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991.
《Journal of separation science》2003,26(5):425-428
This paper describes a method for analysing some acids of milk whey by Capillary Zone Electrophoresis. After eliminating the whey proteins by ultrafiltration, the whey underwent electrophoretic separation in the presence of anodic electroosmotic flow. The following analytes were detected: citric, orotic, uric, and hippuric acids. A procedure is described for sample preparation and the operating conditions for electrophoretic capillary separation established. Finally, orotic acid is quantitatively determined. 相似文献
992.
Summary Interferences in the flameless determination of cadmium using the HGA 72 were studied for HCl, HNO3, H2SO4, HClO4 and HF and found to be depending on different thermal pretreatment. The interferences of cations were much smaller than for anions. The results are discussed with respect to thermal stability as well as atomization rate of the compositions under investigation. Special emphasis is put upon the presence of interactions between interferents, which in some cases can be used to eliminate interferences.
Statistische Untersuchungen über Störungen bei der flammenlosen AtomabsorptionsspektralphotometrieII. Cadmium
Zusammenfassung Interferenzen, die bei der flammenlosen Bestimmung von Cadmium in der HGA 72 auftreten, wurden bei HCl, HNO3, H2SO4, H3PO4, HClO4 und HF studiert; die AbhÄngigkeit ihres Auftretens von der thermischen Vorbehandlung wird gezeigt. Interferenzen von Kationen sind kleiner. Die Ergebnisse werden im Hinblick auf die thermische StabilitÄt und die Atomisierungsgeschwindigkeit der Proben diskutiert. Besonders betont wird die Gegenwart von Wechselwirkungen zwischen Störungen, die manchmal auch benützt werden können, um Interferenzen auszuschalten.
Part I: Z. Anal. Chem. [10] 相似文献
993.
Franz Pertlik 《Monatshefte für Chemie / Chemical Monthly》1990,121(2-3):129-139
Summary 2-Hydroxy-benzamide, C7H7NO2; monoclinic; I2/a-C
2h
6
;a=12.901 (2),b=4.982 (1),c=20.987 (3) Å; =91.50 (2)°;Z=8. 2-Hydroxy-thiobenzamide, C7H7NOS; monoclinic; P21/n-C
2h
5
;a=13.508 (5),b=6.780 (2),c=15.878 (6) Å; =93.74 (5)°;Z=8. 2-Hydroxy-N,N-dimethyl-benzamide, C9H11NO2; orthorhombic; Pbca-D
2h
15
;a=11.752 (2),b=16.680 (3),c=9.079 (2) Å;Z=8. 2-Hydroxy-N,N-dimethyl-thiobenzamide, C9H11NOS; monoclinic; P21/c-C
2h
5
;a=6.983 (1),b=11.652 (3),c=11.704 (3) Å; =100.02 (2)°;Z=4. The crystal structures of these four compounds were determined (respectively refined: 2-hydroxy-benzamide) by single crystal X-ray data. The refinements of the structure parameters by least squares methods yielded in all casesR<0.056. The hydrogen atoms were located by means of difference Fourier summations. The O-H ... O distances are 2.513 (1) Å in 2-hydroxy-benzamide (intramolecular) and 2.625 (1) Å in 2-hydroxy-N,N-dimethyl-benzamide (intermolecular). The two O-H ... S distances in 2-hydroxy-thiobenzamide are 2.904 (2) Å and 2.918 (2) Å (intramolecular, two molecules in the asymmetric unit) and 3.228 (2) Å in 2-hydroxy-N,N-dimethyl-thiobenzamide (intermolecular). Clear N-H ... O hydrogen bonds with 2.926 (1) Å and 3.006 (1) Å occur only in the structure of 2-hydroxy-benzamide (intermolecular).
Die Kristallstrukturen und Wasserstoffbrücken-Bindungsschemata in vier Benzamid-Derivaten
Zusammenfassung 2-Hydroxy-benzamid, C7H7NO2; monoklin; I2/a-C 2h 6 ;a=12.901 (2),b=4.982 (1),c=20.987 (3) Å; =91.50 (2)°;Z=8. 2-Hydroxy-thiobenzamid, C7H7NOS; monoklin; P21/n-C 2h 5 ;a=13.508 (5),b=6.780 (2),c=15.878 (6) Å; =93.74 (5)°;Z=8. 2-Hydroxy-N,N-dimethyl-benzamid, C9H11NO2; orthorhombisch; Pbca-D 2h 15 ;a=11.752 (2),b=16.680 (3),c=9.079 (2) Å;Z=8. 2-Hydroxy-N,N-dimethyl-thiobenzamid, C9H11NOS; monoklin; P21/c-C 2h 5 ;a=6.983 (1),b=11.652 (3),c=11.704 (3) Å; =100.02 (2)°;Z=4. Die Kristallstrukturen dieser vier Verbindungen wurden mittels Röntgen-Einkristalldaten bestimmt (bzw. verfeinert: 2-Hydroxy-benzamid). Die Verfeinerungen der Strukturparameter nach der Methode der kleinsten Quadrate ergab in allen FällenR<0.056. Die Wasserstoffatome konnten anhand von Differenz-Fourier-Summationen belegt werden. Die O-H ... O-Abstände haben folgende Werte: 2.513(1)Å in 2-Hydroxy-benzamid (intramolekular) und 2.625(1) Å in 2-Hydroxy-N,N-dimethyl-benzamid (intermolekular). Die zwei O-H ... S-Abstände sind in 2-Hydroxy-thiobenzamid 2.904(2)Å und 2.918(2)Å (intramolekular, zwei moleküle in der asymmetrischen Einheit) und 3.228(2)Å in 2-Hydroxy-N,N-dimethyl-thiobenzamid(intermollekular). Klar zuzuordnende N-H ... O-Wasserstoffbrücken mit 2.926(1)Å und 3.006(1)Å treten lediglich in der Struktur des 2-Hydroxy-benzamid auf (intermolekular).相似文献
994.
The Perthioborates RbBS3, TIBS3, and Tl3B3S10 . RbBS3 (P21/c, a=7.082(2) Å, b=11.863(4) Å, c=5.794(2) Å, β=106.54(2)°) was prepared as colourless, plate-shaped crystals by reaction of stoichiometric amounts of rubidium sulfide, boron, and sulfur at 600°C and subsequent annealing. TlBS3 (P21/c, a=6.874(3) Å, b=11.739(3) Å, c=5.775(2) Å, β=113.08(2)°) which is isotypic with RbBS3 was synthesized from a sample of the composition Tl2S · 2 B2S3. The glassy product which was obtained after 7 h at 850°C was annealed in a two zone furnace for 400 h at 400→350°C. Yellow crystals of TlBS3 formed at the warmer side of the furnace. Tl3B3S10 (P1 , a=6.828(2) Å, b=7.713(2) Å, c=13.769(5) Å, α=104.32(2)°, β=94.03(3)°, γ=94.69(2)°) was prepared as yellow plates from stoichiometric amounts of thallium sulfide, boron, and sulfur at 850°C and subsequent annealing. All compounds contain tetrahedrally coordinated boron. The crystal structures consist of polymeric anion chains. In the case of RbBS3 and TlBS3 nonplanar five-membered B2S3 rings are spirocyclically connected via the boron atoms. To obtain the anionic structure of Tl3B3S10 every third B2S3 ring of the polymeric chains of MBS3 is to be substituted by a six-membered B(S2)2B ring. 相似文献
995.
Alkylidynephosphanes and -arsanes. I [P ≡ C? S]?[Li(dme)3]+ – Synthesis and Structure O,O′-Diethyl thiocarbonate and bis(tetrahydrofuran)-lithium bis(trimethylsilyl)phosphanide dissolved in 1,2-dimethoxyethane, react below 0°C to give ethoxy trimethylsilane and tris(1,2-dimethoxyethane-O,O′)lithium 2λ3-phosphaethynylsulfanide – [P≡C? S]? [Li(dme)3]+ – ( 1a ). Apart from bis(trimethylsilyl)sulfane or carbon oxide sulfide, dark red concentrated solutions of λ3-phosphaalkyne 1 are also obtained from reactions of carbon disulfide with bis(tetrahydrofuran)-lithium bis(trimethylsilyl)phosphanide or with the homologous lithoxy-methylidynephosphane ( 2 ) [1]. The ir spectrum shows two absorptions at 1762 and 747 cm?1 characteristic for the P≡C and C? S stretching vibrations. The nmr parameters {δ(31P) ? 121.3; δ(13C) 190.8 ppm; 1JCP 18.2 Hz} resemble much more values of diorganylamino-2λ3-phosphaalkynes than those of bis(1,2-dimethoxyethane-O,O′)lithoxy-methylidyne-phosphane ( 2a ). As found by an X-ray structure analysis (P21/c; a = 1192.6(16); b = 1239.1(19); c = 1414.8(26) pm; β = 105.91(13)° at ?100 ± 3°C; Z = 4 formula units; wR = 0.064) of pale yellow crystals (mp. + 16°C) isolated from the reaction with O,O′-diethyl thiocarbonate, the solid is built up of separate [P≡C? S]? and [Li(dme)3]+ ions. Typical bond lengths and angles are: P≡C 155.5(11); C? S 162.0(11); Li? O 206.4(17) to 220.3(20) pm; P≡C? S 178.9(7)°. 相似文献
996.
Jií Davídek Miloslava Neméthová Josef Seifert 《Fresenius' Journal of Analytical Chemistry》1977,287(4-5):286-287
Summary An indirect polarographic method for the determination of phosmet was elaborated. It is based on the fact that N-hydroxymethylphthalimide formed by the reaction of phosmet with sulphuric acid is polarographically active and exhibits a behaviour during electrolysis at a Hg dropping-electrode similar to that of phthalimide. The method has been applied to the determination of phosmet in apples. The sensitivity is 0.1 ppm.
Indirekte polarographische Bestimmung von Phosmet O,O-Dimethyl-S-(phthalimidomethyl)dithiophosphat
Zusammenfassung Das Verfahren beruht darauf, daß N-Hydroxymethylphthalimid, das bei der Reaktion von Phosmet mit Schwefelsäure gebildet wird, polarographisch aktiv ist und sich bei der Elektrolyse mit der Quecksilber-Tropfelektrode ähnlich wie Phthalimid verhält. Die Methode wurde zur Bestimmung von Phosmet in Äpfeln angewandt. Die Empfindlichkeit beträgt 0,1 ppm.相似文献
997.
J. Musil 《Fresenius' Journal of Analytical Chemistry》1974,271(5):352-354
Summary The following substances have been investigated with regard to their interfering effect in the determination of aluminium by atomic absorption spectrophotometry: HCl, H2SO4, HNO3, H3PO4, alkali and alkaline earth metals, Cu, Fe, Zn, Ni, Mn, Co, Mo, Ti, Cr, V, Si. Ternary systems with La have been examined also. Si exerts a strong depressive effect, whereas other elements in certain concentration ranges exhibit positive effects.
Störungen bei der atomabsorptionsspektralphotometrischen Bestimmung von Aluminium
Zusammenfassung Folgende Substanzen wurden hinsichtlich einer möglichen Beeinflussung der Aluminiumbestimmung untersucht: HCl, H2SO4, HNO3, H3PO4, Alkalimetalle, Erdalkalimetalle, Cu, Fe, Zn, Ni, Mn, Co, Mo, Ti, Cr, V, Si. Ternäre Systeme mit La wurden ebenfalls geprüft. Si übt eine stark depressive Wirkung aus, während andere Elemente in bestimmten Konzentrationsbereichen positiv wirken.
Lecture given on the 2nd Czechoslovak Conference on Flame Speotroscopy, Zvíkov, June 5–8, 1973. 相似文献
998.
A. Manjon J. A. Ferragut J. C. Garcia-Borron J. L. Iborra 《Applied biochemistry and biotechnology》1984,9(2):173-185
Fluorescence spectra and soluble quenching of intrinsic protein fluorescence were used as indexes of conformational changes
suffered by frog epidermis tyrosinase. The activation process and the immobilization of the enzyme involving either free amino
groups or its carbohydrate moiety were studied. The conformational changes resulting from denaturation of each one of the
protein derivatives, as well as the effect of active center copper extraction, were followed by fluorescence studies.
The results showed that: (a) both activation and immobilization were accompanied by conformational changes of the protein
leading to more unfolded states; (b) neither enzyme nor immobilized enzyme were fully unfolded upon denaturation although
enzymic activity was lost; (c) the enzyme immobilized through its carbohydrate moiety was more unfolded upon denaturation
than the enzyme immobilized through amino groups, thus pointing to a higher conformational stabilization in the last situation;
and (d), that tryptophyl residues moved to a localization near the active site upon activation. 相似文献
999.
A new kinetic-catalytic method by the initial rate procedure for the determination of nanogram level of iron(III) is developed, which is based on its catalytic effect on the oxidative coupling of 3-methyl-2-benzothiazolinone hydrazone (MBTH) with N,N-dimethylaniline (DMA) to form an indamine dye (λmax=590 nm) in the presence of hydrogen peroxide. Iron(II) is also determined, being oxidized to iron(III) by hydrogen peroxide. Calibration graphs obtained by the initial rate method are linear in the range 1–1000 ng ml−1 Fe and as low as 10−8 M Fe(II, III) can easily be determined. The relative standard deviations are 6.6, 2.5 and 1.5% for ten determinations of 1, 20 and 60 ng ml−1 of Fe(III), respectively. The method is applicable to the determination of iron in natural waters without preconcentration and separation. 相似文献
1000.
A starter culture ofTrichoderma reesei (Rut-C30) prepared in a liquid fluidized bed reactor (LFBR) gave better growth and greater cellulase production in submerged
fermentation than a conventional shake flask inoculum. The LFBR starter was prepared by first coatingT. reesei spores to 0.25 mm size corncob (1.0x108g-1) in a medium containing 1.0% corncob, 0.5 gL-1 xylose and 0.1 gL-1 lactose in a balanced salt solution, then fluidizing the particles in the LFBR for 36 h to allow germination of the spores,
and covering the particles with an approx 30 μm thick biofilm. This biofilm that developed in constant adherence to the lignocellulosic
carrier, apparently became well adapted to grow rapidly on insoluble cellulose substrates (Solca Floc), and had the enzymes
of the cellulase complex induced for increased cellulase production.
The LFBR starter used in a stirred tank reactor (STR) gave 15 gL-1 biomass production and 6.5 IU mL-1 overall cellulase activity with a volumetric productivity of 64 IU L-1h-1 in a 5 d fermentation, compared with a 7 d shake flask inoculum that gave 11 gL-1 biomass and 3.2 IU mL-1 cellulase activity, with a volumetric productivity of 31IU L-1h-1. The LFBR starter culture retained its viability in dry storage for 6–9 mo. 相似文献