Spectrophotometric Determination of Azide with Ferric Perchlorate

Anton, Anthony; Dodd, J. G.; Harvey, Aubrey E.

doi:10.1021/ac60165a055

Cited by 36 publications

(16 citation statements)

References 5 publications

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“…The solubility product ( Ksp) of thallium(r) azide was measured at 0 "C as previously recommended in the literature,29 because of its appreciable solubility at ambient temperature. The Ksp ~ values obtained for lead(u), copper(rI), mercury(1) and thallium (1) azides, presented in Table 3, compare favourably with values previously reported and obtained by other measurement techniques. "v29…”

Section: Determination Of Solubility Products Of Metal Azidessupporting

confidence: 87%

See 1 more Smart Citation

Poly(vinyl chloride) matrix membrane electrodes for manual and flow injection determination of metal azides

Hassan¹,

Zawawy²,

Marzouk³

et al. 1992

Analyst

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Novel poly(viny1 chloride) matrix membrane electrodes for the azide ion are developed, electrochemically evaluated and used for manual and flow injection determinations of soluble and insoluble metal azides. These electrodes incorporate iron(ii) and nickel(i1) bathophenanthroline-azide ion-pair complexes as ion exchangers and 2-nitrophenyl phenyl ether as a plasticizing solvent mediator. The electrodes exhi bit ( i ) near-Nernstian response for 1 x 10-1-3.5 x 10-5 mol dm-3 N3-with an anionic slope of 56-57 mV decade-' of concentration; ( i i ) a wide working range of pH (6-12); ( i i i ) a fast response time (<40 s ) ; ( i v ) long-term stability (>I month); and ( v ) reasonable selectivity for N3over many common anions. Interference caused by C104-, C103and NO3can be easily tolerated by appropriate ion-exchange separation. Determination of a s little as 0.8 pg crn-3 of soluble azides shows an average recovery of 99.4% and a mean standard deviation of 0.4%. Insoluble metal azides can be similarly determined after prior solubilization with alkaline ethylenediaminetetraacetic acid solution. Methods for measuring the solubility products of some sparingly soluble metal azides and for monitoring the concentration level of azide in primer mixtures are described. Significant advantages in terms of simplicity, sensitivity, selectivity and accuracy are offered by these electrodes.

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Section: Determination Of Solubility Products Of Metal Azidessupporting

confidence: 87%

“…The results obtained show an average recovery of 99.3% and a mean standard deviation of 1.1% (n = 36). Insoluble lead(n), silver (1) and thallium(1) azides were also determined by FI after solubilization. The results obtained show an average recovery of 101.0% and a mean standard deviation of 0.8% (n = 36).…”

Section: Fi Of Azidesmentioning

confidence: 99%

Poly(vinyl chloride) matrix membrane electrodes for manual and flow injection determination of metal azides

Hassan¹,

Zawawy²,

Marzouk³

et al. 1992

Analyst

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“…The aim of this study was to develop an efficient assay to monitor the changes of azide in the ring-opening process. A spectrophotometric determination of azide by ferric perchlorate solution has been reported previously (Anton et al 1960), which was based on the blood red complex (iron(III)/azide) with a characteristic absorbance at 454 nm. Herein, ferric chloride solution (FCS) was used and optimized to establish a proper colorimetric assay for determining HHDH activity.…”

Section: Resultsmentioning

confidence: 99%

An efficient high-throughput screening assay for rapid directed evolution of halohydrin dehalogenase for preparation of β-substituted alcohols

Wan

Liu

Xue

et al. 2015

Appl Microbiol Biotechnol

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Halohydrin dehalogenases (HHDHs) are an important class of enzymes for preparing optically active haloalcohols, epoxides, and β-substituted alcohols. However, natural HHDHs rarely meet the requirements of industrial applications. Here, a novel high-throughput screening (HTS) methodology for directed evolution of HHDH was developed based on the colorimetric determination of azide. In this method, azide was involved in the HHDH-catalyzed ring-opening process and the decrease of azide was used to quantitatively evaluate HHDH activity. The HTS methodology was simple and sensitive (ε460 = 1.2173 × 10(4) L mol(-1) cm(-1)) and could be performed in a microplate format using whole cells. To verify the efficiency of the HTS methodology, it was adopted to engineer a HHDH (HHDH-PL) from Parvibaculum lavamentivorans DS-1, which was applied in the process for ethyl (R)-4-cyano-3-hydroxybutanoate (HN) by the conversion of ethyl (S)-4-chloro-3-hydroxybutanoate ((S)-CHBE)). A random mutant library containing 2500 colonies was screened using the HTS methodology, and three beneficial mutants F176M, A187R, and A187S were obtained. By combining the beneficial mutated residues, the variant F176M/A187R was identified with 2.8-fold higher catalytic efficiency for preparation of HN. The high-throughput colorimetric assay would be very useful for directed evolution of HHDH for preparing β-substituted alcohols.

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“…A massive release of nitric oxide after ingestion leads to hypotension and arrhythmia 1 . The earliest methods for sodium azide determination are spectrophotometric 2 , 3 and volumetric 4 , which appeared in the early 1960s. Over time, a number of chromatographic methods have been developed: high performance liquid chromatography with ultra-visible detector (HPLC-UV) 5 , high performance liquid chromatography with diode array detector (HPLC-DAD) 6 – 8 , ion chromatography (IC) 9 , headspace gas chromatography with nitrogen phosphorus detector (HS-GC-NPD) 10 , gas chromatography with nitrogen phosphorus detector (GC-NPD) 11 , and gas chromatography coupled with mass spectrometry (GC–MS) 12 – 14 .…”

Section: Introductionmentioning

confidence: 99%

A novel procedure for stabilization of azide in biological samples and method for its determination (HS-GC-FID/FID)

Wachełko¹,

Zawadzki

Szpot

2021

Sci Rep

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Sodium azide is an old poison with toxicity comparable to potassium cyanide. It would seem to be completely forgotten however, between 2000 and 2020, the number of intentional ingestions and murders committed with sodium azide significantly increased. Furthermore, due to its extreme instability, sodium azide is difficult to detect, which poses an additional risk when used to commit a crime. In this study, the epidemiology of sodium azide exposures between 1920 and 2020 was investigated. For the determination the azide concentration in biological samples, a simple, precise and selective headspace gas chromatography method (HS-GC-FID/FID) was developed and fully validated. The limit of quantification was 0.65 µg/mL; and the limit of detection was 0.35 µg/mL; precision and accuracy did not exceed 20%. The stability study was conducted for various biological fluids (urine, bile, blood, gastric content) for 91 days in the refrigerator (4 °C) and the method for stabilization of azide was presented. The addition of a mixture of borax and sodium fluoride (w/w 3:1) to the test tubes can stabilize this poison. The described unique technique of collecting the biological samples poses a great potential for azide detection in clinical and toxicology laboratories even long time after human exposure to this substance.

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Spectrophotometric Determination of Azide with Ferric Perchlorate

Cited by 36 publications

References 5 publications

Poly(vinyl chloride) matrix membrane electrodes for manual and flow injection determination of metal azides

Poly(vinyl chloride) matrix membrane electrodes for manual and flow injection determination of metal azides

An efficient high-throughput screening assay for rapid directed evolution of halohydrin dehalogenase for preparation of β-substituted alcohols

A novel procedure for stabilization of azide in biological samples and method for its determination (HS-GC-FID/FID)

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