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  • 1985-1989  (915)
  • 1965-1969
  • 1945-1949
  • 1890-1899
  • 1820-1829
  • 1800-1809
  • 1985  (915)
  • Analytical Chemistry and Spectroscopy  (901)
  • Insulin
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  • 1985-1989  (915)
  • 1965-1969
  • 1945-1949
  • 1890-1899
  • 1820-1829
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Year
  • 1
    ISSN: 1432-0428
    Keywords: Insulin ; free insulin assay ; insulin antibodies ; radioimmunoassay
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Plasma insulin concentrations of insulin-treated diabetic patients must be measured after removal of insulin antibodies, usually by precipitation with polyethylene glycol (PEG). Details of the procedure vary between laboratories; commonly, frozen plasma is thawed and incubated at 37 °C to restore a presumed equilibrium between free and antibody bound insulin before extraction. The present study was designed to investigate methodological factors that could affect the measured free insulin concentration. In normal subjects PEG extraction of globulins did not disturb measurement of insulin concentrations, whether carried out after incubation for 2 h at 37 °C, or storage at -20 °C, in either order. Freezing or incubation of PEG extracts of plasma from insulin-treated patients also failed to disturb the measured concentrations of free insulin. When plasma from patients was incubated for 2 h after storage, a marked scatter (51–272%) of measured results occurred when compared to bedside extraction. This problem was not overcome by buffering with HEPES or storage at a lower temperature (-40 °C). Incubation at 0 °C also severely disturbed the apparent concentrations. Incubation of plasma before extraction and freezing also disturbed the measured result, a problem not corrected by maintaining near physiological pH. Total insulin concentrations measured on acid extracts were not disturbed by any of these manoeuvres. The temperature of centrifugation of blood at the time of venepuncture did not influence the result. Furthermore, when insulin concentrations were rising or falling similar percentage changes were seen over a 30-min incubation of plasma before extraction on the day of venepuncture, suggesting that equilibrium between free and bound insulin is maintained in vivo. We suggest that, for accurate estimation of free insulin concentrations in insulin-treated diabetic patients, immediate centrifugation of blood and extraction of insulin antibodies is mandatory.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-0428
    Keywords: Insulin ; myocardial contraction ; heart rate ; diabetes mellitus
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary To evaluate the acute effects of intravenous insulin on myocardial contractility and heart rate, echocardiography was performed in 12 healthy subjects and continuous heart rate recording in 11 healthy subjects before and during eugly-caemic insulin and glucose infusion. The rate of insulin infusion was 0.5–1.0 mU·kg−1·min−1. Serum insulin concentration was increased from 14.1±5.5 (mean±SD) to a plateau level of 91.3±22.8 mU/l. Left ventricular end-diastolic diameter, ejection phase indices and the heart rate remained at basal levels during the intervention. Thus moderate hyperinsulinaemia, induced by euglycaemic insulin and glucose infusion, has no inotropic or chronotropic effects in healthy supine subjects.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Diabetologia 28 (1985), S. 295-301 
    ISSN: 1432-0428
    Keywords: Insulin ; insulin resistance ; obesity ; exercise ; glucose metabolism ; glycogen synthase ; fructose 2–6 bisphosphate ; skeletal muscle ; goldthioglucose obese mice ; hypertrophy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The effect of work-induced hypertrophy (without any concomitant change in circulating parameters) on skeletal muscle metabolism was studied in lean mice and in goldthioglucose obese-mice. Soleus muscle was functionally overloaded in one leg by tenotomy of gastrocnemius muscle 4 days before muscle isolation, muscle in the other leg being used as control. Basal deoxyglucose uptake and glycolysis were markedly increased in overloaded muscles compared with control muscles, together with a ten-fold increase in fructose 2–6 bisphosphate content. In the presence of maximally effective insulin concentrations, deoxyglucose uptake and glycolysis were identical in overloaded and control muscles of lean mice, while the effects of overload and insulin were partly additive in muscles of goldthioglucose-obese mice. The sensitivity to insulin and insulin binding to muscles were not modified in overloaded muscles. Insulin-stimulated glycogenogenesis was decreased by about 50% probably due to a lower amount of glycogen synthase in overloaded than in control muscles. Thus, in muscles of goldthioglucose-obese mice work-induced hypertrophy increased the response to maximal insulin concentrations without modifying the altered insulin sensitivity and decreased insulin binding.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1432-0428
    Keywords: Insulin ; proinsulin ; insulin-like growth factors ; multiplication-stimulating activity ; insulin effects on growth ; embryogenesis ; chick embryo
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The teratogenic effect of insulin in early vertebrate embryos is controversial and the mechanisms involved are unknown. We studied the effects of pharmacological doses of insulin in chick embryos during the period of differentiation. We compared the effects of insulin with two proinsulins, desoctapeptide-insulin and multiplication-stimulating activity, peptides that have little insulin-like metabolic activity while they have significant growth effects. Chick embryos at 46 h of development were injected with the different peptides. At 96 h the mortality and abnormal growth elicited by the peptides were dose-dependent. Considering the indices of lethality (LD50) and affected embryos (ED50) as 100% for insulin, proinsulin was 59–66% as potent as insulin, desoctapeptide-insulin 2–6% and multiplication-stimulating activity 176–204%. In the surviving embryos, insulin (5 μg, decreased DNA, RNA and protein content by 49%, 40% and 48% respectively compared with controls. The effects of insulin were not corrected by simultaneous glucose injections. These data suggest that insulin, at pharmacological doses, interferes with embryo development through a non-metabolic pathway, probably via a growth-type receptor.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Diabetologia 28 (1985), S. 458-463 
    ISSN: 1432-0428
    Keywords: Insulin ; insulin stability ; insulin delivery systems
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Exposure of insulin solutions to elevated temperatures for prolonged periods of time will inevitably lead to chemical modifications of the hormon. Contact with different materials in dosing devices, other design-related factors and motion appear to be chemically more detrimental than storage in glass vials at the same temperature. An in vitro test, designed to mimick the in vivo situation, consisted of delivery of insulin at 37 °C while the device was constantly moved on a shaking apparatus. Insulin quality was assessed using high performance liquid chromatography. A polyethylenepoly-propylene glycol-stabilized neutral human insulin solution (HOE 21 PH) was used. A single insulin derivative is the major modification product which, after passage of the complete infusion system, amounts to up to 10%. The biological potency of the derivative is indistinguishable from native insulin. Delivery of acidic insulin under implant conditions, leads to extensive and multiple insulin derivatization, even though the biological potency remains 95% after 4 weeks.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    Experimental brain research 61 (1985), S. 87-90 
    ISSN: 1432-1106
    Keywords: Prostaglandins ; Brain ; Insulin ; 2-deoxy glucose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Prostaglandin synthesis in the brain has been suggested as a component in the control mechanism of the cerebral circulation. During insulininduced hypoglycemia there is a significant increase in local cerebral blood flow in various brain regions, however, regional loss of autoregulation occurs under these conditions. In the present study the regional distribution of PGE2, TXB2 (the stable metabolite of thromboxane) and 6-keto-PGF1α (the stable metabolite of prostacyclin) was determined in rat brain following decapitation. Three groups of rats were treated with either saline, insulin or 2-deoxyglucose and their brains were rapidly removed one hour later. Samples from the cortex hypothalamus, hippocampus, striatum, nucleus accumbens and cerebellum were assayed by RIA for the content of PGE2, TXB2 and 6-keto-PGF1α The levels of all three compounds in control rats were the lowest in the striatum and cerebellum, while in the cortex and hippocampus their levels were 4–6 times higher. Insulin had selective effect on the post decapitation levels of prostanoids. It increased PGE2 in the n. accumbens and TXB2 in the hippocampus, and reduced 6-keto-PGF1α and TXB2 in the cortex. 2-DG reduced all PGs in the cortex and 6-keto-PGF1α in the hypothalamus and hippocampus. The results demonstrate that discrete brain areas have a differential capacity to accumulate PGs following decapitation. This capacity is selectively affected by insulin and 2-DG.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Springer
    European journal of pediatrics 143 (1985), S. 183-186 
    ISSN: 1432-1076
    Keywords: C-peptide ; Growth hormone deficiency ; Obesity ; Insulin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The daily excretion of C-peptide in the urine was measured in 105 healthy infants and children from birth to 14 years of age. For technical reasons no studies were performed from 1–3 years of age. The excretion of C-peptide showed a close positive correlation with age and weight. The relationship with weight was already apparent in the 1st days of life. The C-peptide/weight and the C-peptide/creatinine ratios were constant throughout most of childhood with the exception of the age range of 1 month-1 year when the C-peptide/creatinine was significantly higher. In obese children the C-peptide/weight and C-peptide/creatinine ratios were similar to those found in children with normal weight. In growth hormone deficiency these ratios were low and increased during the 1st week of growth hormone therapy. It is concluded that urinary C-peptide is a reliable indicator of integrated insulin production and gives new information about insulin secretion in various conditions.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    Pflügers Archiv 405 (1985), S. S33 
    ISSN: 1432-2013
    Keywords: Sodium transport ; Epithelial transport ; Transport regulation ; Frog skin ; Oxytocin ; Ouabain ; Insulin ; Neurohypophysial hormones
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract 1. Application of transepithelial square voltage pulses to the frog skin leads to responses in the transepithelial current and intracellular potential which include transient components. Determinations at 600 ms allow for meaningful estimates of basolateral membrane responses to transport modifiers. 2. Oxytocin produced a large and sustained increase in the amiloride-inhibitable short circuit current (I m) which was accompanied by a large increase of both apical and basolateral membrane conductance (g a andg b, respectively). WhileI m andg a increased nearly simultaneously,g b started to increase several minutes after the increase in the two other parameters. 3. Insulin also increasedI m,g a andg b. As with oxytocin, the increases inI m andg a often preceded the changes ing b. 4. Ouabain reducedI m andg a. The effects ofg b were more complex, since sometimes the inhibition ofI m was first accompanied by an increase followed by a decrease while in other instances only minor changes in conductance could be observed. 5. The currently available information regarding the control of cytoplasmic [Ca2+] and the effects of Ca2+ on cell membrane properties are used to construct a model in which changes in cytoplasmic [Ca2+] account for the observed behavior of the basolateral membrane.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Naunyn-Schmiedeberg's archives of pharmacology 328 (1985), S. 253-257 
    ISSN: 1432-1912
    Keywords: Clonidine ; Insulin ; Glucose ; Hyper-responsiveness ; Rat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Effect of chronic clonidine treatment on the response to glucose of rat pancreatic B-cells was investigated. Clonidine treatment was carried out for 10 days by dissolving the drug into drinking water at a concentration of 10 μg/ml. Control rats were given drug-free tap water. Serum insulin responses to glucose (750 mg/kg, i. v.) of clonidinetreated rats were much smaller than those of control rats. However, after 1 day's withdrawal of clonidine, the rise in the serum insulin level induced by glucose was approximately 2-fold larger in clonidine-treated rats as compared to that in control rats. Since clonidine treatment decreased body weight of the rat by 10%–20% in 10 days, the same experiments were carried out with rats whose body weight loss was made comparable to that of clonidine-treated rats by restricting food for 10 days. Then, some animals of the group thus treated had food-restriction discontinued for 1 day. In both of the above two groups, no increment in glucoseinduced rise in serum insulin level was observed. Islets of Langerhans isolated from clonidine-treated rats showed pronounced insulin releasing capacity in response to glucose. Insulin content per islet of the clonidine-treated rat was slightly larger than that of control rat. These results indicate that the enhancement of serum insulin response to glucose following clonidine treatment is mainly attributable to the hyper-responsiveness developed in the pancreatic B-cells.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Cell & tissue research 239 (1985), S. 537-545 
    ISSN: 1432-0878
    Keywords: Mouse ; Pancreas, endocrine ; Insulin ; Acid phosphatase ; Lysosomes ; Crinophagy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The relation between qualitative and quantitative glucose-dependent alterations of lysosomes in pancreatic islets and the function of the islets was studied. Isolated islets of the mouse were maintained in tissue culture for one week in either 28, 5.5 or 3.3 mmol/l glucose. Insulin biosynthesis, insulin secretion and insulin content of the cultured islets were determined. After culture, the islets were subjected to acid phosphatase cytochemistry and examined by electron microscopy and ultrastructural morphometry. Islets cultured in 28 mmol/l glucose both produced and secreted insulin rapidly. Such islets seemed, however, unable to maintain more than small amounts of granule-stored insulin. Islets cultured at the lower concentrations of glucose displayed a reduced insulin secretion, which apparently resulted in considerable amounts of intracellularly stored insulin. In all cultured islets different types of lysosomes, identified by their acid phosphatase reactivity, could be seen. Dense bodies, i.e., lysosomes characterized by a homogeneous, very fine, particulate content of high density, seemed to predominate at all concentrations of glucose. It is suggested that, in the islets, the dense bodies correspond morphologically to primary lysosomes. Other types of lysosomes with inclusions of various kinds, which were frequent at the two lower concentrations of glucose, may correspond to secondary lysosomes. Morphometry revealed differences between the size distributions of lysosomes in the three experimental groups. Thus, the average lysosomal size was inversely proportional to the concentration of glucose in the culture medium. However, the numerical density of lysosomes was greatest at the highest glucose concentration. The observation of secondary lysosomes, containing material resembling secretory granules, suggests that the increased size and lowered number of lysosomes in islets cultured at low glucose concentrations may depend on a crinophagic process. Such a process, together with insulin biosynthesis and insulin secretion, may be of physiological importance for control of the secretory granule content within the pancreatic B-cell.
    Type of Medium: Electronic Resource
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  • 11
    Electronic Resource
    Electronic Resource
    Springer
    European journal of applied physiology 54 (1985), S. 420-426 
    ISSN: 1439-6327
    Keywords: Glycemia ; Glucose infusion ; Diet ; Free fatty acids ; Insulin ; Exercise in humans
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Extant literature dealing with metabolic and hormonal adaptations to exercise following carbohydrate (CHO) reduced diets is not sufficiently precise to allow researchers to partial out the effects of reduced blood glucose levels from other general effects produced by low CHO diets. In order to shed light on this issue, a study was conducted to examine the effects of a 24-h CHO-poor diet on substrate and endocrine responses during prolonged (75 min; 60% $$\dot V_{O_{2max} } $$ ) glucose-infused leg exercise. Eight subjects exercised on a cycle ergometer in the two following conditions: 1) after a normal diet (CHON), and 2) after a 24-h low CHO diet (CHOL). In both conditions, glucose was constantly infused intravenously (2.2 mg · kg−1 · min−1) from the 10th to the 75th min of exercise in relatively small amounts (10.4±0.8 g). No significant differences in blood glucose concentrations were found between the two conditions at rest and during exercise although a significant increase (p〈0.01) in glucose level was observed in both conditions after 40 min of exercise. The CHOL as compared to the CHON condition, was associated with significantly (p〈0.05) lower resting concentrations of insulin, muscle glycogen (8.7 vs 10.6 g · kg−1), and triacylglycerol, and greater concentrations of Β-hydroxybutyrate (0.5 vs 0.2 mmol · L−1), and free fatty acids. During exercise, the CHOL condition as compared to the CHON condition, was associated with significantly (p〈0.05) lower insulin and R values, as well as greater free fatty acid (from min 20 to 60) and epinephrine (min 60 to 75) concentrations. Norepinephrine and glucagon concentrations also showed a net tendency (p〈0.06) to be higher in the CHOL condition. There were no significant differences at rest and during exercise in blood lactate and cortisol concentrations between the two conditions. These results demonstrate that blood glucose is not the sole determinant of the metabolic and hormonal responses during prolonged exercise following a low CHO intake and indicate that other factors may be involved in the regulatory mechanism.
    Type of Medium: Electronic Resource
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  • 12
    ISSN: 1439-6327
    Keywords: Glucose storage ; Insulin ; Exercise-training ; Athletes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The present study was designed to evaluate the contribution of the exercise-induced increment in glucose storage to the increased insulin sensitivity characterizing endurance athletes. Plasma glucose and insulin were measured during an oral glucose tolerance test (OGTT) in six endurance athletes. Glucose storage and lipid oxidation during this test were also determined using indirect calorimetry. These measurements were compared to those obtained in five non-trained subjects who were tested before and during the three days following a 90-min cycle ergometer exercise performed at 69% of their $$\dot V_{{\text{O}}_{{\text{2max}}} }$$ . As expected, preexercise values of non-trained subjects revealed a much higher insulin response to glucose, and a lower glucose storage and lipid oxidation compared to results obtained in endurance trained individuals. Glucose tolerance was comparable in both groups. The morning following the exercise test, i. e. about 16 h after exercise, glucose storage was significantly increased in non-trained subjects to a level similar to that found in trained subjects. Surprisingly, this was accompanied by higher values of glucose during the OGTT without significant changes in insulinaemia. This impairment in glucose homeostasis was transitory since glucose tolerance had returned to control level on day 2 after exercise. At that time, the increase in glucose storage was less pronounced than in day 1. On day 3 after exercise, glucose and insulin responses to glucose were similar to preexercise values. These results indicate that the increase in glucose storage by acute exercise is not systematically associated with an improved glucose homeostasis, suggesting that other adaptive mechanisms also contribute to the improvement of insulin sensitivity in endurance athletes.
    Type of Medium: Electronic Resource
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  • 13
    Electronic Resource
    Electronic Resource
    Springer
    European journal of applied physiology 54 (1985), S. 337-342 
    ISSN: 1439-6327
    Keywords: Exercise ; Anaerobic ; Aerobic ; Cortisol ; Glucagon ; Insulin ; Lactate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Five normal men, aged 20–30 years, participated in three types of exercise (I, II, III) of equal duration (20 min) and total external work output (120–180 kJ) separated by ten days of rest. Exercises consisted of seven sets of squats with barbells on the shoulders (I; Maximal Power Output $$\dot W$$ max=600−900 W), continuous cycling at 50 rev · min−1 (II; $$\dot W$$ max=100−150 W) and seven bouts of intermittent cycling at 70 rev · min−1 (III; $$\dot W$$ max=300−450 W). Plasma cortisol, glucagon and lactate increased significantly (P〈0.05) during the exercise and recovery periods of the anaerobic, intermittent exercise (I and III) but not in the continuous, aerobic exercise (II). No consistent significant changes were found in plasma glucose. Plasma insulin levels decreased only during exercise II. The highest increase in cortisol and glucagon was not associated with the highest $$\dot V_E $$ , $$\dot V_{O_2 } $$ , $$\dot W$$ max or HR; however it was associated with the anaerobic component of exercise (lactic acid). It is suggested that in exercises of equal duration and total external work output, the continuous, aerobic exercise (II) led to lowest levels of glucogenic hormones.
    Type of Medium: Electronic Resource
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  • 14
    Electronic Resource
    Electronic Resource
    Springer
    Clinical rheumatology 4 (1985), S. 294-300 
    ISSN: 1434-9949
    Keywords: Insulin ; Hyperostosis ; DISH ; New Bone Formation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The tendency of patients with DISH towards obesity or an adult onset of diabetes has been reflected in marked hyperinsulinaemia following glucose challenge. It is hypothesized that insulin at prolonged and high physiologic levels promotes new bone growth, particularly in the entheseal regions. These areas are also subject to various mechanical forces. The resulting new bone produces the radiological changes which characterise DISH.
    Type of Medium: Electronic Resource
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 224-229 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Pharmacokinetics ; Quantitation in human serum ; Antihypertensive agents ; Ebrantil ; Urapidil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The antihypertensive agent urapidil (Ebrantil Byk-Gulden, Konstanz) can be reliably quantitated with three metabolites in human serum using high performance liquid chromatography. Serum is alkalinized and extracted with ethyl acetate. The organic phase is back-extracted with diluted acid. An aliquot is sampled automatically and chromatographed in an optimized combination of mobile and stationary phase. UV-detection at 273 nm allows a quantitation limit of 5 ng/ml for all analytes. Precise handling of exact volumes facilitates external calibration. The coefficient of variation for spiked samples is less than 5% within and less than 7% between studies. Application of the method to experimental and clinical pharmacokinetic studies of urapidil is illustrated.
    Additional Material: 4 Ill.
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 256-258 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Non-aqueous ion exchange ; Abietanoic diterpenoids ; Coleons, royleanones ; Quinone methides, hydroxyquinones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the HPLC separation of moderately acidic, dehydrated, and multi-oxygenated diterpenoids, compounds which hitherto could not be handled by HPLC. It is based on chemically bonded silica strong cation exchangers in the protonated form, using organic solvents of the full polarity range as eluents. Thus a stable and easy-to-regenerate substitute for buffered silica gel is obtained.
    Additional Material: 4 Ill.
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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 320-320 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 332-336 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Packed columns ; Two-dimensional system ; Multidimensional system ; Deans switching ; Cold trap ; Reinjection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The construction and evaluation of an interface for two-dimensional gas chromatography is described. The interface consists of commercially available components and is attachable to available gas chromatographs without any major modifications. The interface has been constructed so as to permit “heartcutting” as well as solute band concentration. Trapping is performed in a simple cold trap of fused silica. Flow switching is accomplished by Deans switching. Factors of the over-all chromatographic performance are examined.
    Additional Material: 4 Ill.
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  • 19
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 347-355 
    ISSN: 0935-6304
    Keywords: Simulation of chromatograms ; Data processing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A digital chromatogram simulator has been used to evaluate the performance of data handling systems. The simulator can synthesize chromatograms with any desired shape from a library of peaks based on real peak shapes. Once generated, the chromatograms can be reproduced exactly any number of times.The algorithms used in data handling systems have a significant effect on the results they produce. An object of this work was to examine how well the true size of a peak was reported when the peak was detected overlapping with other peaks. A series of experiments was therefore performed in which peaks were overlapped by different amounts and in different situations. The reported results from the data systems were compared with the results which would have been reported had the peaks been fully resolved. A significant difference was found between the overlap results and the fully resolved results, which did not have a linear relationship with the parameters tested.The chromatogram simulator was found to be a powerful tool in assessing the performance of the data systems. It offers a valuable means of evaluating the quality of the results produced by these systems.
    Additional Material: 16 Ill.
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 369-369 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 366-367 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Quantitative analysis ; Metallic complexes ; Diethyldithiocarbomates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 22
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 385-387 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Column switching ; Fourier transform infrared spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A dual oven gas chromatograph incorporating a micro, mechanical switching valve has been interfaced to an FTIR spectrometer. With this system, each oven can be operated with independent temperature control. Complete choice of the columns' type and capacity gives flexibility in the separation prior to spectroscopic evaluation. An application which demonstrates some of the advantages of column switching in GC/FTIR is presented. Minor sample components have been successfully analyzed by heart-cutting the appropriate section of the separation from a high to a low capacity column. In this way, the dynamic range of the technique is effectively increased while an efficient chromatographic inlet to the FTIR is maintained.
    Additional Material: 4 Ill.
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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 400-403 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns, FSOT ; Steroid profiling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The accuracy and reproducibility of steroid and steroid conjugate determinations using capillary GC are evaluated. It is possible to analyze many unconjugated steroids, steroid sulfates, and some steroid glucuronides simultaneously, simply by using group fractionation based on successive hydrolysis and solvent extraction steps. However, a reliable determination of corticosteroid glucuronides can only be obtained after previous isolation of the glucuronides as a group, with ion exchange chromatography. In complex chromatograms, the combined use of nitrogen specific detection and flame ionization detection facilitates peak identification.
    Additional Material: 1 Ill.
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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 415-422 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillaries ; High-temperature phases ; Triglyceride analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of triglycerides on FSOT columns coated with a phenylmethylsilicone gum opens up new perspectives in fat and oil characterization. On phenylmethylsilicone, besides a “carbon number” or CN separation, the triglycerides are also separated according to the different combinations of saturated and unsaturated fatty acids in the triglycerides.
    Additional Material: 20 Ill.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 436-439 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Large-volume injection onto capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A modification of a packed GC injector to a capillary injector is presented using a simple device which is connected to the GC column by an adsorption-free connector. It permits injections of large sample volumes up to 500 μl hexane solutions on normal 0.3 mm i.d. capillary columns. No special requirements for the stationary phase are necessary. Involatile residues remain inside the device which can be exchanged easily. High performance of separation and quantification is achieved.
    Additional Material: 5 Ill.
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  • 26
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 456-458 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica and glass capillary columns ; Helium ionization detector ; Trace gas analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capability of the helium ionization detector (HID) to operate in connection with capillary columns for trace gas analyses has been evaluated. Two different capillary columns were considered: a PLOT fused silica column with molecular sleve and a thick film WCOT glass column with PS-255. The determination of trace impurities in gases can be achieved with evident advantages over classical adsorption columns, even using a split injection system. Direct on-column injections also have been investigated with promising results.
    Additional Material: 7 Ill.
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  • 27
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Split-splitless injection ; Drinking water treatment ; Helogenated hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this paper we report a way to evaluate the removal of volatile halogenated hydrocarbons formed after break-point chlorination in the Arno river raw water at the Mantignano Utility, Florence, Italy, following dechlorination by hydrogen peroxide. The removal evaluation is performed by GC-ECD on fused silica capillary columns with split-splitless injection on n-pentane extracts and by other analytical techniques such as UV254 absorption, TOC and TOX. Both laboratory and pilot plant data on Arno river raw water are reported and discussed.
    Additional Material: 5 Ill.
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  • 28
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 267-269 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Organic geochemistry ; Thermodesorption/cold trap injection ; Petroleum hydrocarbons in sedimentary rocks ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 29
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 30
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 283-289 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Microbial mutagenicity ; Solvent refined coal ; Creosote oils ; Polyaromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical composition of a commercially available creosote was compared to a direct coal liquefaction product, i.e., solvent refined coal-II fuel oil blend (SRC-II FOB) using high resolution gas chromatography (HRGC). In addition, hydrogenated products of these materials were studied. Samples were fractionated by chemical class on neutral alumina. Those fractions previously shown to be the most mutagenic and tumorigenic in laboratory bioassays of coal-derived materials were analyzed and compared by HRGC and gas chromatography/mass spectrometry (GC/MS). Individual components were tentatively identified and quantitated. Although similar chemical components were present in the creosote and SRC-II FOB fractions studied, the creosotes had higher concentrations of heavy molecular weight materials and a lower ratio of alkylated to parent polycyclic aromatic compounds than the coal liquefaction products. The creosote samples also had a significantly higher concentration of components which eluted in the polycyclic aromatic hydrocarbon (PAH) chemical class fraction. Amino-substituted PAH were present in both nonhydrogenated coal liquid and creosote materials. The creosote and SRC-II FOB crudes and nitrogen-containing polycyclic aromatic compound (NPAC) chemical class fractions expressed similar microbial mutagenicity. Based on chemical analysis data, the predicted tumorigenic potency of the creosote in laboratory bioassay systems would be equivalent to or greater than the SRC-II FOB.
    Additional Material: 2 Ill.
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  • 31
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    Journal of High Resolution Chromatography 8 (1985), S. 308-308 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 32
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    Journal of High Resolution Chromatography 8 (1985), S. 627-628 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 33
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Elution profiles ; Sorption effect ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The elution profiles observed with overloaded capillary columns are well described by a four-parameter theoretical model derived from the basic mass balance equations which relies on an expansion of the partition isotherm to the second term and takes the sorption effect into account. The reliability of the model is demonstrated by the fact that the peak leaning coefficient obtained from a least squares fit of the model to the experimental peak is in good agreement with that obtained from the variation of peak height with retention time at peak maximum. The coefficeint of apparent axial dispersion is independent of sample size and can be used to characterize the plate height at zero concentration of an overloaded capillary column.
    Additional Material: 4 Ill.
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  • 34
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    Journal of High Resolution Chromatography 8 (1985), S. 607-610 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Temperature programmed retention indices ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Direct conversion of isothermal to temperature programmed indices is not possible. In this work it is shown that linear temperature programmed retention indices can only be calculated from isothermal retention data if the temperature dependence of both the distribution coefficients and the column dead time are taken into account.Procedures are described which allow calculation of retention temperatures and from these, accurate programmed retention indices. Within certain limits the initial oven temperature and programming rate can be chosen freely. The prerequisite for this calculation is the availability of reliable isothermal retention data (retention times, retention factors, relative retention times, or retention indices) at two different temperatures for one column.The use of compiled isothermal retention indices at two different temperatures for the calculation of retention temperatures and thus temperature programmed indices is demonstrated. For the column for which programmed retention indices have to be determined, the isothermal retention times of the n-alkanes and the column dead time as a function of temperature have to be known in addition to the compiled data for a given stationary phase.Once the programmed retention indices have been calculated for a given column the concept allows the calculation of temperature programmed indices for columns with different specifications. The characteristics which can be varied are: column length, column inner diameter, phase-ratio, initial oven temperature, and programming rate.
    Additional Material: 2 Tab.
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  • 35
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    Journal of High Resolution Chromatography 8 (1985) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 36
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    Journal of High Resolution Chromatography 8 (1985), S. 664-672 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; CP-MAS NMR ; Deactivation methods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of deactivating a fused silica surface by silylation with 1,1,3,3-tetraphenyl-1,3-dimethylilazane (TPDMDS), triphenylsilylamine (TPSA), and octamethylcyclotetrasiloxane (D4) and by polydimethylsiloxane degradation (PSD) is studied. Rehydrated, dried, and deactivated Cab-O-Sil M5 samples are used as model materials for 29Si CP-MAS NMR analysis.At about 350 °C, TPDMDS yelds mainly diphenylmethylsiloxysilane, dimethyldisiloxysilane, and triphenylsiloxysilane groups. TPSA yields phenyltrisiloxysilane, diphenyldisiloxysilane, and triphenylsiloxysilane groups. At 400°C, the products formed initially are eventually replaced by methyltrisiloxysilane or phenyltrisiloxysilane groups, while a substantial number of silanol groups still remains. The possible consequences for wettability are discussed.D4 reacts with Cab-O-Sil even at 200°C, but a large number of silanol groups remains. This number decreases gradually at higher temperatures and becomes negligible above 400°C. The formation of methyltrisiloxysilane groups, which starts at 425°C, is predominant at 490°C.
    Additional Material: 9 Ill.
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  • 37
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    Journal of High Resolution Chromatography 8 (1985), S. 691-691 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 38
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 696-697 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Trapping volatiles ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 39
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    Journal of High Resolution Chromatography 8 (1985), S. 704-704 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 40
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 362-363 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Normal and reversed phase ; Pentafluorobenzamidopropyl silica gel ; Donor-acceptor complexes ; Aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 41
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 42
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    Journal of High Resolution Chromatography 8 (1985), S. 391-394 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Crosslinking ; Enantiomeric separation ; Polymeric chiral phases ; Polysiloxane skeleton ; Polyethylene glycol skeleton ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Crosslinking experiments for immobilization of the well-known chiral stationary phases XE 60-L-valine-(S)- and XE 60-L-valine-(R)-α-phenylethylamide within capillary columns have been successfully carried out. Crosslinking was also obtained with mixtures of the chiral compound acrylyl-L-valine-(S)-α-phenylethylamide and the polyethylene glycol Carbowax 20M. Immobilization of 75% to 90% was achieved by crosslinking the polymeric chiral phases, but sometimes up to 100% of these phases remained within the columns after the usual subsequent solvent treatment. The crosslinking of Carbowax 20M with acrylyl-L-valine-(S)-α-phenylethylamide led to a chiral polymer of a polarity different from that of the common siloxane type chiral phases.
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  • 43
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    Journal of High Resolution Chromatography 8 (1985), S. 407-411 
    ISSN: 0935-6304
    Keywords: Electrophoresis ; Electroosmosis ; Borosilicate, fused silica, and teflon capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Separation efficiency in capillary zone electrophoresis was examined as a function of capillary length and diameter as well as solute concentration for a borosilicate glass capillary/phosphate buffer system. Electroosmotic flow coefficients in borosilicate, fused silica, and teflon capillaries were measured over the useful operating pH range of 3-8 at constant applied power (0.333 W). Sample introduction by a simple, low-dispersion electromigration method was found to be a reliable procedure for solute quantitation.
    Additional Material: 4 Ill.
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  • 44
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Simulated distillation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characterization of heavy petroleum fractions is essential for the design and improvement of cracking plants converting heavy feedstock into valuable “white” products. Conventional simulated distillation methods using packed columns are unsuitable for this purposes, being limited to boiling points up to about 600°C. The method presented is able to cover a boiling points interval ranging from about 150°C up to around 800°C. It employs a short, nonpolar, highly thermostable capillary column routinely operated at temperatures around 430°C. The analytical system is based on a high temperature versions of a fully automatic, capillary dedicated gas chromatograph. The experimental data demonstrate that cold on-column injection is the sole sampling system suitable for such heavy compounds. The conversion of the retention times into boiling points, based on the use of low molecular weight polyethylenes, is extremely reliable, as demonstrated by the excellent retention time reproducibilities. The lower part (up to 550-600°C TBP) of the boiling point distribution curves of heavy petroleum fractions obtained on capillary columns fits well with the corresponding distribution curves based on packed column data. For the petroleum fractions fully eluted from the column the quantitative results obtained either using internal standards or by direct processing of the elution curves are in excellent agreement (less than 0.3 weight% differences). The method has been applied to the determination of the true boiling points corresponding to short path vacuum distillation (DISTACT) cut points over 300°C.
    Additional Material: 18 Ill.
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  • 45
    ISSN: 0935-6304
    Keywords: Coupled HPLC-GC ; Retention gap ; Partially concurrent solvent evaporation ; Gasoline ; Group-type separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two-dimensional chromatography of gasoline by on-line coupled HPLC-HRGC, as described in this paper, allows separate GC analysis of paraffins and aromatics. The GC system contains a retention gap of only 10 m length for introducing HPLC fractions of 100 μl volume. This becomes possible through evaporation of part of the solvent during introduction of the HPLC eluent. This “partially concurrent solvent evaporation” technique allows transfer of large volumes of HPLC eluent into relatively short retention gaps, maintaining the full efficiency of the solvent effects in reconcentrating the bands of the early eluted solutes.
    Additional Material: 7 Ill.
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  • 46
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    Journal of High Resolution Chromatography 8 (1985), S. 625-626 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 47
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    Journal of High Resolution Chromatography 8 (1985), S. 632-650 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 8 Ill.
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  • 48
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    Journal of High Resolution Chromatography 8 (1985), S. 659-664 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Packed micro columns ; Breakthrough gradients ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new approach is described for micro-HPLC for generating nearly linear gradients in the 40 to 550 μl volume range. These “linear” gradients have a straight line middle portion with a gentle curved onset of the gradient andd rapid attainment of the final 100% composition. Such “breakthrough-gradients” are produced by the interface between weak and strong eluent when a small (3 × 0.46 cm) packed “gradient-generator” column is switched abruptly from weak to strong eluent. The model system described here, without an analytical column, shows gradients from weak eluent (water) to strong eluent (modele with water plus acetone) using a 12-port high pressure valve to 1) vent the “flush” eluent, and simultaneously 2) begin the gradient and 3) make the sample injection.The volume of the gradient can be changed in two ways. If the breakthrough-generator is packed with very large (300 to 1600 μm nonporous particles, the gradient volume is nearly independent of the flush flow rate. The flush flow is used to quickly move the breakthrough-interface to the head of the micro-HPLC column. However, the gradient volume can be increased by using larger solid particles in the gradient-generator column because of increased eddy diffusion. If the gradient-generator is packed with porous particles (75-150 μm), the gradient volume can be changed over a broad range by simply changing the flush flow rate. This simple control over the gradient volume is due to the increased mass transfer of weak eluent out of the porous particles into the strong eluent at higher flush flows.The breakthrough-interface gradient-generator column approach provides the following advantages for micro-HPLC: - Gradient volumes can be readily varied over the micro-HPLC range 40-550 μl.- Gradient are linear with smooth and rapid onset of intial and final concentrations.- Gradient are produced inexpensively with a single high-pressure precision pump.- Gradient can be automated with a timer and single 12-port valve that provides both column regeneration and sample injection.
    Additional Material: 9 Ill.
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  • 49
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    Journal of High Resolution Chromatography 8 (1985), S. 693-694 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography, GLC ; Capillary columns ; Static coating ; Monitoring device ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 50
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    Journal of High Resolution Chromatography 8 (1985), S. 19-22 
    ISSN: 0935-6304
    Keywords: Thin layer chromatography, HPTLC ; Anticircular mode ; Cosmetic emulsions ; Jojoba wax ester quantitation ; Triglyceride quantitation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cosmetic creams were analyzed for their content of jojoba wax and shea fat using anticircular HPTLC, a fast, precise, and reliable method. After optimization of the solvent system (petrol ether/diethyl ether) for the separation of jojoba wax and shea fat, the spots were visualized with phosphomolybdic acid by the “dip-in” technique, subsequently heated, and finally recorded by scanning with a densitometer at 546 nm. Results showed that one particular concentration range gives an optimum correlation between calibration curves and sample evaluations.
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  • 51
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    Journal of High Resolution Chromatography 8 (1985), S. 30-31 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass packed columns ; Glass capillary columns ; Interference ; Medicinal plants ; DDT-residues ; PCB-residues ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 52
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    Journal of High Resolution Chromatography 8 (1985) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 53
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Electron capture detection ; Octachlorobenzo-p-dioxin ; Heptachlorobenzo-p-dioxin ; Polychlorinated dibenzofurans ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the analysis of contaminated building dust samples and surface swab samples for octachlorodibenzo-p-dioxin (OCDD) and heptachlorodibenzo-p-dioxins (HpCDDs). The samples were analyzed by fused silica capillary GC combined with electron capture detection. Analysis was preceded by a short HPLC cleanup step designed to remove polychlorinated biphenyls (PCBs) and other compounds that might interfere. The method was found to work successfully on surface swab and dust samples known to contain PCBs, OCDD, and HpCDDs. The overall recovery of the analysis procedure for OCDD was found to be approximately 80%. The detection limit for the method was sample dependent, but for one typical set of surface swab samples was 0.2 μg/m2 of OCDD.
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  • 54
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    Journal of High Resolution Chromatography 8 (1985), S. 102-103 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 55
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    Journal of High Resolution Chromatography 8 (1985), S. 112-118 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Packed absorption columns ; Thick liquid phase films ; Natural, refinery, and reactor gas analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic system consisting of one multiport valve, two (hot-wire and flame-ionization) detectors and two analytical columns (one thick-film capillary and one packed adsorption column) is used for the analysis of gas samples containing a number of inorganic compounds (hydrogen, argon, oxygen, nitrogen, carbon monoxide, and carbon dioxide) and organic compounds. Examples include samples containing hydrocarbons up to n-nonane and benzene and toluene. The system also permits the analysis of more complicated samples containing, for example, alcohols, in addition to hydrocarbons.
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  • 56
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    Journal of High Resolution Chromatography 8 (1985), S. 143-143 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Chromosorb 102 ; C1—C6 Hydrocarbons ; CO2 and H2S ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 57
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    Journal of High Resolution Chromatography 8 (1985), S. 148-149 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Slurry packing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 58
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    Journal of High Resolution Chromatography 8 (1985), S. 154-155 
    ISSN: 0935-6304
    Keywords: High performance ion-exchange chromatography ; Recovery of proteins ; TSKgel DEAE-5PW and SP-5PW ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Tab.
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  • 59
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    Journal of High Resolution Chromatography 8 (1985), S. 158-162 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 60
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    Journal of High Resolution Chromatography 8 (1985), S. 78-79 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Gel filtration of proteins ; Protein-support interaction ; TSKgel G3000SW ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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    Journal of High Resolution Chromatography 8 (1985), S. 88-89 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; High speed HPLC ; Profiling ; Prostaglandins ; 2,3-Dinor-6-keto-prostaglandin F1α ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 62
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    Journal of High Resolution Chromatography 8 (1985), S. 230-242 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography, GC ; Fused silica wall-coated open tubular columns ; Dual column analysis ; Retention indices ; “Delta I-pt” effect ; Shale-derived fuels ; Petroleum-derived fuels ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Overlapping chromatographic peaks of components from different hydrocarbon classes can be disengaged by exploiting their shifts in relative retention behavior with changes in linear rates of programmed temperature. Many co-eluting species in complex chromatograms of shale- and petroleum-derived jet fuels can be resolved without varying stationary phase, column length, or initial column temperature.Retention indices were simultaneously determined on two bonded-phase, fused silica capillary columns of slightly different polarities at three different linear programmed temperature rates. For certain hydrocarbon types, no change in index values was observed with an alteration in programming rate. However, the indices of other hydrocarbon classes shifted uniformly with programmed temperature rates on each of the two stationary phases. When applied, this phenomenon could help resolve coeluting members of different or even the same hydrocarbon type and elucidate their probable structure. The overall precision of the retention indices, i.e., the mean standard deviation at the 95% confidence levels, was less than ±0.13 for either column at any of the three programming rates. Since the above technique is automated, it could also be a useful screening tool to search for specific hydrocarbons in a myriad of unknown components of a complex hydrocarbon mixture.
    Additional Material: 6 Ill.
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  • 63
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    Journal of High Resolution Chromatography 8 (1985), S. 169-169 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 64
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    Journal of High Resolution Chromatography 8 (1985), S. 193-195 
    ISSN: 0935-6304
    Keywords: Atmospheric residue ; Capilary columns ; Gas chromatography ; Pyrex ; Simulated distillation (SIMDIS) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 65
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    Journal of High Resolution Chromatography 8 (1985), S. 200-208 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 66
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    Journal of High Resolution Chromatography 8 (1985), S. 301-302 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Kovats retention indices ; Monocyclic terpene alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 67
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    Journal of High Resolution Chromatography 8 (1985), S. 304-305 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Chiral-stationary phase ; 1-Nitrobenzo[a]pyrene ; 3-Nitrobenzo[a]pyrene ; 1-Nitro-7,8,9,10-tetrahydrobenzo[a]pyrene ; 3-Nitro-7,8,9,10-tetrahydrobenzo[a]pyrene ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 68
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    Journal of High Resolution Chromatography 8 (1985), S. 469-474 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Packed capillary columns ; On-Line multidimensional chromatography ; Gas chromatography, GC ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The introduction of selected fractions from a liquid chromatograph into a gas chromatograph has been described; however, analyses were performed by off-line experiments requiring collection and reinjection of the separate fractions or by on-line procedures where disadvantageously, only a fraction of the separated peak or a well resolved component in a mixture could be introduced into a gas chromatograph. This disadvantage is overcome by the apparatus and method described in this paper, which utilizes a multidimensional chromatography system employing a high efficiency, packed capillary LC column coupled on-line to a capillary gas chromatograph.The liquid chromatograph (so designed) can act as a highly efficient clean-up or chemical class fractionation step prior to introduction into the gas chromatograph, significantly reducing sample preparation times in many applications. Thus minor components in a complex matrix can be determined without prior sample clean-up, an example of which is the determination of polychlorinated biphenyls in a complex hydrocarbon matrix.
    Additional Material: 12 Ill.
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  • 69
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    Journal of High Resolution Chromatography 8 (1985), S. 480-484 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Supercritical fluid chromatography, SFC ; Packed columns ; Fused silica and glass capillary columns ; Liquid crystal stationary phases ; Polyaromatic hydrocarbons ; Insect sex pheromones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel monomeric and polymeric liquid crystalline compounds were synthesized as stationary phases for gas chromatography (GC) and supercritical fluid chromatography (SFC). Monomeric liquid crystalline compounds were used in packed column gas chromatography for the separation of isomeric aromatic compounds and insect sex pheromones. Liquid crystalline polymers possess long nematic ranges and a uniform coating was easily achieved in glass and fused silica capillaries, which could stand temperatures up to 250°C in GC and pressures of 200 MPa at 160°C in SFC. The columns provide excellent selectivity and resolution for fused ring aromatic compounds such as the isomers anthracene and phenanthrene or triphenylene and chrysene.
    Additional Material: 7 Ill.
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  • 70
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    Journal of High Resolution Chromatography 8 (1985), S. 510-513 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Curie point pyrolysis ; Polystyrenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pyrolysis-capillary GC has been applied to the analysis of chemically derivatized polystyrenes. The reproducibility of the method and the influence of instrumentation has been discussed.
    Additional Material: 3 Ill.
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  • 71
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    Journal of High Resolution Chromatography 8 (1985), S. 531-534 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Open tubular columns ; Post column derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The practical applications of open tubes in liquid chromatography as separation columns and as reactors for post column derivatization are discussed. With present technology, the potential efficiency of open tubular columns cannot be fully exploited. As reactors in post column derivatization, these tubes offer many advantages if knitted or stitched to enhance radial mass transfer. The application of open tubes with diameters between 0.12 mm and 0.6 mm as reactors in the selective and sensitive detection of amino acids is demonstrated.
    Additional Material: 5 Ill.
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  • 72
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    Journal of High Resolution Chromatography 8 (1985), S. 551-557 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Thick films ; Polyphenylmethylsiloxane films ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The efficiency of FSOT columns coated with thick films of polyphenylmethylsiloxane was theoretically and experimentally compared to thin apolar and medium polar coatings and to thick apolar coatings. Experimental hū and TZū plots clearly demonstrate the enormous loss in chromatographic efficiency of thick films of medium polar siloxane stationary phases. The low diffusion coefficient in the liquid phaese is responsible for this behavior. The influence of the temperature and the nature of the solute on the efficiency was also studied.
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  • 73
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    Journal of High Resolution Chromatography 8 (1985), S. 547-550 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Amino acid profiles ; Yeasts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Saccharomyces strains uvarum, montuliensis, bayanus, capensis and florentinus were grown in liquid media prepared from a 1% aqueous glucose solution to which 0.05% of ammonium sulfate or urea were added as the only nitrogen supply. The amino acids exuded during incubation were isolated by cation exchange and derivatized as the corresponding N,O-heptafluorobutyryl isopropyl esters. Separation was achieved on a highly deactivated glass capillary column coated with OV-101. A characteristic amino acid profile was obtained for each of the species studied, allowing the construction of a chemotaxonomic tree, on the basis of present or absent acids.
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  • 74
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    Journal of High Resolution Chromatography 8 (1985), S. 566-571 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; Cooled needle split injection ; Temperature programmed (PTV) injection ; On-column injection ; Automation ; Quantitation ; Sampling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sampling techniques for practical quantitative capillary GC have to meet certain principal requirements. Both the absolute and the relative peak areas (e.g. column loads) must be reproducible with high precision and at high accuracy; discrimination of certain constituents according to their volatility should not take place on sampling. On the basis of systematic studies, the three most reliable sampling techniques used for GC analyses with the aim of achieving precise and accurate quantitative data proved to be the following: On-column, injection, splitless PTV injection, and an optimized version of split sampling called “cooled needle split” injection. The on-column technique can be optimized by using precolumns with wider internal diameters and without stationary phase coatings to overcome the problems of large liquid sampling volumes and for automation. The PTV technique should only be used in the splitless mode because discrimination cannot be suppressed completely with the split mode. All three of the techniques can be operated automatically, either to avoid “human interference”, i.e. to improve precision or for unattended operation to save man-power.
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  • 75
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    Journal of High Resolution Chromatography 8 (1985), S. 672-677 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Slurry-packed capillary columns ; Fluorimetric photodiode array detector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A high sensitivity, multichannel fluorescence detector with small volume has been developed for capillary column liquid chromatography. Using an intensified linear photodiode array to monitor fluorescence emission, several important mixtures exhibiting native fluorescence have been examined following high efficiency separation on a capillary column. By correlating mass spectral, fluorescence spectral, and retention time data, information of potential utility in the structural elucidation of aromatic molecules contained in complex mixtures can be obtained. Examples include the separation and spectral examination of the polyaromatic compounds in samples of both biological and environmental interest.
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  • 76
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    Journal of High Resolution Chromatography 8 (1985), S. 690-690 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 77
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    Journal of High Resolution Chromatography 8 (1985), S. 705-708 
    ISSN: 0935-6304
    Keywords: Capillary columns ; Glass ; Fused silica ; Acid leaching ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A study was carried out on the effects of acid leaching of capillary column wall materials. Leaching experiments with glass and fused silica were performed under static and dynamic conditions; moreover, the influence of the temperature was investigated. The amount of water released during different temperature programs was measured with a microwave plasma detector. Different leaching conditions and column wall materials cause considerable variations in water production. These results probably explain the disappointing deactivation efficiency obtained for fused silica and dynamically leached soft glass if HMDS is used. Evidence was found for an increase in surface area due to acid leaching.
    Additional Material: 3 Ill.
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  • 78
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    Journal of High Resolution Chromatography 8 (1985), S. 726-733 
    ISSN: 0935-6304
    Keywords: Coupled HPLC-capillary GC ; Retention gap ; Concurrent solvent evaporation ; Extraction techniques ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: HPLC fractions involving eluents of low to intermediate polarity can be introduced into capillary GC using the retention gap technique. Partial or complete solvent evaporation during sample introduction reduces the length of, or almost eliminates, the zone in the column inlet (retention gap) flooded by the introduced liquid, allowing introduction of larger HPLC fractions and/or use of shorter retention gaps. The corresponding techniques are reviewed. The retention gap technique is poorly suited for water-containing HPLC eluents (reversed phase HPLC) and fails completely if HPLC eluents contain, e.g., buffer salts. Various techniques for extracting such HPLC eluents are considered, preference being given to extraction into GC stationary phases from where solutes are thermally desorbed into the GC separation column. Limiting factors are diffusion of solutes within the liquid phase to be extracted and retention power of the extraction tubes.
    Additional Material: 6 Ill.
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  • 79
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Automatic analysis of volatiles ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system for automatic analysis of volatile compounds by purge-and-cold-trapping/capillary gas chromatography is described. It is suitable for analysis of volatile compounds in a wide variety of samples, such as water, food products and environmental samples. Possibilities and limitations of the system are evaluated in relation to several parameters. The efficiency of different types of cryogenic trap (open tubular, coated, packed) is also investigated; it depends on purge-flow rate, temperature of trapping, and total purge volume. Examples of the analysis of volatile compounds in foods and water are given.
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  • 80
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    Journal of High Resolution Chromatography 8 (1985), S. 804-806 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Stationary-phase focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 81
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    Journal of High Resolution Chromatography 8 (1985), S. 824-828 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Aromatic hydrocarbons ; Multidimensional chromatography ; Normal and reversed phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A two-dimensional chromatographic separation is described which makes use of the unusual properties of supercritical carbon dioxide mobile phase. This solvent has the property of giving a separation of polycyclic aromatic hydrocarbons (PAH) on amine-bonded columns similar to that given by usual normal-phase solvents, and on octadecylsilane-bonded columns similar to that given by usual reversed-phase solvents.Packed columns were used, arranged so that they could be switched in or out of the solvent flow. Polycyclic aromatic hydrocarbon mixtures isolated from coal tar were fractionated according to number of aromatic carbon atoms on an amine-bonded column, and these fractions were trapped on an octadecysilane-bonded column. They were subsequently eluted according to the polarity of the individual compounds. Separations from fractions containing 16 and 18 aromatic carbon atoms are shown.
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  • 82
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    Journal of High Resolution Chromatography 8 (1985), S. 838-842 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, HPTLC ; Elution characteristics ; Temperature effect ; Solvent polarity effect ; Polar lipids ; Boric acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 83
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    Journal of High Resolution Chromatography 8 (1985), S. 852-853 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Gas sampling ; Gas analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 84
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    Journal of High Resolution Chromatography 8 (1985), S. 860-862 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Solvent peaks ; Mixed eluents ; UV-visualization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 85
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    Journal of High Resolution Chromatography 8 (1985), S. 426-431 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns, fused silica ; Ultra-narrow bore columns ; Increased residence time ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The resolution of the diastereoisomers of norpristane, pristane, and phytane was studied as a function of the column internal diameter and/or the residence time of the compounds in the column. Increasing the residence time in the column by operating the column at a lower temperature program rate enhances the resolution more than reducing the internal diameter of the column. Practical experience with ultra narrow bore columns is also presented.
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  • 86
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    Journal of High Resolution Chromatography 8 (1985), S. 440-443 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Capillary column, fused silica ; EI-MS/CI-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to facilitate the gas chromatographic determination of butyric as well as other short chain fatty acids, triglycerides containing these fatty acids were transbutylated and transpentylated to give FABES (fatty acid butyl esters) and FAPES (fatty acid pentyl esters), respectively. This method allows the molecular weight of the compounds to be increased while their polarity is decreased. Short chain esters elute sufficiently separated from the solvent; due to the decreased polarity, elution of long chain fatty acids is only slightly retarded compared to the corresponding methyl esters. Quantitative evaluation over a large series of injections proved the linearity of correction factors in both cases, FABES and FAPES, with a slight deviation for 16:0 and 18:0, respectively. Structural characterization was performed by GC/MS. It was shown that there are characterstic fragmentations for FABES as well as for FAPES. The El-mass spectra give structural information about the alcohol and acid moieties, the ester molecule and the Cl-spectra indicate the molecular weight. The absence of abundant highly characteristic peaks in the spectra of these esters makes the detection of FABES or FAPES in complex mixtures more difficult than the detection of FAMES with their very characteristic ions at m/z 74 and 87.
    Additional Material: 4 Ill.
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  • 87
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    Journal of High Resolution Chromatography 8 (1985), S. 709-714 
    ISSN: 0935-6304
    Keywords: Deactivation ; Capillary columns ; Silylation ; HPLC-silica ; Surface group concentration ; Pore alterations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-temperature silylation (HTS) used for the deactivation of capillary columns was studied on the silica commonly used in HPLC to gain a better insight into this process. LiChrosorb Si 100 was silylated with disilazanes at different temperatures and the materials obtained were compared in terms of organic and silanol group surface concentration, IR reflection spectra, HPLC behavior, and pore distribution parameters. Applying diphenyltetramethyldisilazane, the volatile reaction products were monitored during the HTS process. With increasing silylation temperature up to 400°C the silanol surface concentration is reduced to a very small level independent of the organic group concentration which exhibits a broad maximum depending upon substituents and temperature. Up to 350°C triorganosiloxy groups prevail as bonded organic groups. It could be proved that HTS is accompanied by pore alterations of the silica matrix. Arguments proposed by different authors in explaining HTS effects are discussed.
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  • 88
    ISSN: 0935-6304
    Keywords: Gas chromatography-mass spectrometry ; Capillary columns ; Stationary phases ; Silicones ; Thermal degradation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability of capillary columns for gas chromatography is often limited by stationary phase degradation at elevated temperatures. In order to achieve a better understanding of column thermostability, column bleed products have been analyzed qualitatively by gas chromatography-mass spectrometry (GC-MS). Three silicone stationary phases were studied: SE-52, SE-54, and OV-1701. Each of these was immobilized in the columns. The proportion of cyclics containing diphenyl in column bleed from SE-52 reflected to a large extent the composition of the polymer, while for SE-54 the proportion of such cyclics was unexpectedly high. The polar moiety of OV-1701, the cyanopropyl(phenyl)siloxy unit, was found to exert a highly destabilizing effect on the polymer, and the thermal degradation products consisted mainly of cyclosiloxanes containing this unit.
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  • 89
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    Journal of High Resolution Chromatography 8 (1985), S. 741-747 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Cyanopropylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for surface deactivation and modification of fused silica capillary columns with a cyanopropyl-containing reagent. The deactivation procedure involved a dehydrocondensation reaction between a bis(cyanopropyl)methylhydropolysiloxane reagent and surface silanol groups at an optimum temperature of only 250°C. Actual critical surface tension measurements were made using the capillary rise method. Excellent deactivation for acidic and basic compounds at the low ng level, and wettability for nonpolar and polar polysiloxane stationary phases were obtained. A procedure was developed to remove acidic impurities that are present in polar stationary phases.
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  • 90
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    Journal of High Resolution Chromatography 8 (1985), S. 831-837 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Characterization of antacida ; Gastric juice ; Bile acids ; Lysolecithin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Work-up procedures and HPLC separation systems for determination of taurocholic, glycocholic, chenodeoxycholic, and cholic acids and lysolecithin in artificial and natural gastric juice are described. These compounds are used for testing the binding capacity of antacida to the individual analytes. Work-up is simple, no extraction or filtration being required. The optimized combinations of stationary and mobile phases allow selective and sensitive determination of the respective bile acids in gastric juice. For optimization, the capacity factors of two related bile acids were evaluated for numerous commercial stationary phases. The mechanism of retention is different for free and conjugated bile acids. Special aspects of routine analysis are discussed.
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  • 91
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Electron impact mass spectrometry ; Retention data ; Nitrofluoranthenes ; Nitropyrenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 92
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    Journal of High Resolution Chromatography 8 (1985), S. 42-44 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Immobilization ; 60Co gamma radiation ; Polyethylene glycol-type phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 93
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    Journal of High Resolution Chromatography 8 (1985), S. 50-56 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 94
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    Journal of High Resolution Chromatography 8 (1985), S. 77-78 
    ISSN: 0935-6304
    Keywords: Gas liquid chromatography, GLC ; Capillary columns ; Polytetrafluoroethylene joint ; Solvent effect inlet ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 95
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 80-81 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Trifluoropropyl silicone capillary columns ; Ketoesters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 96
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 90-92 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Liquid crystal stationary phases ; Shape parameter ; Monomethylbenz[a]anthracenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
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  • 97
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 32-33 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass and fused silica capillary columns ; Coating time and efficiency ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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  • 98
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 34-36 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Injecting liquid samples ; Septumless sample injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 99
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 39-41 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Mass detector ; Carbohydrates ; Heavy petroleum distillates ; Hormonal steroids ; Nonionic surfactants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 100
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 44-45 
    ISSN: 0935-6304
    Keywords: Thin-layer chromatography, TLC ; TLC bonded phases ; 3-Aminopropyltriethoxysilane-treated plates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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