace autosampler
as interface. To obtain high sampling rates, the use of fast graphite furnace programmes was studied. Conventional programmes
of 96 s were reduced to 18 s by using hot injection (120 °C) and reducing the charring step to 2 s. The increase of the injection
volume from 20 to 60 μl lengthened the programme to 46 s. Nickel had to be added to get a comparable response for both inorganic
and organic selenium species (selenite and selenomethionine) and to reduce the interferent effect produced in presence of
the chromatographic eluent (TRIS 0.01 mol l-1, NH4NO3 0.1 mol l-1, pH 7). The optimized conditions were applied to the speciation of selenium in human erythrocyte lysates by size exclusion
LC-ETAAS. Using a high performance size exclusion column selenium could be assigned to proteins of 100 and 35 kDa. Detection
limits in the range of 1 ng (2 μg l-1 for 500 μl injection volume) were obtained for the combined technique.
Received: 9 October 1996/Revised: 8 July 1996/Accepted: 14 July 1996 相似文献
14.
Traces of uranium and thorium in barium(II), strontium(II) titanate ((Ba, Sr)TiO3) ferroelectric materials were determined by inductively coupled plasma mass spectrometry (ICP-MS). Samples were completely
dissolved by a mixture of 1.4% H2O2 and 1.0 mol⋅l-1 HNO3. For a complete separation of the analytes from the matrix elements, a two step separation technique involving leaching and
anion-exchange was applied. By the leaching step with HNO3 more than 90% of the matrix can be removed whereas the analytes completely remained in the solution. The anion-exchange step
was carried out on a BIO⋅RAD AG1-X8 column with a mixture of 1.0 mol⋅l-1 HF and 0.5 mol⋅l-1 HNO3 as eluent. The content of uranium and thorium was subsequently measured by ICP-MS. The detection limits (D.L.) obtained were
0.043 ng g-1 and 0.035 ng g-1 for U and Th, respectively. The reproducibility was satisfactory with a relative standard deviation of less than 3% (at the
1 ng g-1 level, n=5). The matrix concentrations in the final solution were reduced to the sub-μg ml-1 level which is in the range of the detection limits of USN-ICP-AES (ultrasonic nebulization-ICP-atomic emission spectroscopy).
The method was successfully applied to the determination of uranium and thorium in three synthetic (Ba, Sr)TiO3 samples spiked with the analytes at levels of 1, 5 and 10 ng g-1 and three (Ba, Sr)TiO3 ferroelectric samples containing sub-ng g-1 levels of the analytes.
Received: 26 February 1996/Revised: 28 May 1996/Accepted: 5 June 1996 相似文献
15.
Suwa K. Yamamoto K. Akashi M. Takano K. Tanaka N. Kunugi S. 《Colloid and polymer science》1998,276(6):529-533
We examined the effects of salt on the lower critical solution temperature (LCST) and lower critical solution pressure (LCSP)
of aqueous solutions of poly (N-vinylisobutyramide), polyNVIBA, and compared them with those on poly(N-isopropylacrylamide), polyNIPAAm. We found that the addition of salt (such as Na2SO4, NaCl, or KCl) decreased the LCST of aqueous polyNVIBA from 45 °C to below 20 °C, almost linearly with the salt concentrations
and dependent on the type of salt. We observed a similar concentration-dependent decrease in LCST for polyNIPAAm. When KI
or NaSCN was added to each aqueous polymer solution, some smaller increases in LCST were observed at relatively low salt concentrations;
higher concentrations of salt gave an almost linear decrease in LCST. As for LCSP, the addition of most types of salt lowered
the transition pressure, but the effects were much more dependent on the type and the valence of the salt (especially of anion)
in both polymers. Salt with divalent anion showed a larger decrease in LCSP, but those with mono valent anion showed a relatively
small decrease, even showed a slight increase at lower salt concentrations in the case of polyNVIBA. Salt with I- or SCN- showed evident increases in LCSP up to 1 M and was maintained higher than the control even at 2 M. We discuss the interactions
of the amide group in the side chains of polymers and water and their perturbation by ions.
Received: 13 November 1997 Accepted: 22 January 1998 相似文献
16.
A novel surfactant peptide consisting of an arginine cation with laurate anion has been synthesized, purified and characterized.
The critical micellar concentration (cmc) of peptide in aqueous solutions has been determined using spectroscopic techniques
and is found to increase from 0.06 to 0.11 mM with increasing temperature (15–45 °C). Cmc is also determined in the presence
of salts like NaCl, KCl and sodium acetate and it is found that these electrolytes hinder aggregation with a significant increase
in the case of sodium acetate. The aggregation number of the surfactant peptide has been determined using fluorescence quenching
measurements and is observed to decrease from 14 to 6 with increasing temperature (15–45 °C). The standard free energy change
(ΔG
0
m) and standard enthalpy change (ΔH
0
m) of the peptide aggregate are found to be negative with a small positive value for standard entropy change (ΔS
0
m). The peptide aggregate seems to undergo phase transition above 50 °C as observed from UV–vis and fluorescence spectroscopy.
From pyrene binding studies, it is shown that the interior dielectric constant increases from 5.08 at 34 °C to 8.77 at 50 °C
and further decreases with increase in temperature indicating a phase change at 50 °C. Also, the ratio of excimer intensity
to monomer intensity, which is a measure of microviscosity of the aggregate, decreases with increase in temperature with a
change at 50 °C indicating a phase change.
Received: 14 February 1997 Accepted: 13 August 1997 相似文献
17.
A new method for the separation and determination of trace amounts of cadmium and zinc in water as their thenoyltrifluoroacetone
(TTA) complexes with dibenzo-18-crown-6 (DB18C6) in o-dichlorobenzene has been established by means of synergistic extraction
and back-extraction combined with atomic absorption spectrometry. The effect of various factors (synergism with TTA and DB18C6,
shaking time, composition of the extracted species, and mutual separation etc.) on the extraction and back-extraction of cadmium
and zinc has been in- vestigated. When the mixtures were extracted for 4 min at pH 4.9, only zinc was extracted quantitatively,
whereas cadmium remained in the aqueous phase. After the phases were separated, cadmium was again extracted quantitatively
at pH 7.5. Then, the two phases were each shaken with 0.05–0.1 mol/l HCl in order to back-extract cadmium and zinc from the
organic phases; the ions were determined individually by atomic absorption spectrometry. In the process cadmium and zinc TTA
chelates in o-dichlorobenzene form stable adducts with DB18C6 (Cd(TTA)2 ⋅ nDB18C6 and Zn(TTA)2 ⋅ nDB18C6, n=0∼2). The stability constants (βn) of the adducts determined by means of the curve fitting method were log β1=4.62 and log β2=6.74 for cadmium, and log β1=3.48 and log β2=5.18 for zinc.
Received: 8 September 1995/Revised: 22 January 1996/Accepted: 24 January 1996 相似文献
18.
Solid-phase spectrophotometric microdetermination of iron with ascorbic acid and ferrozine 总被引:1,自引:0,他引:1
M. L. Fernández-de Córdova A. Ruíz-Medina A. Molina-Díaz 《Analytical and bioanalytical chemistry》1997,357(1):44-49
A very sensitive and selective method for the determination of trace amounts of iron has been developed, based on the reduction
of Fe(III) to Fe(II) by ascorbic acid, followed by chromogenic chelation of Fe(II) with ferrozine. The complex Fe(II)-ferrozine
is easily sorbed on a dextran-type anion-exchange gel packed in a 1 mm cell, and the absorbance of the gel is measured directly
at 569 and 800 nm. The extended linear range of the determination is 0.5–10 ng ml-1 of iron (apparent molar absorptivity=4.4×107 l mol-1 cm-1) and the precision (RSD) 1.3% for a concentration of 5 ng ml-1 of iron (n=10). The detection limit for a sample volume of 1000 ml, using 0.040 g of anion-exchanger, corresponds to 0.12 ng ml-1. The method has been successfully applied to the determination of iron in natural and waste waters, wine, soil extract and
previously digested vegetal tissues, drugs and human hair.
Received: 20 November 1995/Revised: 23 January 1996/Accepted: 26 January 1996 相似文献
19.
An effective, rapid and simple analytical method for the determination of Na, K, Ca, Mg, Cd, Pb, Ba, Fe, Mn, Sr, Zr, Cu, Zn
and Al at mg kg−1 levels in the ultrapure salts MgCl2 and CaCl2 using optical emission spectrometry was developed. Optimisation of the operation conditions was performed with real samples
of ultrapure MgCl2 and CaCl2. The results of the determination with multi-elemental water standards were compared to the internal standardisation, the
standard addition method, and the maximum allowable content of the above mentioned elements in pure chemicals. The method
was shown to be very sensitive with the following limits of detection: Na 1.01, K 3.12, Ca 0.263, Mg 0.275, Cd 0.0832, Pb
0.482, Ba 0.0153, Fe 0.0528, Mn 0.0473, Sr 0.0203, Zr 0.638, Cu 0.0732, Zn 0.0686 and Al 0.459 (all in mg kg−1). The method exhibited satisfactory precision, high analytical recoveries, linear responses of an accuracy of at least 4
orders of magnitude and low contamination susceptibility. 相似文献
20.
Christopher J. G. Plummer Rudolf Gensler Hans-Henning Kausch 《Colloid and polymer science》1997,275(11):1068-1077
Melt crystallized isotactic polypropylene thin films of thickness between 30 and 100 nm have been investigated by high-resolution
transmission electron microscopy at room temperature. The c-axis projection of the 2*31 helices and their packing in the lattice were clearly visible in flat-on lamellae of the α-phase following reconstruction
from the components of the image Fourier transform corresponding to the (1 1 0) and (0 4 0) lattice planes, and the image
power spectra also indicated contributions from (1 3 0) and (0 6 0) relfections, corresponding to a line resolution of about
0.35 nm. These results are discussed in terms of Bloch wave calculations based on the generally accepted structure for the
α-phase. Attempts to obtain lattice images of the β-phase in isotactic polypropylene and melt crystallized syndiotactic polypropylene
under similar operating conditions are also briefly discussed, although these provided relatively little structural information.
Received: 27 June 1997 Accepted: 15 August 1997 相似文献