应用酸性铬蓝K的A_N=0双波长补偿系数光度法测定铜(Ⅱ)

在pH=12.7的NaOH介质中,铜(Ⅱ)与酸性铬蓝K(ACBK)形成深红色配合物,应用该配合物生色对试剂ACBK褪色产生100%相消干扰的波长533 nm作为负峰波长,建立了ACBK测定铜(Ⅱ)的A_N=0双波长补偿系数光度法.该法能消除显色剂ACBK褪色对生成物Cu(ACBK)生色的相消干扰,测得生色法真实吸光度,消除生成物生色对有色剂ACBK褪色的相消干扰;测得褪色法近似真实吸光度,其灵敏度是上述两法之和.于波长λp 573 nm,λN 533 nm测得信号吸光度补偿系数fs为4.135,信号摩尔吸光系数为4.56×10~4 L·5moL~(-1)·5cm~(-1),是经典光度法的3.73倍.方法线性范围为0.02～1.60 mg·~(-1),配合物的摩尔比为Cu∶ACBK=1∶1.测定了某些水样中的铜(Ⅱ),并对方法进行了检验,回收率为96%～104%.     

双波长补偿光度法的研究及对微量铁的测定

提出了新的双波长法并应用于茜素S(ARS)光度法测定铁.该法能消除显色剂ARS褪色对生成物Fe[ARS]3生色的相消干扰,测得生色法真实吸光度,消除生成物生色对有色剂ARS褪色的相消干扰,测得褪色法真实吸光度,以其生色吸光度与褪色吸光度绝对值之和作为信号,按信号吸光度法测定.于波长λN=423 nm,λp=555 nm测得信号吸光度补偿系数fs为2.227,测得摩尔吸光系数为2.154 × 104L·mol-1,cm-1,为经典法的2.135倍,线性范围为0-2 mg/L,反应摩尔比为1:3.应用该法测定了某些样品中的铁.结果表明,该法用于存在相消干扰的光度分析及反应摩尔比测定等研究的效果优于经典光度法.     

邻—甲酚酞络合酮吸光光度法连续测定血清中钙和镁

利用邻－甲酚酞络合剂为显色剂建立了连续测定血清钙和镁的吸光光度法,钙和镁与该显色剂在ＰＨ１１的碱性缓冲液中形成紫色络合物,于５７０ｎｍ波长处均表最大吸收,且曲线具有加和性。先测得钙镁吸光度之和,加入８－羟基喹啉以掩蔽镁离子的干扰后测得钙的吸光度,两者之差即为镁的吸光度。钙和镁的摩尔吸光系数分别为２．１４×１０＾４和１．５１×１０＾４,方法应用于血清样品中钙和镁的连续测定,结果令人满意。     

双波长吸光光度法同时测定水样中的钙和镁

本文以4-甲基偶氮胂-TB为显色剂，研究了双波长吸光光度法对钙、镁的同时测定。试验中发现，钙、镁与4-甲基偶氮胂-TB络合时，λmax分别为613nm和580nm，相差33nm。本文拟定的方法可消除钙、镁的相互干扰，用于水样中钙、镁的同时测定，无需分离和加掩蔽剂，方法简便、快速、结果可靠。     

双波长叠加法测定样品中槲皮素含量

在pH= 7.45的B-R缓冲介质中,槲皮素在256 nm和368 nm波长处有两个强度不等的吸收峰,实验发现两个峰的吸光度值之和与槲皮素的浓度呈良好的线性关系,据此提出了双波长叠加分光光度法测定微量槲皮素的新方法.槲皮素的质量浓度在0.84～42 μg· mL-1范围内符合比耳定律,表观摩尔吸光系数高达4.24×10...     

以固绿FCF或茜素红作反应剂分光光度法测定城市土壤中的铬

在盐酸介质中,铬(Ⅵ)氧化固绿FCF使其褪色导致在最大吸收波长628nm处的吸光度下降;而在相同介质中,铬(Ⅵ)使茜素红氧化而显色,导致在其最大吸收波长520nm处的吸光度增加。上述褪色反应的吸光度下降幅度和显色反应的吸光度增加幅度分别与铬(Ⅵ)的质量浓度在0.2~4.0 mg·L~(-1)和0.5~14 mg·L~(-1)内呈线性关系,其检出限(3s/k)分别为0.014,0.051mg·L~(-1)。据此,分别应用上述两种方法测定了城市土壤中铬(Ⅵ)的含量,测定结果与电感耦合等离子体原子发射光谱法测得的结果一致。     

双波长光度法测定阿米卡星的研究

在酸性条件下,水溶苯胺蓝(ANB)与硫酸阿米卡星(AMK)反应,生成蓝色离子缔合物,其最大正吸收波长位于682nm,最大负吸收波长位于602nm,正负峰吸光度绝对值之和与AMK的浓度线性相关,AMK的浓度在0～1.8×10-5mol·L-1的范围内遵从朗伯比耳定律,表观摩尔吸光系数为9.50×104L·mol-1·cm-1,由此建立了测定阿米卡星的双波长光度法。方法用于市售药物及人体尿液中阿米卡星含量的测定,结果满意。     

银碘络阴离子-丁基罗丹明B-吐温-80体系双波长分光光度法测定岩矿中痕量银

方法基于CAgI_3]~(2-)络阴离子与丁基罗丹明B形成离子缔合物,用非离子表面活性剂吐温-80实现增溶增稳。提出了一个高灵敏度的双波长分光光度测定银的方法。缔合物最大吸收波长为605nm,负峰波长为555nm,摩尔吸光系数为3.26×10~5L·mol~(-1)·cm~(-1),0～8μgAg/25ml符合比耳定律。用于岩矿中痕量银的测定,结果满意。     

Zn~(2+)-邻菲啰啉-亮黄缔合体系双波长光度法测定锌

在pH5.7的NaAc-HAc缓冲溶液中,Zn2+与邻菲啰啉(phen)和亮黄(BY)反应生成稳定的离子缔合物[Zn(phen)3]BY,使BY褪色,492 nm处出现正吸收峰,379 nm处出现负吸收峰。选定测量波长为492 nm,参比波长为379 nm,建立了双波长光度法测定微量锌的新方法。表观摩尔吸光系数为3.01×104L.mol-1.cm-1,线性范围为0~1.5μg/mL,检出限为18.5μg/L。方法用于测定锌强化营养盐和健康平衡盐中锌,相对标准偏差为0.69%~0.87%(n=5),回收率为98.4%~99.3%。     

同步扫描-双波长荧光分光光度法同时测定三种儿茶酚胺类神经递质

提出了用同步扫描-双波长荧光分光光度法同时测定肾上腺素(EP)、去甲肾上腺素素(NEP)和多巴胺(DA)3种儿茶酚胺类神经递质.试验表明:荧光检测宜选定发射波长(λen)与激发波长(λex)的波长差为70 nm(△λ=λem-λex)的条件下进行同步扫描.在λem为385.0 nm时DA的荧光信号不受EP和NEP的干扰,而EP和NEP相互的干扰,采用双波长荧光检测模式可消除.选择测定NEP的波长对为470.0 nm(λem,1)和531.8 nm(λem,2),测定EP的波长对为500.0 nm(λ'em,1)和445.6 nm(λ'em,2).测得荧光强度与3种儿茶酚胺浓度在320 μg·L-1(EP),640 μg·L-1(NEP)及160μg·L-1(DA)内呈线性关系,检出限(3σ/k)依次为0.20,0.97,0.73 μg·L-1.     

Simultaneous determination of calcium and magnesium by derivative spectrophotometry in pharmaceutical products

First- and second-derivative spectrophotometric methods for the simultaneous determination of calcium and magnesium in their mixtures are described. The methods are based on the colored complexes formed by calcium and magnesium with bromopyrogallol red in presence of Tween 80 as a surfactant. The zero-crossing method has been utilized to measure the first- and second-derivative value of the derivative spectrum. Calcium (0.8-4.8microgml(-1)) is determined in the presence of magnesium (0.5-3.5microgml(-1)) at the pH 10 and vice versa at zero-crossing wavelengths of 544.5 and 570nm in the first-derivative procedure and 574 and 531nm in the second-derivative procedure, respectively. The detection limits achieved were 0.0575microgml(-1) of calcium and 0.03microgml(-1) of magnesium. The relative standard deviations were in all instances less than 2%. The proposed method has been applied to the simultaneous determination of calcium and magnesium in different samples: commercial multivitamin, human serum and drinking water where excellent agreement between reported and obtained results was achieved.     

Preconcentration and determination of calcium and magnesium in brine with flow-injection systems

On-line preconcentration on a chelating resin (Dowex A-1) and elution with 0.1 M hydorchloric acid is followed by spectrophotometry based on the metal complexes formed with 1- (2-hydroxy-4-diethylamino-1-phenylazo)-2-hydroxynaphthalene-3,6-disulfonic acid. The total concentration of calcium and magnesium is determined; in a second sample, calcium is masked with a ligand buffer containing excess of barium(II) and EGTA, and magnesium is determined. The calcium concentration is measured by difference. Magnesium (1–30 μg l^?1 and calcium (8– 10 μg l^?1) in 2.5 M sodium chloride can be determined. Calcium and magnesium in analytical reagent-grade sodium chloride and potassium chloride and primary standard sodium chloride are aslo determined. The method based on the exchange between calcium ions and Mg(EDTA) is proposed to enchance the sensitivity for calcium.     

Coulometric titration in the study of metal ion-ligand equilibria

The coulometric titration technique is applied to evaluation of stability constants of metal complexes with ligands which have protolytic properties. The validity of the procedure was checked by studying several well-known systems. The proposed method can be used with success when metal ions are not reduced at the working cathode. Constants for calcium and magnesium complexes with components of some biologically important buffers, so-called Good buffers, were evaluated under experimental conditions (ionic strength of 0.16M, 37 degrees ) used in clinical analysis.     

Improved scheme for the analysis of high-purity talc

An improved method is proposed for the determination of silica, magnesium oxide, R(2)O(3), ferric oxide, calcium oxide, and aluminium oxide in high-purity talc. In the method for silica and magnesium oxide, the sample is fused with sodium carbonate and the cooled melt is dissolved with perchloric acid in such a manner that it floats free from the crucible (in previous schemes for the analysis of talc there are frequently mechanical losses due to the difficulty of removing the magnesium silicate melt from the crucible). The solution is then evaporated to fumes of perchloric acid and the silica is filtered off and ignited. The magnesium oxide is determined in the filtrate by precipitation as magnesium ammonium phosphate and a correction is made for the calcium which is precipitated along with the magnesium ammonium phosphate. R(2)O(3) is determined after treatment of the sample with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Iron oxide and calcium oxide are determined by atomic absorption, after treatment with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Al(2)O(3) is calculated by difference.     

An ab initio mo study of calcium and magnesium complexes with malonate and formate

Quantum mechanical SCF calculations were performed on magnesium and calcium complexes of malonate and malonate/formate coordination. The calcium malonate structure is in substantial agreement with recent X-ray results on -ethylmalonate. The magnesium complexes are generally more tightly bound than calcium, although qualitatively, the calcium and magnesium structures are similar. Experimental binding results for divalent ions with malonates and EDTA are discussed in view of the current calculations.     

Dosage electrochimique rapide,en une seule operation et sans separation,du calcium et du magnesium en presence lún de láutre: Application aux dosages de ces elements dans le serum sanguin et dans lúrine

An important simplification is proposed for the simultaneous electrochemical titration of calcium and magnesium in blood serum and urine. By using platinum wire and mercury electrodes, calcium can be titrated with EGTA and then magnesium with EDTA in the presence of a buffer (pH 10.5) and possibly a citrate-tartrate masking agent. A current due to oxidation of mercury in presence of EGTA or EDTA marks the end-point, and can be read directly or recorded. For blood serum, no preliminary operation is needed; for urine, prior addition of a little silver nitrate makes the method satisfactory.     

Polargraphic adsorptive waves of alkaline-earth metal complexes with thymolphthalexone

Sensitive derivative polarographic adsorption waves have been observed for alkaline-earth metal-TP complexes in 0.15M potassium hydroxide containing 3 x 10(-5)M thymolphthalexone (TP). The limit of detection for calcium, strontium and barium was 7.5 x 10(-7)M and for magnesium 4.0 x 10(-6)M. The proposed method has been used successfully for determining trace amounts of calcium in natural waters and hair samples. The composition of the complex has been shown to be 1:1 alkaline-earth metal:TP and various experiments have confirmed that the wave is an adsorption wave. The reaction mechanism has been studied by a number of methods.     

Concentration and Thermodynamic Stability Constants of Magnesium(II) and Calcium(II) Tartrate Complexes in Aqueous Solutions

The formation of calcium and magnesium tartrate complexes was studied by potentiometric titration at ionic strengths of 0.1 and 0.3 (in the presence of tetraethylammonium chloride) at a temperature of 298.15 K. The composition and the stability constants of the complexes formed in the system were determined. The known stability constants were used to optimize the conditions of calorimetric determination of the heats of formation of calcium and magnesium tartrates in an aqueous solution.     

Carboxyterfenadine antacid interaction monitoring by UV spectrophotometry and RP-HPLC techniques

Carboxyterfenadine, a primary metabolite of terfenadine, a second generation antihistaminic compound was introduced in therapy as a successor of terfenadine due to its cardiac arrhythmia. There are number of drug interactions of fexofenadine with erythromycin, ketoconazole and alike reported in the literature. In this paper, fexofenadine antacid interaction has been studied in presence of sodium bicarbonate, megaldrate, calcium carbonate, magnesium carbonate, aluminum hydroxide, magnesium hydroxide, magnesium trisilicate, simethicone (dimethylpolysiloxane) and calcium hydroxide by UV–Vis spectrophotometer and high performance liquid chromatography (HPLC). These in vitro fexofenadine–antacid interactions were carried out in simulated gastric and intestinal juices and in buffer of pH 7.4 (simulating blood pH) on BP 2005 dissolution apparatus. The results show non-concordant availability of fexofenadine envisaged due to formation of unstable charge transfer complexes.     

Determination of magnesium and calcium ions in seawater by capillary zone electrophoresis

Capillary zone electrophoresis is proposed for the determination of magnesium and calcium ions in seawater. A carrier solution containing EDTA was adopted for the complexation of these ions and the effect of sodium chloride concentration in the sample solutions on the results was examined. It was found that magnesium and calcium ions could be determined without any pretreatment by injecting 100-fold diluted seawater samples. Linear calibration graphs were obtained for standard solutions containing up to 10.0 mg/l of calcium ion when both peak area and peak height were used. On the other hand, a linear calibration graph was obtained for standard solutions containing up to 20.0 mg/l of magnesium ion when the peak area was used, while a curved one was obtained when the peak height was used. Relative standard deviations were 0.8 and 1.2% when a standard solution containing 5.0 mg/l of magnesium and 8.0 mg/l of calcium ions was analysed 8 times using the peak area. Limits of detection for magnesium and calcium ions were 0.13 and 0.26 mg/l, respectively. The proposed method was applied to the determination of magnesium and calcium ions in surface and bottom seawater samples.