Determination of cyanide or thiocyanate at trace levels by derivatization and gas chromatography with flame thermionic detection

Funazo, Koichi; Tanaka, Minoru; Shono, Toshiyuki

doi:10.1021/ac00232a017

Cited by 27 publications

(20 citation statements)

References 18 publications

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“…Gas chromatography (GC) with electron capture detection (ECD) [7][8][9] and with nitrogen-phosphorus detection (NPD) [10,11], after suitable derivatization of cyanide, has been reported. GC measurements of cyanide without any derivatization with NPD have also been used after headspace extraction [2,[12][13][14].…”

Section: Introductionmentioning

confidence: 99%

Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography

et al. 1998

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SummaryCyanide can be extracted from whole blood samples by headspace solid-phase microextraction (SPME) with a Carbowax/divinylbenzene-coated fiber. Dm'ing heating a vial of a whole blood sample containing cyanide and acetonitrile as internal standard (IS) at 50 ~ in the presence of Na2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial for 45 rain to allow adsorption of cyanide and IS. The fiber needle was then injected into a capillary gas chromatography (GC) instrument equipped with nitrogen-phosphorus detection. The headspace SPME-GC with a Supel-Q PLOT fused silica capillary column gave large peaks for cyanide and IS; almost no interfering peaks appeared. Recoveries of cyanide and IS flom human whole blood were 3.02-4.06 % and 0.21%, respectively. The calibration curve for cyanide added to human blood showed excellent linearity in the range of 0.04-4.0 pg mL-1; the detection limit was about 0.02 pg mL -1. The coefficients of intra-day and inter-day variation were not greater than 7.1 and 9.2 %. Good correlation (r 2 = 0.999) was found between the present SPME-GC method and the conventional microdiffusion colorimetric method. Data on determination of cyanide in rat blood after intraperitoneal administration are also presented.

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Section: Introductionmentioning

confidence: 99%

Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography

et al. 1998

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“…Approximately a four-fold increase in the concentration of ethyl fluoroacetate in the headspace was observed when the phosphate system was employed. This appears to be a function of the identity of the supporting electrolyte since the apparent pH of each of the two systems is quite close (12.2 for the phosphate system vs. 12.5 for the carbonate system as measured with a pH (7) 54 ( 5 ) 95 (2) 85 (10) 87 (6) 91 ( "The antilog of the intercept of the linear regression of log (area) vs. log (concentration). The slope of the linear regression of area vs. concentration for comparison to a similar number derived from the intercept of the log-log plot.…”

Section: Resultsmentioning

confidence: 90%

“…In 1981, Shono, Funazo, and Tanaka [6] reported the use of dimethylsulfate to produce acetonitrile (from cyanide) and methyl thiocyanate (from thiocyanate) in basic aqueous solutions. These derivatives were subsequently extracted into ethyl acetate for injection into the gas chromatograph.…”

Section: Introductionmentioning

confidence: 99%

“…Other workers have reported the determination of a variety of inorganic and organic anions by conventional gas chromatography after the formation of alkyl derivatives. In 1981, Shono, Funazo, and Tanaka [6] reported the use of dimethylsulfate to produce acetonitrile (from cyanide) and methyl thiocyanate (from thiocyanate) in basic aqueous solutions. These derivatives were subsequently extracted into ethyl acetate for injection into the gas chromatograph.…”

Section: Introductionmentioning

confidence: 99%

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Aqueous alkylation of anions for static headspace sampling with analysis by capillary gas chromatography‐mass spectrometry

Mulligan

1995

J Microcolumn Separations

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Abstract. The formation of ethyl derivative from anions and the conjugate bases of weak acids through the reaction with ethyl p-toluenesulfonate in strongly basic aqueous systems was used as a precursor to analysis by static headspace sampling with capillary gas chromatography-mass spectrometry. A host of materials are amenable to the technique including: cyanide, butyrate, caproate, fluoroacetate, iodide, and phenol. These analytes were used to study the performance of the system in relation to the behavior of commercially obtained ethyl derivatives. 18-Crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) effectively catalyzes the reaction which appears to require the presence of high concentrations (5 M) of a basic salt, such as potassium carbonate. A 1:l (molar) mixture of dibasic and tribasic potassium phosphate effectively substitutes for potassium carbonate and provides improved performance for fluoroacetate while reducing interferences such as diethyl carbonate. Quantitative yields were obtained in the concentration range 0.05-2 mM, except for cyanide which produced propionitrile with an efficiency of 55580%. Fructose, at the 10% w/v level, exerted little influence upon the reaction. Calibration curves (selected ion monitoring) were linear between 0.001 and 1 mM.This approach extends the applicability of static headspace sampling and offers a potentially simple alternative to ion chromatography for complicated matrices. It should prove useful for confirming results obtained by other methods or for screening poorly characterized samples. o 1995 John Wiley & Sons, Inc.

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“…Gas chromatography has been utilized for the determination of cyanide primarily in biological samples with a minimum detection limit of 50 gg/L [8][9][10][11][12]. Several electrochemical procedures have been developed using pulse polarography [13], coulometry [14,15], amperometry with flow-injection [16,17], and ion-selective electrodes [18][19][20][21][22][23][24].…”

Section: Introductionmentioning

confidence: 99%

The Determination of Trace Levels of Cyanide by Ion Chromatography with Electrochemical Detection

Koch

1983

J. RES. NATL. BUR. STAN.

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An improved method for the determination of trace quantities of free cyanide has been developed using ion chromatography with electrochemical detection. Detection limits of I Ag/L have been achieved with linearity of response over the range I to 1000 pg/L. The precision of replicate injections is 0.6 percent, expressed as the relative standard deviation. The method has been applied to the analysis of dust samples.

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Determination of cyanide or thiocyanate at trace levels by derivatization and gas chromatography with flame thermionic detection

Cited by 27 publications

References 18 publications

Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography

Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography

Aqueous alkylation of anions for static headspace sampling with analysis by capillary gas chromatography‐mass spectrometry

The Determination of Trace Levels of Cyanide by Ion Chromatography with Electrochemical Detection

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