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Qualitative and quantitative organic analysis. Elementary and functional groups
ABSTRACTS
403
Oxidation of sulfides with alkaline permanganate, I. M. Issa and M. Hamdy, 2. anal. Chem., 169, 334 (1959). Sulfides can be oxidized with alkaline permanganate in presence of telluric acid. Determination of small quantities of chromium in minerals with diphenylcarbazide, F. FrBhlich, Z. anal. Chem., 170, 387 (1959). Cr(IV) in weakly acidic solution can be determined calorimetrically with diphenylcarbaeide at a level of lo-80 pg. Cr/lOO ml. Determination of uranium content in rocks and crude phosphates, G. Jaugg, W. Ochsenfeld, and F. Habashi, Z. anal. Chem., 171, 27 (1959). After separation of interfering metals, uranium is determined polarographically by use of the catalytic nitrate wave. Use of p-cresotic acid and its derivatives for the estimation of thorium and zirconium, S. P. Agrawal, R. C. Agrawal, and T. N. Srivastava, Z. anal. Chem., 171,91 (1959). pcresotic acid and its derivatives are used for the gravimetric determination of thorium and zirconium. The extracticn of transition metals as polyglycol-oxonium complexes and the detection of cobalt as polyethylene-glycol-rhodano-cobaltate. II, M. Ziegler, Z. anal. Chem. 171, 111 (1959). A review of the extraction of transition metals as polyglycoloxonium complexes and the detection of Co is presented. As little as 0.5 pg. of cobalt can be detected in presence of larger quantities of other metal ions. Complexometric aluminum determination with dithizone as indicator, G. Gottschalk, Z. anal. Chem., 172, 192 (1960). The determination of Al by back-titration of the excess EDTA with zinc sulfate with dithiasone as indicator is described. Determination of microgram quantities of thorium in silicates, sediments, and other materials after preliminary enrichment by means of ion exchange, J. Korkish and P. Antal, Z. anal. Chem., 173, 126 (1960). Microgram quantities of Th can be enriched on Dowex 50 resin and determined calorimetrically with thorine. Solochrome Green V as a new analytical reagent, A. M. Amin, H. Khalifa, and A. S. Moustafa, Z. anal. Chem., 173, 138 (1960). Solochrome Green V is a good indicator for EDTA titrations of Zn and Mn and for the calorimetric determination of Zn.
Qualitative and Quantitative Organic Analysis. Elementary and Functional Groups Application of gas chromatography to microdetermination of carbon and hydrogen. 0. E. Sundberg and C. Maresh, Anal. Chem., 32, 274-77 (1960). Organic compounds are converted into component parts by combustion. Water is converted
404
ABSTRACTS
chemically to a.cetylene, and COz and acetylene column. Detection is by thermal conductivity.
are separated
on a silica gel
Rapid decomposition and analysis procedure for microdetermination of chlorine compounds in petroleum fractions, H. V. Mahnstadt and J. D. Winefordner, Anal. Chem., 32, 281-84 (1960). A new apparatus for converting organically-bound chlorine to chloride is used with a sensitive, precision null-point potentiometric method for determining chloride. The method is rapid and permits measurement of 10 a. chlorine. Determination of microgram quantities of sulfate in organic linkages, G. Zdybek, D. S. McCann, and A. J. Boyle, Anal. Chem., 32, 558-60 (1960). The sulfate content of mucopolysaccharides is determined by a turbidimetric procedure involving wet digestion with chloric acid. Simultaneous determination of 20 samples is possible; sulfur contents of lo-300 pg. may be determined. Spot test detection of esters of noncarboxylic acids, F. Feigl and V. Anger, Chemist Analyst, 49, 13-14 (1960). A simple test for detection (as low as 5 pg.) of alkyl and aryl esters of phosphorothioic, phosphorodithioic, phosphonic, arylsulfonic, sulfuric, and boric acids, is described. It is based on liberation of SO2 when heated with hydrated or anhydrous sodium thiosulfate at 180”. Spot test for formaldehyde and jormaldehyde-liberating compounds, E. Jungreis, Chemist-Analyst, 49, 14 (1960). Formaldehyde or compounds such as hexamethylenetetramine that release formaldehyde under pyrohydrolytic conditions can be detected by condensation of the product, formaldoxime, formed with hydroxylamine and which undergoes a color reaction with Mn(I1). Identification limit is 5 pg. of formaldehyde with a dilution limit of 1: 10,000 and 15 pg. of hexamethylenetetramine. Photometric determination of 2,4,6-trichlorophenol, R. U. Schenk, Chemist-Analyst, 49, 14-15 (1960). By steam distillation and measurement of the absorbance at a pH of 7.6-8.0, the variability in the determination of 2,4,6-trichlorophenol can be reduced to less than 1% at concentrations of 0.14.6 mg./lOO ml. Diuzo reaction following chloramine-T-oxidation as a sensitive and specijk tesl for aspartic acid, H. Stegeman and H. F. Griffin, J. Chromatog., 3, 15&53 (1960). As little as 1 gg./ml. asparatic acid can be differentiated from other amino acids, especially glutamic acid. Investigation of the determination of phosphorus in organic compounds, W. J. Kirsten and M. E. Carlsson, Micro&em. J., 4,3-31 (1960). Several methods for the determination of phosphorus in organic compounds have been tested, and improved procedures for the mineralization and spectrophotometric measurement have been developed. MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3
ABSTRACTS
405
Determination of traces of hydroperoxide by reaction of arsenic (III). Application to determination in polymer latex, I. M. Kolthoff, E. J. Meehan, S. Bruckenstein, of the use of and H. Minato, Micro&em. J., 4, 33-41 (1960). An investigation Measurements of the arsenic method below lO-?M hydroperoxide is described. rate of reaction at various pH, temperature, and concentration of reactants are included. A simple, rapid automatic micro-Dumas apparatus for nitrogen determination, G. M. Gustin, Microchem. J., 4, 43-54 (1960). A completely automatic extremely accurate, very compact (occupies only 1 ft.* of bench space), and simply operated micro-Dumas nitrogen apparatus is described. Microdetermination of sulfur in organic compounds utilizing the Schiiniger combustion, A. Steyermark, E. A. Bass, C. C. Johnston, and J. C. Dell, Microchem. J., 4, 55-58 (1960). Two procedures are described: (a) the use of fuming and to make certain that all of the sulfur is in the hexavalent state and (b) the use of bromine to effect the same change. Volumetric microdetermination of organic sulju~ following the &h6niger combustion, H. Soep and P. Demoen, Microchem. J., 4,77-87 (1960). A comparative study of three titration methods for the determination of the sulfate ion on the microscale is presented. Microtitration of organic bases in nonaqueous solvents, M. Gutterson Mikrochim. Acta, 1960, l-11. Visual and potentiometric titration acetic anhydride, formic acid, and propionic acid are investigated.
and T. S. Ma, in acetic acid,
Contribution to the determination of isonicotinic hydrazide and N-acetyl-D-glucosaminylisonicotinic hydra&de with %naphthoquinone-4-suljonate, W. Nielsch and L. Giefer, Mikrochim. Acta, 1960, 17-26. A critical investigation of the spectrophotometeric determination of microgram quantities is reported. Zmproved spot test for cardiac glycosides, K.-H. Segel, Mikrochim. Acta, 1960, 2730. Color changes obtained in the course of 2 hr. after addition of 80% H&+X& and furfural are listed. Concerning the anomalous reactions in the determination of amino nitrogen. VZZ. Anomalous behavior of suljonic acid amides, G. Kainz and H. Huber, Mikroehim. Acta, 1960,38-43. Nitrous acid reacts to give NzO and Nz. Paper chromatography of olefins, W. Huber, Mikrochim. Acta, 1960, 44-53. By adding mercuric acetate to the methanol solution and chromatographic separation it is possible by simple means and quickly to detect olefins in any hydrocarbon mixture, to give their molecular weight, and to give the approximate composition of mixtures of isomers.
ABSTRACTS
406
Concerning the combustion of liquids according to Schtiniger, It. Bennewita, Mikrochim. A&, 1960,54-57. A simple modification makes possible the combustion of liquids if the halogen content does not exceed 80%. A new spot test for nitroso compounds, V. Anger, Mikrochim. Acta, 1960, 58-61. From 0.2 to 30 pg. of nitroso compound gives a blue coloration with concentrated HsSOc and diphenylbenzidine. Nitrate, nitrite, chlorate, bromates, esters of nitric and nitrous acid, various quinones, and other oxidants interfere. Concerning the anomalous reactions in the determination of amino nitrogen. VIZI. Anomalous behavior of some amino acids, G. Kainz and F. Kasler, Mikrochim. Acta, 1960, 62-71. Deamination seems to give an hydroxyl compound and a nitrolic acid which decomposes with liberation of N20 and NP. Additional gas is formed by the reaction of the phenol grouping of tyrosine and of the disulfide of cystine. Chromatography in thin films of silica gel for use in toxicology, G. Machata, Mikrochim. Acta, 1960, 79-86. A detailed description of the separation of alkaloids is given. Contributions to combustion analysis, H. Malissa, Mikrochim. Acta, 1960, 12744. By recording the conductivity of suitable absorbants, carbon, hydrogen, and sulfur may be determined in inorganic and organic substances within 10 min. A new simple nitrometer for Dumas nitrogen determination, Acta, 1960, 150-56. Stehr’s nitrometer has been modified fluoroethylene polymer in place of the ball-socket valve and bottle for the KOH solution in place of a leveling bulb and
T. Mitsui, Mikrochim. by using a plug of dia polyethylene storage rubber tubing.
Mikrochim. A new rapid method for the determination of nitrogen, H. Trutnovsky, Acta, 1960, 157-59. The combustion is carried out with NiO and pure oxygen which is removed by copper. A convenient weighing tube for volatile liquids in carbon-hydrogen and Dumas nitrogen microdetermination, T. Mitsui and C. Furuki, Mikrochim. Acta, 1960, 169-74. With the weighing tube described the use of liquid samples is markedly simplified. The effect of some organic alcohol, M. R. F. Ashworth,
only a negligible
solvents on the turbidimetric analysis of tertiary butyl Mikrochim. Acta, 1960, 175-82. Most solvents exert
influence.
Studies on oxygen determination in organic microanalysis. I. A modified purzfication method of nitrogen gas, S. Mizukami, T. Ieky, and, K. Numoto, Mikrochim. Acta, 1960, 183-87. In the modified purification described, Raney nickel is used in place of copper. MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3
ABSTRACTS Studies analysis T. Ieki, HIsO6 is
407
on oxygen determination in organic microanalysis. II. On the microof oxygen by decrease in the quantify of anhydroiodic acid, S. Mizukami and Mikrochim. Acta, 1960, 188-91. The loss of weight of the tube with determined.
an acoustical control of the combustion process in microdetermination according to Dumas, K. Eder, Milcrochim. Acta, 1960, 197-99. The rate of gas flow is regulated via a combination of loud speaker, sound pickup, and amplifier.
Concerning of nitrogen
Calorimetric micro Kjeldahl method for the routine determination of nitrogen not present in jorm of nitro or nitroso groups, H. C. Burck, Milcrochim. Acta, 1960, 200-203. A calorimetric procedure is described in which Nessler reagent is added directly to the digest. A new method for the iodometric determination of halogens in organic substances, In this method the halogen reacts E. Meier, Mikrochim. Acta, 1960, 204-207. with AgI, and the liberated I, is oxidized and determined as iodate. A rapid method for the microdetermination oj nitrogen in organic substances with the use of Co304 as catalyst in the combustion, M. Vereia and L. Synek, Mikrochim. Acta, 1960, 208-19. A determination of a series may be carried out in 30 min. if two azotometers are used. Detection oj primary Goldstein, Mikrochim. pound is presented.
halogen alkyls in spot analysis, F. Feigl, V. Anger, and D. A spot test for 0.005+.1 mg. of comActa, 1960, 231-34.
The reactions reactions in the determination of amino nitrogen. IX. and oxazoline compounds with nitrous acid, G. Kainz and H. Huber, The reaction of various pyrroline and oxaline Mikrochim. Acta, 1960, 245-53. compounds with nitrous acid yields l-l.4 moles of gas/mole. Anomalous
of pyrroline
Microdetermination of glycol ether compounds, G. Kainz, Mikrochim. Acta, 1960 254-60. Boiling glycol ethers with HI gives ethyl iodide and ethylene, both of which are determined. On the use of nitrite in the determination oj halogen in organic compounds, W. Kirsten, Mikrochim. Acta, 1960, 272-81. Nitrite converts Brz, CL, CIOa, and BrOt to the halides and may consequently be added to the absorbing liquids used in combustion and flask combustion. A new test for the detection of aryl alkyl and dialkyl ketones containing the -CO-CHZgroup, E. Sawicki, J. Noe, and T. W. Stanley, Mikroehim. Acta, 1960, 286-W. A new test for aryl alkyl or dialkyl ketone is based on the blue or violet coloration obtained with 2,2’-dinitrobiphenyl.
408
ABSTRACTS
Determination of carbon and hydrogen in organic compounds. Eflectiveness of combustion catalysts. II, J. Hor&fek, J. Korbl, and V. Pechanec, Mikrochim. Acta, 1960, 294-98. Catalysts could be divided into 2 classes; CoaOd, Co203 + Ag, FezOj + Ag, MnOz, Fez03, NiO, and decomposition products of AgMnO, burn methane quantitatively below 500°C.; others, like CuO, Pt foil, VZO,, and CeO*, do not give complete combustion at 650°C. Quantitative determination of cyanohydrins, C. Berther, K. Kreis, and 0. Buchmann, 2. anal. Chem., 169, 184 (1959). A titration method for cyanohydrins is described which permits the following of the saponification to a-hydroxy acids and formation of aminonitriles with ammonia. Determination of pyridine and its derivatives with chlorcyan and barbituric acid, W. Nielsch and L. Giefer, 2. anal. Chem., 171, 26 (1959). Pyridine, isonicotinic acid, and y-picoline can be determined down to 0.01 Hg. by photometric or paper chromatographic procedures, even in presence of each other. Calorimetric determination of penicillin as Fe(II1) hydroxamate complex, L. M&or and M. K. Papay, Z. anal. Chem., 171, 98 (1959). The high blank value in the calorimetric determination of penicillin by this procedure can be overcome by extraction of the complex with isobutanol. The use of bromchloride for volumetric analysis, K. Burger and E. Schulek, Z. anal. Chem., 172,98 (1960). Maleic and fumaric acid can be determined by an addition reaction with bromochloride, which is accelerated in presence of Hg(I1) salts. Difjkrent tube fillings for nitrogen determinations, G. Kainz and L. Hainberger, Z. anal. Chem., 179, 406 (1959). Metha.ne was to test the Dumas determination of N. The efficiency of tube filling increased in the following sequence: NiO, CorO, is best, oxidizing CH, quantitaCuO, MnsOl, Co304, Pb304 and MnOz. tively at 660°C.
Microfractionation
Procedures
Applications of thin-layer chromatography to steroids, M. Barbier, H. Jiiger, H. Tobias, and F. Wyss, Helv. Chim. Acta, 42, 2446-46 (1959). Adsorbent is spread in a thin layer on a glass plate. Gas chromatographic characterization of organic substances. III. Calculation of retention indices of aliphatic, alicyclic, and aromatic substances, A. Wehrli and E. Kovats, Helv. Chim. Acta, 42, 270936 (1959). Retention indices are given for a large number of compounds; group and structural values are calculated therefrom. Chromatographic fractionation of polysaccharides on cellulose anion exchangers, H. Newkom, H. Dewel, W. J. Heri, and W. Kundig, Helv. Chim. Acta, 43,64-71 (1960). Neutral polysaccharides are adsorbed and eluted at pH 6, acidic compounds at lower pH. Borate improves the fractionation. Preparation of commercial DEAE cellulose is described (see specifically pages 69-71). MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3
403
Oxidation of sulfides with alkaline permanganate, I. M. Issa and M. Hamdy, 2. anal. Chem., 169, 334 (1959). Sulfides can be oxidized with alkaline permanganate in presence of telluric acid. Determination of small quantities of chromium in minerals with diphenylcarbazide, F. FrBhlich, Z. anal. Chem., 170, 387 (1959). Cr(IV) in weakly acidic solution can be determined calorimetrically with diphenylcarbaeide at a level of lo-80 pg. Cr/lOO ml. Determination of uranium content in rocks and crude phosphates, G. Jaugg, W. Ochsenfeld, and F. Habashi, Z. anal. Chem., 171, 27 (1959). After separation of interfering metals, uranium is determined polarographically by use of the catalytic nitrate wave. Use of p-cresotic acid and its derivatives for the estimation of thorium and zirconium, S. P. Agrawal, R. C. Agrawal, and T. N. Srivastava, Z. anal. Chem., 171,91 (1959). pcresotic acid and its derivatives are used for the gravimetric determination of thorium and zirconium. The extracticn of transition metals as polyglycol-oxonium complexes and the detection of cobalt as polyethylene-glycol-rhodano-cobaltate. II, M. Ziegler, Z. anal. Chem. 171, 111 (1959). A review of the extraction of transition metals as polyglycoloxonium complexes and the detection of Co is presented. As little as 0.5 pg. of cobalt can be detected in presence of larger quantities of other metal ions. Complexometric aluminum determination with dithizone as indicator, G. Gottschalk, Z. anal. Chem., 172, 192 (1960). The determination of Al by back-titration of the excess EDTA with zinc sulfate with dithiasone as indicator is described. Determination of microgram quantities of thorium in silicates, sediments, and other materials after preliminary enrichment by means of ion exchange, J. Korkish and P. Antal, Z. anal. Chem., 173, 126 (1960). Microgram quantities of Th can be enriched on Dowex 50 resin and determined calorimetrically with thorine. Solochrome Green V as a new analytical reagent, A. M. Amin, H. Khalifa, and A. S. Moustafa, Z. anal. Chem., 173, 138 (1960). Solochrome Green V is a good indicator for EDTA titrations of Zn and Mn and for the calorimetric determination of Zn.
Qualitative and Quantitative Organic Analysis. Elementary and Functional Groups Application of gas chromatography to microdetermination of carbon and hydrogen. 0. E. Sundberg and C. Maresh, Anal. Chem., 32, 274-77 (1960). Organic compounds are converted into component parts by combustion. Water is converted
404
ABSTRACTS
chemically to a.cetylene, and COz and acetylene column. Detection is by thermal conductivity.
are separated
on a silica gel
Rapid decomposition and analysis procedure for microdetermination of chlorine compounds in petroleum fractions, H. V. Mahnstadt and J. D. Winefordner, Anal. Chem., 32, 281-84 (1960). A new apparatus for converting organically-bound chlorine to chloride is used with a sensitive, precision null-point potentiometric method for determining chloride. The method is rapid and permits measurement of 10 a. chlorine. Determination of microgram quantities of sulfate in organic linkages, G. Zdybek, D. S. McCann, and A. J. Boyle, Anal. Chem., 32, 558-60 (1960). The sulfate content of mucopolysaccharides is determined by a turbidimetric procedure involving wet digestion with chloric acid. Simultaneous determination of 20 samples is possible; sulfur contents of lo-300 pg. may be determined. Spot test detection of esters of noncarboxylic acids, F. Feigl and V. Anger, Chemist Analyst, 49, 13-14 (1960). A simple test for detection (as low as 5 pg.) of alkyl and aryl esters of phosphorothioic, phosphorodithioic, phosphonic, arylsulfonic, sulfuric, and boric acids, is described. It is based on liberation of SO2 when heated with hydrated or anhydrous sodium thiosulfate at 180”. Spot test for formaldehyde and jormaldehyde-liberating compounds, E. Jungreis, Chemist-Analyst, 49, 14 (1960). Formaldehyde or compounds such as hexamethylenetetramine that release formaldehyde under pyrohydrolytic conditions can be detected by condensation of the product, formaldoxime, formed with hydroxylamine and which undergoes a color reaction with Mn(I1). Identification limit is 5 pg. of formaldehyde with a dilution limit of 1: 10,000 and 15 pg. of hexamethylenetetramine. Photometric determination of 2,4,6-trichlorophenol, R. U. Schenk, Chemist-Analyst, 49, 14-15 (1960). By steam distillation and measurement of the absorbance at a pH of 7.6-8.0, the variability in the determination of 2,4,6-trichlorophenol can be reduced to less than 1% at concentrations of 0.14.6 mg./lOO ml. Diuzo reaction following chloramine-T-oxidation as a sensitive and specijk tesl for aspartic acid, H. Stegeman and H. F. Griffin, J. Chromatog., 3, 15&53 (1960). As little as 1 gg./ml. asparatic acid can be differentiated from other amino acids, especially glutamic acid. Investigation of the determination of phosphorus in organic compounds, W. J. Kirsten and M. E. Carlsson, Micro&em. J., 4,3-31 (1960). Several methods for the determination of phosphorus in organic compounds have been tested, and improved procedures for the mineralization and spectrophotometric measurement have been developed. MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3
ABSTRACTS
405
Determination of traces of hydroperoxide by reaction of arsenic (III). Application to determination in polymer latex, I. M. Kolthoff, E. J. Meehan, S. Bruckenstein, of the use of and H. Minato, Micro&em. J., 4, 33-41 (1960). An investigation Measurements of the arsenic method below lO-?M hydroperoxide is described. rate of reaction at various pH, temperature, and concentration of reactants are included. A simple, rapid automatic micro-Dumas apparatus for nitrogen determination, G. M. Gustin, Microchem. J., 4, 43-54 (1960). A completely automatic extremely accurate, very compact (occupies only 1 ft.* of bench space), and simply operated micro-Dumas nitrogen apparatus is described. Microdetermination of sulfur in organic compounds utilizing the Schiiniger combustion, A. Steyermark, E. A. Bass, C. C. Johnston, and J. C. Dell, Microchem. J., 4, 55-58 (1960). Two procedures are described: (a) the use of fuming and to make certain that all of the sulfur is in the hexavalent state and (b) the use of bromine to effect the same change. Volumetric microdetermination of organic sulju~ following the &h6niger combustion, H. Soep and P. Demoen, Microchem. J., 4,77-87 (1960). A comparative study of three titration methods for the determination of the sulfate ion on the microscale is presented. Microtitration of organic bases in nonaqueous solvents, M. Gutterson Mikrochim. Acta, 1960, l-11. Visual and potentiometric titration acetic anhydride, formic acid, and propionic acid are investigated.
and T. S. Ma, in acetic acid,
Contribution to the determination of isonicotinic hydrazide and N-acetyl-D-glucosaminylisonicotinic hydra&de with %naphthoquinone-4-suljonate, W. Nielsch and L. Giefer, Mikrochim. Acta, 1960, 17-26. A critical investigation of the spectrophotometeric determination of microgram quantities is reported. Zmproved spot test for cardiac glycosides, K.-H. Segel, Mikrochim. Acta, 1960, 2730. Color changes obtained in the course of 2 hr. after addition of 80% H&+X& and furfural are listed. Concerning the anomalous reactions in the determination of amino nitrogen. VZZ. Anomalous behavior of suljonic acid amides, G. Kainz and H. Huber, Mikroehim. Acta, 1960,38-43. Nitrous acid reacts to give NzO and Nz. Paper chromatography of olefins, W. Huber, Mikrochim. Acta, 1960, 44-53. By adding mercuric acetate to the methanol solution and chromatographic separation it is possible by simple means and quickly to detect olefins in any hydrocarbon mixture, to give their molecular weight, and to give the approximate composition of mixtures of isomers.
ABSTRACTS
406
Concerning the combustion of liquids according to Schtiniger, It. Bennewita, Mikrochim. A&, 1960,54-57. A simple modification makes possible the combustion of liquids if the halogen content does not exceed 80%. A new spot test for nitroso compounds, V. Anger, Mikrochim. Acta, 1960, 58-61. From 0.2 to 30 pg. of nitroso compound gives a blue coloration with concentrated HsSOc and diphenylbenzidine. Nitrate, nitrite, chlorate, bromates, esters of nitric and nitrous acid, various quinones, and other oxidants interfere. Concerning the anomalous reactions in the determination of amino nitrogen. VIZI. Anomalous behavior of some amino acids, G. Kainz and F. Kasler, Mikrochim. Acta, 1960, 62-71. Deamination seems to give an hydroxyl compound and a nitrolic acid which decomposes with liberation of N20 and NP. Additional gas is formed by the reaction of the phenol grouping of tyrosine and of the disulfide of cystine. Chromatography in thin films of silica gel for use in toxicology, G. Machata, Mikrochim. Acta, 1960, 79-86. A detailed description of the separation of alkaloids is given. Contributions to combustion analysis, H. Malissa, Mikrochim. Acta, 1960, 12744. By recording the conductivity of suitable absorbants, carbon, hydrogen, and sulfur may be determined in inorganic and organic substances within 10 min. A new simple nitrometer for Dumas nitrogen determination, Acta, 1960, 150-56. Stehr’s nitrometer has been modified fluoroethylene polymer in place of the ball-socket valve and bottle for the KOH solution in place of a leveling bulb and
T. Mitsui, Mikrochim. by using a plug of dia polyethylene storage rubber tubing.
Mikrochim. A new rapid method for the determination of nitrogen, H. Trutnovsky, Acta, 1960, 157-59. The combustion is carried out with NiO and pure oxygen which is removed by copper. A convenient weighing tube for volatile liquids in carbon-hydrogen and Dumas nitrogen microdetermination, T. Mitsui and C. Furuki, Mikrochim. Acta, 1960, 169-74. With the weighing tube described the use of liquid samples is markedly simplified. The effect of some organic alcohol, M. R. F. Ashworth,
only a negligible
solvents on the turbidimetric analysis of tertiary butyl Mikrochim. Acta, 1960, 175-82. Most solvents exert
influence.
Studies on oxygen determination in organic microanalysis. I. A modified purzfication method of nitrogen gas, S. Mizukami, T. Ieky, and, K. Numoto, Mikrochim. Acta, 1960, 183-87. In the modified purification described, Raney nickel is used in place of copper. MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3
ABSTRACTS Studies analysis T. Ieki, HIsO6 is
407
on oxygen determination in organic microanalysis. II. On the microof oxygen by decrease in the quantify of anhydroiodic acid, S. Mizukami and Mikrochim. Acta, 1960, 188-91. The loss of weight of the tube with determined.
an acoustical control of the combustion process in microdetermination according to Dumas, K. Eder, Milcrochim. Acta, 1960, 197-99. The rate of gas flow is regulated via a combination of loud speaker, sound pickup, and amplifier.
Concerning of nitrogen
Calorimetric micro Kjeldahl method for the routine determination of nitrogen not present in jorm of nitro or nitroso groups, H. C. Burck, Milcrochim. Acta, 1960, 200-203. A calorimetric procedure is described in which Nessler reagent is added directly to the digest. A new method for the iodometric determination of halogens in organic substances, In this method the halogen reacts E. Meier, Mikrochim. Acta, 1960, 204-207. with AgI, and the liberated I, is oxidized and determined as iodate. A rapid method for the microdetermination oj nitrogen in organic substances with the use of Co304 as catalyst in the combustion, M. Vereia and L. Synek, Mikrochim. Acta, 1960, 208-19. A determination of a series may be carried out in 30 min. if two azotometers are used. Detection oj primary Goldstein, Mikrochim. pound is presented.
halogen alkyls in spot analysis, F. Feigl, V. Anger, and D. A spot test for 0.005+.1 mg. of comActa, 1960, 231-34.
The reactions reactions in the determination of amino nitrogen. IX. and oxazoline compounds with nitrous acid, G. Kainz and H. Huber, The reaction of various pyrroline and oxaline Mikrochim. Acta, 1960, 245-53. compounds with nitrous acid yields l-l.4 moles of gas/mole. Anomalous
of pyrroline
Microdetermination of glycol ether compounds, G. Kainz, Mikrochim. Acta, 1960 254-60. Boiling glycol ethers with HI gives ethyl iodide and ethylene, both of which are determined. On the use of nitrite in the determination oj halogen in organic compounds, W. Kirsten, Mikrochim. Acta, 1960, 272-81. Nitrite converts Brz, CL, CIOa, and BrOt to the halides and may consequently be added to the absorbing liquids used in combustion and flask combustion. A new test for the detection of aryl alkyl and dialkyl ketones containing the -CO-CHZgroup, E. Sawicki, J. Noe, and T. W. Stanley, Mikroehim. Acta, 1960, 286-W. A new test for aryl alkyl or dialkyl ketone is based on the blue or violet coloration obtained with 2,2’-dinitrobiphenyl.
408
ABSTRACTS
Determination of carbon and hydrogen in organic compounds. Eflectiveness of combustion catalysts. II, J. Hor&fek, J. Korbl, and V. Pechanec, Mikrochim. Acta, 1960, 294-98. Catalysts could be divided into 2 classes; CoaOd, Co203 + Ag, FezOj + Ag, MnOz, Fez03, NiO, and decomposition products of AgMnO, burn methane quantitatively below 500°C.; others, like CuO, Pt foil, VZO,, and CeO*, do not give complete combustion at 650°C. Quantitative determination of cyanohydrins, C. Berther, K. Kreis, and 0. Buchmann, 2. anal. Chem., 169, 184 (1959). A titration method for cyanohydrins is described which permits the following of the saponification to a-hydroxy acids and formation of aminonitriles with ammonia. Determination of pyridine and its derivatives with chlorcyan and barbituric acid, W. Nielsch and L. Giefer, 2. anal. Chem., 171, 26 (1959). Pyridine, isonicotinic acid, and y-picoline can be determined down to 0.01 Hg. by photometric or paper chromatographic procedures, even in presence of each other. Calorimetric determination of penicillin as Fe(II1) hydroxamate complex, L. M&or and M. K. Papay, Z. anal. Chem., 171, 98 (1959). The high blank value in the calorimetric determination of penicillin by this procedure can be overcome by extraction of the complex with isobutanol. The use of bromchloride for volumetric analysis, K. Burger and E. Schulek, Z. anal. Chem., 172,98 (1960). Maleic and fumaric acid can be determined by an addition reaction with bromochloride, which is accelerated in presence of Hg(I1) salts. Difjkrent tube fillings for nitrogen determinations, G. Kainz and L. Hainberger, Z. anal. Chem., 179, 406 (1959). Metha.ne was to test the Dumas determination of N. The efficiency of tube filling increased in the following sequence: NiO, CorO, is best, oxidizing CH, quantitaCuO, MnsOl, Co304, Pb304 and MnOz. tively at 660°C.
Microfractionation
Procedures
Applications of thin-layer chromatography to steroids, M. Barbier, H. Jiiger, H. Tobias, and F. Wyss, Helv. Chim. Acta, 42, 2446-46 (1959). Adsorbent is spread in a thin layer on a glass plate. Gas chromatographic characterization of organic substances. III. Calculation of retention indices of aliphatic, alicyclic, and aromatic substances, A. Wehrli and E. Kovats, Helv. Chim. Acta, 42, 270936 (1959). Retention indices are given for a large number of compounds; group and structural values are calculated therefrom. Chromatographic fractionation of polysaccharides on cellulose anion exchangers, H. Newkom, H. Dewel, W. J. Heri, and W. Kundig, Helv. Chim. Acta, 43,64-71 (1960). Neutral polysaccharides are adsorbed and eluted at pH 6, acidic compounds at lower pH. Borate improves the fractionation. Preparation of commercial DEAE cellulose is described (see specifically pages 69-71). MICROCHEMICAL
JOURNAL,
VOL.
IV,
ISSUE
3