1-(5-溴-2吡啶偶氮)-2-萘酚-6-磺酸作指示剂络合滴定连续测定铝和钛

在酸性溶液中加入对铝、钛过量的EDTA标准溶液,在pH4．0煮沸下,铝（Ⅲ）、钛（Ⅳ）与EDTA生成稳定的络合物。以5-Br-PAN-S作指示剂,用硫酸铜标准溶液返滴定过量的EDTA,测定铝钛合量,再用置换法测定钛的量。终点变色敏锐,准确度高,方法用于硅酸盐矿物中铝钛的连续测定,结果满意。     

2-(5-硝基-2-吡啶偶氮)-5-二甲氨基苯胺作络合滴定指示剂测定铜

试验了用光度显色剂2-(5-硝基-2-吡啶偶氮)-5-二甲氨基苯胺(5-NO2-PADMA)作为螯合滴定铜的指示剂.在pH 4.5的乙酸盐缓冲介质中,5-NO2-PADMA与铜(Ⅱ)生成紫红色螯合物,其吸收峰在550 nm波长处,在无铜(Ⅱ)存在时,该试剂本身的吸收峰在450 nm处,对比度达100 nm.在相同缓冲介质中用EDTA标准溶液滴定铜(Ⅱ)时,滴定终点时溶液由紫红色突变为黄绿色(铜量大于5 mg时接近绿色),终点敏锐可辨.方法中采用指示剂溶液浓度为1 g·L-1溶剂为N,N-二甲基甲酰胺,滴定时加入5～10滴指示剂较为适宜.用此方法测定了化学试剂硝酸铜及铝合金中铜量.     

2-(四氮唑偶氮)-5-二乙氨基苯甲酸指示剂络合滴定法测定钴

探讨 2 (四氮唑偶氮 ) 5 二乙氨基苯甲酸 (TTZDBA)作为络合滴定钴的指示剂的分析性能。在pH值为 7.0的NH3 ·H2 O -NH4Ac缓冲溶液中 ,加入 5滴TTZDBA作指示剂 ,用EDTA标准溶液进行滴定 ,滴定终点溶液的颜色变化敏锐 ,由紫红色变为亮橙色。将该方法用于试剂和钴基合金样品中钴的测定 ,测定结果与标准值相符 ,RSD(n =6 )为 0 .38%～ 1.5 2 %。     

2—（3,5—二溴—2—吡啶偶氮）—5—二乙氨基苯酚作络合滴定指示剂连续测 …

对２－（３,５－二溴－２吡啶偶氮）－５－二乙氨基苯酚作铁（Ⅲ）,铜（Ⅱ）的配位滴定指示剂进行了研究。在ＰＨ１．８￣２．０时用ＥＤＴＡ标准溶液滴定铁（Ⅱ）。在滴定铁（Ⅲ）后的溶液中,加处对铝过量的ＥＤＴＡ标准溶液,在ＰＨ３．８￣４．０煮沸下,铝（Ⅲ）与ＥＤＴＡ生成稳定的络合物,过量的ＥＤＴＡ用硫酸铜标准溶液滴定,从而测定铝（Ⅲ）（。     

络合滴定法测定硅铁中铝含量的改进

络合滴定法测定硅铁中铝量,GB4333.5—84中用甲基异丁基酮将铁萃取后,用硫酸铜标准溶液滴定过量的EDTA,加入氟化钠释放与铝络合的EDTA,再用硫酸铜标准溶液回滴,由于该法操作条件严格,费时,不能适用于一般中小企业生产控制要求.本文在试样以硝酸、氢氟酸溶解,高氨酸冒烟驱除氟后,采用氢氧化钠一氯化钠体系沉淀Fe(Ⅲ),过滤后加入过量EDTA,在pH 5.5条件下,用硫酸铜标准溶液滴定过量的EDTA,获得了令人满意的结果.1 主要试剂与仪器吡啶基偶氮萘酚(PAN)乙醇溶液:2g·L~(-1)乙酸-乙酸钠缓冲溶液:PH 5.5混合液:50g·L~(-1)氯化钠与10g·L~(-1)氢氧化钠溶液按1:1混合.对硝基酚乙醇溶液:2g·L~(-1)EDTA标准溶液:0.02mol·L~(-1),称取基准乙     

关于常温下EDTA络合滴定铝的几个问题

常温下EDTA络合滴定铝的有关实验已有详细报告。在一份试液中,以半二甲酚橙为指示剂,用铋盐回滴法连续测定铁、钛,然后加入对铝过量的EDTA标准溶液,以pH4.0的乙酸-乙酸钠缓冲溶液调节溶液pH至3.0～3.5,放置10分钟,用氨水(1:1)将溶液pH调节至5.5～6.0,再以半二甲酚橙为指示剂,用铅盐溶液回滴过剩的EDTA。本文拟对涉及方法有关的几个基本问题阐述于下。 1.溶液中铝的存在形态及其络合滴定的最佳pH范围。由实验可知Al~(8+)与EDTA络合     

EDTA滴定法快速测定铝锰镁合金中铝和镁方法探讨

以HCl溶解HClO4冒烟使试样完全溶解后,利用铝是两性元素的特性,加入过量的NaOH使Mg、Fe、Mn生成氢氧化物沉淀,过滤与铝分离.将滤液定容,移取部分在过量EDTA存在下,用HCl调节pH 4左右,加热煮沸使铝与EDTA配位络合,以PAN为指示剂,用CuSO4标准溶液返滴定过量的EDTA,加氟化钠取代出与铝定量配位络合的EDTA,再用CuSo4标准溶液滴定取代出的EDTA,求得铝量.将过滤出的Mg、Fe、Mn等氢氧化物沉淀,用热的稀HCl及H2O2溶解后,用NH3·H20(1+1)调节pH 5～6,加入铜试剂使Fe、Mn沉淀与Mg分离,于滤液中加NH4Cl缓冲液,以铬黑T为指示剂,用EDA标准溶液滴定镁量.     

2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸-过氧化氢催化动力学光度法测定痕量铁的研究

研究了铁(Ⅲ)催化H2O2氧化2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基苯甲酸(CTZDBA)的褪色反应及其动力学条件,褪色反应程度与铁(Ⅲ)量在一定范围内呈线性关系,建立了测定痕量铁(Ⅲ)的催化动力学光度法。在pH4.0的HAc-NaAc缓冲溶液介质中,褪色体系的最大吸收波长581nm,Fe(Ⅲ)的质量浓度在0.0008～0.04μg/mL范围内符合线性关系,回归方程为ΔA=25.325ρ-8.02×10-3(ρ:μg/mL),相关系数为0.9977,检出限3.78×10-10g/mL,方法用于头发和面粉中痕量铁的测定,结果与AAS测定结果相符。     

2-[2′-苯并噻唑偶氮]-1,8-二羟基萘-3,6-二磺酸的合成及与铝的显色反应研究

本文合成了新的显色试剂2-〔2’-苯并噻唑偶氮〕-1,8-二羟基萘-3,6-二磺酸,并研究了与铝的显色反应.在CTMAB存在下,铝与试剂于pH7.0～8.0的缓冲溶液中形成稳定的深紫红色络合物,组成为Al(Ⅱ):R=1:2表观摩尔吸光系数为1.46×10~5L·mol_(-1)·cm~(-1).铝浓度在0～5.0 μg/25mL范围内符合比尔定律.该方法灵敏度高,选择性好,并用于测定低合金钢、稀土硅镁合金和硅铁等试样中的微量铝.     

2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺与铱(Ⅲ)显色反应的研究及其应用

研究了新试剂2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺(5-I-PADMA)与铱(Ⅲ)的高灵敏显色反应。结果表明,在pH 5.6～7.3的HAc-NaAc缓冲溶液中,铱(Ⅲ)与5-I-PADMA可形成稳定的1：2配合物,其最大吸收峰位于475 nm;铱配合物形成后,当以适量的无机酸(HCl,H2SO4,HClO4,...     

A rapid complexometric scheme for analysis of iron, aluminium, calcium and magnesium in slags

A simple and rapid complexometric method has been developed for the simultaneous determination of iron, aluminium, calcium and magnesium in a single solution in slags. Phosphorous and small amounts of chromium (1.5 mg) and vanadium (1 mg) do not interfere in the titration. Titanium and manganese are suitably masked with lactic acid and tetra sodium pyrophosphate, respectively. In a suitable aliquot, iron is titrated at pH 2 with EDTA, using sulphosalicylic acid as indicator. To this solution, excess disodium 1,2-cyclohexane diamine tetra acetic acid (DCTA) is added and aluminium is titrated by titrating the excess DCTA with standard copper sulphate solution at pH 3.5, using 1-(2-pyridylazo)-2-naphthol (PAN) as an indicator. A known excess of EDTA is added, the pH is raised to 10 and calcium and magnesium are jointly titrated by titrating the excess EDTA with copper sulphate solution, using PAN indicator. The Ca-EDTA complex is demasked with ammonium oxalate at pH 5 and the released EDTA equivalent to calcium is titrated with copper sulphate solution at pH 10 with PAN indicator. Results of analysis compare favourably with certified values and values obtained by standard methods for BCS and other slags. A set of five samples can be analysed for iron, aluminium, calcium and magnesium in four hours as compared to three days by the classical conventional method.     

Extraction-spectrophotometric determination of trace iron (II) in sea water with 2-[2-(3,5-dibromopyridyl)azo]-5-diethylaminobenzoic acid

An extraction-spectrophotometric method is described for the determination of traces of iron(II) with 2-[2-(3,5-dibromopyridyl)azo]-5-diethyl-aminobenzoic acid. The reagent forms a stable and blue 12 iron/reagent complex that can be extracted into chloroform. The apparent molar absorptivity of the iron(II) complex is 1.09 × 10⁵ 1 mol^–1 cm^–1 at 624 nm in chloroform. The reagent is relatively selective; interferences from cobalt, copper, nickel and vanadium can be removed by using dimethylglyoxime and EDTA. The method is applied to the determination of iron (II) in sea water and aluminium alloys with good precision and accuracy.     

1—（5—溴—2—吡啶偶氮）—2—萘酚—6—磺酸作指示剂络合滴定连续测定铜和锌

对５－Ｂｒ－ＰＡＮ－Ｓ作指示剂络合滴定连续测定铜和锌进行了研究，在ｐＨ６．０的乙酸乙酸的钠介质中，以５－Ｂｒ－ＰＡＮ－Ｓ作指示剂，ＥＤＴＡ为滴定剂连续测定铜和锌，滴定终点颜色变化敏锐，准确度高，铜和锌量各在０～２０ｍｇ范围内与ＥＤＴＡ用量成正比，铜，锌比例在１：１０～１０：１范围内相互无影响，方法用于合金中铜，锌的连续测定，结果满意。     

PAN-6S作络合指示剂连续滴定测定汞和铅的研究

试验研究了pH3.0和pH5.4的介质中,以1 (2 吡啶偶氮) 2 萘酚 6 磺酸(PAN 6S)作为指示剂,以EDTA为滴定剂连续滴定汞和铅,其终点颜色变化敏锐,准确度高。     

Selective edta titration of gallium or aluminium in the presence of other metals

The selective determination of aluminium or gallium by EDTA titration is reported. Gallium or aluminium is titrated together with other multivalent ions with EDTA at pH 3-7 and then the pH is raised above 10.5. Aluminates or galliumates are formed with the consequent release of EDTA from the EDTA complexes. The released EDTA is titrated with lead solution using Xylenol Orange as an indicator and with copper using photometric detection of the end-point, for the determination of gallium and aluminium respectively. The theoretical basis of the procedure is discussed.     

新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸分光光度法测定微量钴

近年来,杂环偶氮苯甲酸类显色剂取得了较快的发展。由于氨基取代结构对试剂性能有较大的影响^[1],因此本文合成了新显色剂2-(2-噻唑偶氮)-5-二乙氨基苯甲酸,(TAEB)并研究了它与钴的显色反应。     

2-(5-硝基-2-吡啶偶氮)-5-二甲氨基苯胺与铑显色反应的研究及应用

本文报道了以新试剂2-(5-硝基-2吡啶偶氮)-5-二甲氨基苯胺(5-NO_2-PADMA)作分光光度法测定铑的新体系.结果表明,在 PH=5.25～6.75范围内,铑与 5-NO_2-PADMA形成 1:1的紫红色络合物,其 λ_(max)在 525 nm处,该络合物在 1.8mol/L的盐酸溶液中转变为绿兰色,其最大吸收峰位于620nm处,表观摩尔吸光系数为1.39×10～5L·mol～1·cm～1.反应具有良好的选择性,常见金属离子在一定范围内无干扰.铑含量为0～0.56μg/mL范围内遵守比耳定律.所拟方法操作简便,灵敏度高,用于催化剂中微量铑的测定,结果满意.     

Direct complexometric determination of magnesium in the presence of uranium, iron and aluminium

Conditions for the direct complexometric determination of magnesium in the presence of uranium, iron and aluminium are described. The method is based on the masking of uranium by hydroxylamine, and of iron and aluminium by triethanolamine. Methylthymol Blue is used as indicator for the EDTA titration of magnesium at pH 10.     

Rapid chelatometric determination of bismuth, titanium and aluminium using Semi-Xylenol Orange with visual end-point indication

A rapid and simple general complexometric method was presented for the determination of bismuth, titanium and aluminium in laboratory synthesized alloys similar to those of some bauxites, clay, ilmenite, Portland cements and ceramic products. The precision and accuracy attainable in successive titrations of Bi(3+), Ti(4+) and Al(3+) with 0.01 and/or 0.001M solutions of disodium ethylenediaminetetraacetate (Na(2)EDTA) and standard ZnCl(2) of the same concentration, using Semi-Xylenol Orange (SXO) as a metallochromic indicator with visual end-point indication were studied. For one aliquot Bi(3+) was at first directly titrated at pH 1-2 (HNO(3)) with Na(2)EDTA using SXO as indicator in the presence of L-ascorbic acid to reduce Fe(3+) to Fe(2+). At the bismuth end-point, an excess of Na(2)EDTA was added, the pH was adjusted with hexamine buffer (pH 5) and the excess of Na(2)EDTA was back-titrated with solution of standard zinc(II) chloride for both the simultaneous and consecutive titrations in the presence of (SXO) as indicator. For the simultaneous titration, fluoride was added to release the Na(2)EDTA combined with both Al(3+) and Ti(4+). For the consecutive titration, phosphate was added to release the Na(2)EDTA combined with Ti(4+) and then fluoride to release the Na(2)EDTA combined with Al(3+). The interference of various anions and cations in the determination of Bi(3+), Ti(4+) and Al(3+) was studied. A comparison of the accuracy of both the simultaneous and consecutive titration was also carried out. The proposed methods were applied successfully to some real samples of bauxites, clay, ilmenite, Portland cements and ceramic products and the results were satisfactory.