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1.
A first-order derivative spectrophotometric method has been developed for the simultaneous determination of copper, mercury and lead at g/L levels using dithizone as reagent. The procedure involves the simultaneous extraction of these elements by dithizone in chloroform from weakly alkaline solutions. Linear calibration curves were obtained in the ranges 0.5–10 (Cu), 1–10 (Hg) and 1–10 (Pb) g present in 40 ml of aqueous phase with detection limits of 5 g/L (Cu) and 20 g/L (Hg and Pb). The R.S.D.s for 100 g/L of copper, mercury and lead were 2.5, 2.6 and 3.1% respectively, for 5 determinations. The method is applicable for the determination of copper and lead in marine sediment samples with good precision and accuracy.  相似文献   

2.
Zusammenfassung Eine neue Methode zur Durchführung gravimetrischer Bestimmungen im Mikrogrammbereich wurde beschrieben; diese beruht im wesentlichen darauf, daß der Niederschlag nicht mehr zusammen mit dem Filter, sondern nach Überführen mit einem geeigneten Lösungsmittel in einem separaten Wägegefäß gewogen wird.Die dazu nötigen Geräte und deren Herstellung wurden beschrieben. Nach dieser Methode wurden folgende Bestimmungen mit zufriedenstellender Richtigkeit durchgeführt: 2,5–25g Al, 5–50g Cu und 5–50g Zn mit Oxin, 2,5–25g Fe(III) und 2,5–25g Ti(IV) mit N-Benzoyl-phenylhydroxylamin, 5–50g Ni und 5–50g Cu mit Salicylaldoxim, 2,5–50g Co(II) und 2,5–50g Fe(III) mit -Nitroso--naphthol sowie 5–50g Chlorid als Silberchlorid.
Precipitation analysis in the microgram-scale: A new method
Summary A new method for gravimetric determinations in the microgram-scale is described. This method is based on the fact that the precipitate is not weighed together with the filter but is transferred to a separate weighingvessel using a suitable solvent. The necessary simple devices and their use are described. The following determinations were carried out with satisfying accuracy: 2,5–25g Al, 5–50g Cu and 5–50g Zn with Oxine, 2,5–25g Fe and 2,5–25g Ti withN-benzoylphenylhydroxylamine, 5–50g Ni and 5–50g Cu with salicylaldoxime, 2,52–50g Co and 2,5–50g Fe with -nitroso--naphthol and 5–50g chloride as silver chloride.
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3.
The diacetylenic adducts, Fe2(CO)6{-EC(H) = C(C CMe)E} (E = E, E E; E, E = S, Se, Te) (1–8) have been obtained from the room temperature stirring of Fe2(CO)6(-EE) with HC CC CMe in methanol solvent containing sodium acetate. Compounds 1–8 have been characterized by IR and multinuclear NMR (1H, 13C, 77Se, and l25Te) spectroscopy. Trends in the chemical shifts of 77Se and 125Te NMR spectra of Fe2(CO)6{-EC(H) = C(C CMe)E} with a variation of EE are discussed.  相似文献   

4.
The absorption spectra of 4f electron transitions of the complexes of neodymium and erbium with 5,7-dibromo-8-hydroxyquinoline in the presence of octylphenol poly(ethyleneglycol)ether have been studied by normal and third-derivative spectrophotometry. The proposed method is free of interference of other rare earths. The calibration graphs were linear up to 18 g/ml of neodymium and 21 g/ml of erbium (in the final solution). The derivative molar absorptivities are 395 l.mol–1.cm–1 for neodymium and 3421.mol–1.cm–1 for erbium. The corresponding values of Sandell's sensitivity were 0.36 and 0.49 g.cm–1, respectively. The relative standard deviations evaluated from ten independent determinations of 2.5 g/ml of neodymium and erbium are 1.5 and 3.8% for neodymium and 1.8 and 4.1% for erbium in absence and presence of 70 g of lanthanum, respectively. The detection limits (signal to noise ratio=2) are 0.23 g/ml for neodymium and 0.30 g/ml for erbium. The method has been used for the determination of neodymium and erbium in mixed rare earths with satisfactory results.  相似文献   

5.
Packed-column supercritical-fluid chromatography (pSFC) is presented as a novel method for separating and analyzing gramicidin samples. By use of methanol-modified carbon dioxide as a mobile phase the pentadecapeptides gramicidin A (gA), gramicidin B (gB), and gramicidin C (gC) are readily separated and eluted from a PRP-1 poly(styrene–divinylbenzene) column. Although optimum separation conditions are typically achieved near a column temperature of 40°C, a column pressure of 11 MPa, and 30% methanol modifier, pressure and modifier gradients around these values are also found to improve the overall separation time. Measurements indicate that the mobile phase solubility of gramicidin under these conditions is 5.0±0.4 g mL–1. Collection of individual peaks during chromatography achieved analytical-scale isolation of 2 g refined gC from 20 g injected gramicidin D. Further, supercritical-fluid extraction of 200 g gramicidin D from a Chromosorb 102 support packed into the vessel produced 57 g gA in 90% purity. The results establish that carbon dioxide-based mobile phases can be successfully used for the separation of individual gramicidin species.  相似文献   

6.
A procedure was developed for the gas-chromatographic determination of promedol (trimeperidine) and ketamine in whole blood with mass-selective detection. The detection limit for trimeperidine and ketamine in blood is 0.05 g/mL. The analytical range is 0.1–5.0 g/mL. The maximum within-series errors in the determination of the studied compounds are no higher than 14.1% for concentrations of 0.10 g/mL and 7.47% for concentrations of 1.0 g/mL. The maximum between-series relative errors are 5.75% for concentrations of 0.10 g/mL and 2.7% for concentrations of 1.0 g/mL. The procedure can be used in toxicological and clinical analyses.  相似文献   

7.
Crystallization of iron phosphate glasses   总被引:1,自引:0,他引:1  
Differential thermal analysis (DTA), thermogravimetric analysis (TG), X-ray diffraction and Mössbauer spectroscopy were employed in the investigation of crystalline products of FeOx-P2O5 glasses generated by various heat treatments. In glasses with a high value of =Fe2+/(Fe2+ + Fe3+), absorption of oxygen occurs in a broad temperature range identified by TG. Depending on the value of , two exotherms appear in the DTA curves, the low-temperature one corresponding to crystallization of the Fe3(PO4)2 type regions, and the high-temperature one being related to various phases with dominating FePO4. Each exotherm has its own transformation region, identical in absolute value. The Mössbauer spectra of glasses which underwent thermal treatment at higher temperatures exhibit some indication of phases of the types Fe3(PO4)2 · xH2O and FePO4 · xH2O.
Zusammenfassung Differentialthermoanalyse (DTA), thermogravimetrische Analyse (TG), Röntgendiffraktion und Mössbauerspektroskopie wurden bei der Untersuchung (von kristalliner Produkte) durch verschiedene thermische Behandlungen hergestellten FeOx-P2O5 Gläsern eingesetzt. In den Glasarten mit einem hohen Wert von =Fe2+/(Fe2+ + Fe3+) erfolgt die Sauerstoffabsorption in einem durch TG [nachgewiesenen breiten Temperaturbereich. In Abhängigkeit von dem -Wert erscheinen zwei Exothermen in den DTA-Kurven, von denen der bei niedriger Temperatur die Kristallisation des Fe3(PO4)2 entspricht, und jener bei höheren Temperaturen in verschiedenen Phasen dem FePO4. Jede Exotherme hat ihr eigenes Umwandlungsgebiet, das in absolutem Wert identisch ist. Die Mössbauer-Spektren der Gläser welche einer Wärmebehandlung bei höheren Temperaturen unterzogen worden sind, weisen einige Indikationsphasen der Typen Fe3(PO4)2 · xH2O und FePO4 · xH2O auf.

, , FeOx-P2O5, . , =Fe2+/(Fe2++Fe3+) . , - : Fe3(PO4)2, – FePO4. , . , , Fe3(PO4)2 · 2 FePO4 · 2.


The authors thank Mrs. Simonyiová for assistance in the experimental part of these investigations, and Dr. Horváth and Dr. Vondrovic for performing the X-ray and TG analyses.  相似文献   

8.
    
A computer-controlled flow injection system was developed for the determination of cadmium in a hydrometallurgical zinc refining process stream. An anion-exchange method in acidic potassium iodide medium was used for the on-line separation of cadmium from the matrix zinc. 1-(4-Nitrophenyl)-3-(4-phenylazophenyl)triazene (Cadion) was used as the chromogenic reagent for the spectrophotometric detection of cadmium. In order to expand the dynamic range of the flow injection - spectrophotometry, a computer-aided time-based variable-volume injection method has been employed for the introduction of the sample into the flow injection system. Samples ranging from 0.56 to 350 l can be delivered by controlling the time period of the sample introduction valve and the flow rate of the carrier solution. The system permits a throughput of 5 samples per hour. The reproducibility has been proven to be satisfactory with a relative standard deviation of less than 6.2% (sample injected: 0.56 l of 850 g Cd/ml; n=100) and 5.0% (350 l of 0.14 g Cd/ml; n=5). The determination limit was 20 g Cd/ml with 0.56 l sample injection and 0.05 g Cd/ml with 350 l sample injection (the absolute amount of cadmium injected into the system was 11 ng and 17.5 ng, respectively).  相似文献   

9.
The phase changes in the solid state in E AlMgSi alloy are discussed. The dissolution and precipitation processes are investigated by DTA, and the results can be applied to control the technological parameters of dissolution heat treatments.
Zusammenfassung Die Autoren erörtern die Phasenänderungen in festem Zustand in E AlMgSi-Legierungen. Die Lösungen- und Fällungsvorgänge werden mittels der DTA-Methode untersucht, wodurch die Versuchsegebnisse bei der Kontrolle der technologischen Parameter der Hitzebehandlung von Lösungen eingesetzt werden5 können.

Résumé Etude par ATD des changements de phases dans l'état solide de l'alliage E AlMgSi et des processus de dissolution et de précipitation. Les résultats peuvent être appliqués au contrôle des paramètres technologiques des traitments thermiques.

E AlMgSi, . . .


Paper presented at the Scientific Session on Thermal Analysis held at Balatonfüred, Hungary, on 14–16 October 1976.  相似文献   

10.
Chemical processing for the preparation of Nb-coated barium titanate composite particles was investigated using surface modification technology, hydrolyzing Nb ethoxide on the surface of barium titanate particles dispersed in hydrophobic solvent.It was confirmed from the measurements of specific surface area and zeta potential as well as SEM, TEM and EDX observations of the resulting composite particles that the original barium titanate particles were coated uniformly with hydrolysis product of Nb ethoxide.Barium titanates coated with 1 wt% of Nb as oxide were well sintered at 1200–1300°C. The dielectric constants of the sintered barium titanates showed flattened temperature dependence, but it depended upon the average particle size of original barium titanate. The sintered bodies of Nb-coated barium titanate powders with average particle size of 0.2 m gave dielectric constants of 2000–3000 and those of barium titanate with average particle size of 0.5 m showed dielectric constants of 3000–4000 at room temperature.The microstructure of the sintered barium titanate coated with Nb oxide consisted of grains of about 1 m, smaller than those of sintered original barium titanate.  相似文献   

11.
Cyclic voltammetry and galvanostatic coulometry techniques were used to determine how the redox properties of osmium binuclear -oxocarboxylates [Os2 IV(-O)(-O2CR)2Cl4L2] (R = CH3, CCl3; L = PPh3 and R = CH3; L = AsPh3) are influenced by the nature of the bridging carboxylate ligand RCOO and ligand L. It was shown that all compounds in solution of dichloromethane undergo two single-electron reduction processes. The data obtained were compared with the DFT calculations of the electronic structure of the model complexes [Os2 IV(-O)(-O2CR)2Cl4L2] (R = CH3, CCl3; L = PH3 and R = CH3; L = AsH3).  相似文献   

12.
The stoichiometry of thermal decomposition of a particular group of clathrate compounds, of the type Cd(en)Pd(CN)4·2G, with the same coordination component but different clathrate-enclosed components, was investigated. Irrespective of the experimental conditions, the liberation of the enclosed component G always proceeded in one step. Thermal investigation of the decomposition stoichiometry under identical experimental conditions showed that the temperature intervals in which the enclosed components are given off shift to lower temperatures in the order C6H5OH=> C6H6 > > C4H5N > C4H4S. Diffraction measurements indicated a considerable change in the structures of the original clathrate compounds after thermal release of the enclosed componentG.
Zusammenfassung Die Stöchiometrie der thermischen Zersetzung einer bestimmten Gruppe von Klathratverbindungen vom Typ Cd(en)Pd(CN)4·2G mit der gleichen Koordinationskomponente und verschiedenen Klathrat-Einschlußkomponenten wurde in dieser Studie untersucht. Ungeachtet der Versuchsbedingungen vollzieht sich die Freisetzung der eingeschlossenen KomponenteG stets in einer Stufe. Die unter gleichen Versuchsbedingungen durchgeführte thermische Untersuchung der Zersetzungsstöchiometrie zeigte, daß die Temperaturbereiche, in denen die eingeschlossenen Komponenten freigesetzt werden in der Reihenfolge C6H5OH > C6H6 > C4H5N > C4H4S in Richtung der niedrigeren Temperaturwerte verschoben werden. Die Diffraktionsmessungen weisen darauf hin, daß eine beträchtliche Änderung der Struktur der ursprünglichen Klathratverbindung nach thermischer Freisetzung der eingeschlossenen KomponenteG sichtbar wird.

Résumé Dans cette étude on a établi la stoechiométrie de la décomposition thermique d'un groupe particulier de clathrates du type Cd(en)Pd(CN)4·2G, avec le même composant de coordination et différents composants occlus. Indépendamment des conditions d'expériences, la libération du composant occlusG s'effectue toujours en une étape. L'étude thermique de la stoechiométrie de la décomposition effectuée dans les mêmes conditions d'expériences, a montré que les intervalles des températures dans lesquels les composants occlus sont libérés, se déplacent vers les températures plus faibles dans l'ordre suivant: C6H5OH > C6H6 > > C4H5N > C4H4S. Les mesures de diffraction indiquent qu'après la libération thermique du composant occlusG, une variation considérable de la structure initiale des clathrates originaux apparaît.

Cd(en)Pd(CN)4. 2G . , G . , , , ] 65>66>C4H6N>C4H4S. - , G.
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13.
To obtain the kinetic curves of thermal decomposition of ammonium nitrate occurring together with decomposition of metal nitrates contained in a mixture, the ammonia contents evolved from samples heated under thermoanalytical conditions were determined by the Kjeldahl method.
Zusammenfassung Der aus unter thermoanalytischen -Bedingungen erhitzten Proben freigesetzte Ammoniakgehalt wird durch das Kjeldahlverfahren bestimmt, um die kinetischen Kurven der thermischen Zersetzung von Ammoniumnitrat zusammen mit der Zersetzung von Metallnitraten in Gemischen zu erhalten.

, , , .
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14.
Summary A simple and fast determination of trace amounts of commercially used cationic surfactants is described. After extraction from water cationic surfactants are separated by HPLC and detected by conductometry. The detection limit is 3 g/l for distearyldimethylammonium chloride, 16 g/l for ditallowimidazolinium methosulphate, and 6 g/l for dodecylpyridinium chloride.  相似文献   

15.
Summary For the trace determination of sodium alkylbenzenesulphonate (ABS) by HPLC the following conditions were employed: Shimadzu ZORBAX SIL Column (5 m, 4.6 mm i.d. x 150 mm) as stationary phase, 0.2% ammoniaethanol (v/v) as mobile phase, UV detector at 225 nm, injection volume 12 l. The chromatograms of ABS were simple and sharp (detection limit of ABS 0.02 g in 12 l of ethanol). The calibration curves of ABS were linear in a concentration range of 0.03 0.3 g in 12 l of ethanol. In the case of linear sodium dodecylbenzenesulphonate positive errors of 1 4% were caused by non-ionic surfactants or laurylsulphate (6 times excess), 10 50% positive errors were caused by 2 6 times excess of household detergents.Standard water samples containing ABS were treated with a weak base anion-exchange resin, the adsorbed ABS were eluted, and then determined either by HPLC or by the methylene blue spectrophotometric method. Recoveries of ABS in water were about 92 107% by HPLC.
Bestimmung von Spuren Natriumalkylbenzolsulfonat mit Hilfe der HPLC. Anwendung auf Wasser
Zusammenfassung Für die Spurenbestimmung von Natriumalkylbenzolsulfonat (ABS) durch HPLC werden die folgenden Bedingungen empfohlen:Shimadzu ZORBAX SIL (5 m, 4,6 mm x 150 mm) als stationäre Phase, 0,2% Ammoniak/Ethanol als mobile Phase, UV-Detektor bei 225 nm, Injektionsvolumen 12 l. Die erhaltenen Chromatogramme sind einfach und scharf (Nachweisgrenze 0,02 g in 12 ml Ethanol). Die Eichkurven sind im Konzentrationsbereich von 0,03–0,3 g in 12 l Ethanol linear. Im Falle des linearen Natriumdodecylbenzolsulfonats werden bei Anwesenheit von nicht-ionischen oberflächenaktiven Substanzen oder von Laurylsulfat in 6fachem Überschuß positiver Fehler von 1–4% erhalten; bei 2–6fachem Überschuß von Haushaltswaschmitteln ergeben sich positive Fehler von 10–50%.Standard-Wasserproben werden zunächst einer Behandlung mit einem Anionenaustauscher unterzogen, die adsorbierten ABS eluiert und durch HPLC oder nach der Methylenblaumethode analysiert. Wiederfindungsraten liegen bei 92–107%.
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16.
The general kinetic equation for two-component chemical systems is analyzed. It is shown that the positions of steady states in concentration spaces can be detected by a qualitative analysis of the chemical mechanism.
. , .
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17.
The optimum conditions for the extractive spectrophotometric determination of dioxouranium(VI) with hexamethyleneiminecarbodithioate(HMICdt) have been established. Dioxouranium(VI) reacts with this ligand at pH 4.5 to form a yellowish-orange uncharged 12 metal-ligand complex which can be extracted by chloroform. The calibration graph was linear in the range of 1–20 g ml–1 of dioxouranium(VI) at 335 nm. The molar absorptivity of the extracted species is 5.952×103 l mol–1 cm–1 with Sandell's sensitivity of 0.04 g cm–2. The average of 10 determinations of dioxouranium was 49.75 g for the samples containing 50 g of U(VI) and the variation from the mean at 95% confidence limit was 49.75±0.5955.  相似文献   

18.
Most optimized vitreous electrolytes are obtained by doping an oxide glass with a salt (MX); the resulting substance has an increased ionic conductivity, but a reduced thermal stability. On the other hand, this paper shows that it is possible to obtain vitreous electrolytes with enhanced electrical and thermal performances by mixing two glass formers. This phenomenon may be called the mixed anion effect. The Ag2OB2O3P2O5 system is shown to offer a very interesting example of such a phenomenon.
Zusammenfassung Optimale glasartige Elektrolyte werden durch Dopen eines Oxydglases mit einem Salz (MX) erhalten; die Produkte weisen eine erhöhte ionische Leitfähigkeit, jedoch auch eine verminderte thermische Stabilität auf. Andererseits wird gezeigt, daß glasartige Elektrolyte mit besseren elektrischen und thermischen Eigenschaften durch Mischen von zwei Glasbildnern erhalten werden können. Für dieses Phänomen wird die Bezeichnung mixed anion effect in Vorschlag gebracht. Es wird gezeigt, daß das System Ag2OB2O3P2O5 ein sehr interessantes Beispiel dieses Phänomens bietet.

MX. , . . . , Ag2O2325 .


The NMR data were collected at the Regional NMR Center of the Colorado State University (Fort Collins, Co, USA), funded by NSF Grant CHE-8208821). This research was funded in part by the Italian Department of Education (MPI 40%).  相似文献   

19.
Summary Less than 1 milligram of suspended particulate matter in a 50-ml water sample was separated by centrifugation, decomposed with 22l of 21010 perchloric-nitric-hydrofluoric acid mixture, and analyzed for copper, lead, cadmium and zinc by microscale differential pulse anodic stripping voltammetry with a hanging mercury drop electrode in 300l of 0.06M perchloric acid. The procedure was simple and rapid, because a single Teflon microvessel was used throughout the whole procedure.
Bestimmung von Schwermetallspuren in suspendierten Teilchen in Teichwasser durch Anodic Stripping Voltammetry im Mikromaßstab
Zusammenfassung Weniger als 1 mg suspendierter Teilchenmaterie wurde durch Zentrifugieren abgetrennt, mit 22l eines Gemisches HClO4HNO3HF (21010) zersetzt und darin Cu, Pb, Cd und Zn durchDifferential-Pulse-Anodic-Stripping-Voltammetrymit hängender Hg-Tropfelektrode in 300 l 0.06M Perchlorsäure bestimmt. Das Verfahren ist einfach und schnell, es bedarf dazu nur eines Mikrokölbchens aus Teflon.
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20.
Summary A rapid ion-exchange method for the determination of 144Ce, 137Cs, 89Sr, 90Sr and 140Ba in 2–30 liter samples of atmospheric water precipitations is described. The samples, containing up to 300 mg of calcium, are sorbed on a specially shaped column filled with Dowex 50, X-8 or Dowex 50W, X-8. Radio-cerium and radio-caesium are stripped from the column with 0.6 M ammonium glycolate/ 0.2 M NaCl, pH 5, radio-strontium and radio-barium with 0.15 M ammonium citrate, pH 7.5. The isolated radio-nuclides are counted on a low-background beta-counter: 144Ce as CeO2, 137Cs as Cs-dipicrylaminate, 89Sr/90Sr as SrCO3, 90Y as Y2O3, and 140Ba as BaCO3. The mean chemical yields amount to 95% for cerium, 85% for caesium, 95% for strontium, 95% for yttrium and 65% for barium. With parallel determinations at levels of a few picocuries, the deviations of the results from the respective mean values generally do not exceed ± 5%. With a 30 l sample the limit of detection amounts to 0.005 Ci/l for 144Ce, 0.006 Ci/l for 137Cs, 0.005 Ci/l for 90Sr, and 0.006 Ci/l for 140Ba.
Zusammenfassung Es wird eine schnelle Ionenaustauschmethode für die Bestimmung von 144Ce, 137Cs, 89Sr, 90Sr und 140Ba in 2–30 l Proben von atmosphärischen Wasser-Niederschlägen beschrieben. Die Proben, mit einem Calciumgehalt bis zu 300 mg, werden in eine besonders gestaltete, mit Dowex 50, X-8 oder Dowex 50 W, X-8 gefüllte Säule eingewaschen. Radio-Cer und Radio-Caesium werden mit 0,6 M Ammoniumglykolat/0,2 M NaCl, pH 5, Radio-Strontium und Radio-Barium mit 0,15 M Ammoniumcitrat pH 7,5 eluiert. Die isolierten Radio-Nuklide werden in einem Beta-Antikoinzidenzzähler gemessen: 144Ce als CeO2, 137Cs als Cs-dipikrylaminat, 89Sr/90Sr als SrCO3, 90Y als Y2O3 und 140Ba als BaCO3. Die mittlere Rückgewinnung der zugesetzten Träger beträgt für Cer 95%, 85% für Caesium, 95% für Strontium, 95% für Yttrium und 65% für Barium. In Parallelbestimmungen mit Gehalten von einigen Ci/l, überschreiten die Abweichungen der Ergebnisse von den entsprechenden Mittelwerten im allgemein nicht 5%. Bei einer 30 l-Probe beträgt die untere Nachweisgrenze 0,005 Ci/l für 144Ce, 0,006 Ci/l für 137Cs, 0,005 Ci/l für 90Sr und 0,006 Ci/l für 140Ba.
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