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Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs

The determination of the alcoholic strength in spirits and liqueurs is required to control the labelling of alcoholic beverages. The reference methodology prescribes a distillation step followed by densimetric measurement. The classic distillation using a Vigreux rectifying column and a West condens...

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Autores principales: Lachenmeier, Dirk W., Plato, Leander, Suessmann, Manuela, Di Carmine, Matthew, Krueger, Bjoern, Kukuck, Armin, Kranz, Markus
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Springer International Publishing 2015
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4684557/
https://www.ncbi.nlm.nih.gov/pubmed/26702372
http://dx.doi.org/10.1186/s40064-015-1574-6
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author Lachenmeier, Dirk W.
Plato, Leander
Suessmann, Manuela
Di Carmine, Matthew
Krueger, Bjoern
Kukuck, Armin
Kranz, Markus
author_facet Lachenmeier, Dirk W.
Plato, Leander
Suessmann, Manuela
Di Carmine, Matthew
Krueger, Bjoern
Kukuck, Armin
Kranz, Markus
author_sort Lachenmeier, Dirk W.
collection PubMed
description The determination of the alcoholic strength in spirits and liqueurs is required to control the labelling of alcoholic beverages. The reference methodology prescribes a distillation step followed by densimetric measurement. The classic distillation using a Vigreux rectifying column and a West condenser is time consuming and error-prone, especially for liqueurs that may have problems with entrainment and charring. For this reason, this methodology suggests the use of an automated steam distillation device as alternative. The novel instrument comprises an increased steam power, a redesigned geometry of the condenser and a larger cooling coil with controllable flow, compared to previously available devices. Method optimization applying D-optimal and central composite designs showed significant influence of sample volume, distillation time and coolant flow, while other investigated parameters such as steam power, receiver volume, or the use of pipettes or flasks for sample measurement did not significantly influence the results. The method validation was conducted using the following settings: steam power 70 %, sample volume 25 mL transferred using pipettes, receiver volume 50 mL, coolant flow 7 L/min, and distillation time as long as possible just below the calibration mark. For four different liqueurs covering the typical range of these products between 15 and 35 % vol, the method showed an adequate precision, with relative standard deviations below 0.4 % (intraday) and below 0.6 % (interday). The absolute standard deviations were between 0.06 % vol and 0.08 % vol (intraday) and between 0.07 % vol and 0.10 % vol (interday). The improved automatic steam distillation devices offer an excellent alternative for sample cleanup of volatiles from complex matrices. A major advantage are the low costs for consumables per analysis (only distilled water is needed). For alcoholic strength determination, the method has become more rugged than before, and there are only few influences that would lead to incomplete distillation. Our validation parameters have shown that the performance of the method corresponds to the data presented for the reference method and we believe that automated steam distillation, can be used for the purpose of labelling control of alcoholic beverages.
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spelling pubmed-46845572015-12-23 Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs Lachenmeier, Dirk W. Plato, Leander Suessmann, Manuela Di Carmine, Matthew Krueger, Bjoern Kukuck, Armin Kranz, Markus Springerplus Methodology The determination of the alcoholic strength in spirits and liqueurs is required to control the labelling of alcoholic beverages. The reference methodology prescribes a distillation step followed by densimetric measurement. The classic distillation using a Vigreux rectifying column and a West condenser is time consuming and error-prone, especially for liqueurs that may have problems with entrainment and charring. For this reason, this methodology suggests the use of an automated steam distillation device as alternative. The novel instrument comprises an increased steam power, a redesigned geometry of the condenser and a larger cooling coil with controllable flow, compared to previously available devices. Method optimization applying D-optimal and central composite designs showed significant influence of sample volume, distillation time and coolant flow, while other investigated parameters such as steam power, receiver volume, or the use of pipettes or flasks for sample measurement did not significantly influence the results. The method validation was conducted using the following settings: steam power 70 %, sample volume 25 mL transferred using pipettes, receiver volume 50 mL, coolant flow 7 L/min, and distillation time as long as possible just below the calibration mark. For four different liqueurs covering the typical range of these products between 15 and 35 % vol, the method showed an adequate precision, with relative standard deviations below 0.4 % (intraday) and below 0.6 % (interday). The absolute standard deviations were between 0.06 % vol and 0.08 % vol (intraday) and between 0.07 % vol and 0.10 % vol (interday). The improved automatic steam distillation devices offer an excellent alternative for sample cleanup of volatiles from complex matrices. A major advantage are the low costs for consumables per analysis (only distilled water is needed). For alcoholic strength determination, the method has become more rugged than before, and there are only few influences that would lead to incomplete distillation. Our validation parameters have shown that the performance of the method corresponds to the data presented for the reference method and we believe that automated steam distillation, can be used for the purpose of labelling control of alcoholic beverages. Springer International Publishing 2015-12-18 /pmc/articles/PMC4684557/ /pubmed/26702372 http://dx.doi.org/10.1186/s40064-015-1574-6 Text en © Lachenmeier et al. 2015 Open AccessThis article is distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made.
spellingShingle Methodology
Lachenmeier, Dirk W.
Plato, Leander
Suessmann, Manuela
Di Carmine, Matthew
Krueger, Bjoern
Kukuck, Armin
Kranz, Markus
Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title_full Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title_fullStr Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title_full_unstemmed Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title_short Improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
title_sort improved automatic steam distillation combined with oscillation-type densimetry for determining alcoholic strength in spirits and liqueurs
topic Methodology
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC4684557/
https://www.ncbi.nlm.nih.gov/pubmed/26702372
http://dx.doi.org/10.1186/s40064-015-1574-6
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