- Email: [email protected]
Briefs
Microchemical Journal, Volume 23, Number 3, September 1978
Briefs Determination of Sub-Nanogram Quantities of Ruthenium by Flameless Atomic Absorption Spectrometry. CRAIG M. YOUNG AND JON M. BALDWIN, A/lied Chemical Corporation, Idaho Chemical Programs Operations Office. 550 Second Street, Iduho Falls, Ida ho 83401.
The determination has been applied to sub-nanogramquantities of ruthenium in a variety of matrices encountered in the solidification of nuclear waste. Detection limits ranged to below lo-“’ g, depending on the sample matrix. Microchem. J. 23,265-284
(1978).
Analytical Reactions of Substituted Cyanoferrates. 2. Pentacyanoamminoferrate (II) in Catalytic Spectrophotometric Determination of Sub-Parts per Million Amounts of Ag+, Au3+, and Hg2+ in Solution. M. K. GADIA AND M. C. MEHRA, Environmental Contaminants Research Group, Department Moncton. New Brunswick, Canada EIA 3E9.
de chimie,
UniversitP
de Moncton,
The ions catalyze ligand exchange reaction between pentacyanomminoferrate (II) ion and ferrozine to produce a strongly colored chelate absorbing at 562 nm. A mechanism is proposed and the effects of the experimental parameters have been determined. Microchem. J. 23,278-W
The Linear Correlation of the (AR’& Function Determined for the Ortho Derivatives of Phenol, Aniline, Benzaldehyde, and Nitrobenzene. LEONARD OGIERMAN AND J~ZEF SLIWIOK, Institute
of Chemistry, Silesian University,
40-006 Katowice, Poland.
Selected chromatographic data from a group of ortho derivatives of phenol, aniline, benzaldehyde, and nitrobenzene are helpful in attempting to predict Rf values of substances with known structures or in elucidating such structures with compounds having known R, values. Microchem. J. 23, 285-290 (1978).
Spectrophotometric Determination of Cerium(IV), Arsenic(III), and Nitrite with Promazine Hydrochloride. H. SANKE GOWDA AND K. N. THIMMAIAH, Department of Postgraduate Studies and Research in Chemistry, gotri, Mysore-570006, India.
University
of Mysore, Manasa Gan-
Promazine hydrochloride reacts with cerium(IV) in acid solution to form a red compound which exhibits maximum absorbance at 505 nm. Arsenic(II1) and nitrite are determined indirectly. Microchem.
J. 23, 291-296 (1977).
Benzothiazole-2-aldehyde-2-quinolylhydrazone as a Reagent for the Extractive trophotometric Determination of Copper(I1). MAKOTO OTOMO AND HIDEMASA Department of Synthetic Chemistry, 466, Japan.
Nagoya Institute
SpecNODA,
of Technology, ShoMa-ku. Nagoya
Copper(I1) was reacted with benzothiazole-2-aldehyde-2-quinolylhydrazone (BTAQH) at pH 8.3-12.6 to form a water-insoluble 1:2 complex, which was extracted with various organic solvents. Microchem.
Metallic BES~GNI,
J. 23, 297-304
(1978)
Excess Determination in Nonstoichiometric Oxides and Chalcogenides. T. F. Ltccr, .WD L. ZANOTTI, Laboratorio Maspec de1 C. N. R., Via Spezia. 73,
43100 Parma. Italy.
A polarographic procedure is described for determining the excess of a metallic element in nonstoichiometric oxides and chalcogenides. The method is based on the possibility of changing the reduction potential of an element in the presence of a strong complexing agent (EDTA). Microchem.
J. 23, 305-311 (1978).
The Use of Redox Reactions in the Analysis of Dyes and Dye Industry Intermediates. III. An Indirect Determination of Brilliant Green with Ceric Sulfate. J. BAREK, A. BERKA, AND K. JAKUBEC, Department of Analytical Chemistry, Charles University, 128 40 Prague 2, Czechoslovakia.
The stoichiometry of the reaction of brilliant green with ceric sulfate was studied. An indirect determination of brilliant green was developed based on this oxidation. Microchem.
J. 23, 312-320 (1978).
A New Reagent for the Spectrophotometric ALEXAKI-TZIVANIDOU, G. KOUIVENIS, AND B. erinary Faculty,
University
of Thessaloniki.
Microdetermination Laboratory Thessaloniki. Greece. ELLLOGLOU,
of Cadmium. ofPhysiology.
H. Vet-
2,2’-Dipyridyl-2-pyridylhydrazone (DPPH) is used in aqueous solution for the determination of cadmium. The yellow 1:2 metal-to-ligand complex formed has a molecular extinction coefficient of 5.5 x 104liters mole-’ cm-’ at the absorption maximum of 444 nm. Microchem.
J. 23, 329-335 (1978).
2,4-Dioxo-4-(4-hydroxy-6-methyl-2-pyrone-3-yl)butyric Acid Ethyl Ester: Reagent for Identifying and Estimating Metal Ions in Ring Oven Analysis. ANTUN GERTNER AND DUBRAVKA PAVI&, Institute of Chemistry, Faculty of Pharmacy versity of Zagreb, A. KovaWa I, 4100 Zagreb, Yugoslavia.
and Biochemistry,
Vni-
The ligand gave variously colored or fluorescent rings when reacted with several kinds of ions on a ring oven. With some ions, the reactions were sensitive enough to enable application of ring calorimetry or fluorometry for quantitation. Microchem.
J. 23, 336-340 (1978).
The Use of Redox Reactions in the Analysis of Dyes and Dye Industry Intermediates. IV. The Oxidation of Benzidine, o-Tolidine, and o-Dianisidine with Chloramine T and N-Bromosuccinimide. J. B.~HLK. A. BF..RK-\. ISII K. JAKYBFC. Drpc~rtmrttr ctf A,~c~/~tictr/
C/wmi.\tr,v,
Chtrrle,\
ur7i\~cw.\ir~.
128 40 Prrr).~lcc 2. C;c~c~12o.\lo~~llhirr.
An extraction-photometric determination of the diamines was developed based on the reaction with an excess of the reagents and the measurement of the absorbance of the reaction product
Analytical Applications of Picolinealdehyde Salicyloylhydrazone. I. Spectrophotometric Determination of Nickel and Zinc. M. GALLE(:O. + M. G~\Rc:IA-V.~KG.U, X F PINO. *
of Ancrlyticnl
AND M. V:\LC.ARCFL,+ * Department
Chemistry,
Faculty
sity of‘ Sc\,illtr. SatY//rl. Spclin, crud fl~eportmrnt of‘ Anctlytical Sc,ierrc,rc\, Uuil,rrsify of C‘ordohtr. Cordohu. Spc~in.
of Sciences.
Chemistry.
Uniter-
Faculty
of
A study of the physical properties of the hydrazone was undertaken with the view that it could be used as an analytical reagent. With both nickel and zinc, yellow complexes are formed. In both cases. the method can determine parts per million amounts. Microchem.
J. 23, 353-359
( 1978)
Spectrophotometric Determination of Arsenic with Diethyldithiocarbamic Acid Silver Salt and Borohydride as Reducing Agent. MA~S~REL B.G~DRF POMPON. A. ALVAREZDepartment of de Compostela, San-
DLVFS~, F. BER~~F,~o-MART~s~~, *ND M,\HERMISI.A B~LL~~x-R~DR~cuEz, Ancrlytical Chemistry, ticrgo dr Composteltr,
Fuculfy Spain.
The method is a modification Microchem.
of ChrmiAtty.
of a previously
University
of Santiago
published method.
J. 23, 360 -365 ( 1978)
Analytical Study of the Phenyl-2-pyridyl Ketone Azine-Palladium System. Photometric Determination of Palladium. M. GAHCIA-V.~RG,AS .4x" M. VALCARCFL, Department
of Antr/\fictr/
Chemistry, Frrc,ulty of’Scienc~c.v. sity of Cordohu, Cordohu, Sptrir~.
A yellow I:1 complex determination. Microc~hrm.
is formed
.I. 23, 366
Hrrc,hioji.
in aqueous ethanolic
c?f‘Sevillcr,
solution
Srvilla,
crnd Uni\,er-
which is used for the
373 ( 1978).
Consecutive Determination ments. MIZUHO S~Ra~lolo Horinouchi
Uni\,ersity
Tokyo
of Rutin and Quercetin by Spectrophotometric .\h~ Kr~olco TAIC~XICRA, Tokyo 192-03,
College
of Pharmuc?,
Measure1432-1.
Jupcln.
Quercetin forms a more stable metal complex without interference from rutin and is determined as a tin complex. After quercetin is removed by using its oxidation with
copper(
rutin is determined as a rutin-copper(I1)
concentrations Microchem.
of the order of IO-’ M. J. 23,374
-383
( 1978).
complex. The method is applicable to
Identification Thin-Layer Chemistry,
of the Order of Aromatic Alcohols and Their Derivatives by Means of Chromatography. J~ZEF $LIU'IOK AND LEOXARD OGIFRMAN, Insfitute of Silrsian University, 40-006 Kato~ice, Poland.
Separation conditions their acetates. Microchem.
were established for aromatic primary
and secondary alcohols and
J. 23, 384 -389 (1978).
Preliminary Evaluation of Biacetyl Bis(2-Pyridyl)Hydrazone as an Analytical Reagent. A. G. ASLWXO, Department of Analytica/ Chemistry, Faculty of Sciences and Pharmacy, The University of Seville, Seville-4. Spain. The compound acts as a general chromogenic reagent, and the fundamental chemistry of the complexes formed with metal ions was studied. Microchem.
J. 23, 390-399
solution
(1978)
A Study of the Stability of Pyrimidine Series Cytostatics, Ftorafur and 5Fluorouracil. The Effect of Oxidation on the Stability of Ftorafur and S-Fluorouracil. HANA To ~~x~ovA* ASD JAROSLAV Z~KA.~ “The State Institute for Control of Drugs, Prague, and tDepartment of Analytical Chemistry, Char/es University, 128-40 Albertov 2030, Prague, Czechoslovakia. The stability of solutions of the compounds was studied during oxidation with alkaline peroxide, acidic peroxide, and weakly acidic peroxide by means of thin-layer chromatography. The decrease in content was monitored spectrophotometrically in the ultraviolet region. The greatest decrease occurred in alkaline solutions, where the pyrimidine ring opened, yielding urea. Microchem.
J. 23, 400-406
(1978)
A Device to Aid Installing and Removing Glass Gas Chromatographic STAHR* ASD A. WUNDERL1TH.t *Veterinary Diagnostic Laboratory Shop, lon~tr State Uniljersirg. Ames, IoM,a 50011.
Columns. H. M. and ~Insrrumcnt
This device allows columns to be removed and replaced in a matter of seconds without stress. Microchem.
J. 23, 407-408
(1978)
Briefs Determination of Sub-Nanogram Quantities of Ruthenium by Flameless Atomic Absorption Spectrometry. CRAIG M. YOUNG AND JON M. BALDWIN, A/lied Chemical Corporation, Idaho Chemical Programs Operations Office. 550 Second Street, Iduho Falls, Ida ho 83401.
The determination has been applied to sub-nanogramquantities of ruthenium in a variety of matrices encountered in the solidification of nuclear waste. Detection limits ranged to below lo-“’ g, depending on the sample matrix. Microchem. J. 23,265-284
(1978).
Analytical Reactions of Substituted Cyanoferrates. 2. Pentacyanoamminoferrate (II) in Catalytic Spectrophotometric Determination of Sub-Parts per Million Amounts of Ag+, Au3+, and Hg2+ in Solution. M. K. GADIA AND M. C. MEHRA, Environmental Contaminants Research Group, Department Moncton. New Brunswick, Canada EIA 3E9.
de chimie,
UniversitP
de Moncton,
The ions catalyze ligand exchange reaction between pentacyanomminoferrate (II) ion and ferrozine to produce a strongly colored chelate absorbing at 562 nm. A mechanism is proposed and the effects of the experimental parameters have been determined. Microchem. J. 23,278-W
The Linear Correlation of the (AR’& Function Determined for the Ortho Derivatives of Phenol, Aniline, Benzaldehyde, and Nitrobenzene. LEONARD OGIERMAN AND J~ZEF SLIWIOK, Institute
of Chemistry, Silesian University,
40-006 Katowice, Poland.
Selected chromatographic data from a group of ortho derivatives of phenol, aniline, benzaldehyde, and nitrobenzene are helpful in attempting to predict Rf values of substances with known structures or in elucidating such structures with compounds having known R, values. Microchem. J. 23, 285-290 (1978).
Spectrophotometric Determination of Cerium(IV), Arsenic(III), and Nitrite with Promazine Hydrochloride. H. SANKE GOWDA AND K. N. THIMMAIAH, Department of Postgraduate Studies and Research in Chemistry, gotri, Mysore-570006, India.
University
of Mysore, Manasa Gan-
Promazine hydrochloride reacts with cerium(IV) in acid solution to form a red compound which exhibits maximum absorbance at 505 nm. Arsenic(II1) and nitrite are determined indirectly. Microchem.
J. 23, 291-296 (1977).
Benzothiazole-2-aldehyde-2-quinolylhydrazone as a Reagent for the Extractive trophotometric Determination of Copper(I1). MAKOTO OTOMO AND HIDEMASA Department of Synthetic Chemistry, 466, Japan.
Nagoya Institute
SpecNODA,
of Technology, ShoMa-ku. Nagoya
Copper(I1) was reacted with benzothiazole-2-aldehyde-2-quinolylhydrazone (BTAQH) at pH 8.3-12.6 to form a water-insoluble 1:2 complex, which was extracted with various organic solvents. Microchem.
Metallic BES~GNI,
J. 23, 297-304
(1978)
Excess Determination in Nonstoichiometric Oxides and Chalcogenides. T. F. Ltccr, .WD L. ZANOTTI, Laboratorio Maspec de1 C. N. R., Via Spezia. 73,
43100 Parma. Italy.
A polarographic procedure is described for determining the excess of a metallic element in nonstoichiometric oxides and chalcogenides. The method is based on the possibility of changing the reduction potential of an element in the presence of a strong complexing agent (EDTA). Microchem.
J. 23, 305-311 (1978).
The Use of Redox Reactions in the Analysis of Dyes and Dye Industry Intermediates. III. An Indirect Determination of Brilliant Green with Ceric Sulfate. J. BAREK, A. BERKA, AND K. JAKUBEC, Department of Analytical Chemistry, Charles University, 128 40 Prague 2, Czechoslovakia.
The stoichiometry of the reaction of brilliant green with ceric sulfate was studied. An indirect determination of brilliant green was developed based on this oxidation. Microchem.
J. 23, 312-320 (1978).
A New Reagent for the Spectrophotometric ALEXAKI-TZIVANIDOU, G. KOUIVENIS, AND B. erinary Faculty,
University
of Thessaloniki.
Microdetermination Laboratory Thessaloniki. Greece. ELLLOGLOU,
of Cadmium. ofPhysiology.
H. Vet-
2,2’-Dipyridyl-2-pyridylhydrazone (DPPH) is used in aqueous solution for the determination of cadmium. The yellow 1:2 metal-to-ligand complex formed has a molecular extinction coefficient of 5.5 x 104liters mole-’ cm-’ at the absorption maximum of 444 nm. Microchem.
J. 23, 329-335 (1978).
2,4-Dioxo-4-(4-hydroxy-6-methyl-2-pyrone-3-yl)butyric Acid Ethyl Ester: Reagent for Identifying and Estimating Metal Ions in Ring Oven Analysis. ANTUN GERTNER AND DUBRAVKA PAVI&, Institute of Chemistry, Faculty of Pharmacy versity of Zagreb, A. KovaWa I, 4100 Zagreb, Yugoslavia.
and Biochemistry,
Vni-
The ligand gave variously colored or fluorescent rings when reacted with several kinds of ions on a ring oven. With some ions, the reactions were sensitive enough to enable application of ring calorimetry or fluorometry for quantitation. Microchem.
J. 23, 336-340 (1978).
The Use of Redox Reactions in the Analysis of Dyes and Dye Industry Intermediates. IV. The Oxidation of Benzidine, o-Tolidine, and o-Dianisidine with Chloramine T and N-Bromosuccinimide. J. B.~HLK. A. BF..RK-\. ISII K. JAKYBFC. Drpc~rtmrttr ctf A,~c~/~tictr/
C/wmi.\tr,v,
Chtrrle,\
ur7i\~cw.\ir~.
128 40 Prrr).~lcc 2. C;c~c~12o.\lo~~llhirr.
An extraction-photometric determination of the diamines was developed based on the reaction with an excess of the reagents and the measurement of the absorbance of the reaction product
Analytical Applications of Picolinealdehyde Salicyloylhydrazone. I. Spectrophotometric Determination of Nickel and Zinc. M. GALLE(:O. + M. G~\Rc:IA-V.~KG.U, X F PINO. *
of Ancrlyticnl
AND M. V:\LC.ARCFL,+ * Department
Chemistry,
Faculty
sity of‘ Sc\,illtr. SatY//rl. Spclin, crud fl~eportmrnt of‘ Anctlytical Sc,ierrc,rc\, Uuil,rrsify of C‘ordohtr. Cordohu. Spc~in.
of Sciences.
Chemistry.
Uniter-
Faculty
of
A study of the physical properties of the hydrazone was undertaken with the view that it could be used as an analytical reagent. With both nickel and zinc, yellow complexes are formed. In both cases. the method can determine parts per million amounts. Microchem.
J. 23, 353-359
( 1978)
Spectrophotometric Determination of Arsenic with Diethyldithiocarbamic Acid Silver Salt and Borohydride as Reducing Agent. MA~S~REL B.G~DRF POMPON. A. ALVAREZDepartment of de Compostela, San-
DLVFS~, F. BER~~F,~o-MART~s~~, *ND M,\HERMISI.A B~LL~~x-R~DR~cuEz, Ancrlytical Chemistry, ticrgo dr Composteltr,
Fuculfy Spain.
The method is a modification Microchem.
of ChrmiAtty.
of a previously
University
of Santiago
published method.
J. 23, 360 -365 ( 1978)
Analytical Study of the Phenyl-2-pyridyl Ketone Azine-Palladium System. Photometric Determination of Palladium. M. GAHCIA-V.~RG,AS .4x" M. VALCARCFL, Department
of Antr/\fictr/
Chemistry, Frrc,ulty of’Scienc~c.v. sity of Cordohu, Cordohu, Sptrir~.
A yellow I:1 complex determination. Microc~hrm.
is formed
.I. 23, 366
Hrrc,hioji.
in aqueous ethanolic
c?f‘Sevillcr,
solution
Srvilla,
crnd Uni\,er-
which is used for the
373 ( 1978).
Consecutive Determination ments. MIZUHO S~Ra~lolo Horinouchi
Uni\,ersity
Tokyo
of Rutin and Quercetin by Spectrophotometric .\h~ Kr~olco TAIC~XICRA, Tokyo 192-03,
College
of Pharmuc?,
Measure1432-1.
Jupcln.
Quercetin forms a more stable metal complex without interference from rutin and is determined as a tin complex. After quercetin is removed by using its oxidation with
copper(
rutin is determined as a rutin-copper(I1)
concentrations Microchem.
of the order of IO-’ M. J. 23,374
-383
( 1978).
complex. The method is applicable to
Identification Thin-Layer Chemistry,
of the Order of Aromatic Alcohols and Their Derivatives by Means of Chromatography. J~ZEF $LIU'IOK AND LEOXARD OGIFRMAN, Insfitute of Silrsian University, 40-006 Kato~ice, Poland.
Separation conditions their acetates. Microchem.
were established for aromatic primary
and secondary alcohols and
J. 23, 384 -389 (1978).
Preliminary Evaluation of Biacetyl Bis(2-Pyridyl)Hydrazone as an Analytical Reagent. A. G. ASLWXO, Department of Analytica/ Chemistry, Faculty of Sciences and Pharmacy, The University of Seville, Seville-4. Spain. The compound acts as a general chromogenic reagent, and the fundamental chemistry of the complexes formed with metal ions was studied. Microchem.
J. 23, 390-399
solution
(1978)
A Study of the Stability of Pyrimidine Series Cytostatics, Ftorafur and 5Fluorouracil. The Effect of Oxidation on the Stability of Ftorafur and S-Fluorouracil. HANA To ~~x~ovA* ASD JAROSLAV Z~KA.~ “The State Institute for Control of Drugs, Prague, and tDepartment of Analytical Chemistry, Char/es University, 128-40 Albertov 2030, Prague, Czechoslovakia. The stability of solutions of the compounds was studied during oxidation with alkaline peroxide, acidic peroxide, and weakly acidic peroxide by means of thin-layer chromatography. The decrease in content was monitored spectrophotometrically in the ultraviolet region. The greatest decrease occurred in alkaline solutions, where the pyrimidine ring opened, yielding urea. Microchem.
J. 23, 400-406
(1978)
A Device to Aid Installing and Removing Glass Gas Chromatographic STAHR* ASD A. WUNDERL1TH.t *Veterinary Diagnostic Laboratory Shop, lon~tr State Uniljersirg. Ames, IoM,a 50011.
Columns. H. M. and ~Insrrumcnt
This device allows columns to be removed and replaced in a matter of seconds without stress. Microchem.
J. 23, 407-408
(1978)