• Analytical Science and Technology
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• v.9 no.1
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• pp.26-34
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• 1996

A method to determine the trace amount of Se and Bi in the scalp hair using the hydride generation inductively coupled plasma atomic emmission spectrometry was studied. The optimum operation conditions of ICP for hydride generation are 0.6~0.8L/min for the carrier gas flow rate, and 6mm above the induction coil for the observation height. Hydrochloric acid concentrations for the optimum hydride generation conditions were greater than 1.5M when 2.5% $NaBH_4$ and NaOH were used, and greater than 0.5M when 2.5% $NaBH_4$ and 0.1% NaOH were used. Severe interference effects are observed from transition metals such as Cu and Ni, and they could be circumvented by the coprecipitation with lanthanum hydroxide.

• Analytical Science and Technology
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• v.14 no.5
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• pp.410-415
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• 2001

An analytical method has been developed which determines lead in steel samples by inductively coupled plasma mass spectrometry (ICP-MS) with sample introduction by the hydride generation. The lead hydride is not stable and requires and oxidant for the oxidation into metastable Pb(IV) before reduction to $PbH_4$ with $NaBH_4$. A study was carried out to find and optimum lead hydride generation condition for a sample solution with more than $1000{\mu}g/mL$ Fe matrix. $K_2Cr_2O_7$ was found to work as an efficient oxidant when more than $10{\mu}g/mL$ Fe matrix was present. Lactic acid was used with the oxidant as a complexing agent of the metastable Pb(IV) to enhance sensitivity. Optimum concentrations of the sample acidity, oxidant and lactic acid were different depending on the matrix concentration. The isotope dilution method was employed for the quantitation of lead. The determined Pb concentrations of the NIST steel SRM 361 and 362 were in good agreement with the certified values within the uncertainty range.

• Journal of the Korean Society of Food Science and Nutrition
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• v.41 no.5
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• pp.674-680
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• 2012

As(III) and As(V) were analyzed in bamboo salts by hydride generation ICP-AES. In order to quantify the total amount of As in bamboo salts, $AsH_3$ was producted by reacting with 6 mol/L hydrochloric acid and $NaBH_4$, which was then analyzed by hydride generation ICP-AES. As(V) was quantified simultaneously after selectively quantifying As(III). As(III) was quantified by determining the total amount of As and then correcting for the amount of As(III). To improve the reliability of the analysis we repeated the experiment several times to check the detection limit, quantification limit, and measurements of our testing methods. According to the result of our quantification analysis of As existing in bamboo salt, the range of total As content was 0.05 mg/kg~0.2 mg/kg and As(V) was over 90% of the total As.

• Bulletin of the Korean Chemical Society
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• v.8 no.5
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• pp.372-376
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• 1987

Acetone solution of quinoline-8-carbaldehyde reacts with $[Rh(cod)(PPh_3)_2] PF_6$and $[Ir(cod)(PPh_3)_2] PF_6$ to yield $[Rh(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (1) and $[Ir(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (2), respectively. The compound $[Ir(cod)(PPh_3)_2] PF_6$ also reacts with $Ph_2PC_6H_4-o-CHO$ in the acetone / $H_2O$ mixture to give $[Ir(Ph_2PC_6H_4-o-CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (3). Compounds 1, 2, and 3 were characterized by infrared, $^1H$ NMR, $^{31}P$ NMR spectra and conductivity measurement. The $^1H$ NMR spectra of 1, 2, and 3 support the presence of a terminal hydride that is cis to the phosphine. The IR band of 3 at 2185 $cm^{-1}$, which is assigned to $\nu$(Ir-H), and the hydride cleavage reaction of 3 with $CCl_4$, provide evidence for the Ir-H bond.

• Bulletin of the Korean Chemical Society
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• v.15 no.6
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• pp.448-452
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• 1994

2-Hydroxymethyl-2,5-dihydrothiophene 1,1-dioxide (1) was prepared from thiophene-2-carboxylic acid by consecutive reactions involving the Birch reduction, esterification, reduction with lithium aluminum hydride, and oxidation with Oxone$^{\circledR}$. The esterification of alcohol 1 with various unsaturated carboxylic acids provided the precursors 8 for the intramolecular Diels-Alder reaction. The cheletropic expulsion of sulfur dioxide from the esters 8 followed by intramolecular Diels-Alder reaction furnished bicyclic ${\gamma}$-and ${\delta}$-lactones.

• Transactions of the Korean hydrogen and new energy society
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• v.26 no.3
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• pp.271-277
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• 2015

The present paper discusses about noble idea on various reactions including hydrides, hydrogen peroxide and nano-sized metal powders, which do not emit toxic materials as well as carbon dioxide. Here in this paper, the very first-ever concept that heat energy can be generated from the direct reaction between sodium borohydride and hydrogen peroxide is presented. Sodium hydride as fuel can supply hydrogen reacting with oxygen provided by the decomposition of hydrogen peroxide solution. Solid sodium borohydride can be resolved in water and treated as liquid solution for the easy handling and the practical usage although its solid powder can be directly mixed with hydrogen peroxide for the higher reactivity. The thermodynamic analysis was conducted to estimate adiabatic reaction temperatures from these materials. The preliminary experiment on the reactions conducted using sodium borohydride powder and hydrogen peroxide water solution revealed that the self-propagating reaction can occur and that its reactivity increases with an increase of hydrogen peroxide concentration.

• Transactions of the Korean hydrogen and new energy society
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• v.26 no.4
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• pp.308-317
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• 2015

To investigate the effect of microstructure on the formation of the desorption peak, the volumetric thermal analysis technique (VTA) was applied to the Mg-13.5 wt% Ni hydride system. The sample made by the HCS (hydriding combustion synthesis) process had two kinds of Mg microstructures. Linear heating was started with various constant heating rates. Only one peak was appeared in the case of the small initial hydrogen wt% (0.83 wt%). Yet, two peaks were appeared with increasing initial hydrogen wt% (1.85 and 3.73 wt%) when only Mg was hydrogenated. The first peak was formed through the evolution of hydrogen from $MgH_2$, made by eutectic Mg. The second peak was formed through the evolution of hydrogen from $MgH_2$, made by primary Mg. Therefore, this result shows that the microstructure also has a considerable effect on forming the desorption peak. We have also derived the hydrogen desorption equations by VTA to get apparent activation energy when the rate-controlling step for the desorption of the hydrided system is the diffusion of hydrogen through the ${\alpha}$ phase and the chemical reaction ${\beta}{\rightarrow}{\alpha}$.

• Journal of the Korean Society of Propulsion Engineers
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• v.25 no.3
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• pp.26-41
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• 2021

Titanium hydride potassium perchlorate (THPP) has played an important role as initiators of the propulsion system. However, the 'aging' may cause performance degradation and even give rise to a failure in the total system. In this study, various hygrothermal aging conditions were considered and the aging effects on thermodynamic and ignition characteristics of THPP are provided via thermal analysis and ignition measurements. Also, physical-chemical changes were identified by morphological analysis. In conclusion, thermal aging led to E_α decrease-high reactivity due to oxidizer decomposition whereas hygrothermal aging gave rise to an opposite tendency by fuel oxidation.

• Analytical Science and Technology
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• v.14 no.5
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• pp.416-421
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• 2001

The optimization of the reductant and acid concentration for stannane($SnH_4$) generation was investigated by using a continuous flow hydride generator combined with an inductively coupled plasma-atomic emission spectrometer. Several different prereductants were studied to remove the interfering effect of fluoride ion on the hydride generating of tin. The optimum acid concentration was 0.5-1.0 M for the 1-2% $NaBH_4$ and 1.0 M NaOH and the interfering effect of fluoride ion was minimized using boric acid and L-cysteine mixed solution as a prereductant. The reconveries of tin at 20 ng/mL level in the solution containing fluoride ion were 100~108 %.

• Journal of the Korean Chemical Society
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• v.21 no.2
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• pp.108-120
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• 1977

The approximate rates and stoichiometries of the reaction of lithium borohydride, with fifty two selected organic compounds containing representative functional groups under the standard condition (tetrahydrofuran, $0^{\circ}$), were studied.Among the active hydrogen compounds,primary alcohols and compounds containing an acidic proton liberated hydrogen relatively fast, but secondary and tertiary alcohols very sluggishly. All the carbonyl compounds examined were reduced rapidly within one hour. Especially, among the ${\alpha}{\beta}$-unsaturated carbonyl compounds tested, the aldehydes consumed one hydride cleanly, however the cyclic ketones consumed more than one hydride even at $-20^{\circ}$. Carboxylic acids were reduced very slowly, showing about 60% reduction in 6 days at $25^{\circ}$, however acyl chlorides reduced immediately within 30 minutes. On the other hand, the reductions of cyclic anhydrides proceeded moderately to the hydroxy acid stage, however the further reductions were very slow. Aromatic and aliphatic esters, with exception of the relatively moderate reduction of acetate, were reduced very slowly, however lactones were reduced at a moderate rate. Epoxides reacted slowly, but amides and nitriles as well as the nitro compounds were all inert to this reagent. And cyclohexanone oxime and phenyl isocyanate were reduced very sluggishly. Last of all, all sulfur compounds studied were inert to this hydride.