WO2003062818A1 - Method for the spectroscopic analysis of viscose constituents - Google Patents

Method for the spectroscopic analysis of viscose constituents Download PDF

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WO2003062818A1
WO2003062818A1 PCT/AT2003/000016 AT0300016W WO03062818A1 WO 2003062818 A1 WO2003062818 A1 WO 2003062818A1 AT 0300016 W AT0300016 W AT 0300016W WO 03062818 A1 WO03062818 A1 WO 03062818A1
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viscose
determined
calibration
constituents
spectra
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PCT/AT2003/000016
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German (de)
French (fr)
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Thomas Baldinger
Johann Moosbauer
Susanne Jary
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Lenzing Aktiengesellschaft
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/36—Textiles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N21/552—Attenuated total reflection

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  • the present invention relates to a method for the spectroscopic determination of viscose constituents, in particular by infrared spectroscopy.
  • the method is primarily intended to examine viscose spinning solutions spectroscopically.
  • the chemical composition of viscose spinning solutions has a decisive influence on the quality of the viscose fibers. It is particularly important for the spinning process to achieve consistent product quality. It is therefore absolutely necessary to know the chemical composition of the spinning solution and to monitor it in the process.
  • the classic methods for determining the quality parameters of viscose spinning solutions are e.g. in an iodometric determination of the cellulose xanthate (gamma value), an acidometric titration of the ⁇ aOH content, a spectroscopic (UV-VIS) determination of the trithiocarbonate content (TTC) and in a gravimetric determination of the cellulose content. This determination is time-consuming and has been replaced by spectroscopic methods.
  • VIS- ⁇ IR near infrared
  • TTC trithiocarbonate
  • cellulose xanthate cellulose by means of spectroscopic measurements in the VIS- ⁇ IR range, coupled with mathematical methods such as e.g. Multivariate data analysis.
  • infrared spectroscopy is considered an important tool for the analysis of substance mixtures and for process monitoring.
  • the basis was the development of Fourier transform infrared spectrometers (FTIR).
  • FTIR Fourier transform infrared spectrometers
  • ATR attenuated total eflection probe system
  • the described spectroscopic methods for examining viscose spinning solutions have the disadvantage that they require complex sample preparation, since the spinning solutions to be examined have a high viscosity, the measuring cuvette is to be infested with as little bubbles as possible, and the temperature is kept as constant as possible during the measuring process got to. Sample preparation and measurement In addition, it should be possible to complete the test as quickly as possible, since the spinning solutions are chemically sensitive, change quickly and falsify the measurement result.
  • the object of the present invention is to provide an analytical method which does not have the above disadvantages.
  • This object is achieved in a method of the type described at the outset by using ATR technology for the determination.
  • the ATR technique is advantageous for examining the viscose and allows very precise determinations, although the analysis beam is not guided through the sample. This allows easy sample preparation, since only a drop of viscose spinning solution on a high-index medium, e.g. a diamond plate needs to be applied and the sample is recorded in total reflection.
  • a high-index medium e.g. a diamond plate
  • At least one of cellulose, total alkali, sulfur, NaOH, Na 2 CO 3 , Na 2 CS 3 and gamma value can be determined in the sample.
  • a preferred embodiment of the method according to the invention is that the four constituents cellulose, total alkali and sulfur are determined.
  • Another preferred embodiment of the method according to the invention consists in that NaOH, Na 2 CO 3 , Na 2 CS 3 and gamma values are additionally determined.
  • the method according to the invention has the further advantage that the spectroscopic examination in the middle infrared can be carried out with a wavelength in the range between 600 and 4000 cm “1 (MIR range).
  • MIR range 600 and 4000 cm “1
  • This allows a better assignment of the individual absorptions to the atomic groups or molecular residues of the Components to be determined as possible in the near infrared (NCR.)
  • NCR. near infrared
  • mainly harmonics of the molecules are registered, whereby the assignment to the individual components to be determined is not so easy. It is clear to the person skilled in the art that in this If the highly refractive medium used for ATR technology has to be matched to the wavelength range of the measuring light.
  • the parameters or components of interest are determined as precisely as possible using conventional methods and a spectrum is recorded in each case.
  • the distribution of the individual parameter values should, as far as possible, cover the measuring range to be expected, and it is also advantageous if the individual parameters do not vary in parallel (eg no dilutions as “independent” samples).
  • the number of samples required depends, among other things, on the number of samples to be determined Parameters and the reliability of the individual conventional analysis methods.
  • a spectral pre-treatment is selected (e.g. baseline correction, normalization, derivation) or tested empirically.
  • a suitable multivariant calibration program is then used to select a suitable spectral range for the calibration from the parameter vectors and spectra of these samples and to generate a set of factor spectra.
  • Each sample spectrum can be represented by a linear combination of these factor spectra plus a residual error spectrum.
  • the coefficients result in a specific value for each parameter.
  • the optimal number of factor spectra to be used can be determined by minimizing the residual error.
  • Most of the commercially available software packages offer automatic routines for selecting the spectral pretreatment and spectral ranges as well as for determining the optimal number of factor spectra.
  • the parameters of interest (X) are again determined as precisely as possible using conventional methods and a spectrum is recorded in each case; Calculated parameters result from these spectra and the above-mentioned calibration.
  • the comparison with the directly determined parameters again results in a correlation measure (R 2 ) and a standard prediction error, the practice-relevant variables for assessing the quality of the analysis methods.
  • R 2 correlation measure
  • the entire set of the calibrated parameters can be determined in a very short time from a spectrum of an unknown sample recorded in the same way.
  • a set of approx. 400 viscose samples was characterized as completely as possible with regard to the 8 parameters cellulose content, total alkali, sulfur content, NaOH content, Na 2 CO 3 , Na 2 CS 3 , gamma value and ripeness, and an infrared spectrum of between 4,000 and 600 cm "1 added.
  • the table shows satisfactory results for all 7 calibrated parameters (standard prediction error).
  • the maturity of the viscose can also be determined with the method according to the invention, the calibration range [ ⁇ o] being between 8 and 15.

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  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
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Abstract

The invention relates to a method for the spectroscopic analysis of viscose constituents, whereby the ATR technique is used for said analysis.

Description

Verfahren zur spektroskopischen Bestimmung von NiskosebestandteilenMethod for the spectroscopic determination of components of anesthetic
Die vorliegende Erfindung betrifft ein Verfahren zur spektroskopischen Bestimmung von Viskosebestandteilen, insbesondere durch Infrarotspektroskopie. Mit dem Verfahren sollen vor allem Viskose-Spinnlösungen spektroskopisch untersucht werden.The present invention relates to a method for the spectroscopic determination of viscose constituents, in particular by infrared spectroscopy. The method is primarily intended to examine viscose spinning solutions spectroscopically.
Die chemische Zusammensetzung von Viskose-Spinnlösungen hat einen entscheidenden Einfluß auf die Qualität der Viskosefasern. Für den Spinnprozeß ist es insbesondere wichtig, eine gleichbleibende Produktqualität zu erzielen. Es ist deshalb unbedingt notwendig, die chemische Zusammensetzung der Spinnlösung zu kennen und im Prozeß zu überwachen.The chemical composition of viscose spinning solutions has a decisive influence on the quality of the viscose fibers. It is particularly important for the spinning process to achieve consistent product quality. It is therefore absolutely necessary to know the chemical composition of the spinning solution and to monitor it in the process.
Die klassischen Methoden zur Bestimmung der Qualitätsparameter von Viskose- Spinnlösungen bestehen z.B. in einer jodometrischen Bestimmung des Cellulosexanthogenates (gamma-Wert), einer acidometrischen Titration des ΝaOH-Gehaltes, einer spektroskopischen (UV-VIS) Bestimmung des Trithiocarbonat-Gehaltes (TTC) und in einer gravimetrischen Bestimmung des Cellulose-Gehaltes. Diese Bestimmung ist zeitaufwendig und wurde von spektroskopischen Methoden abgelöst.The classic methods for determining the quality parameters of viscose spinning solutions are e.g. in an iodometric determination of the cellulose xanthate (gamma value), an acidometric titration of the ΝaOH content, a spectroscopic (UV-VIS) determination of the trithiocarbonate content (TTC) and in a gravimetric determination of the cellulose content. This determination is time-consuming and has been replaced by spectroscopic methods.
Die simultane Bestimmung der Hauptbestandteile von Viskose-Spinnlösungen im nahen Infrarot (VIS-ΝIR) ist bekannt (siehe z.B. S. Sollinger und M. Noges, J. Νear Infrared Spectrosc. 5, 135-148 (1997)). Gemäß diesem Verfahren gelingt die gleichzeitige Bestimmung der folgenden Viskose-Bestandteile: ΝaOH, Trithiocarbonat (TTC), Cellulosexanthogenat und Cellulose mittels spektroskopischer Messungen im VIS-ΝIR- Bereich, gekoppelt mit mathematischen Methoden , wie z.B. Multivarianten-Datenanalyse.The simultaneous determination of the main components of viscose spinning solutions in the near infrared (VIS-ΝIR) is known (see e.g. S. Sollinger and M. Noges, J. Νear Infrared Spectrosc. 5, 135-148 (1997)). According to this method, the following viscose components can be determined simultaneously: ΝaOH, trithiocarbonate (TTC), cellulose xanthate and cellulose by means of spectroscopic measurements in the VIS-ΝIR range, coupled with mathematical methods such as e.g. Multivariate data analysis.
Ganz allgemein gilt die Infrarotspektroskopie heute als ein bedeutendes Instrument zur Analyse von Stoffgemischen und zur Prozeßüberwachung. Grundlage war die Entwicklung von Fourier-Transform Infrarotspektrometern (FTIR). In Kombination mit einem Attenuated-Total- eflection Meßsondensystem (ATR) hat sich diese Methode zur Untersuchung von schnell ablaufenden chemischen Reaktionen bewährt, wobei dieses System direkt in den Reaktionsraum eingebaut wird.In general, infrared spectroscopy is considered an important tool for the analysis of substance mixtures and for process monitoring. The basis was the development of Fourier transform infrared spectrometers (FTIR). In combination with an attenuated total eflection probe system (ATR), this method has proven itself for the investigation of rapid chemical reactions, whereby this system is built directly into the reaction space.
Die beschriebenen spektroskopischen Methoden zur Untersuchung von Viskose- Spinnlösungen haben aber den Nachteil, dass sie eine aufwendige Probenvorbereitung erfordern, da die zu untersuchenden Spinnlösungen eine hohe Viskosität aufweisen, die Meßküvette möglichst blasenfrei zu befallen ist, und die Temperatur während des Messvorganges möglichst konstant gehalten werden muß. Probenvorbereitung und Messung sollen darüber hinaus möglichst rasch absolviert werden können, da die Spinnlösungen in chemischer Hinsicht empfindlich sind, sich rasch verändern und das Messergebnis verfälschen.However, the described spectroscopic methods for examining viscose spinning solutions have the disadvantage that they require complex sample preparation, since the spinning solutions to be examined have a high viscosity, the measuring cuvette is to be infested with as little bubbles as possible, and the temperature is kept as constant as possible during the measuring process got to. Sample preparation and measurement In addition, it should be possible to complete the test as quickly as possible, since the spinning solutions are chemically sensitive, change quickly and falsify the measurement result.
Die vorliegende Erfindung stellt sich die Aufgabe, ein Analysenverfahren zur Verfügung zu stellen, das die obigen Nachteile nicht aufweist.The object of the present invention is to provide an analytical method which does not have the above disadvantages.
Diese Aufgabe wird bei einem Verfahren der eingangs dargestellten Art dadurch gelöst, dass zur Bestimmung die ATR-Technik eingesetzt wird.This object is achieved in a method of the type described at the outset by using ATR technology for the determination.
Es hat sich gezeigt, dass sich die ATR-Technik vorteilhaft zur Untersuchung der Viskose eignet und sehr genaue Bestimmungen erlaubt, obwohl der Analysenstrahl nicht durch die Probe geleitet wird. Dies gestattet eine einfache Probenvorbereitung, da zur Messung lediglich ein Tropfen Viskose-Spinnlöung auf ein hochbrechendes Medium, z.B. ein Diamantplät chen, aufgebracht zu werden braucht und die Probe in Totalreflexion erfasst wird.It has been shown that the ATR technique is advantageous for examining the viscose and allows very precise determinations, although the analysis beam is not guided through the sample. This allows easy sample preparation, since only a drop of viscose spinning solution on a high-index medium, e.g. a diamond plate needs to be applied and the sample is recorded in total reflection.
Mit dem erfindungsgemäßen Verfahren lässt sich in der Probe mindestens eines von Zellulose, Gesamtalkali, Schwefel, NaOH, Na2CO3, Na2CS3 und gamma-Wert bestimmen.With the method according to the invention, at least one of cellulose, total alkali, sulfur, NaOH, Na 2 CO 3 , Na 2 CS 3 and gamma value can be determined in the sample.
Eine bevorzugte Ausfurhrungsform des erfindungsgemäßen Verfahrens besteht darin, dass die vier Bestandteile Zellulose, Gesamtalkali und Schwefel bestimmt werden.A preferred embodiment of the method according to the invention is that the four constituents cellulose, total alkali and sulfur are determined.
Eine weitere bevorzugte Ausfuhrungsform des erfindungsgemäßen Verfahrens besteht darin, dass noch zusätzlich NaOH, Na2CO3, Na2CS3 und gamma-Wert bestimmt werden.Another preferred embodiment of the method according to the invention consists in that NaOH, Na 2 CO 3 , Na 2 CS 3 and gamma values are additionally determined.
Das erfindungsgemäße Verfahren hat weiters den Vorteil, dass die spektroskopische Untersuchung im mittleren Infrarot mit einer Wellenlänge im Bereich zwischen 600 und 4000 cm"1 (MIR-Bereich) durchgeführt werden kann. Dies erlaubt eine bessere Zuordnung der einzelnen Absorptionen zu den Atomgruppen oder Molekülresten der zu bestimmenden Bestabdteile als dies im nahen Infrarot (NCR.) möglich ist. Im NDR. werden hauptsächlich Obeschwingungen der Moleküle registriert, wobei die Zuordnung zu den einzelnen zu bestimmenden Bestandteilen nicht so leicht möglich ist. Es ist dem Fachmann dabei klar, dass in diesem Fall das zur ATR-Technik eingesetzte, hochbrechende Medium auf den Wellenlängenbereich des Messlichtes abgestimmt werden muß.The method according to the invention has the further advantage that the spectroscopic examination in the middle infrared can be carried out with a wavelength in the range between 600 and 4000 cm "1 (MIR range). This allows a better assignment of the individual absorptions to the atomic groups or molecular residues of the Components to be determined as possible in the near infrared (NCR.) In the NDR. mainly harmonics of the molecules are registered, whereby the assignment to the individual components to be determined is not so easy. It is clear to the person skilled in the art that in this If the highly refractive medium used for ATR technology has to be matched to the wavelength range of the measuring light.
Mit den nachfolgenden Beispielen wird die Erfindung noch näher erläutert. Eichung (Kalibrierung)The invention is explained in more detail with the following examples. Calibration
Von einem genügend großen Satz (A) von Meß-Proben werden die interessierenden Parameter bzw. Bestandteile mittels herkömmlicher Methoden möglichst genau bestimmt und jeweils ein Spektrum aufgenommen. Die Verteilung der einzelnen Parameterwerte soll dabei möglichst den zu erwartenden Meßbereich abdecken, vorteilhaft ist auch, wenn die einzelnen Parameter nicht parallel variieren (z.B. keine Verdünnungen als „unabhängige" Proben). Die erforderliche Zahl von Proben hängt u.a. ab von der Zahl der zu bestimmenden Parameter und der Zuverlässigkeit der einzelnen herkömmlichen Analysenmethoden.From a sufficiently large set (A) of measurement samples, the parameters or components of interest are determined as precisely as possible using conventional methods and a spectrum is recorded in each case. The distribution of the individual parameter values should, as far as possible, cover the measuring range to be expected, and it is also advantageous if the individual parameters do not vary in parallel (eg no dilutions as “independent” samples). The number of samples required depends, among other things, on the number of samples to be determined Parameters and the reliability of the individual conventional analysis methods.
Falls nötig, wird eine Spektrenvorbehandlung gewählt (z.B. Basislinienkorrektur, Norminierung, Ableitung) oder empirisch getestet. Aus den Parametervektoren und Spektren dieser Proben wird nun mithilfe eines geeigneten multivarianten Eichprogramms ein geeigneter Spektralbereich für die Eichung ausgewählt und ein Satz von Faktorspektren erzeugt. Jedes Probenspektrum läßt sich durch eine Linearkombination dieser Faktorspektren plus einem Restfehlerspektrum darstellen. Aus den Koeffizienten ergibt sich für jeden Parameter ein bestimmter Wert. Durch Minimierung des Restfehlers kann die optimale Zahl der zu verwendenden Faktorspektren ermittelt werden. Sowohl für die Wahl der Spektrenvorbehandlung und der Spektralbereiche als auch zur Ermittlung der optimalen Zahl an Faktorspektren bieten die meisten der käuflichen Softwarepakete automatische Routinen an.If necessary, a spectral pre-treatment is selected (e.g. baseline correction, normalization, derivation) or tested empirically. A suitable multivariant calibration program is then used to select a suitable spectral range for the calibration from the parameter vectors and spectra of these samples and to generate a set of factor spectra. Each sample spectrum can be represented by a linear combination of these factor spectra plus a residual error spectrum. The coefficients result in a specific value for each parameter. The optimal number of factor spectra to be used can be determined by minimizing the residual error. Most of the commercially available software packages offer automatic routines for selecting the spectral pretreatment and spectral ranges as well as for determining the optimal number of factor spectra.
In einem nächsten Schritt werden allfällige Ausreißer gesucht und eliminiert (meist ebenfalls programmierte clusteranalytische Routinen in den Softwarepaketen) und mit den verbleibenden Proben die Faktorspektren neu berechnet. Aus den Berechnungen ergibt sich dabei für jeden Parameter ein Korrelationsmaß (R2) und ein Standardeichfehler, ein Maß für die Qualität der Eichung.In a next step, possible outliers are searched for and eliminated (usually also programmed cluster analysis routines in the software packages) and the factor spectra are recalculated with the remaining samples. For each parameter, the calculations result in a correlation measure (R 2 ) and a standard calibration error, a measure of the quality of the calibration.
Validierungvalidation
Von einem weiteren genügend großen Satz (B) von Proben werden wieder die interessierenden Parameter (X) mittels herkömmlicher Methoden möglichst genau bestimmt und jeweils ein Spektrum aufgenommen; aus diesen Spektren und der o.a. Eichung ergeben sich errechnete Parameter. Der Vergleich mit den direkt bestimmten Parametern ergibt wieder ein Korrelationsmaß (R2) und einen Standardvorhersagefehler, die praxisrelevanten Größen zur Beurteilung der Qualität der Analysemethoden. Sind diese Werte in einem durch die Anforderungen vorgegebenen Rahmen, so kann aus einem in gleicher Weise aufgenommenen Spektrum einer unbekannten Probe der gesamte Satz der geeichten Parameter in kürzester Zeit bestimmt werden.From another sufficiently large set (B) of samples, the parameters of interest (X) are again determined as precisely as possible using conventional methods and a spectrum is recorded in each case; Calculated parameters result from these spectra and the above-mentioned calibration. The comparison with the directly determined parameters again results in a correlation measure (R 2 ) and a standard prediction error, the practice-relevant variables for assessing the quality of the analysis methods. Are these values in one through the requirements given the framework, the entire set of the calibrated parameters can be determined in a very short time from a spectrum of an unknown sample recorded in the same way.
Bestimmungenprovisions
Ein Satz von ca. 400 Viskoseproben wurde bezüglich der 8 Parameter Zellulosegehalt, Gesamtalkali, Schwefelgehalt, NaOH-Gehalt, Na2CO3, Na2CS3, Gammawert und Spinnreife, möglichst vollständig charakterisiert und von sämtlichen Proben ein Infrarotspektrum im Bereich zwischen 4.000 und 600 cm"1 aufgenommen.A set of approx. 400 viscose samples was characterized as completely as possible with regard to the 8 parameters cellulose content, total alkali, sulfur content, NaOH content, Na 2 CO 3 , Na 2 CS 3 , gamma value and ripeness, and an infrared spectrum of between 4,000 and 600 cm "1 added.
Zur Aufnahme der Spektren diente ein FT-ER Spektrometer der Fa. Bruker (DFS 66) und eine Diamant Horizontal- ATR-Einheit mit hermetisch abgedichtetem Strahlengang; die Auflösung betrug 2 cm"1.An FT-ER spectrometer from Bruker (DFS 66) and a diamond horizontal ATR unit with hermetically sealed beam path were used to record the spectra; the resolution was 2 cm "1 .
Die Auswertungen (Spektrenvorbehandlung und multivariante Kalibration nach einem PLS- Algorithmus) mit der Software „Opus" und dem Zusatzpaket „Opus Quant 2" der Fa. Bruker bzw. dem PLS Paket zur GRAMS Software der Fa. Galactic (PLS = „partial least Squares").The evaluations (spectrum pretreatment and multivariate calibration according to a PLS algorithm) with the software "Opus" and the additional package "Opus Quant 2" from Bruker or the PLS package for GRAMS software from Galactic (PLS = "partial least squares ").
Ein Teil der Datensätze (ca. 60, alle vollständige charakterisiert) wurde für die spätere Validierung reserviert, mit den übrigen ca. 340 Datensätzen wurde eine Multivariante Eichung nach einem PLS Algorithmus durchgeführt, indem zunächst für jeden Parameter die optimale Spektrenvorbehandlung und der geeignete Spektralbereich ermittelt wurden (Bereich zwischen 2.000 und 675 cm"1). Im nächsten Schritt wurden die Faktorspektren errechnet und aus einer Auftragung Zahl der verwendeten Farbaktivspektren gegen Restfehler die für jeden Parameter optimale Zahl der zu verwendenden Faktorspektren (= „ Rank") bestimmt.Some of the data sets (approx. 60, all fully characterized) were reserved for later validation, with the remaining approx. 340 data sets, a multivariate calibration was carried out according to a PLS algorithm by first determining the optimal spectra pretreatment and the suitable spectral range for each parameter (range between 2,000 and 675 cm "1 ). In the next step the factor spectra were calculated and the optimal number of factor spectra to be used for each parameter (=" rank ") was determined from a plot of the number of active color spectra against residual errors.
Mit diesem „Rank" wurde nun eine erste Eichung aufgestellt und sämtliche Proben einem Ausreißertest unterzogen. Dann wurde unter Eliminierung der Ausreißer (es verblieben bis zu 314 Proben) die Eichung wiederholt und die statistischen Parameter Standardeichfehler und Regressionskoeffizienten R2 der Eichung ermittelt.With this "rank", a first calibration was set up and all samples were subjected to an outlier test. Then, with the outliers eliminated (up to 314 samples remained), the calibration was repeated and the statistical parameters standard calibration error and regression coefficient R 2 of the calibration were determined.
In einem letzten Schritt wurden aus den IR-Spektren der reservierten Validierproben (als quasi Unbekannte) die kalibrierten Parameter errechnet und diese mit den direkt gemessenen Werten statistisch verglichen (Standardvorhersagefehler und Regressionskoeffizient R2 der Validierung). Die Ergebnisse sind in der nachfolgenden Tabelle ersichtlich:In a last step, the calibrated parameters were calculated from the IR spectra of the reserved validation samples (as quasi unknowns) and these were compared statistically with the directly measured values (standard prediction error and regression coefficient R 2 of the validation). The results are shown in the table below:
Figure imgf000006_0001
Figure imgf000006_0001
Die Tabelle zeigt für alle 7 geeichten Parameter befriedigende Ergebnisse (Standardvorhersagefehler). Als weiterer Parameter läßt sich mit dem erfindungsgemäßen Verfahren auch die Reife der Viskose bestimmten, wobei der Eichbereich [Ηo] zwischen 8 und 15 liegt. The table shows satisfactory results for all 7 calibrated parameters (standard prediction error). As a further parameter, the maturity of the viscose can also be determined with the method according to the invention, the calibration range [Ηo] being between 8 and 15.

Claims

Patentansprüche : Claims:
1. Verfahren zur spektroskopischen Bestimmung von Visko'sebestandteilen, dadurch gekennzeichnet, dass zur Bestimmung die ATR-Technik eingesetzt wird.1. A method for the spectroscopic determination of viscous' sebestandteilen, characterized in that is used to determine the ATR technique.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass mindestens eines von Zellulose, Gesamtalkali, Schwefel, NaOH, Na2CO , Na2CS3 und gamma-Wert bestimmt werden.2. The method according to claim 1, characterized in that at least one of cellulose, total alkali, sulfur, NaOH, Na 2 CO, Na 2 CS 3 and gamma value are determined.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, dass die vier Bestandteile Zellulose, Gesamtalkali, Schwefel und gamma-Wert bestimmt werden.3. The method according to claim 2, characterized in that the four components cellulose, total alkali, sulfur and gamma value are determined.
4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass noch zusätzlich NaOH, Na2CO3, Na2CS3 und gamma-Wert bestimmt werden.4. The method according to claim 3, characterized in that additionally NaOH, Na 2 CO 3 , Na 2 CS 3 and gamma value are determined.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die Bestimmung im mittleren Infrarot mit einer Wellenlänge im Bereich zwischen 600 und 4000 cm"1 (MER-Bereich) durchgeführt wird. 5. The method according to any one of claims 1 to 4, characterized in that the determination in the middle infrared is carried out with a wavelength in the range between 600 and 4000 cm "1 (MER range).
PCT/AT2003/000016 2002-01-23 2003-01-17 Method for the spectroscopic analysis of viscose constituents WO2003062818A1 (en)

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CN108585229A (en) * 2018-01-22 2018-09-28 中国科学院生态环境研究中心 A kind of drinking water softening composite drug and its application

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Publication number Priority date Publication date Assignee Title
CN108585229A (en) * 2018-01-22 2018-09-28 中国科学院生态环境研究中心 A kind of drinking water softening composite drug and its application

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