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  • Chromatographie, Gas  (24)
  • Bone
  • Springer  (36)
  • Periodicals Archive Online (PAO)
  • 1975-1979  (36)
  • 1978  (36)
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  • Springer  (36)
  • Periodicals Archive Online (PAO)
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  • 1975-1979  (36)
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  • 1
    Electronic Resource
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    Springer
    Calcified tissue international 26 (1978), S. 47-49 
    ISSN: 1432-0827
    Keywords: Matrix vesicles ; Calcospherites ; Mineralization ; Bone ; Dentin ; Cartilage ; SEM
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Mineral particle cluster, corresponding to calcospherites or matrix vesicle-initiated clusters in calcifying cartilage and dentin and to collagen bundle-related mineralization in lamellar bone, have been isolated from NaOCl solutions used to dissolve the organic matrix in preparation of anorganic mineralizing fronts for scanning electron microscopy.
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  • 2
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    Calcified tissue international 26 (1978), S. 81-84 
    ISSN: 1432-0827
    Keywords: Osteoclasts ; Bone ; Resorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Osteoclastic bone resorption involves the solubilization of the mineral salts and the degradation of noncollagen bone matrix and collagen fibrils. As no recognizable collagen fibrils have ever been reported within cytoplasmic vacuoles in osteoclasts, it is generally assumed that the collagen fibrils are digested extracellularly in the resorption zone. The extent to which lysis occurs extracellularly and whether or not the osteoclasts phagocytose the degradation products remain to be established. In the present communication, a hypothesis is presented suggesting the possibility that osteoclastic resorption of bone involves the participation of two different cell types. According to this hypothesis, osteoclastic bone resorption is initiated by osteoclasts that demineralize areas of bone and degrade noncollagen bone matrix. After the osteoclasts have moved away or become partially detached from the demineralized site, the exposed collagen fibrils are phagocytosed by mononuclear, fibroblast-like or monocyte-derived cells.
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  • 3
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    Calcified tissue international 26 (1978), S. 155-161 
    ISSN: 1432-0827
    Keywords: Plasma protein ; Glycoprotein ; Bone ; Glucosamine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Plasmaα 2HS-glycoprotein is specifically accumulated in calcified tissues. In the present studies this glycoprotein was isolated from plasma and after iodination with iodine-125 was injected intravenously into young rabbits. The tissue distribution and plasma disappearance rate of this radioactively labeled material were determined. Of the various tissues studied, bone showed the greatest retention of labeled glycoprotein expressed as percentage of the injected dose per gram tissue relative to the plasma content. The rate of loss of iodinatedα 2HS-glycoprotein from plasma was similar to that ofα 2HS-glycoprotein labeled endogenously by using14C-glucosamine or3H-glucosamine. The uptake of exogenously labeled3I-α 2HS-glycoprotein into bone tissue expressed as a percentage of the injected dose was similar to that of endogenously labeled14C-α 2HS-glycoprotein. These results suggest that the125I-labeled material can be used to study further the metabolism ofα 2HS-glycoprotein by bone tissue.
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  • 4
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    Calcified tissue international 26 (1978), S. 209-213 
    ISSN: 1432-0827
    Keywords: Mithramycin ; Bone ; β-Glucuronidase ; KT medium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Mithramycin suppresses bone resorption. Its effect on the synthesis and release of β-glucuronidase (a referent for lysosomal enzymes) in mouse calvarial explants was studied in an in vitro culture system. A newly described medium (designated as KT medium) was introduced in this specific study. Mithramycin initially inhibited the release of β-glucuronidase into the medium and resulted in an ultimate accumulation of this enzyme in the bone. These results suggest that inhibition of bone resorption by mithramycin may be attributed to interference in release of lysosomal enzymes from bone cells.
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  • 5
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    Calcified tissue international 25 (1978), S. 37-43 
    ISSN: 1432-0827
    Keywords: ESR ; Radiation free radicals ; CO3-Apatites ; Bone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Exposure of bone mineral to X-rays generates free radicals. These are usually very labile, but can be stabilized at liquid nitrogen temperatures for study by electron spin resonance spectroscopy. The free radicals thus detected in the present study included one with resonances arising from an electron excess center and 2 species with electron-deficit centers: a phosphate anion radical and a radical associated with carbonate. Each of these radicals seemed to be located chiefly at the mineral surface and was sensitive to the surface environment. Presence of an organic phase, as in whole bone, modified free radical production in a manner that suggests interference with the formation of electron deficit centers. Comparison with other synthetic minerals suggests that precipitated carbonateapatites are good models for bone mineral.
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  • 6
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    Calcified tissue international 25 (1978), S. 227-232 
    ISSN: 1432-0827
    Keywords: Parathyroid hormone ; Bone ; Calcium ; Chick embryo ; Organ culture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary The purpose of this study was to measure in an in vitro system the movement of Ca and phosphate (Pi) out of bone when treated with parathyroid hormone (PTH). Tibiae from 13-day chick embryos were incubated for up to 8 h in a defined medium containing 1.8 mM Ca. Medium samples were collected every 2 h and were analyzed for Ca, Pi and lactate. Net effluxes from the bones were calculated. When bones were incubated with PTH in the medium (1 U/ml), net Ca efflux was increased 44, 60 and 100% at 4, 6 and 8 h, respectively. At no time was net Pi efflux affected by the hormone. The well known PTH-stimulated lactate production was not seen until 8 h. Lower doses of PTH (0.1 and 0.3 U/ml) were also effective. Comparing PTH (1 U/ml) responsiveness at higher (2.2 mM) and lower (0.9 mM) medium Ca concentrations, showed that with 2.2 mM Ca no increased Ca efflux was seen, while with 0.9 mM Ca significant elevation in medium Ca occurred 2 h sooner than in the experiments using 1.8 mM Ca. In another experiment, varying the medium Pi level from 1 to 2 mM had no effect on the Ca response to PTH. In neither experiment was Pi release affected by PTH. The results of this study have led to the following conclusions: (1) PTH acts on bone to cause an early dose related increase in net Ca efflux; (2) the effect is specific for Ca, since it is not accompanied by an increased Pi efflux, and may be saturated by raising the medium Ca level; and (3) PTH-stimulated Ca efflux in this system is not correlated with, and is probably not a result of increased lactate production.
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  • 7
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    Calcified tissue international 25 (1978), S. 233-240 
    ISSN: 1432-0827
    Keywords: Bone ; Bone resorption ; Albumin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary A fraction (brA), which causes resorption of fetal rat bones in vitro, has been concentrated from bovine serum albumin by anion exchange column chromatography on DEAE Sephadex. This active fraction has also been prepared using DEAE Sephadex A-50 by a batch method with a 0.09M NaCl, 0.1M TRIS buffer, pH 8.35. BrA was 10–30 times more potent than the original albumin. The retained material, which constitutes the bulk of the protein and has less activity than the original albumin, elutes with 0.45M NaCl. Similar treatment of serumα,β or γ globulins does not yield brA. Further enhancement of the bone resorbing activity of brA can be obtained with (NH4)2SO4 fractionation or extraction with CH3OH∶CHCl3. Heating at 55° C for 2 h or at 100° C for 10 min does not affect the activity; overnight incubation with protease destroys the bone resorbing effect. The bone resorbing activity is not removed by dialysis and does not correlate with the protease activity of the fraction. The action of brA is inhibited by 3 mM PO4, 1 μg/ml calcitonin or glucagon, 10−7 M dexamethasone or 0.02 μg/ml actinomycin D. The bone resorbing activity of brA is partially inhibited by 10−7–10−5 M indomethacin. PTH did not elicit bone resorption when added to cultures incubated in chemically defined medium supplemented with 0.1 mg/ml brA. However, brA did not inhibit PTH-induced resorption.
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  • 8
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    Calcified tissue international 25 (1978), S. 249-254 
    ISSN: 1432-0827
    Keywords: Bone ; Oestrogens ; Oestrogen receptors ; Binding proteins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Attempts were made to demonstrate the presence of specific oestrogen binding proteins (“receptors”) in bone cells. High speed cytosol preparations of bone were incubated with several concentrations of radioactive oestradiol alone and with radioactive oestradiol in the presence of a specific antioestrogen, Nafoxidine. Separation of bound and free oestradiol was carried out by dextran coated charcoal treatment and by sucrose gradient ultracentrifugation. Several types of bones likely to be oestrogen-sensitive were investigated: human femoral heads, human phalanx, rat and rabbit calvaria, humeri and femora of female rats. In all experiments we were unable to demonstrate the presence of specific oestrogen receptors in bone cell cytosol indicating that the direct effect of oestrogens on bone, if present, is not mediated by specific oestrogen receptors.
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  • 9
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    Calcified tissue international 26 (1978), S. 85-89 
    ISSN: 1432-0827
    Keywords: Bone ; Histology ; Microradiography ; Densitometry ; Computer
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary A comparatively simple quantitative method for assessing bone morphology has been evolved. Microradiographs of thin sections of mandible have been scanned with a Joyce-Loebl double beam recording microdensitometer with a scanning autodensidater attachment, using a white beam. For each image the optical densities for all the pixels (picture elements) were divided into 10 groups. The limits of the division were fixed by the maximum and minimum densities occurring within the image. A computer generated map was produced which indicated the spatial distribution of the pixels within each group to which an arbitrarily chosen shading was attached. The number of pixels within each group is also shown on the map. The computer map was compared with the photomicrograph and, where necessary, the original section. The fractional area of hard tissue was then readily determined using the numerical values of each group of pixels.
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  • 10
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    Calcified tissue international 26 (1978), S. 139-142 
    ISSN: 1432-0827
    Keywords: Chemisorption ; Surface area ; Hydroxyapatite ; Bone ; Enamel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary The surface areas of three different samples of hydroxyapatite, samples of deproteinized bone, and samples of whole and deproteinized enamel were determined by adsorption of an adduct (the diglycidyl ether of bisphenol A with N-phenylglycine) from methylene chloride solution. In all cases, the surface areas of these samples agree well with those obtained by the BET (N2) method.
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  • 11
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    Calcified tissue international 25 (1978), S. 105-110 
    ISSN: 1432-0827
    Keywords: Progesterone ; 17β estradiol ; Testosterone ; Tissue culture ; Bone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary Although sex steroids are known to affect skeletal metabolism, their effects on bone collagen synthesis have not been studied. We have examined the direct effects of progesterone, 17β estradiol, testosterone, 5α dihydrotestosterone and dehydroepiandrosterone on bone collagen and noncollagen protein synthesis in cultures of calvaria obtained from 21-day fetal rats. Bones were incubated for 24 to 168 h and3H-proline was added for the last 2 h of culture. Incorporation of the label into collagenase-digestible protein (CDP)1 and noncollagen protein (NCP) was determined using repurified bacterial collagenase. Progesterone caused a dose dependent inhibition of the labeling of CDP at concentrations of 3×10−7 M to 10−5 M after 96 h of culture. A smaller inhibitory effect was observed on NCP. The inhibitory effect was slow in onset and persisted when bones were incubated for 48 h with progesterone and then transferred to control medium for 48 h. Progesterone also inhibited the incorporation of3H-thymidine and3H-uridine into fetal rat calvaria. After 24 h of culture, 17β estradiol and testosterone had no effects on the labeling of CDP and NCP. After 96 h, 17β estradiol had a small and inconsistent stimulatory effect on the labeling of CDP but testosterone had no effect. Neither hormone altered the inhibitory effects of parathyroid hormone, cortisol and progesterone. Dihydrotestosterone and dehydroepiandrosterone had no effects after 24 h and 96 h of culture. 17β estradiol, testosterone and dihydrotestosterone did not affect the incorporation of3H-uridine or3H-thymidine into fetal rat calvaria. Our studies indicate that progesterone is an inhibitor of bone collagen synthesis and estrogens and androgens are not major regulators of bone formation in vitro.
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  • 12
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    Calcified tissue international 25 (1978), S. 29-35 
    ISSN: 1432-0827
    Keywords: Albumin ; Bone ; Growth retardation ; Osteomalacia
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Notes: Summary 125I-labeled rat albumin injected intravenously into rats was taken up by growing bone. Some of this radioactive albumin could be removed from bone by washing with saline, the proportion so removed decreasing from 82.5% at 1 day to 7.4% at 8 days. Both the total radioactivity, and that remaining in bone after saline wash, were reduced when growth was slowed by alteration or restriction of the diet. Although the amount of125I albumin in rachitic bone was reduced, autoradiography showed that radioactivity was present in rachitic osteoid. Immunoprecipitation using anti-rat-albumin serum showed that about half of the radioactivity released from normal bone by EDTA was still attached to albumin. These results suggest that albumin plays some part in the growth of bone.
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  • 13
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    Fresenius' Zeitschrift für analytische Chemie 291 (1978), S. 299-307 
    ISSN: 1618-2650
    Keywords: Analyse von Kohlenwasserstoffen in Luft ; Chromatographie, Gas ; Tieftemperaturgradientenrohr
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird über ein gas-chromatographisches Verfahren zur Bestimmung von Alkanen, Alkenen und Aromaten in der Außenluft berichtet, bei dem die Probenahme an Tenax GC oder Carbopack mit Hilfe eines Tieftemperaturgradientenrohres erfolgt und die Analyse unter Einsatz eines Doppelsäulensystems in Verbindung mit zwei Flammenionisationsdetektoren durchgeführt wird. Eingehende Untersuchungen zum Verhalten der Substanzen bei der Probenahme zeigen, daß die Trocknung der Probeluft mit Magnesiumperchlorat das Ergebnis nicht beeinflußt und für Kohlenwasserstoffe mit drei oder mehr C-Atomen keine auf Durchbruch zurückzuführenden Substanzverluste zu befürchten sind. Bei einem Probenahmevolumen von 51 Luft können 2 μg Substanz/m3 gut bestimmt werden. Für Außenluft-Konzentrationen von 45 μg Benzol/m3, 95 μg Toluol/m3 und 35 μg n-Pentan/m3 betrugen die Standardabweichungen 3,5, 6,0 bzw. 3,6 μg/m3. Bei leichter Modifikation des Systems ist mit derselben Probenahmevorrichtung die gleichzeitige Bestimmung von Kohlenwasserstoffen mit einem Flammenionisationsdetektor und von Organohalogen Verbindungen mit einem Elektroneneinfangdetektor möglich.
    Notes: Summary A method is described for the gas-chromatographic determination of alkanes, alkenes and aromatics in ambient air. The hydrocarbons are trapped by cryogenic sampling using Tenax GC or Carbopack as adsorbing material and are analyzed in a two-column system equipped with two flame-ionization detectors. A detailed examination of the sampling procedure shows that drying the air with magnesium perchlorate does not affect the results, and losses of substances due to break-through need not be reckoned with for hydrocarbons with three and more carbon atoms. In a 51 air sample 2 μg/m3 of hydrocarbons can be determined readily. The standard deviations for benzene, toluene and n-pentane were 3.5, 6.0 and 3.6 μg/m3 at ambient air concentrations of 45, 95 and 35 μg/m3. A slight modification of the system which includes the combined use of a flame-ionization detector and an electron-capture detector permits the simultaneous determination of hydrocarbons and halogenated hydrocarbons.
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  • 14
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 39-42 
    ISSN: 1618-2650
    Keywords: Analyse von Metaboliten in Biolog. Material ; Chromatographie, Gas ; Fraktionierung durch Extraktion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A new method for the gas-chromatographic multicomponent analysis of metabolites in biological material is described. It is an analytical procedure involving several extractions carried out under different conditions. In this procedure the metabolites are divided according to their functional groups and specific chemical behaviours into eight main fractions: lipids, hydrocarbons, organic acids, neutral substances, phenols, amines, amino acids and carbohydrates. Each of these fractions is derivatized; the components are separated and estimated by gas chromatography. This analytical system was applied to the determination of a number of metabolites in serum, urine, amniotic fluid, sperma, tissues and other biological materials.
    Notes: Zusammenfassung Eine Methode für die Multikomponenten-GC-Analyse von Metaboliten in Biomaterialien wird beschrieben. Das Verfahren umfaßt mehrere Extraktionen, die unter verschiedenen Bedingungen durchgeführt werden. Die Komponenten werden in Abhängigkeit von ihren funktionellen Gruppen und spezifischem chemischen Verhalten in acht Hauptfraktionen geteilt: Lipide, Kohlenwasserstoffe, organische Säuren, neutrale Substanzen, Phenole, Amine, Aminosäuren und Kohlenhydrate. Die Komponenten jeder Gruppe werden nach spezieller Derivatisierung gaschromatographisch getrennt und bestimmt. Dieses neue System ist bei verschiedenen biologischen Materialien (klinische Proben, Pflanzen- und Tiergewebe) angewandt worden.
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  • 15
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 385-390 
    ISSN: 1618-2650
    Keywords: Best. von Carbonsäuren, Sulfonsäuren ; Chromatographie, Gas ; Spuren in wäßrigem Medium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Gas-chromatographische Methoden für die Spurenbestimmung einiger Carbonund Sulfonsäuren in wäßrigem Medium werden beschrieben. Die Nachweisvermögen für Ameisensäure, Essigsäure, Propionsäure, n-Buttersäure, n-Valeriansäure, Capronsäure, Acrylsäure, Benzoesäure und Chloressigsäure sowie für Methansulfonsäure und Äthansulfonsäure liegen zwischen 1 · 10−7 und 8 · 10−7 Mol/Liter. Anreicherung und Derivatisierung werden bei den Carbonsäuren durch Gefriertrocknung der Tetra-n-butylammoniumsalze und deren Umsetzung mit Benzylbromid zu den Benzylestern, bei den Sulfonsäuren durch Gefriertrocknung der Silbersalze und deren Umsetzung mit n-Butyljodid zu den n-Butylestern erreicht.
    Notes: Summary Gas-chromatographic methods for the determination of traces of several carboxylic and sulphonic acids in aqueous media are presented. Detection limits for formic, acetic, propionic, n-butyric, isobutyric, n-valeric, caproic, acrylic, benzoic, and chloroacetic acids as well as of methanesulphonic and ethanesulphonic acids range from 1 · 10−7 moles/liter to 8 · 10−7 moles/liter. Preconcentration and derivatisation of the carboxylic acids are achieved by freezedrying their tetra-n-butylammonium salts and converting the latter into the benzyl carboxylates using benzyl bromide. The sulphonic acids are converted to the corresponding silver salts, freeze-dried, and then esterified using n-butyl iodide.
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  • 16
    ISSN: 1618-2650
    Keywords: Analyse von Umweltmaterial, Pesticiden ; Chromatographie, Gas ; Capillar-, Ident. von Einzelkomponenten in komplexen Gemischen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Der Vergleich von präzise bestimmten Retentionsindices von Probe- und Referenzsubstanzen in der hochauflösenden Capillar-Gas-Chromatographie stellt eine aussagekräftige Methode der Identifizierung von Einzelkomponenten in komplexen Gemischen dar. Neben der Konstanz der GC-Parameter erfordert die präzise Bestimmung von Retentionsindices eine sehr genaue Bestimmung der Netto-Retentionszeiten. Insbesondere ist bei Anwendung einer Totzeitberechnung auf der Basis einer erzwungenen Linearisierung der log t s/Homologenzahl-Beziehung auf eine sehr genaue Retentionszeitmessung zu achten. Die Reproduzierbarkeit von präzise bestimmten Retentionsindices hängt von der Konstanz der Polarität und von der Adsorptivität der Capillarsäule ab. An ausreichend desaktivierten und konditionierten Hochleistungs-Capillarsäulen (TZ≥40) können unter der Voraussetzung einer Retentionszeit-Meßgenauigkeit von besser als 0,05% Retentionsindices über einen Zeitraum von mehreren Wochen innerhalb ±0,15 Indexeinheiten reproduziert werden. Eine Übertragung des n-Alkan bezogenen Retentionsindex-Konzeptes auf die homologe Reihe der n-Allkyl-trichloracetate (ATA) ermöglicht die Verwendung des Elektroneneinfang-Detektors (ECD) zur präzisen RetentionsindexBestimmung als Methode einer zuverlässigen Identifizierung von Substanzen im Picogrammbereich.
    Notes: Summary High resolution glass-capillary gas chromatography can be used as a powerful identification tool for single components in complex mixtures, when the matching of retention indices of reference compounds with those found in the sample is based on precise measurements. Besides the constancy of the GC-parameters high precision measurements of retention indices require an accurate determination of net retention times. Special care has to be taken for an accurate measurement of retention times when using a dead-time calculation on the basis of an enforced linearisation of the log t s/homologues-number relationship. The reproducibility of precise retention-index determinations strongly depends on the constancy of the polarity and on the adsorptivity of the capillary column. Provided a sufficiently deactivated and conditioned high performance capillary column (separation number ≥40) and an accuracy of retention-time measurement of better than 0,05 % retention indices can be reproduced within ±0.15 i.u. over a period of several weeks. A conversion of the n-alkane based retention-index concept to the use of the homologous series of n-alkyl-trichloro-acetates (ATA) allows the use of the electron-capture detector (ECD) for precise retention-index determinations for a reliable identification of compounds in the picogram range.
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  • 17
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    Fresenius' Zeitschrift für analytische Chemie 293 (1978), S. 412-413 
    ISSN: 1618-2650
    Keywords: Analyse von Dimethylterephthalat in Wasser ; Chromatographie, Gas ; Abwasser
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 18
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    Fresenius' Zeitschrift für analytische Chemie 293 (1978), S. 11-15 
    ISSN: 1618-2650
    Keywords: Best. von Blei neben Wismut ; Chromatographie, Gas ; Di(trifluoräthyl)dithiocarbamat. — Verhalten von Kupfer(II), Nickel(II), Kobalt(III), Eisen(III), Wismut(III), Blei(II), Antimon(III) ; Verteilung zwischen wäßriger Lösung und Chloroform
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Das Verteilungsverhalten der oben genannten Di(trifluroäthyl)dithiocarbamato-Chelate zwischen wäßrigen Lösungen und Chloroform wird untersucht. Eine Anwendung zur gleichzeitigen gaschromatographischen Bestimmung von Blei und Wismut im ppm-Bereich (0,2–3 ppm) nach Ausschütteln aus wäßrigen Lösungen wird beschrieben (Säule: 5 % GE SE50 auf Gas Chrom Q; 180–240° C; 4°/min; Einspritzblock: 240° C).
    Notes: Summary The solvent extraction of the above di(trifluoroethyl)dithiocarbamatochelates with chloroform is investigated. An application for the simultaneous gas-chromatographic determination 0.2–3 ppm of lead and bismuth after extraction out of aqueous solutions is reported (column: 5% GE SE 50 on Gas Chrom Q; 180–240° C; 4°/min; injection block: 242°C).
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  • 19
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 199-202 
    ISSN: 1618-2650
    Keywords: Verhalten von Di(trifluoroäthyl)dithiocarbamatochelaten ; Chromatographie, Gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Das gas-chromatographische Verhalten einiger Di(trifluoäthyl)dithiocarbamatochelate unter isothermen und temperaturprogrammierten Arbeitsbedingungen verschiedener Säulen wird beschrieben. Multielementanalyse von bis zu wenigstens neun Elementen dürfte auch nach Ausschütteln aus wäßrigen Lösungen möglich sein.
    Notes: Summary Gas chromatographic behaviour of some di(trifluoroethyl)dithiocarbamatochelates is investigated under isothermal and temperature programmed working conditions of various columns. Multielemental analysis of up to at least nine elements seems to be possible even after extraction out of aqueous solutions.
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  • 20
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 216-218 
    ISSN: 1618-2650
    Keywords: Best. von Pharmazeut. Produkten im Harn ; Chromatographie, Gas ; Extrelut, saure u. neutrale Stoffe
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Zum gas-chromatographischen Nachweis saurer und neutraler Arzneistoffe wurden Harnproben bei pH 6 an Extrelut® (Merck) mit Diäthyläther extrahiert. Die Wiederfindungsraten der meisten untersuchten Arzneistoffe liegen im gleichen Bereich wie bei der üblichen Flüssig-Flüssig-Extraktion im stärker sauren Milieu. Jedoch verbleiben endogene Carbonsäuren, welche die Auswertung der Chromatogramme erschweren, in der wäßrigen Phase.
    Notes: Summary Samples of urine at pH 6 were extracted with diethyl ether from Extrelut® (Merck) columns for the gas-chromatographic identification of acidic and neutral drugs. The recovery rates for most of the investigated substances were similar to those of usual liquid-liquid extraction from strongly acidic media. Endogenous carboxylic acids however, which would otherwise interfere in the chromatogram, remained in the aqueous phase.
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  • 21
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    Fresenius' Zeitschrift für analytische Chemie 289 (1978), S. 91-95 
    ISSN: 1618-2650
    Keywords: Analyse von Kohlenwasserstoffen, polycycl. in Klärschlamm ; Chromatographie, Gas ; Profilanalyse
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird ein einfaches und selektives Anreicherungsverfahren für polycyclische aromatische Verbindungen angegeben (flüssig-flüssig-Verteilung: Dimethylformamid + Wasser + Cyclohexan; Chromatographie an Sephadex LH 20/Isopropanol; Filtration an Aluminiumoxid/Cyclohexan). Das Gemisch der polycyclischen aromatischen Kohlenwasserstoffe (= PAH) wird gas-chromatographisch an gepackten Hochleistungssäulen getrennt und die FID-Signale mit einem anfangs zugegebenen inneren Standard verglichen. Es wurden 18 Hauptkomponenten quantitativ ausgewertet. Die Variationskoeffizienten einer fünffachen Bestimmung derselben Probe lagen zwischen 1,6 und 11,3%. Die Nachweisgrenze des Verfahrens beträgt bei einer mittleren elektronischen Signalverstärkung in Abhängigkeit von der Retentionszeit 0,5–5 ng (für Benzo(a)pyren 1 ng). Die Charakterisierung der PAH mit 4–7 Ringen erfolgte mit einer GC-MS-Kombination, was für den Routinebetrieb aufgrund der großen Ähnlichkeit der PAH-Profile verschiedener Klärschlammproben nicht erforderlich ist.
    Notes: Summary A simple and selective method of enrichment of polycylic aromatic compounds is described (liquid-liquid-distribution with DMF + water + Cyclohexane; chromatography on Sephadex LH 20/isopropanol; filtration on aluminium oxide/cyclohexane). The fraction of polycyclic aromatic hydrocarbons (= PAH), separated gas-chromatographically using high performance columns, is evaluated by comparising the FID-signals with those of the internal standard added to the sample. Eightteen main components are evaluated. The variation coefficient of five analyses of the sample is in the range of 1.6–11.3%. The detection limit by moderate amplification depends on retention time of the PAH (0.5–5 ng; for benzo(a)pyrene 1 ng). As the PAH profiles of different samples of sludge are very similar, it is normally not necessary to characterize the PAH by mass spectrometry.
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    Fresenius' Zeitschrift für analytische Chemie 289 (1978), S. 287-288 
    ISSN: 1618-2650
    Keywords: Best. von Phenylbutazon, Oxyphenbutazon in Plasma, Harn ; Chromatographie, Gas ; Pferde
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 111-112 
    ISSN: 1618-2650
    Keywords: Best. von Pentachlorphenol in Plasma, Urin ; Chromatographie, Gas
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 113-113 
    ISSN: 1618-2650
    Keywords: Best. von Methylquecksilber in Blut ; Chromatographie, Gas
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 114-114 
    ISSN: 1618-2650
    Keywords: Best. von Ameisensäure in Harn ; Chromatographie, Gas
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 132-133 
    ISSN: 1618-2650
    Keywords: Best, von α-Ketosäuren ; Chromatographie, Gas ; N-selektiver Detektor
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    Topics: Chemistry and Pharmacology
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    ISSN: 1618-2650
    Keywords: Analyse von Polycycl. Verbindungen, Carbazole, Acridine ; Chromatographie, Gas ; Carcinogene
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 155-155 
    ISSN: 1618-2650
    Keywords: Best. von Schlafmitteln in Serum ; Chromatographie, Gas
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 158-158 
    ISSN: 1618-2650
    Keywords: Best. von Doxepin, Desmethyldoxepin in Plasma ; Chromatographie, Gas ; cis-trans-Isomere
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 290 (1978), S. 316-316 
    ISSN: 1618-2650
    Keywords: Best. von Dimethylchlorsilan in Trichlorsilan ; Chromatographie, Gas ; Chlorierung
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 293 (1978), S. 211-219 
    ISSN: 1618-2650
    Keywords: Analyse von Metallen mit Dialkyldithiocarbamaten ; Chromatographie, Gas ; Eigenschaften, Extinktionskoeff., Dampfdrucke der Chelate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Darstellung, Eigenschaften, Extinktionskoeffizienten, thermogravimetrisches Verhalten und Dampfdrucke einer Reihe von Dialkyldithiocarbamatochelaten werden beschrieben und die Möglichkeiten zu ihrer gas-chromatographischen Bestimmung umrissen.
    Notes: Summary Preparation, properties, extinction coefficients, thermogravimetric behaviour and vapour pressure are reported of various dialkyldithiocarbamato chelates. Possibilities for their gas-chromatographic determination are outlined.
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    Fresenius' Zeitschrift für analytische Chemie 293 (1978), S. 303-304 
    ISSN: 1618-2650
    Keywords: Best. von Nimetazepam in biolog. Material ; Chromatographie, Gas
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 293 (1978), S. 290-294 
    ISSN: 1618-2650
    Keywords: Best. von Zink, Kupfer, Nickel mit Dipropyldithiocarbamat ; Chromatographie, Gas ; Extraktion aus wäßr. Lösung
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Kleine Mengen Ni, Cu und Zn in wäßrigen Lösungen können nach Ausschütteln ihrer Dipropyldithiocarbamatochelate gas-chromatographisch bestimmt werden. Arbeitsbedingungen für den 0,01–1 ppm-Bereich werden angegeben. Die Reproduzierbarkeit der Bestimmung wird durch Zusatz eines inneren Standards verbessert.
    Notes: Summary Small amounts of Ni, Cu and Zn in aqueous solutions can be determined by gas chromatography after extraction of their dipropyldithiocarbamatochelates. Working details for the 0.01–1 ppm range are reported. Reproducibility is markedly improved by addition of an inner standard.
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 97-107 
    ISSN: 1618-2650
    Keywords: Best. von Biphenylen, polychlorierte, Pesticide, chlorhaltig in Fisch ; Chromatographie, Gas ; Capillar, Persistenz
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Besides 83 structurally defined trichloro- to octachloro-biphenyls (PCB), the following chlorinated pesticides have been identified in fish liver oil (DAB 6) and fish liver extracts: HCB;α-HCH;γ-HCH; 2,4′-DDE; 4,4′-DDE; 2,4′-DDT; 4,4′-DDT; 2,4′-DDD; 4,4′-DDD; dieldrin; endrin. By analysing constant relative amounts of PCB-components present only in defined technical PCB-mixtures, the original PCB-pattern in environmental samples could be calculated. A mixture of Clophen A 60/Clophen A50 or of Aroclor 1260/Aroclor 1254 of 2.2∶1 gives the best fit. The constant ratio of four octachloro-biphenyls in technical mixtures and environmental samples as well requires the assumption of complete environmental stability of these compounds despite of any thinkable differences in environmental pathways. This assumption of environmental persistency is supported by a degree of degradation up to 80% of the calculated input observed for some higher chlorinated PCB-components, e.g. 2,2′,3,4,5′,6-hexachloro-biphenyl. Correlating the amount of each identified PCB-component to the octachloro-biphenyl as the internal standard, a correlation of the degradation with the PCB-substitution pattern is possible. Persistency is observed, if vicinal hydrogens are missing or a 4-position is chlorinated. A 4,4′-disubstitution favours persistency most.
    Notes: Zusammenfassung Neben 83 strukturell definierten Trichlor- bis Octachlor-biphenylen (PCB) wurden folgende chlorierte Biocide in Lebertran (DAB6) und Fischleberextrakten identifiziert: HCB;α-HCH;γ- HCH; 2,4′-DDE; 4,4′-DDE; 2,4′-DDT; 4,4′-DDT; 2,4′-DDD; 4,4′-DDD; Dieldrin; Endrin. Aus den Verhältnissen von nur in PCB-Produkten mit bestimmtem Chlorierungsgrad vorkommenden, schwer abbaubaren PCB-Komponenten konnte die ursprünglich in die Umwelt gelangte Zusammensetzung der PCB berechnet werden: eine Mischung aus Aroclor 1260/Aroclor 1254 (Monsanto, USA) oder Clophen A 60/Chlophen A 50 (Bayer, Deutschland) im Verhältnis 2,2∶1 ergibt die beste Näherung. Aus dem in technischen Produkten und den Umweltproben gleichen relativen Vorkommen von vier Octachlor-biphenylen muß auf deren völlige Stabilität unter Umweltbedingungen geschlossen werden. Diese Annahme wird durch den Abbau von bis zu 80% des ursprünglichen Gehalts anderer hochchlorierter Biphenyle, wie des 2,2′,3,4,5′,6-Hexachlor-biphenyls, gestützt. Wird das Vorkommen der identifizierten Chlorbiphenyle, auf die als persistent angenommenen Octachlor-biphenyle als internen Standard bezogen, ergibt sich eine klare Persistenz-Abbau-Beziehung zu dem PCB-Substitutionsmuster. Persistenz ist gegeben bei fehlenden vicinalen Wasserstoffatomen oder 4-Chlorsubstitution, wobei die 4,4′-Di-Substitution die Persistenz am stärksten fördert.
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 207-212 
    ISSN: 1618-2650
    Keywords: Analyse von Carbiden in Aluminium, Magnesium ; Chromatographie, Gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A quantitative gas-chromatographic method (molecular sieve column, FID) for the determination of Al4C3 in aluminium and magnesium has been developed. The effect of methane from external sources has been investigated and eliminated. Metallographic analysis of carbides in polished specimens were consistent with the gas-chromatographic measurements within a factor of 2. The discrepancy can be explained by the large uncertainties in light microscopy analysis of the small carbides. Analysis of commercial magnesium shows that the metal contains ca. 2–9 ppm of Al4C3. The concentration of carbides in aluminium from the electrolysis cell is in the range of 10–35 ppm and in the final product of ca. 2–12 ppm Al4C3. CaC2 has been detected in a few magnesium and aluminium samples by means of gas-chromatography and microprobe analysis.
    Notes: Zusammenfassung Zur Bestimmung von Al4C3 in Aluminium und Magnesium wurde eine quantitative gas-chromatographische Methode (MolekularsiebSäule, FID) entwickelt. Der Einfluß von Methan aus äußeren Quellen, wurde untersucht und ausgeschaltet. Die metallographischen Untersuchungen von Carbiden an polierten Proben stimmten mit den Ergebnissen der gas-chromatographischen Messungen mit einem Faktor von 2 überein. Der Unterschied kann durch die großen Unsicherheiten bei der lichtmikroskopischen Analyse der kleinen Carbide erklärt werden. Die Analyse des technisch reinen Magnesiums zeigt, daß das Metall ca. 2–9 ppm Al4C3 enthält. Die Konzentration von Carbiden in elektrolytisch raffiniertem Aluminium liegt im Bereich 10–35 ppm und im Endprodukt bei ca. 2–12 ppm Al4C3. CaC2 wurde in einigen Magnesium- und Aluminiumproben mit Hilfe von gas-chromatographischen und Mikrosondenuntersuchungen festgestellt.
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    Fresenius' Zeitschrift für analytische Chemie 292 (1978), S. 236-236 
    ISSN: 1618-2650
    Keywords: Analyse von Dimethylterephthalat ; Chromatographie, Gas ; Oxidationsgemisch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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