Sie sind auf Seite 1von 5

Food Chemistry 213 (2016) 529533

Contents lists available at ScienceDirect

Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Analytical Methods

Determination of total sulfur concentrations in different types of


vinegars using high resolution flame molecular absorption spectrometry
Nil Ozbek , Suleyman Akman
Department of Chemistry, Faculty of Arts and Sciences, Istanbul Technical University, 34469 Maslak, Istanbul, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: Total sulfur concentrations in vinegars were determined using molecular absorption of carbon monosul-
Received 3 July 2015 fide (CS) determined with a high-resolution continuum source flame atomic absorption spectrometer.
Received in revised form 29 June 2016 The molecular absorption of CS was measured at 258.056 nm in an airacetylene flame. Due to non-
Accepted 3 July 2016
spectral interference, as well as the different sensitivities to some sulfur compounds, all sulfur species
Available online 5 July 2016
were oxidized to sulfate using a HNO3 and H2O2 mixture and the analyte addition technique was applied
for quantification. The limit of detection (LOD) and limit of quantification (LOQ) were 11.6 and
Keywords:
38.6 mg L 1, respectively. The concentrations of sulfur in various vinegars ranged from 6LOD to
Carbon monosulfide
Sulfur
163.6 mg L 1.
Vinegar 2016 Elsevier Ltd. All rights reserved.
High-resolution continuum source
molecular absorption spectrometry

1. Introduction bactericide and antiseptic characteristics (Quirs, Herrero, Garca,


& Daz, 2012).
Vinegar is an acidic liquid that is produced by fermentation of Sulfur can cause allergic reactions, leading to anaphylaxis, or
wine (or, strictly speaking, ethanol) or fruit pulps and juices with respiratory reactions, such as asthma (Metcalfe, Sampson, &
the help of bacteria. It consists mainly of acetic acid, water and Simon, 2009). Because of its negative health effects, the addition
other trace chemicals to give flavor and taste (Nakayama, 1959). of sulfur as a preservative is authorized according to defined stan-
Vinegar is commonly used as a condiment, a preservative, an dards. According to the US Environmental Protection Agency (US
antiseptic and a cleaning agent. Annual vinegar production in Tur- EPA), sulfur dioxide between 50 and 100 mg L 1 is allowed in grape
key is more than 35,000 tonnes and increases year-by-year. Grape juice and wine vinegar (International for the USDA National
vinegar is the most commonly used in Turkey as well as globally. Organic Program ICF, 2011; U.S. EPA, 2007). According to EU Regu-
Generally, grapes are treated with sulfur dioxide during produc- lation (EC) No. 1333/2008, the maximum should be expressed as
tion and transportation to prevent mold and decay. When these SO2 content of not more than 10 mg kg 1 or 10 mg L 1 (Council
grapes are used for vinegar, sulfur compounds can still be present. of the European Union, 2011). In Turkey, the maximum allowable
In addition, sulfur compounds, mainly sodium metabisulfite (Na2- sulfur dioxide concentration, as a preservative in vinegar set by
S2O5), are added to vinegars as preservatives for their antibacterial regulation, is 170 mg L 1 (Republic of Turkey Ministry of Food
and antioxidant properties. In an acidic matrix, sodium metabisul- Agriculture & Livestock, 2004).
fite releases sulfur oxides. In vinegars, sulfur can be present as free There are several methods for the determination of sulfur, such
sulfur dioxide in the forms of H2SO3, HSO3 and SO23 as well as as flow injection turbidimetry (Brienza, Sartini, Neto, & Zagatto,
bound to compounds, such as phenols, acetaldehyde and sugar. 1995), inductively coupled plasma-atomic emission spectrometry
Sulfate also occurs in vinegars through oxidation of free sulfur (Santelli, Oliveira, de Carvalho, Bezerra, & Freire, 2008), inductively
dioxide as well as from other sources. The sum of free and bound coupled plasma-mass spectrometry (Heilmann, Boulyga, &
SO2 makes up total SO2. The bound SO2 is inactive and has no Heumann, 2004), X-ray fluorescence spectrometry (Kendall,
antimicrobial efficacy whereas free sulfur dioxide has antioxidant, Schoenwald, Siao, & Hendricks, 1995) and chromatography (Bak,
Schuhmann, & Jansen, 1993). Each method has advantages and dis-
advantages with respect to cost, precision, selectivity, limit of
detection and simplicity.
Corresponding author. Since the atomic absorption lines of non-metals are in the vac-
E-mail addresses: nil.ozbek@itu.edu.tr (N. Ozbek), akmans@itu.edu.tr
uum UV range, they cannot be determined by conventional AAS.
(S. Akman).

http://dx.doi.org/10.1016/j.foodchem.2016.07.007
0308-8146/ 2016 Elsevier Ltd. All rights reserved.
530 N. Ozbek, S. Akman / Food Chemistry 213 (2016) 529533

Following the availability of commercial HR-CS AAS, non-metals 2.2. Reagents


including sulfur have been determined based on the molecular
absorption of diatomic molecules formed with another element, High-purity water (resistivity 18.2 MO cm) obtained by a TKA
a so-called molecule forming element, in a flame or graphite fur- reverse osmosis and a TKA deionizer system (TKA Wasseraufbere-
nace. Sulfur is commonly determined at one of the rotational itungsysteme GmbH, Niederelbert, Germany) was used in solution
absorption lines of CS. Generally, carbon is chosen as a molecule preparations and dilutions. The reagents used in this work were of
forming element because it is found abundantly both in the flame analytical grade (HNO3, 65% (w/w), Merck, Darmstadt, Ger-
and the graphite furnace as well as in the sample matrix. Thus, it is manyH2O2, 30%, Carlo Erba, Italy).
not necessary to add it to the sample, externally. The sulfur standards, potassium pyrosulfate (K2S2O7), potas-
Since LOD values in the graphite furnace are lower than those in sium sulfate (K2SO4), magnesium sulfate heptahydrate (MgSO4-
flame, in most studies, the former was used as an atomizer. How- 7H2O), sodium sulfate decahydrate (Na2SO410H2O), sodium
ever, in the graphite furnace, the sensitivities of sulfur compounds thiosulfate (Na2S2O3), sodium sulfite (Na2SO3), sodium persulfate
in standards and samples as well as their thermal behaviors, such (Na2S2O8) and sodium metabisulfite (Na2S2O5) were obtained from
as conversion efficiencies of sulfur to CS and volatilities of sulfur Merck (Darmstadt, Germany). The waste water standard reference
compounds, are not always the same, causing dissimilar pyrolysis material SPS-NUTR-WW2 (which includes 10.0 0.1 lg mL 1 of
curves prior to the molecule formation step and also inaccurate F , 50.0 0.5 lg mL 1 of Cl , 7.5 0.08 lg mL of PO34 ,
results (Huang, Becker-Ross, Florek, Heitmann, & Okruss, 2005). 5.0 0.05 lg mL of NO and 100 1 lg mL of SO4 ) was pro-
1 3 1 2

Therefore, a systematic study would be needed to optimize instru- vided by LGC Standards (Teddington, UK).
mental conditions for the graphite furnace as well as selection of Different types of vinegars (grape, apple, balsamic, pomegra-
an appropriate calibrant with similar sensitivity and thermal nate and fig), produced in 2015 by different factories, were pur-
behavior to those of the analyte in the sample. In case of the flame chased from markets in Istanbul. The samples were chosen from
atomizer, since the sample is not thermally treated prior to the amongst the most commonly consumed brands in Turkey.
molecule formation, such problems (i.e. removal of the volatile
compounds at lower temperatures) do not occur. Moreover, non- 2.3. Procedure
spectral interferences, due to reactions with sulfur, are less likely
in the flame environment. Finally, optimization and analysis using The analyte addition technique was applied to determine sulfur
the flame technique are faster and more practical than the graphite in vinegar. Standards were prepared from sodium metabisulfite
furnace. daily. Vinegars were analyzed seven days after opening the bottle.
Until now, sulfur was determined by flame HR-CS AAS (HR-CS In order to convert the sulfur forms to sulfate, 0.20 mL of H2O2
FAAS) in foods (Ozbek & Baysal, 2015; Zambrzycka & God (30%) and 0.20 mL HNO3 (65%) were added to 5 mL of vinegar
_
lewska-Zykiewicz, 2014), coal samples (Baysal & Akman, 2011), and the mixture was made up to 10 mL with distilled water or
plant leaves (Oliveira, Gomes Neto, Nbrega, & Jones, 2010), agri- standards. In order to prepare the analyte addition graph, three
cultural samples (Virgilio, Raposo, Cardoso, Nbrega, & Gomes solutions were used. While the first was made up to volume with
Neto, 2011), petroleum products (Kowalewska, 2011) and by gra- distilled water, the others were made up to volume with 20 mg L 1
phite furnace HR-CS AAS (HR-CS GFAAS) in food samples and 50 mg L 1 of sodium metabisulfite, respectively. For each sam-
(Gunduz & Akman, 2014; Ozbek & Akman, 2013), biological sam- ple type (grape vinegar, apple vinegar etc.), different standard
ples (Ferreira, Lepri, Welz, Carasek, & Huang, 2010), coal samples addition graphs were developed since their matrices were different
(Mior, Mors, Welz, Carasek, & de Andrade, 2013) and airborne from one another. After standing for 30 min, the solutions were
particulates (Ozbek & Baysal, 2016). Moreover determination of aspirated into the fuel-rich airacetylene flame. The results were
sulfur in water samples was done by molecular absorption of SnS evaluated as the mean of triplicate analysis.
by HR-CS GFAAS (Baumbach, Limburg, & Einax, 2013). Sulfur deter-
mination methods, based on molecular absorption of carbon
3. Results and discussion
monosulfide (CS) using high resolution-continuum source atomic
absorption spectrometers, were extensively reviewed (Butcher,
3.1. Selection of atomizer
2013; Resano, Flrez, & Garca-Ruiz, 2014; Welz et al., 2009). The
aim of this study was, therefore, to develop and optimize a proce-
In this study, the flame technique was selected because it was
dure for the determination of total sulfur in vinegars based on
anticipated that the sulfur concentrations in most of the vinegars
molecular absorption of CS using HR-CS FAAS, and to discuss the
samples would be higher than the LOD. Sulfur determination, even
effects of different sulfur species on the CS sensitivity and elimina-
in a flame, is not completely free of problems. It has been reported
tion of errors due to interference.
that the sensitivities of CS obtained from different compounds
might not always be the same (Huang et al., 2008). However, the
2. Experimental problems are less significant and their elimination is less trouble-
some compared to the graphite furnace.
2.1. Instrumentation
3.2. Selection of wavelength
An Analytik Jena ContrAA 700 High-Resolution Continuum
Source Flame Atomic Absorption Spectrometer (Analytik Jena, Jena, The primary CS lines, 257.593, 257.959 and 258.056 nm, are
Germany) equipped with an airacetylene-flame, 300 W xenon well documented in the literature with respect to sensitivity
short-arc lamp (XBO 301, GLE, Jena, Germany), a high-resolution (Ferreira et al., 2010; Huang, Becker-Ross, Florek, Heitmann, &
double monochromator with a prism pre-monochromator, a Okruss, 2006; Huang et al., 2005; Virgilio et al., 2011). The highest
high-resolution echelle monochromator and a charge coupled sensitivity was obtained at 258.056 nm, corresponding to one of
device (CCD) array as a detector was used. The molecular absorp- the Dm = 0 vibrational sequences of the electronic transition X1R
tion of CS was measured at 258.056 nm (central pixel 1). All mea- + ? A1P (Kowalewska, 2011). The wavelength resolved absorption
surements were made in at least three replicates. Samples were spectrum of a vinegar sample in the vicinity of 258.056 nm is
prepared using Eppendorf pipettes in polyethylene wares. shown in Fig. 1. No molecular and atomic absorption signal
N. Ozbek, S. Akman / Food Chemistry 213 (2016) 529533 531

tivities of some sulfur species in the vinegar (free and bound sulfur
dioxide, sulfite, bisulfite, sulfate etc.), and those of the standards
added to the samples, might not be the same, even with the ana-
lyte addition technique.
In a series of experiments, we compared the sensitivities for CS
in aqueous solutions of sulfur prepared from potassium pyrosul-
fate (K2S2O7), potassium sulfate (K2SO4), magnesium sulfate
(MgSO4), sodium sulfate (Na2SO4.), sodium thiosulfate (Na2S2O3),
sodium sulfite (Na2SO3), sodium persulfate (Na2S2O8) and sodium
metabisulfite (Na2S2O5) and similar sensitivities were obtained.
As examples, the calibration curves obtained from sodium salts
of sulfate, sulfite and metabisulfite are shown in Fig. 2. When the
standards were prepared in the acetic acid, which is the main com-
ponent of vinegar as well as an addition to vinegar, the CS sensitiv-
ities dramatically increased, depending on the acidity, whereas
sulfates hardly changed (Fig. 3).
Therefore, in this study, in order to eliminate the errors due to
Fig. 1. Wavelength resolved spectrum for CS at 258.056 nm of blank (black) and a different sensitivities of various sulfur forms, HNO3 and H2O2 were
vinegar sample (blue). (For interpretation of the references to color in this figure added to oxidize all the sulfur species to the sulfate. Since a certi-
legend, the reader is referred to the web version of this article.)
fied reference material (CRM) was not available, in order to test
some errors independent of the sample matrix, such as instrumen-
originating from the sample matrix was detected. Thus, tal errors, weighing errors, pipetting errors etc., sulfur in a waste
258.056 nm was used subsequently without any problems. water CRM sample was subjected to the same procedure as the
vinegar samples. The value was found to be within the uncertainty
limits for the CRM, which showed there were no major errors influ-
3.3. Flame conditions encing the accuracy of analysis.

Both airacetylene and nitrous oxide/acetylene flames are suit-


able for sulfur determination. In this study, airacetylene was
selected due to the satisfactory results and ease of use. Flame con-
ditions, namely burner height and fuel rate (airacetylene ratio),
were adjusted automatically for the maximum sensitivity by the
instrument following aspirating of a 100 mg L 1 standard sulfur
solution prepared from sodium metabisulfite dissolved in 3% acetic
acid. The highest absorbance was obtained with 10 mm of burner
height and 100 L h 1 of flow rate. The flame parameters were
checked with a few samples prior to running them all whilst max-
imum sensitivities were obtained using the same conditions as
those applied for the standards.

3.4. The interferences and choice of calibration technique

Due to competitive reactions of sample matrix components


with sulfur, changing aspirating rate, nebulization efficiency, flame
temperature etc. can cause non-spectral interferences and influ-
ence the sensitivity, which would lead to errors (Welz, Becker-
Ross, Florek, & Heitmann, 2005).
Similarly, the distribution of sulfur forms depends on pH. Lower
pH shifts the equilibrium towards molecular free SO2 while at
higher pH more SO2 is found in the sulfite and bisulfite forms.
Therefore, in the acidic medium of vinegar, the increasing concen-
tration of free SO2 should cause higher sensitivity compared to
matrix-free aqueous standards. However, Huang et al. (2005,
2008) showed that in an acidic medium, following addition of
H2O2/HNO3 or KI/I2 to the sample, CS sensitivity to sulfite was
reduced to that of sulfate due to oxidation of sulfur to sulfate
(Huang et al., 2005, 2008).
Even if the standards for calibration are prepared around the
acidity of vinegar, using acetic acid, the sulfur added to the vinegar
cannot be determined quantitatively. Thus, interferences caused by
chemical and physical effects (positive or negative) should not be
compensated for using external standards. Since the linear calibra-
tion technique could not be applied, the analyte addition technique
was used instead. However, the most significant drawback of this
approach is the non-identical sensitivities of the analyte and the Fig. 2. Linear calibration graphs prepared in water (r: Na2S2O5; N:Na2SO3; j:
standard, even in the same environment (Welz, 1986). The sensi- Na2SO4) (N:3).
532 N. Ozbek, S. Akman / Food Chemistry 213 (2016) 529533

made grape vinegar were determined using the analyte addition


technique, and the results at seven days after opening are shown
in Table 1. According to the labels, sodium metabisulfite had been
added to the vinegars but the concentrations were not given so it
was used as a calibrant throughout this study.
The sulfur concentrations found after oxidation with HNO3/
H2O2 were between 2% and 10% (mostly less than 5%) higher than
those without oxidation, which suggests that only a small fraction
of total sulfur was present in the form of free SO2. Huang et al.
(2008) found the free SO2 concentrations in wine were below
10% total sulfur, which is similar to the vinegars in this study.
The total sulfur concentrations varied in a range between <LOD
and 85.0 mg L 1 in grape vinegars, between 39.6 and 163.6 mg L 1
Fig. 3. The effect of acetic acid concentration on the CS molecular absorption for in balsamic vinegars, between <LOD and 76.6 mg L 1 in apple vine-
100 mg L 1 of sulfur prepared from different compounds (r: Na2S2O5; N:Na2SO3; gars (mostly less than the LOD), and <LOD in a pomegranate vine-
j:Na2SO4) (N:3). gar, one homemade vinegar and one fig vinegar. All these values
were below the permitted limits set by the Turkish Ministry of
3.5. Analysis of vinegars
Food, Agriculture and Livestock (170 mg L 1) (Republic of Turkey
Ministry of Food Agriculture and Livestock, 2004).
The total sulfur concentrations of various grape, apple, fig and
To investigate losses due to volatilization or oxidation of SO2 by
balsamic vinegars obtained from markets in Turkey and a home-
air etc., the sulfur concentrations in a grape vinegar and an apple
Table 1 vinegar were determined immediately after opening and for a
Total sulfur concentrations of various types of vinegars (N:3). month afterwards. The sulfur concentration was significantly
reduced (by almost one third) shortly after being exposed to air
Sample Production place Sulfur
concentrationb and then remained almost the same for one month (Fig. 4). It can
(mg L 1) be assumed that free SO2 was lost from the bottle upon opening
SPS-NUTR WW2a 97.2 3.2 although this is speculative.
Grape Vinegar-1 Eskisehir, Central Anatolia Region 36.6 2.1
Grape Vinegar-2 Adana, Central Anatolia Region 43.0 2.2 3.6. Figures of merit
Grape Vinegar-3 _
Istanbul, Marmara Region 16.0 1.0
Grape Vinegar-4 _
Izmir, Aegean Region 19.8 1.1
Figures of merit for sulfur determination in vinegar are summa-
Grape Vinegar-5 _
Izmir, Aegean Region 19.0 1.0
rized in Table 2. The limit of detection (LOD) and limit of quantifi-
Grape Vinegar-6 _
Izmir, Aegean Region 14.3 0.9
_
cation (LOQ) were concentrations corresponding to three- and 10-
Grape Vinegar-7 Izmir, Aegean Region 19.5 1.1
Grape Vinegar-8 Adana, Southern Anatolia Region 50.1 2.4
times the standard deviations for 10 measurements of a sample
Grape Vinegar-9 _
Izmir, Aegean Region 17.8 1.0 that gave an absorbance at baseline level, respectively. The charac-
Grape Vinegar-10 Nevsehir, Central Anatolia Region 35.6 1.5 teristic concentration (C0), which is a measure of sensitivity, was
Grape Vinegar-11 _
Istanbul, Marmara Region 26.6 1.2 calculated as the concentration corresponding to an absorbance
Grape Vinegar-12 _
Izmir, Aegean Region 39.8 2.0 of 0.0044, where 0.0044 is divided by the slope of the linear cali-
Grape Vinegar-13 Adana, Southern Anatolia Region 85.0 4.3 bration curve. The LOD, LOQ and C0 were 11.6, 38.6 and
Grape Vinegar-14 _ 20.8 1.2
Izmir, Aegean Region 44.0 mg L 1, respectively. Instrumental RSD for the three repetitive
Grape Vinegar-15 _
Istanbul, Marmara Region <LOD
aspirations of each sample, as well as the method RSD for an aver-
Grape Vinegar-16 _
Izmir, Aegean Region 22.8 1.1
age of three independent analyses of each sample, were 56%,
Grape Vinegar-17 _
Istanbul, Marmara Region 30.0 1.4
respectively.
Grape Vinegar-18 _
Izmir, Aegean Region 33.2 1.5
Grape Vinegar-19 _
Izmir, Aegean Region <LOD
Grape Vinegar-20 _
Izmir, Aegean Region 28.6 1.4
Apple Vinegar-1 _
Istanbul, Marmara Region 22.2 1.2
Apple Vinegar-2 _
Izmir, Aegean Region <LOD
Apple Vinegar-3 _
Izmir, Aegean Region <LOD
Apple Vinegar-4 _
Izmir, Aegean Region 19.1 1.0
Apple Vinegar-5 Afyon-Karahisar, Egean Region 62.3 3.1
Apple Vinegar-6 _
Izmir, Aegean Region 15.3 0.9
Apple Vinegar-7 _
Izmir, Aegean Region 12.9 0.8
Apple Vinegar-8 Adana, Southern Anatolia Region 76.6 4.1
Apple Vinegar-9 _
Izmir, Aegean Region 18.6 1.2
Apple Vinegar-10 _
Izmir, Aegean Region 17.6 1.0
Apple Vinegar-11 _
Izmir, Aegean Region 15.1 0.8
Apple Vinegar-12 Ankara, Central Anatolia Region 40.1 2.1
Balsamic Vinegar-1 _
Izmir, Aegean Region 163.6 7.8
Balsamic Vinegar-2 Eskisehir, Central Anatolia Region 39.6 2.0
Balsamic Vinegar-3 _
Izmir, Aegean Region 130.3 6.1
Home-made Vinegar _
Istanbul, Marmara Region <LOD
Pomegranate Vinegar _
Izmir, Aegean Region <LOD
Fig. Vinegar Mugla, Aegean Region <LOD
a
Certified value for SO24 is 100 1 lg mL 1. Therefore, the S concentration was
converted to SO4.
b
The values between LOD (11.66 mg L 1) and LOQ (38.6 mg L 1) were given for Fig. 4. Change of CS absorbance in a grape and an apple vinegar samples with time
information. after opening the bottle.
N. Ozbek, S. Akman / Food Chemistry 213 (2016) 529533 533

Table 2 Ferreira, H. S., Lepri, F. G., Welz, B., Carasek, E., & Huang, M.-D. (2010).
Figures of merit for the proposed method. Determination of sulfur in biological samples using high-resolution molecular
absorption spectrometry in a graphite furnace with direct solid sampling.
Parameter Value Journal of Analytical Atomic Spectrometry, 25(7), 10391045.
1 Gunduz, S., & Akman, S. (2014). Sulfur determination in some nuts and dried fruits
Characteristic concentration, (mg L ) 44.0
sold in Turkey by high resolution graphite furnace molecular absorption
Limit of detection, (mg L 1) 11.6
spectrometry. LWT Food Science and Technology, 59(2, Part 1), 718723.
Limit of quantification, (mg L 1) 38.6 Heilmann, J., Boulyga, S., & Heumann, K. (2004). Accurate determination of sulfur in
1
Linearity up to 1000 mg L of S gasoline and related fuel samples using isotope dilution ICPMS with direct
Regression coefficient R2: 0.999 sample injection and microwave-assisted digestion. Analytical and Bioanalytical
Instrumental RSD (N:3 successive aspirations) 56% Chemistry, 380(2), 190197.
Method RSD (N:3 independent analyses) 56% Huang, M. D., Becker-Ross, H., Florek, S., Heitmann, U., & Okruss, M. (2005). Direct
determination of total sulfur in wine using a continuum-source atomic-
absorption spectrometer and an airacetylene flame. Analytical and
Bioanalytical Chemistry, 382(8), 18771881.
4. Conclusion Huang, M. D., Becker-Ross, H., Florek, S., Heitmann, U., & Okruss, M. (2006).
Determination of sulfur by molecular absorption of carbon monosulfide using a
high-resolution continuum source absorption spectrometer and an air
The method described for the determination of total sulfur in acetylene flame. Spectrochimica Acta Part B, 61(2), 181188.
vinegars was based on measurement of the molecular absorption Huang, M. D., Becker-Ross, H., Florek, S., Heitmann, U., Okruss, M., & Patz, C.-D.
of carbon monosulfide (CS) using HR-CS FAAS. The method is rapid, (2008). Determination of sulfur forms in wine including free and total sulfur
dioxide based on molecular absorption of carbon monosulfide in the air
robust, practical and simple. The study describes the successful acetylene flame. Analytical and Bioanalytical Chemistry, 390(1), 361367.
application of an atomic absorption spectrometer for sulfur deter- International for the USDA National Organic Program ICF (2011). Sulphur dioxide,
mination that is not determined by a conventional AAS using a hol- Technical Evaluation Report.
Kendall, D. S., Schoenwald, S. D., Siao, M., & Hendricks, S. (1995). The determination
low cathode lamp. Most of the sulfur concentrations in vinegars of sulfur and chlorine in used oil by X-Ray fluorescence, ICP and ion
were above the limit of detection in flame avoiding the need for chromatography. Hazardous Waste and Hazardous Materials, 12(4), 373380.
the more time consuming and expensive graphite furnace Kowalewska, Z. (2011). Feasibility of high-resolution continuum source molecular
absorption spectrometry in flame and furnace for sulphur determination in
technique. petroleum products. Spectrochimica Acta Part B: Atomic Spectroscopy, 66(7),
546556.
Funding Metcalfe, D. D., Sampson, H. A., & Simon, R. A. (2009). Food allergy: Adverse reactions
to foods and food additives. Wiley.
Mior, R., Mors, S., Welz, B., Carasek, E., & de Andrade, J. B. (2013). Determination of
This study was not funded by any agencies/institutes. sulfur in coal using direct solid sampling and high-resolution continuum source
molecular absorption spectrometry of the CS molecule in a graphite furnace.
Talanta, 106, 368374.
Conflict of interest Nakayama, T. (1959). Studies on acetic acid-bacteria I. Biochemical studies on
ethanol oxidation. Journal of Biochemistry, 46(9), 12171225.
Oliveira, S. R., Gomes Neto, J. A., Nbrega, J. A., & Jones, B. T. (2010). Determination of
Nil Ozbek declares that she has no conflict of interest.
macro- and micronutrients in plant leaves by high-resolution continuum source
Suleyman Akman declares that he has no conflict of interest. flame atomic absorption spectrometry combining instrumental and sample
preparation strategies. Spectrochimica Acta Part B: Atomic Spectroscopy, 65(4),
Ethical approval 316320.
Ozbek, N., & Akman, S. (2013). Determination of total sulfur in food samples by solid
sampling high-resolution continuum source graphite furnace molecular
For this type of study formal consent is not required. This study
absorption spectrometry. Journal of Agricultural and Food Chemistry, 61(20),
does not contain any studies with human participants or animals 48164821.
performed by any of the authors. Ozbek, N., & Baysal, A. (2015). A new approach for the determination of sulphur in
food samples by high-resolution continuum source flame atomic absorption
spectrometer. Food Chemistry, 168, 460463.
Informed constent Ozbek, N., & Baysal, A. (2016). A new approach for the determination of sulphur in
airborne particles by HR-CS ETAAS. International Journal of Environmental
Analytical Chemistry, 96(6), 505514.
Not applicable. Quirs, C., Herrero, M., Garca, L. A., & Daz, M. (2012). Effects of SO2 on lactic acid
bacteria physiology when used as a preservative compound in malolactic
Acknowledgements fermentation. Journal of the Institute of Brewing, 118(1), 8996.
Republic of Turkey Ministry of Food Agriculture and Livestock (2004). Trk Gda
Kodeksi-Renklendiriciler ve Tatlandrclar Dsndaki Gda Katk Maddeleri Tebligi.
We are grateful to Mrs Ece Ozcelik for her helpful work for this Resano, M., Flrez, M. A., & Garca-Ruiz, E. (2014). Progress in the determination of
study. metalloids and non-metals by means of high-resolution continuum source
atomic or molecular absorption spectrometry. A critical review. Analytical and
Bioanalytical Chemistry, 406(910), 22392259.
References Santelli, R. E., Oliveira, E. P., de Carvalho, M. D. F. B., Bezerra, M. A., & Freire, A. S.
(2008). Total sulfur determination in gasoline, kerosene and diesel fuel using
Bak, F., Schuhmann, A., & Jansen, K.-H. (1993). Determination of tetrathionate and inductively coupled plasma optical emission spectrometry after direct sample
thiosulfate in natural samples and microbial cultures by a new, fast and introduction as detergent emulsions. Spectrochimica Acta Part B: Atomic
sensitive ion chromatographic technique. FEMS Microbiology Ecology, 12(4), Spectroscopy, 63(7), 800804.
257264. U.S. EPA (2007). Reregistration Eligibility Decision - Inorganic Sulfites.
Baumbach, G., Limburg, T., & Einax, J. W. (2013). Quantitative determination of Virgilio, A., Raposo, J. L., Cardoso, A. A., Nbrega, J. A., & Gomes Neto, J. A. (2011).
sulfur by high-resolution graphite furnace molecular absorption spectrometry. Determination of total sulfur in agricultural samples by high-resolution
Microchemical Journal, 106, 295299. continuum source flame molecular absorption spectrometry. Journal of
Baysal, A., & Akman, S. (2011). A practical method for the determination of sulphur Agricultural and Food Chemistry, 59(6), 21972201.
in coal samples by high-resolution continuum source flame atomic absorption Welz, B. (1986). Abuse of the analyte addition technique in atomic absorption
spectrometry. Talanta, 85(5), 26622665. spectrometry. Fresenius Zeitschrift fr analytische Chemie, 325(1), 95101.
Brienza, S. M. B., Sartini, R. P., Neto, J. A. G., & Zagatto, E. A. G. (1995). Crystal seeding Welz, B., Becker-Ross, H., Florek, S., & Heitmann, U. (2005). High resolution
in flow-injection turbidimetry: Determination of total sulfur in plants. Analytica continuum source AAS. Weinhein: Wiley-VC.
Chimica Acta, 308(13), 269274. Welz, B., Lepri, F. G., Araujo, R. G. O., Ferreira, S. L. C., Huang, M.-D., Okruss, M., &
Butcher, D. J. (2013). Molecular absorption spectrometry in flames and furnaces: A Becker-Ross, H. (2009). Determination of phosphorus, sulfur and the halogens
review. Analytica Chimica Acta, 804, 115. using high-temperature molecular absorption spectrometry in flames and
Council of the European Union (2011). Commission Regulation (EU) No 1129/2011, of furnacesA review. Analytica Chimica Acta, 647(2), 137148.
11 November 2011 amending Annex II to Regulation (EC) No 1333/2008 of the _
Zambrzycka, E., & Godlewska-Zykiewicz, B. (2014). Determination of sulfur in food
European Parliament and of the Council by establishing a Union list of food by high resolution continuum source flame molecular absorption spectrometry.
additives. European Parliament (Ed.), 1129/2011). Spectrochimica Acta Part B: Atomic Spectroscopy, 101, 234239.

Das könnte Ihnen auch gefallen