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  • Articles  (34)
  • Chromatographie, Gas
  • Drosophila melanogaster
  • Microtubules
  • Pisum
  • Springer  (34)
  • 1980-1984  (34)
  • 1945-1949
  • 1925-1929
  • 1920-1924
  • 1983  (11)
  • 1980  (23)
  • Chemistry and Pharmacology  (34)
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  • Articles  (34)
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  • 1980-1984  (34)
  • 1945-1949
  • 1925-1929
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  • 1
    ISSN: 1573-4927
    Keywords: alcohol dehydrogenase ; Drosophila melanogaster ; multiple forms ; conversion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The nature and the interconversion of the three multiple forms Adh-5, Adh-4, and Adh-3 of the purified alleloenzymes AdhS, AdhF, and AdhUF from the fruitflyDrosophila melanogaster have been examined. The experiments show that these multiple forms differ from those in crude extracts of flies homozygous at the Adh locus. On electrophoresis in a starch gel containing NAD or NADH, of purified AdhS which consists of the three Adh forms S-5, S-4, and S-3, five enzymatically active zones appear. This contrasts with the single active zone that arises with crude extracts. Of the five zones that appear with purified enzyme, S-5 gives rise to one, while the other four zones come from the two minor forms S-4 and S-3. The occurrence of the three multiple forms Adh-5, Adh-4, and Adh-3 for each of the purified alleloenzymes is considered due to Adh-5 and, in the case of Adh-4 and Adh-3, deamidation of Adh-5, with the Adh-3 fraction also containing some reversible modified Adh-5. Of the labile amides, at least one must be located in the coenzyme binding region with deamidation preventing coenzyme binding. Pure NAD does not convert Adh-5 to Adh-3 and Adh-1. To produce conversion, the presence of either acetone or butanone along with NAD is necessary. Increased amounts of either acetone or butanone result in increased conversion. In contrast to this, none of the carbonyl compounds cyclohexanone, (+)- and (−)-verbenone, acetaldehyde, acrolein, or crotonaldehyde produces conversion. The ketone group binds to the alcohol binding site in the enzyme-NAD complex. Conversion is considered due to the ketone group binding to a nucleophilic amino acid residue and forming a bridge to the C-4 of the nicotinamide moiety of NAD.
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  • 2
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; common and rare allozymes ; esterase-6 ; biochemical properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The biochemical properties of three allozymes coded by theEst-6 locus, two common forms (EST-6S and EST-6F) and one rare form (EST-6VF), were studied. The results show the existence of differences in isoelectric point, activity, activation energy, Km, and temperature coefficient among the three variants, especially between the two common forms and the one rare form. The specific activity of the rare enzymatic variant seems to be less affected by temperature variation. The possible significance of these findings in relation to the mechanism of reproduction is briefly discussed.
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  • 3
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; esterase 6 ; isozymes ; enzyme kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Esterase-6 (EST 6; carboxylic-ester hydrolase; EC 3.1.1.1) from Drosophila melanogaster was purified to homogenity. Purified enzyme occurs as two closely moving isozymes, slow (EST 6S) and fast (EST 6F), on native polyacrylamide gel electrophoresis. Except for slight differences in their mobility, the two isozymes share similar molecular and catalytic properties. Both isozymes are glycoproteins and have an apparent molecular weight of 62,000 to 65,000 as judged by analytical gel filtration and sodium dodecyl sulfate (SDS) electrophoresis. They have identical mobility on SDS-polyacrylamide gels and an isoelectric point of 4.5. Each isozyme has a single active catalytic site as confirmed by titration with 0,0-diethyl-p-nitrophenyl phosphate (Paraoxon). We conclude that EST 6 is a monomeric enzyme. The amino acid composition of the two isozymes is very similar and both variants lack half-cystine residues. The low pI of the enzyme is due in part to a relatively high proportion of glutamic and aspartic amino acid residues. Characterization of the kinetic parameters of the isozymes using β-naphthyl and p-nitrophenyl esters revealed no statistically significant differences in catalytic efficiency. There is, however, a suggestion that the two isozymes may differ in their substrate specificity.
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  • 4
    ISSN: 1573-4927
    Keywords: two-dimensional electrophoresis ; Drosophila melanogaster ; yellow (y) gene ; protein purification ; development
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Analysis of temperature-sensitive mutants suggests that the yellow (y) gene in Drosophila melanogaster is expressed at a different time in each cell type that gives rise to the various structures of the adult cuticle. An important step in analyzing the regulation of this gene requires identification of the y structural protein. A polypeptide has been identified which correlates with the presence or absence of a functional y gene. Furthermore, this protein has the tissue distribution profile expected of the y structural gene product. The ability to locate this gene was facilitated by the use of coisogenic stocks, two-dimensional electrophoretic protein separation, and an ultrasensitive silver protein stain.
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  • 5
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    Biochemical genetics 21 (1983), S. 49-62 
    ISSN: 1573-4927
    Keywords: glycerol-3-phosphate dehydrogenase ; enzyme synthesis ; Drosophila melanogaster
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Methods have been developed to measure the synthesis of glycerol-3-phosphate dehydrogenase (GPDH) during the development of Drosophila melanogaster. In emerged adult flies, GPDH is a principal component of protein synthesis, comprising between 1 and 2% of the protein synthetic effort. This high relative rate of protein synthesis continues throughout adult life during a period of stable enzyme concentration. Therefore, it is evident that GPDH undergoes continual turnover. Analysis of GPDH synthesis in the adult segments reveals that this enzyme is synthesized in head, thorax, and abdomen. In 5-day-old flies, the relative rates of GPDH synthesis in the thorax and abdomen are similar. However, the concentration of GPDH in the thorax greatly exceeds that found in the abdomen. Therefore, it appears that the turnover rate of GPDH in the abdomen must be greater than the turnover rate of GPDH in the GPDH-containing cells (flight muscle) of the thorax. GPDH represents between 0.5 and 0.9% of the protein synthetic effort of larvae. The principle GPDH-containing tissue of larvae is fat body. The turnover of GPDH in larvae is similar to that in adult abdomen. This may be related to the concurrent presence of GPDH isozyme-3 in both tissues. Our studies indicate that the cell type-specific control of GPDH occurs at several levels.
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  • 6
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    Biochemical genetics 18 (1980), S. 65-76 
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; cuticle ; chitin ; β-alanine ; N-acetyldopamine ; tanning ; melanization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract In Drosophila melanogaster, the chitinous microfibrils arising from the tips of the epidermal villi in adult cuticles remain irregular and loose in the mutant ebony (which fails in cuticular incorporation of β-alanine) but closely knit and regular in normal flies. Addition of β-alanine to cuticles from which nonchitinous materials have been removed with alkali converts the loose arrangement of the microfibrils to a compact and sharply delineated arrangement. β-alanine also accelerates tyrosinase-catalyzed oxidation of N-acetyldopamine by reacting with the oxidized product of the reaction to produce an orange-red complex. Similarly, β-alanine accelerates oxidation of N-acetyldopamine when these two substances are added to fluids from the hemocoel, to lead to tanning instead of normal blackening. These findings may help explain why β-alanine induces tanning while inhibiting melanization in insects.
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  • 7
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; 6-phosphogluconate dehydrogenase ; isozyme
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract 6-Phosphogluconate dehyrogenase is evident at all developmental stages of Drosophila melanogaster. The activity level is highest in early third instar larvae and declines to a lower, but relatively constant, level at all later stages of development. The enzyme is localized in the cytosolic portion of the cell. The A-isozymic form of 6-phosphogluconate dehydrogenase was purified to homogeneity and has a molecular weight of 105,000. The enzyme is a dimer consisting of subunits with molecular weights of 55,000 and 53,000. For the oxidative decarboxylation of 6-phosphogluconate the Km for substrate is 81 µm while that for NADP+ is 22.3 µm. The optimum pH for activity is 7.8 while the optimum temperature is 37 C.
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  • 8
    ISSN: 1573-4927
    Keywords: Tryptophan ; kynurenine ; white ; Drosophila melanogaster ; amino acid transport ; Malpighian tubules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Dissected Malpighian tubules from wild type and the eye color mutant white of Drosophila were compared with respect to their abilities to transport tryptophan and kynurenine into tubule cells. It was determined that mutation at white greatly impairs the ability of Malpighian tubule cells to take up tryptophan. Functional studies on the extracellular spaces and ultrastructural observations indicated no differences in these respects between wild type and white tubules. It is consistent with several observations that much of the tryptophan associated with white exists in the intercellular spaces. Furthermore, the uptake of tryptophan by the w + system of wild type tubules is inhibited by the analogue 5-methyl-tryptophan. However, the incorporation of radioactive tryptophan into protein in tubule cells from wild type and white occurs at the same rates and is not affected by 5-methyl-tryptophan. Therefore, it is apparent that Malpighian tubules have a transport system that enables entry of tryptophan into a cellular pool and that this cellular pool is initially independent of the tryptophan pool used for protein synthesis. The mutant white lacks this transport system. From these studies and others it appears that compartmentalization of cellular pools may be brought about via the utilization of specific membrane transport systems.
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  • 9
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    Biochemical genetics 18 (1980), S. 303-309 
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; allozymes ; GPT ; genetic mapping
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract We have used electrophoretic variants of glutamate-pyruvate transaminase (GPT, E.C. 2.6.1.2) in Drosophila melanogaster to genetically map the structural gene to position 42.6 on the X chromosome. By pseudodominance tests over several deficiencies we have localized it cytogenetically to the interval 11Fl-2 to 12Al-2. The sedimentation constant (s 20,w) of the native enzyme was determined in sucrose density gradients to be 5.9 and the native molecular weight approximately 87,000. The similarity in physical properties to mammalian enzymes suggests that the enzyme may also be dimeric in D. melanogaster.
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  • 10
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    Biochemical genetics 18 (1980), S. 699-715 
    ISSN: 1573-4927
    Keywords: modifying genes ; G6PD activity ; 6PGD activity ; Drosophila melanogaster ; enzyme polymorphism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Different homozygous lines of similar genotype with respect to G6pd and 6Pgd were shown to have different enzyme activities for G6PD and 6PGD. Crosses between high and low lines suggested that there were modifying genes present on the autosomes, while others were probably located on the X chromosome. Allelic variation within each electrophoretic class of G6pd and 6Pgd might, however, also have contributed to this variation. An experiment on adaptation to sodium octanoate demonstrated that in adapted flies selection for lower enzyme activity had occurred, which provided further evidence for the existence of genetic differences in activity. Furthermore, a strong positive correlation between the activities of G6PD and 6PGD was found for each genotype. Since no correlation was found between MDH and the two enzymes G6PD and 6PGD, it could be concluded that this correlation was probably rather specific for G6PD and 6PGD. Interaction between genotypes with respect to activity was also found. It was shown that the variation at 6Pgd influenced the activity of G6PD within a genotype. The data are discussed in relation to fitness differences presented in foregoing articles.
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  • 11
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    Biochemical genetics 18 (1980), S. 905-913 
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; allozymes ; α-glycerophosphate dehydrogenase ; frequency-dependent selection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Polymorphism at the α-Gpdh locus was studied in Drosophila melanogaster. Using two different lines, one marked by the F allele (FF line) another by the S allele (SS line), four populations were initiated, two in which the initial frequency of F was 0.1 and two in which it was 0.9. They have been observed for 34 generations. From the fifth generation on, the equilibrium frequency in the four cages was about 0.60. Viability has been measured during the evolution of the populations while F frequencies changed and recombinations between the FF and SS lines occurred. It has also been evaluated in synthetic populations built with different frequencies: (1) from the original FF and SS lines and (2) from FF and SS lines extracted after 34 generations of joint evolution. In all three cases, the FF viability depended on the frequency of the F allele. The similarity of the three linear regressions implies that the α-Gpdh locus or other closely linked loci is the target of the selection in the populations analyzed here.
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  • 12
    ISSN: 1573-4927
    Keywords: alcohol dehydrogenase ; Drosophila melanogaster ; multiple forms ; conversion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The nature and the interconversion of the three multiple forms Adh-5, Adh-4, and Adh-3 of the purified alleloenzymes AdhS, AdhF, and AdhUF from the fruitfly Drosophila melanogaster have been examined. The experiments show that these multiple forms differ from those in crude extracts of flies homozygous at the Adh locus. On electrophoresis in a starch gel containing NAD or NADH, of purified AdhS which consists of the three Adh forms S-5, S-4, and S-3, five enzymatically active zones appear. This contrasts with the single active zone that arises with crude extracts. Of the five zones that appear with purified enzyme, S-5 gives rise to one, while the other four zones come from the two minor forms S-4 and S-3. The occurrence of the three multiple forms Adh-5, Adh-4, and Adh-3 for each of the purified alleloenzymes is considered due to Adh-5 and, in the case of Adh-4 and Adh-3, deamidation of Adh-5, with the Adh-3 fraction also containing some reversible modified Adh-5. Of the labile amides, at least one must be located in the coenzyme binding region with deamidation preventing coenzyme binding. Pure NAD does not convert Adh-5 to Adh-3 and Adh-1. To produce conversion, the presence of either acetone or butanone along with NAD is necessary. Increased amounts of either acetone or butanone result in increased conversion. In contrast to this, none of the carbonyl compounds cyclohexanone, (+)- and (−)-verbenone, acetaldehyde, acrolein, or crotonaldehyde produces conversion. The ketone group binds to the alcohol binding site in the enzyme-NAD complex. Conversion is considered due to the ketone group binding to a nucleophilic amino acid residue and forming a bridge to the C-4 of the nicotinamide moiety of NAD.
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  • 13
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    Biochemical genetics 21 (1983), S. 49-62 
    ISSN: 1573-4927
    Keywords: glycerol-3-phosphate dehydrogenase ; enzyme synthesis ; Drosophila melanogaster
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Methods have been developed to measure the synthesis of glycerol-3-phosphate dehydrogenase (GPDH) during the development ofDrosophila melanogaster. In emerged adult flies, GPDH is a principal component of protein synthesis, comprising between 1 and 2% of the protein synthetic effort. This high relative rate of protein synthesis continues throughout adult life during a period of stable enzyme concentration. Therefore, it is evident that GPDH undergoes continual turnover. Analysis of GPDH synthesis in the adult segments reveals that this enzyme is synthesized in head, thorax, and abdomen. In 5-day-old flies, the relative rates of GPDH synthesis in the thorax and abdomen are similar. However, the concentration of GPDH in the thorax greatly exceeds that found in the abdomen. Therefore, it appears that the turnover rate of GPDH in the abdomen must be greater than the turnover rate of GPDH in the GPDH-containing cells (flight muscle) of the thorax. GPDH represents between 0.5 and 0.9% of the protein synthetic effort of larvae. The principle GPDH-containing tissue of larvae is fat body. The turnover of GPDH in larvae is similar to that in adult abdomen. This may be related to the concurrent presence of GPDH isozyme-3 in both tissues. Our studies indicate that the cell type-specific control of GPDH occurs at several levels.
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  • 14
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    Biochemical genetics 21 (1983), S. 375-390 
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; segmental aneuploidy ; octanol dehydrogenase ; allozymes ; cytogenetic localization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract A gene-dosage effect is characteristic of eukaryotic structural genes and is therefore useful in gene mapping. However, attributing quantitative variations in enzyme activity to a gene-dosage effect or other putative regulatory loci can be suspect when the locus in question may be inducible by variations in culture conditions. The problem of controlling for allele-specific variations in activity and regulation can be circumvented in Drosophila melanogaster by the use of synthetic duplications and deficiencies in conjunction with enzyme polymorphism. A method for constructing segmental aneupliods heterozygous for electrophoretic variants of octanol dehydrogenase (Odh) is presented which permitted variations in allozyme phenotype and enzyme activity—which show a strict dosage dependency—to be produced simultaneously. The structural gene region for Odh was identified using T(Y;A) stocks and the deficiency M(3)S31 was used to assign the locus to polytene band region 86D1–4. With this method a segmental aneuploid survey of Drosophila for purposes of gene localization can be accomplished in one generation with appropriate stocks.
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  • 15
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; NADP+-dependent isocitrate dehydrogenase (NADP-IDH) ; cis-acting regulation ; population null alleles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract We have characterized biochemical effects of Idh GB1 in Drosophila melanogaster. This is a “null”-activity allele for NADP+-dependent isocitrate dehydrogenase (NADP-IDH) isolated from a natural population. The homozygous mutant strain has 5% of the NADP-IDH specific activity found in controls and less than 24% of the immunologically cross-reacting material (CRM). This mutation maps to 27.2 on the third chromosome, to the right of h. The biochemical phenotype of this mutant strain includes a coordinate reduction in malic enzyme (ME) specific activity and CRM and an increase in specific activity for the pentose-phosphate shunt enzymes, 6-phosphogluconate dehydrogenase and glucose-6-phosphate dehydrogenase. The K m values for purified NADP-IDH are not different from those found for the purified control enzyme for NADP+ or isocitrate. It is suggested that this allele may represent a cis-acting control mutation for one of at least two loci involved in the production of NADP-IDH in D. melanogaster.
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  • 16
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; common and rare allozymes ; esterase-6 ; biochemical properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract The biochemical properties of three allozymes coded by the Est-6 locus, two common forms (EST-6S and EST-6F) and one rare form (EST-6VF), were studied. The results show the existence of differences in isoelectric point, activity, activation energy, Km, and temperature coefficient among the three variants, especially between the two common forms and the one rare form. The specific activity of the rare enzymatic variant seems to be less affected by temperature variation. The possible significance of these findings in relation to the mechanism of reproduction is briefly discussed.
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  • 17
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    Biochemical genetics 21 (1983), S. 1153-1166 
    ISSN: 1573-4927
    Keywords: Drosophila melanogaster ; glucose-6-phosphate dehydrogenase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Three alleles of the Zw locus of Drosophila melanogaster—Zw A, ZwB,and Zw lol—apparently code for dimeric, tetrameric, and monomeric forms of glucose-6-phosphate dehydrogenase (G6PD), respectively. The three forms of G6PD are characterized by different apparent K mvalues for glucose-6-phosphate but similar apparent K mvalues for NAPD+. When high concentrations of NAPD+ were added to enzyme preparations, the Zw Aand Zw lolforms of G6PD assumed tetrameric and dimeric properties, respectively. Although Zw loladults exhibit little G6PD activity, they maintain levels of G6PD-antigen comparable to those in Zw Aand Zw Badults. Thus the low level of G6PD activity in Zw lolindividuals cannot be explained as the consequence of lack of synthesis of the G6PD subunit.
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  • 18
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    Fresenius' Zeitschrift für analytische Chemie 301 (1980), S. 108-109 
    ISSN: 1618-2650
    Keywords: Best. von Ethosuximid, Valproat in Blutserum ; Chromatographie, Gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Conclusion The proposed simultaneous determination of ethosuximide and valproate takes advantage of the similar properties of these substances that differ markedly from the other mainly used antiepileptic drugs. The volatility as well as the high blood concentration that are usual in therapeutics allow the measurement of ethosuximide and valproate directly in the extract without further concentration, e.g. by evaporation. On the other hand, one can optimise the methods for the determination of the other anticonvulsant drugs that are poorly volatile putting ethosuximide and valproate aside [1] and give up procedures using temperature programs with temperature differences of more than 100 ° C between the starting and the endpoint.
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  • 19
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    Fresenius' Zeitschrift für analytische Chemie 302 (1980), S. 264-268 
    ISSN: 1618-2650
    Keywords: Best. von Wasser in Organ. Lösungsmitteln ; Chromatographie, Gas ; ECD, 8–170 ppm
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Wasser ist in organischen Lösungsmitteln im ng-Bereich gas-chromatographisch ohne Derivatisierung mittels eines linearisierten Elektroneneinfangdetektors (ECD) nach Abtrennung auf einer Porapak QS-Säule bestimmbar. Ausreichend wasserfreie Lösungsmittel ließen sich durch Trocknen mit aktivierten 4 Å-Molekularsieben oder superaktiven Aluminiumoxiden W 200, Woelm Pharma, Eschwege, herstellen. Um Wasserblindwerte aus der Raumluft auszuschließen, ist es notwendig, sämtliche Operationen in einer Box mit Umlauftrocknung durchzuführen. Wassermengen bis zu 15 ng absolut sind bestimmbar. Im Konzentrationsbereich 7–150 μg/ml ist die Detektoranzeige für Wasser linear.
    Notes: Summary Water can be determined directly in organic solvents in the ng range after separation on a porapak-QS column using a linear electron-capture detector (ECD). Organic solvents can be dried by activated 4 Å molecular sieves to a water content of 5 μg/ml, about 0.3×10−3 molar. To exclude water contamination all operations, storage of solvents and standards included, were made in a glove box with permanent drying of the inside atmosphere. The EC-detector allows to determine 15 ng of water absolute. In the range of 7–150 μg/ml a linear response for water by the ECD has been found.
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  • 20
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    Fresenius' Zeitschrift für analytische Chemie 303 (1980), S. 20-22 
    ISSN: 1618-2650
    Keywords: Analyse von Biolog. Substanzen, Steroidhormonen ; Chromatographie, Gas ; Anreicherungsverfahren
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A new technique for the quantitation of very low concentrations of biological substances by gas-liquid chromatography is described. It is based on the direct concentration of the substances to be measured at the inlet of the chromatographic column. This is accomplished by injection of the substance into the chromatographic apparatus, whose column is kept at the condensation temperature of the sample. Repeated injection in separate portions results in accumulation of the substance. Chromatography is readily achieved by heating to the optimal temperature. This technique yielded promising results in the quantitation of several steroid hormones.
    Notes: Zusammenfassung Das Verfahren beruht auf der direkten Konzentrierung der zu bestimmenden Substanzen am Eingang der chromatographischen Säule. Sie erfolgt durch Injektion der Substanzlösung in die Säule bei einer Temperatur niedriger als der Schmelzpunkt, so daß die Substanz nicht eluiert werden kann. Eine wiederholte Injektion einzelner Portionen führt zur Anreicherung der Substanz, die dann nach Erhöhung der Säulentemperatur chromatographiert werden kann. Das Verfahren wurde mit guten Ergebnissen zur Bestimmung einiger Steroidhormone angewendet.
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  • 21
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    Fresenius' Zeitschrift für analytische Chemie 300 (1980), S. 387-402 
    ISSN: 1618-2650
    Keywords: Best. von Hexachlorbenzol, Polychlorcamphenen, Toxaphen, Kohlenwasserstoffen, chlorierte in Biolog. Material ; Chromatographie, Gas ; Umweltbelastung
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Fishes have been used to characterize pristine aquatic environments. In samples from a lake in the Tyrolian Alps (arctic char) and Northwest Ireland (pike), the Caspian Sea (sturgeon/Sevruga), the North Atlantic (salmon), the North Pacific (salmon) and the Antarctic Ocean at South Georgia (antarctic cod) hexachlorobenzene and polychlorinated camphene (PCC, Toxaphene) have been found. Samples are extracted by n-hexane/acetone (2+1), following a dimethylformamide/hexane clean-up of the lipid matrix. Adsorption chromatography on Florisil (1.25% water content) allows the elution of hexachlorobenzene, 4,4′-DDE and the polychlorobiphenyls (PCB) with n-hexane, while the mixture nhexane/diethyl ether (90+10) will elute the polychlorocamphenes (PCC) together with the hexachlorocyclohexane isomers and the DDT group. Identification of the PCC has been done by matching their retention indices measured by high resolution ECD glass capillary gas chromatography using the nalkyl-trichloroacetates as references and technical Toxaphene together with a slightly dehydrochlorinated product as authentic samples. The PCC content of the samples from the lakes in the European Alps and Northwest-Ireland, the North Pacific and the Antarctic Ocean was 125, 240, 285 and 68 ng of PCC per g of extractable lipids, respectively. The samples from the Caspian Sea and the North Atlantic had 1,625 and 3,500 ng of PCC per g of extractable lipids, respectively. All samples but the one from the Antarctic Ocean (liver) were spawn. Besides hexachlorobenzene and the PCC all samples contained polychlorobiphenyls (PCB), theα, β andγ-isomers of hexachlorocyclohexane, the compounds of the DDT-group and many other ECD-dectable not yet identified compounds.
    Notes: Zusammenfassung In Fischproben aus in erster Näherung unbelasteten Gebieten, dem Nordatlantik (Lachs), einem See in Nordwest-Irland (Hecht), einem Hochalpensee (Bergsaibling), dem Kaspischen Meer (Sternhausen), dem Nordpazifik (Lachs) und dem Antarktischen Ozean bei Südgeorgien (Antarktischer Dorsch) lassen sich Hexachlorbenzol und polychlorierte Camphene (PCC, Toxaphen®) nachweisen. Die Probe wird mit n-Hexan/Aceton (2+1) extrahiert. Die Lipide werden über eine Dimethylformamid/Hexan-Verteilung weitgehend abgetrennt. Adsorptions-Chromatographie an Florisil mit 1,25% Wassergehalt erlaubt die Elution von Hexachlorbenzol, 4,4′-DDE und der polychlorierten Biphenyle (PCB) mit n-Hexan; n-Hexan/Diethylether (90+10) eluiert die polychlorierten Camphene zusammen mit den Hexacyclohexan-Isomeren und der DDT-Gruppe. Die Identifizierung der PCC gelang über Vergleich der mit ECD-Capillar-Gas-Chromatographie unter Bezug auf die n-Alkyltrichloracetate gemessenen Retentionsindices. Als Standardsubstanz diente technisches Toxaphen, sowie ein durch methanolische KOH leicht dehydrochloriertes Produkt. Der PCC Gehalt lag bei den Proben aus dem Hochalpensee, einem See in Nordwest-Irland, dem Nordpazifik und dem Antarktischen Ozean bei 125, 240 bzw. 285 und 68 ng PCC/g extrahierbare Lipide. Die Proben aus dem Kaspischen Meer und dem Nordatlantik enthielten 1 625 bzw. 3 500 ng PCC/g extrahierbare Lipide. Bis auf die Probe aus der Antarktis (Leber) handelte es sich jeweils um Rogen. Neben dem Hexachlorbenzol und den Polychlorcamphenen wurden in allen Proben polychlorierte Biphenyle, dieα, β undγ-Isomeren des Hexachlorcyclohexans, die DDT-Gruppe und zahlreiche weitere bisher nicht identifizierte, mit dem ECD nachzuweisende Verbindungen gefunden.
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    Fresenius' Zeitschrift für analytische Chemie 302 (1980), S. 20-31 
    ISSN: 1618-2650
    Keywords: Analyse von Polychlorbiphenylen, Aroclor, Clophen ; Chromatographie, Gas ; Glascapillaren, Electron capture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The composition of seven technical PCB-mixtures (Aroclor [Monsanto, USA] und Clophen A [Bayer, FRG]) has been investigated by high-resolution thin-film glass capillary gas chromatography with electron-capture detector. Methylpolysiloxane (SE 30) and purified Apiezon L have been used as liquid phases. Identification of the single PCB components has been performed by comparison of their retention indices with those of polychlorinated biphenyls defined by synthesis or with values calculated from retention index increments. For marking the individual PCB compounds a systematic numbering has been used.
    Notes: Zusammenfassung Die Zusammensetzung sieben technischer Gemische polychlorierter Biphenyle (PCB) mit unterschiedlichem Chlorierungsgrad (Aroclor- [Monsanto, USA] und Clophen A- [Bayer, Bundesrepublik Deutschland]-Typen) wurde mit hochauflösender Gas-Chromatographie mit Elektroneneinfang-Detektion in Dünnfilm-Glascapillaren mit Methylpolysiloxan (SE 30) und gereinigtem Apiezon L als flüssiger Phase untersucht. Die Identifizierung der Einzelkomponenten erfolgte durch chromatographischen Vergleich mit definierten Referenzsubstanzen oder Vergleich der aus Inkrementen berechneten Retentionsindices. Für die Kennzeichnung der Einzelkomponenten wird eine systematische Numerierung entsprechend der Substituentenbezifferung verwendet.
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    Fresenius' Zeitschrift für analytische Chemie 304 (1980), S. 23-27 
    ISSN: 1618-2650
    Keywords: Best. von n-Butylzinnverbindungen in Luft ; Chromatographie, Gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung n-Butylzinnverbindungen (Tetra-, Tri-, Di-) wurden aus der angesaugten Luft an Chromosorb 102 adsorbiert, mit HCl-haltigem Diethylether desorbiert, falls nötig mit Methylmagnesiumchlorid umgesetzt und die methylierten Verbindungen gas-chromatographisch mit einem zinnspezifischen flammenphotometrischen Detektor bestimmt. Die mittlere Wiederfindungsrate (0,09–40 μg) von Bis(tri-n-butylzinn)oxid (TBTO) betrug: 93,3%; Streubereich der Einzelwerte ± 9,3% (P=95%, N=11). Wird 1 m3 Luft angesaugt, lassen sich noch Konzentrationen an n-Butylzinnverbindungen (Tetra-, Tri-, Di-) von 0,05 μg/m3 bestimmen. In einem mit einer TBTO-haltigen Dispersionsfarbe gestrichenen Raum wurde die Temperaturabhängigkeit der Tri-n-butylzinn-Konzentration in der Luft untersucht. Der Vergleich mit den Resultaten von Bestimmungen des Totalzinngehaltes läßt den Schluß zu, daß in der Luft nur Tri-n-butylzinnverbindungen vorlagen.
    Notes: Summary n-Butyltin compounds (tetra-, tri-, di-) have been adsorbed on Chromosorb 102 from the aspired air, desorbed with HCl-containing diethylether and, if necessary, converted to the corresponding methyl derivatives by reaction with methylmagnesium chloride. The derivatives were determined by GLC with a tin-specific flame photometric detector. The mean recovery (0.09–40 μg) of bis(tri-n-butyltin)oxide (TBTO) was 93.3%; tolerance limit ±9.3% (P=95%, N=11). With an air sample of 1 m3 it is possible to measure n-butyltin compounds (tetra-, tri-, di-) in concentrations down to 0.05 μg/m3. In a room coated with a TBTO-containing latex-based paint, the temperature dependence of the tri-n-butyltin concentration in the air has been studied. Comparison with results of total tin determinations allows the conclusion that the air contained only tri-n-butyltin compounds.
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    Fresenius' Zeitschrift für analytische Chemie 301 (1980), S. 143-143 
    ISSN: 1618-2650
    Keywords: Best. von Phenolen ; Chromatographie, Gas ; neue Methylierungsreagentien
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 301 (1980), S. 432-433 
    ISSN: 1618-2650
    Keywords: Analyse von Abwasser der Dimethylterephthalat-Produktion ; Chromatographie, Gas
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    Fresenius' Zeitschrift für analytische Chemie 303 (1980), S. 126-127 
    ISSN: 1618-2650
    Keywords: Analyse von Hydroxyfettsäuren ; Chromatographie, Gas ; ECD
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    Fresenius' Zeitschrift für analytische Chemie 303 (1980), S. 279-288 
    ISSN: 1618-2650
    Keywords: Analyse von Polysacchariden, Verdikkungsmitteln, Celluloseethern ; Chromatographie, Gas ; Zeisel-Spaltung
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Im vorliegenden zweiten Teil der dreiteiligen Übersicht zur Analytik der Polysaccharide wird am Beispiel einer Methylhydroxyethylcellulose (MHEC) die Erfassung der Celluloseether und -mischether mittels der Gas-Chromatographie vorgestellt. Dabei handelt es sich um die Beschreibung einer quantitativen Methode hoher Empfindlichkeit, die erforderlich ist, um Cellulosederivate mit geringer Mischsubstitution zu identifizieren und zu unterscheiden. Dazu werden die Celluloseether in einer speziell entwickelten Apparatur mit Iodwasserstoffsäure bei 140°C erhitzt. Von den sich bildenden Spaltprodukten werden die abdestillierten Alkyliodide in gekühltem Hexylbromid aufgefangen, gas-chromatographisch getrennt und identifiziert; gebildete Olefine werden durch Bromaddition erfaßt. Reproduzierbarkeit: ≤3% rel. Erfassungsgrenze: = 0,01% Hydroxyethylcellulose (HEC). Die Methode eignet sich auch zur Erfassung von Estern, S-Alkylgruppen, Methylimidverbindungen, Glykolanteilen oder bestimmten Tensiden.
    Notes: Summary In this second part of the three-part review on analysis of polysaccharides the characterization of cellulose ethers and cellulose mixed ethers by means of gaschromatography is described. The identification of the wide varying field of this cellulose ethers is presented using methylhydroxyethylcellulose (MHEC) as an example. To differentiate all cellulose mixed ethers, even those with little substitution of one of the two ether components, the method has to work qualitatively and quantitativly with a high sensitivity. The cellulose ethers are treated with hydriodic acid at 140°C in a special apparatus. The alkyliodides formed are distilled into cooled hexyl bromide. They are separated and identified by gaschromatography. Olefins also formed are determined by addition of bromine. Reproducibility: ≤ 3% rel. Limit of detection: = 0.01 % Hydroxyethylcellulose (HEC). This method can also be used for the determination of esters, S-alkyl groups, methylimides, glycols and some detergents.
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    Fresenius' Zeitschrift für analytische Chemie 303 (1980), S. 397-400 
    ISSN: 1618-2650
    Keywords: Best. von Benzo(a)-pyren in Erdölprodukten ; Chromatographie, Gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A gas-liquid chromatographic method has been developed for the quantitive determination of benzo(a)-pyrene in petroleum products. At the 2 ppb benzo(a)pyrene level in a sample, the recovery is 87–90%. The detection limit is 50 ng. A column was employed with a liquid-crystal phase of bis(p-phenylbenzylidene)-bi-p-toluidine on Chromosorb.
    Notes: Zusammenfassung Das entwickelte gas-chromatographische Verfahren benutzt eine SÄule mit der Flüssig-Kristallphase von Bis(p-phenylbenzyliden)-bi-ptoluidin auf Chromosorb und gestattet im Bereich von 2 ppb Benzo(a)-pyren eine Wiederfindung von 87–90%. Die Nachweisgrenze liegt bei 50 ng.
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    Fresenius' Zeitschrift für analytische Chemie 301 (1980), S. 32-32 
    ISSN: 1618-2650
    Keywords: Best. von Hexachlorcyclohexan, Hexachlorbenzol in Boden ; Chromatographie, Gas ; Extraktion
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 304 (1980), S. 143-143 
    ISSN: 1618-2650
    Keywords: Best. von Hexachlorcyclohexan, Hexachlorbenzol im Wasser ; Chromatographie, Gas ; Extraktion
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 302 (1980), S. 375-381 
    ISSN: 1618-2650
    Keywords: Best. von n-Alkanen, Pristan in Luft ; Chromatographie, Gas ; reine Luft
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary An analytical method was developed for measuring n-alkanes (C9 to C17) and other hydrocarbons in tropospheric air with mixing ratios of a few ppt (10−12) and higher. The hydrocarbons are collected in situ in absorption tubes, carefully protected against contamination and analysed later in the laboratory by gas chromatography. First data are reported for Atlantic air masses at the west coast of Ireland.
    Notes: Zusammenfassung Es wurde eine analytische Methode entwickelt zur Messung der n-Alkane (C9 bis C17) und anderer Kohlenwasserstoffe in reiner troposphärischer Luft mit Mischungsverhältnissen von einigen ppt (10−12) und aufwärts. Die Kohlenwasserstoffe wurden am Beobachtungsort angereichert, sorgfältig gegen Verunreinigung geschützt und später im Laboratorium gas-chromatographisch analysiert. Erste Daten für atlantische Luftmassen an der Westküste Irlands werden mitgeteilt.
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    Fresenius' Zeitschrift für analytische Chemie 302 (1980), S. 398-401 
    ISSN: 1618-2650
    Keywords: Best. von Wasserstoff in Magnesium ; Chromatographie, Gas ; Kapselmethode
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A new method, the capsule method, has been developed for analyzing hydrogen in magnesium with a standard deviation of about 4%. 1–2 g samples are made with a smooth surface and enclosed in a degassed iron capsule. The surface humidity is removed by a short annealing at 400°C, and the sample is subsequently degassed at 500–620°C in vacuum. The extracted hydrogen is measured by gas chromatography. The commercial magnesium analyzed contained from 0.2 to 8 ppm of hydrogen. The diffusion coefficient of hydrogen was measured to be: D=D 0e−Q/RT; where D 0=9.5 · 10−6 m2/s and Q=46,400 Joule/mole. The results obtained were interpreted as interstitial diffusion of hydrogen in magnesium.
    Notes: Zusammenfassung Zur Analyse von Wasserstoff in Magnesium wurde eine neue Methode, die Kapselmethode, entwickelt, 1–2 g schwere Proben werden mit einer glatten Oberfläche hergestellt und in eine gasfreie Kapsel eingeschlossen. Die Oberflächenfeuchtigkeit wird durch kurzes Anlassen bei 400°C entfernt und die Probe wird danach bei 500–620°C im Vakuum entgast. Der entfernte Wasserstoff wird mit einem Gas-Chromatographen gemessen. Die Standardabweichung beträgt etwa 4%. Das untersuchte technische Magnesium enthält zwischen 0,2 und 8 ppm Wasserstoff. Der gemessene Diffusionskoeffizient für Wasserstoff ist: D=D 0e−Q/RT; D 0=9.5 · 10−6 m2/s und Q= 46400 Joule/Mol. Die erhaltenen Resultate wurden als interstitielle Wasserstoffdiffusion im Magnesium interpretiert.
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    Fresenius' Zeitschrift für analytische Chemie 303 (1980), S. 389-393 
    ISSN: 1618-2650
    Keywords: Best. von Chrom(III), Chrom(VI) in Wasser ; Chromatographie, Gas ; Extraktion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The gas-chromatographic determination of Cr(III) and Cr(VI) in aqueous solution using di(trifluoroethyl)dithiocarbamate as an extracting agent (pH 3) is described. Best results were obtained with a column of OV-25 (3% on Chromosorb HPW, 100–120 mesh, 160–210
    Notes: Zusammenfassung Die Extraktion mit dem Reagens wird bei pH 3 durchgeführt. Als SÄulenmaterial hat sich am besten OV-25 (3% auf Chromosorb HPW, 100–120 mesh, 160–210
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    Fresenius' Zeitschrift für analytische Chemie 304 (1980), S. 337-349 
    ISSN: 1618-2650
    Keywords: Analyse von Biphenylen, polychlorierten in Umweltmaterial ; Chromatographie, Gas ; Glascapillar
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The PCB-pattern of biological environmental samples of different trophic levels (fish, bird, man) and geographic areas (Alps, North Sea, North Atlantic) as seen by high-resolution glass capillary gas chromatography with electron capture detection is presented. The most evident variation of the pattern compared to a best fit simulation by technical mixtures is found for warm blooded species (eggs of birds and human milk). Only one trichloro-, but nine tetrachloro-biphenyls and 55 penta-to octachloro-biphenyls have been identified as PCB-components in biological samples. Compounds with 4,4′-disubstitution degrade very slowly, if at all (1,4-recalcitrance principle). Single component analysis of PCB in marine samples using glass capillary gas chromatography needs the preseparation from the ubiquitous polychloroterpenes (toxaphene, polychlorocamphene) and the DDT-group. Both complex mixtures can be separated successfully by adsorption chromatography on Florisil. Quantitation of PCB as a sum has been done by using recalcitrant diagnostic components and PCB-Clophen A 60 as the reference standard.
    Notes: Zusammenfassung Die Bestimmung der Einzelkomponenten der polychlorierten Biphenyle (PCB) in Umweltproben durch Glascapillar-Gas-Chromatographie auf Methylsilicon- oder Apiezon L-Phasen erfordert eine Vortrennung von den Polychlorterpenen (Toxaphen, Polychlorcamphen) und der DDT-Gruppe. Diese Trennung gelingt durch Adsorptions-Chromatographie auf Florisil. Die PCB-Muster im Fett des phytoplanktonfressenden Seefisches Menhaden (Brevoortia tyrannus) aus dem Nordatlantik, im Rogen der zooplanktonfressenden Salmoniden Seesaibling (Salvelinus alpinus) und Bachforelle (Salmo trutta m. fario) aus Bergseen in Tirol, und in der Leber der Süßwasserdorschart Quappe (Lota lota) aus dem Bodensee werden gezeigt. Die stärksten Veränderungen gegenüber einer aus technischen Gemischen hergestellten Simulationsmischung werden für Warmblütlerproben — Eier von Brandgans (Tadorna tadorna) und Küsten-Seeschwalbe (Sterna paradisea); Humanmilch — gefunden. Neben einem Trichlor- und neun Tetrachlorbiphenylen wurden 55 Pentabis Octachlorbiphenyle nachgewiesen. Komponenten mit einer 4 und/oder 3,5-Substitution in beiden Ringen werden beträchtlich langsamer abgebaut als anders strukturierte Komponenten (1,4-Rekalzitranz-Prinzip). Die Quantifizierung der PCB als Summe erfolgte über schwer abbaubare, signifikante Hauptkomponenten unter Verwendung eines Clophen A 60 PCB-Gemisches als Eichstandard.
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