In this paper, we demonstrated the results of ethanol, methanol and higher alcoholic contents of the legally and illegally produced alcoholic samples. For investigation, the samples, which were collected as evidence by officers from the crime scenes or illicit production sites, were sent to our laboratories by prosecutions. 96 Turkish Rakı samples, 8 beer samples, 1 wine sample, 101 other strong drink samples, thus totaling 206 samples, and 2 industrial ethanol samples were examined between years 2015-2017. Fast and reliable analysis of the alcoholic beverages, especially in terms of methanol concentration, has vital importance primarily due to the cases of death arose from metabolic acidosis after consumption of illicit alcoholic beverages with high concentration of methanol produced in clandestine laboratories. In the autumn of 2015, an outbreak of mass methanol poisonings took place and so many people died in Istanbul. An HS-GC-MS system was utilized for qualitative analysis of the higher alcohols and for scanning any volatile compound, whereas the determination of ethanol and methanol concentrations an HS-GC-FID system was performed. So, after all results were investigated in detail, mentioning the key points for evaluations, it was clearly described whether the drinks comply with criteria set by Turkish Food Codex Communiqué on Distilled Alcoholic Beverages. 89 of 96 Rakı samples and 90 of 101 strong alcoholic beverages were not definitely compliant with the Communiqué since they contained either tert-butanol, which is a denaturant, or high levels of methanol.
The study was aimed at developing suitable chromatographic conditions and pretreatment methods for reliable trace analysis of cyanide in drinking water and seawater. Separation of CNˉ (as CNOˉ), Fˉ, Clˉ, NO 2ˉ, Brˉ, NO 3ˉ, CO 3 2ˉ, SO 4 2ˉ, PO 4 3ˉ was carried on a Dionex IonPac AS20 column. Two different methods were developed for different samples. LOD and LOQ values were 7.2 µg L −1 and 24.0 µg L −1 for method I and were 15.4 µg L −1 and 51.3 µg L −1 for method II, respectively. Our results did not indicate the presence of cyanide in drinking water samples commercially supplied from Istanbul markets. By the addition of 250, 500, and 1000 µg L −1 to drinking water, cyanide recoveries were found 100.1 %, 104.5 % and 106.9 %, respectively by employing method I. Method II was applied to an artificial and real seawater sample obtained from the Marmara Sea, Istanbul, where a 50 µg L −1 cyanide spike gave a recovery of 100.1 %. Interferences from excessive amounts of salts in seawater were removed by using strongly acidic cation-exchange resin and melamine-formaldehyde resin. The proposed pre-treatment method (II) and chromatographic conditions provided low LOD's for Downloaded by [Georgetown University] at 01:57 25 August 20152 cyanide in seawater (well below acute toxicity limits), since dilution errors and matrix effects were eliminated.
The first aim of this study was to develop a selective, sensitive and reliable method for direct simultaneous determination of cyanate, thiocyanate and hexavalent chromium by ion chromatography with conductivity detection. The other target was to successfully determine cyanides by utilizing same chromatographic system. Yet, since cyanides can not be detected by the direct method, free cyanide ions were converted into cyanate with chloramine-T at alkaline pH. In addition, strongly complexed metal cyanides were converted into cyanate by using photo-oxidation following chloramine-T. Total cyanate ion obtained from developed methods were analysed with IC. The chromatographic separations on anion exchange column were accomplished by optimized multi-step gradient eluent program using NaOH as the eluent. Proposed method was applied for the simultaneous determination of cyanide and hexavalent chromium in electroplating bath solutions and in industrial wastewater. Cyanide and hexavalent chromium could be measured in the linear dynamic ranges of 0.6 -961.5 µmol L‾ 1 and of 0.9 -118.5 µmol L‾ 1 , respectively. The limit of detection and limit of quantification of cyanide were 0.18 and 0.61 µmol L‾ 1 , and these values for chromium(VI) were 0.26 and 0.86 µmol L‾ 1 , respectively. GRAPHICAL ABSTRACTDownloaded by [University of Cincinnati Libraries] at 06:50 31 May 2016 2 INTRODUCTİONCyanide ion (CNˉ) and hexavalent chromium (Cr(VI)), which are highly toxic compounds, are extensively used in electroplating industry. Since cyanide compounds can form stable complexes with metals in a wide spectrum, they are used in mining, metallurgy, manufacture, photography, etc. The complexes of zinc, nickel, copper and cadmium metals with cyanide can be ionized in acidic medium and they are known as weak acid dissociable (WAD) species. In addition to free cyanide, WAD species, metal cyanide and strongly complexed metal cyanides, thiocyanate, cyanogen chloride, and cyanate show very distinct differences in terms of toxicity, reactivity, and effect on the environment. The ionization constants of metallocyanides have significant differences with oxidation state, pH, temperature, and photodegredation playing as important factors. [1] The toxicity of metallocyanides exhibits diversity according to their stabilization constants. The concentration of cyanate gradually increases with time as the cyanide concentration decreases in environment due to oxidation of cyanide. [2] The most harmful cyanide species to the environment are shown to be free and WAD cyanides. [3] Inhalation of hydrocyanic acid (prussic acid (HCN)) or digestion of cyanide salts causes fast-appearing symptoms. HCN vapors are formed by mixing the salts with acids or in the stomach following oral ingestion. The lethal dose is probably 100 mg for hydrocyanic acid while it is 300 mg for potassium cyanide. [4] Furthermore, according to US EPA, the maximum contaminant level for cyanide in drinking water is 0.2 mg Lˉ1. [5] Downloaded by [University of Cincinnati Libraries] at 06:50 31 Ma...
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The understanding of the impurities in natural snow is important in realizing its atmospheric quality, soil characteristics, and the pollution caused to the environment. Knowledge of the occurrence of major ions and trace metals in the snow in the megacity of Istanbul is very limited. This manuscript attempts to understand the origin of major soluble ions (fluoride, acetate, formate, chlorite, chloride, nitrite, chlorate, bromide, nitrate, sulfate, phosphate, and perchlorate) and some trace metals (Fe, Mn, Cd, Co, Ni, Pb, Zn, Cu) in winter surface snow, collected in Istanbul, Turkey. The sampling of the surface snow was conducted after each precipitation during the winter of 2015-2016 at three sites in the city. Besides the statistical evaluation of the major ions, and some trace metal concentrations, the chemical variations along with atmospheric circulations, which are important modification mechanisms that influence the concentrations, were investigated in the study. At examined locations and times, 12 major anions were investigated and in these anions fluoride, chlorite, chlorate, bromide, and perchlorate in the snow samples were below the detection limit; only SO, NO, and CI were found to be in the range of 1.11-17.90, 0.75-4.52, and 0.19-3.01 mg/L. Also, according to the trace element determination, the concentration was found to be 29.2-53.7, 2.0-16.1, 1.0-2.2, 50.1-71.1, 24.2-35.2, ND-7.9, 43.2-106.6, and 3.0-17.7 μg/L for Fe, Mn, Cd, Co, Ni, Pb, Zn, and Cu, respectively. The major anions and investigated trace elements here originated mainly from anthropogenic and atmospheric circulation and mainly influenced by northerly and southerly circulation patterns. While the main limitations in the present study may be the low number of samples that may not be entirely representative, accurately reflect identification, or support other previously observed local measurements, we believe that the type of data presented in this study has the potential to be used in the field of environmental risk assessment and, as result, for human health.
Ma at te er ri ia al l a an nd d M Me et th ho od ds s: : Formic acid concentration was measured as methylformate in the blood samples by performing headspace-gas chromatography-mass spectrometry (HS-GC-MS) system. R Re es su ul lt ts s: : A wide calibration range (0.1-150 mg dL -1 , r 2 = 0.999, internal standard: acetonitrile) was employed for determination of formic acid. LOD and LOQ values were found to be 0.003 mg dL -1 and 0.011 mg dL -1 , respectively. A positive blood sample was spiked and recovery was found to be 102%. After the analyses, the following results were obtained: In positive blood samples (N= 91), formic acid concentration range was found to be 37-141 mg dL -1 , while control samples (N= 50) had a range 0.3 -5.6 mg dL -1 . In addition, no correlation was found between methanol and formic acid concentrations in the bloods whereas there was a very high correlation between blood and vitreous humor methanol concentrations, as expected. C Co on nc cl lu us si io on n: : The most common reason for the deaths from methanol-induced metabolic acidosis is consumption of illicit alcoholic beverages produced in clandestine places and containing high concentration of methanol. In this paper, we present not only HS-GC-MS method for determination of formic acid in postmortem blood samples, but also the key points for evaluation of its results as well.K Ke ey yw wo or rd ds s: : Acidosis; blood; alcoholism; methanol;headspace gas chromatography-mass spectrometry Ö ÖZ ZE ET T A Am ma aç ç: : Biz bu çalışmada, Ocak 2016 ile Haziran 2018 tarihleri arasında Adli Tıp Kurumu'nda yapılan otopsilerden elde edilen pozitif ve kontrol postmortem kan örneği gruplarındaki formik asit konsantrasyonlarının sonuçlarını değerlendirmeyi hedefledik. G Ge er re eç ç v ve e Y Yö ön nt te em ml le er r: : Kan örneklerinde formik asit konsantrasyonu metilformat olarak headspace-gaz kromatografi-kütle spektrometri (HS-GC-MS) sistemi ile ölçülmüştür. B Bu ul lg gu ul la ar r: : Formik asit tayini için geniş bir kalibrasyon aralığı (0,1-150 mg dL -1 , r 2 = 0.999, İç standart: asetonitril) kullanıldı. LOD ve LOQ değerleri sırasıyla 0,003 mg dL -1 ve 0.011 mg dL -1 olarak bulunmuştur. Pozitif bir kan örneğine spike işlemi uygulandı ve %102 geri kazanım elde edildi. Pozitif kan örneklerinde (N= 91) formik asit konsantrasyon aralığı 37-141 mg dL -1 olarak bulunurken kontrol örneklerinde aralık 0,3-5,6 mg dL -1 (N= 50) bulunmuştur. Ayrıca, kan örneklerinde metanol ile formik asit arasında korelasyon kurulamazken kan ile göz içi sıvılarındaki metanol konsantrasyonları arasında beklendiği gibi yüksek korelasyon bulundu. S So on nu uç ç: : Metanol kaynaklı metabolik asidozdan meydana gelen ölümlerin en yaygın nedeni gizli yerlerde üretilen yüksek konsantasyonda metanol içeren yasadışı içkilerin tüketilmesidir. Biz bu makalede, postmortem kan örneklerinde formik asit tayini için bir HS-GC-MS metodunun yanı sıra formik asit sonuçlarının değerlendirilmesindeki kilit noktaları da sunmaktayız.A An na ah h t ta ar r K Ke e l li i m me e l le
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