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1.
Chromate and cyanide have been determined by their ability to displace iodate from sparingly soluble lead iodate. The released iodate is treated with acidified iodide to give iodine, which is determined either by titration with thiosulphate, or spectrophotometrically as its blue complex with starch. Chromium(III) has been determined as chromate after its oxidation with peroxydisulphate. Sulphate, iodide, bromide, chloride, fluoride, oxalate, tartrate, phosphate and thiocyanate do not interfere. Thiosulphate, sulphite, sulphide, hexacyanoferrate(II) and molybdate ions vitiate the results. Silver, mercury, barium and iron(III) should be masked. Mixtures of cyanide, thiocyanate and halides have been analysed by using complementary procedures that employ the iodates of lead and mercury, and bromine oxidimetry. It has been shown that cyanide or thiocyanate interferes in the determination of iodide by oxidation to iodic acid, because of formation of cyanogen bromide. 相似文献
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Summary Results are given for a two stage oxidation in the ascorbic acid-KIO3 reaction under controlled conditions of acidity. The first step corresponds to the Landolt reaction and the second end point is obtained by the classical Andrews method. The reproducibility and accuracy of the results calculated on the basis of the two successive end points constitute an interesting new feature of this redox reaction involving the use of KIO3 as a primary standard for the determination of ascorbic acid.Our sincere thanks are due to Professor S. S. Joshi for kind interest in the work and to the National Institute of Sciences of India for award of a Research Fellowship to one of us (G. S. D.). 相似文献
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Phytosiderophores of the mugineic acid family are separated by anion-exchange HPLC using NaOH gradient elution. Separation of mugineic acid (MA), 2'-deoxymugineic acid (DMA), 3-hydroxymugineic acid (HMA) and 3-epi-hydroxymugineic acid (epi-HMA) is obtained within 15 min. Detection of the underivatised phytosiderophores is performed using pulsed amperometric detection (PAD) at pH 13. The sensitivity of the detection increases in the order DMA < MA < HMA < epi-HMA and respective detection limits of 5 microM (DMA), 1 microM (MA) and < 0.5 microM (HMA, epi-HMA) are achieved. PAD is discussed in comparison with the well-established fluorimetric detection method after post-column derivatisation with ortho-phthaldialdehyde. The main advantage of PAD is the simplicity of the method (no derivatisation) and the high sensitivity for hydroxylated mugineic acids. The method is used for the determination of phytosiderophores in root washings of iron-deficient and non-deficient wheat and barley plants. 相似文献
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J. B. Luten J. R. W. Woittiez H. A. Das C. L. De Ligny 《Journal of Radioanalytical and Nuclear Chemistry》1978,43(1):175-185
The determination of iodate in rain-water by neutron activation analysis is described. Iodate is separated by anion exchange.
The determination limit of I is 0.02 μg·L−1 for a 20 ml sample. The influence of the sea on the composition of rain-water is demonstrated by the analysis of coastal
rain-water. The results indicate that inorganic iodine (I2 and IO
3
−
) is enriched in filtered coastal rain-water relative to the composition of sea-water. 相似文献
5.
Nitrate (? 6 × 10-4 M) is determined by displacing thiocyanate froman anion-exchange mini-column and determining it spectrophotometrically after reaction with iron (III). The efficiency of lead- and silver-loaded ion-exchange columns in removing anionic interferences is investigated. It is found necessary to incorporate a copperized cadmium reductor to reduce lead or silver ions released by these columns, which otherwise depress the nitrate response. Incorporation of a lead/silver ion-exchange column allows the determination of nitrate in tap water. 相似文献
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High-performance anion-exchange chromatography (HPAC) was used for the determination of aminosaccharides in microbial polymers, chitin, animal waste, sewage sludge, plant residues and soil. The aminosaccharides, galactosamine, mannosamine and glucosamine were separated on a strong anion-exchange column with 1OmM sodium hydroxide as the eluent and determined by pulsed amperometric detection (PAD). The HPAC-PAD methodology was compared with high-performance liquid chromatography (HPLC) with refractive index detection (RI) in terms of selectivity and sensitivity for aminosaccharides. The results indicate that HPAC-PAD required less sample preparation, and was more precise and nearly two orders of magnitude more sensitive than HPLC-RI. HPAC-PAD was not subject to matrix interferences and was highly selective for aminosaccharides. More than 3% of the total nitrogen in alfalfa, and 20% of that in straw, was found to be present as aminosaccharides. 相似文献
7.
A method is described for the determination of cadmium, copper and lead in samples of natural non-saline waters. After acidification with hydrobromic acid, the water sample is filtered and, following the addition of ascorbic acid, passed through a column of the strongly basic anion-exchange resin Dowex 1-X8 (bromide form). On this exchanger cadmium(II). copper(I) and lead(II) are adsorbed as anionic bromide complexes. After elution of these elements with 1 M nitric acid, the determinations by atomic absorption spectrometry are carried out in a medium consisting of 90% () methanol and 10% () 1.5 M hydrobromic acid. The procedure was used for the routine determination of cadmium, copper and lead in water samples collected in Austria. 相似文献
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Summary High performance anion-exchange chromatography (HPAC) coupled with pulsed amperometric detection (PAD) under alkaline conditions (pH 13) separates neutral saccharides based upon their molecular size, saccharide composition, and glycosidic linkages. Carbohydrates were detected by oxidation with a gold-working electrode. HPAC-PAD was compared to high performance liquid chromatography (HPLC) with refractive index (RI) detection in terms of selectivity and sensitivity of saccharides. The results indicate that HPAC-PAD was more precise, two orders of magnitude more sensitive (pmol range) and gives better resolution of saccharides than HPLC-RI. HPAC-PAD required less sample preparation and was not subjected to matrix interferences. The use of HPAC-PAD was applied to the analysis of organic materials (plant residues, animal wastes and sewage sludge) and soil. 相似文献
10.
L. Ma 《Accreditation and quality assurance》2002,7(4):163-167
This paper describes a method of determining the purity of potassium iodate by constant-current coulometry. The determination
can be divided into two steps. First, a Na2S2O3 solution is prepared and its reductive value is determined. Second, the purity value of an oxidimetric quantity of potassium
iodate is determined. This paper discusses the conditions of the reaction process and evaluates type A and B standard uncertainty
of this method. The expanded relative uncertainty of this method is 0.02% (k=2).
Received: 15 June 2000 Accepted: 27 December 2001 相似文献
11.
Ramaier Narayanaswamy Fortunato Sevilla III 《Fresenius' Journal of Analytical Chemistry》1988,329(7):789-792
Summary A flow-through optosensing method for hydrogen sulphide analysis is described, which involves reflectance measurements through optical fibres on paper impregnated with lead acetate. Levels as low as 50 ppb H2S could be measured with high reproducibility within 10 s. The response was affected by flow rate and relative humidity, both of which were controlled during the measurement process. The method provides a sensitive real-time analysis of hydrogen sulphide and could be carried out remote from the instrumentation system.
Schwefelwasserstoffbestimmung durch Bleiacetat-imprägniertes Papier mit Hilfe eines optischen Sensors相似文献
12.
Standard additions experiments for chlortetracycline hydrochloride and virginiamycin at a ratio of 16:1 showed a positive bias for both the plate and turbidimetric methods. The bias was eliminated by anion-exchange chromatography in both the presence and absence of feed components. When chlortetracycline and virginiamycin pre-mixes were used for fortification of laboratory-prepared feeds at chlortetracycline to virginiamycin ratios of 8 or 16:1, the recovery of virginiamycin, without treatment, was 93-100% using the plate assay and 181-236% with the turbidimetric method. The corresponding values obtained using anion-exchange chromatography were 89-99 and 85-91%, respectively. The anion-exchange technique is necessary if the turbidimetric method is used for the assay. 相似文献
13.
建立了以锌粉-氢氧化钠熔融样品,盐酸浸取,用盖氏漏斗作为还原装置,铁粉和铝粒将锡还原,碘酸钾滴定法测定ITO粉末材料中锡的分析方法。方法测定结果稳定,精密度好,相对标准偏差为0.42%~0.67%,加标回收率在99.8%~101%,能够满足ITO粉末中锡的测定要求。 相似文献
14.
建立了阴离子交换色谱分离、抑制型电导检测分析硫磺熏制生姜(简称硫磺姜)中亚硫酸盐的方法。使用NJ-SA-4A阴离子交换分析柱,淋洗液为1.92mmol/L Na2CO3-1.80mmol/L NaHCO3-2%(体积分数)丙酮。通过在样品提取液中加入三乙醇胺,有效地维持了亚硫酸盐的稳定性、并能提高方法的选择性。SO23-在0.02~2.00mg/L范围内线性良好,相关系数为0.9998,峰面积的相对标准偏差为1.9%。方法的检出限为0.015mg/L,加标回收率为84.0%~93.5%。该方法为生姜的市场监测提供了有效的方法。 相似文献
15.
G.E. Taylor 《Journal of chromatography. A》1997,770(1-2):261-271
A validated ion chromatographic method for the determination of anionic impurities in clodronic acid or disodium clodronate is described. Separations are performed by using an anion-exchange column (IonPac AS5) and a sodium hydroxide gradient. Impurities are detected by suppressed conductivity without the need for derivatisation. The most important variable affecting the separation was shown to be the column temperature. 相似文献
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Guanidino compounds were separated and determined by anion-exchange chromatography and electrochemical detection using a basic aqueous eluent and a nickel working electrode. It was found necessary to use a sample clean-up procedure prior to chromatographic analysis of uremic dialysate and serum samples. The effect of eluent hydroxide concentration on the retention of guanidino compounds was studied. Quantitative calibration showed that working curves were non-linear. Electrochemical detection for guanidino compounds with a nickel working electrode, while not selective, has high detection sensitivity. Detection limits for guanidino compounds ranged from 3 to 12 pmol. 相似文献
19.
建立了碘酸钾滴定法测定铜阳极泥分银渣中锡的含量。通过硝酸溶解,过滤除铜,还原铁粉置换分离锑、铋、砷等元素,消除了铜阳极泥分银渣中的铜、锑、砷等杂质元素对锡测定的干扰。方法加标回收率在99.7%~100%。精密度实验结果表明,相对标准偏差(RSD,n=11)小于1.1%。操作过程简单,能满足生产的需要。 相似文献
20.
A simple, rapid and accurate method for the determination of iodate in iodized common salts has been developed. The quantitative determination of iodate was accomplished by anion exchange chromatography with conductimetric detection. The method requires a sample pretreatment for the removal of large excess of chloride from the sample matrix. Onguard silver cartridges were found most suitable for this purpose. The sulphate content in the salt was simultaneously determined. The lower limits for the determination of iodate and sulphate in solution are 0.5 and 0.05 mug ml(-1), respectively. Quantitative recovery of the anions in synthetic samples has been obtained and the interferences from different cations and anions have been studied. The method has been successfully applied to the determination of iodate and sulphate in the commercially available salts. The concentrations of iodate measured by this method are in good agreement with those claimed by the manufacturer. 相似文献