An automatic back titration method for microchemical analysis

An automatic back titration method for microchemical analysis is introduced, which is based on conventional volumetric analysis's principle and the use of flow injection analysis apparatus for the automation and microminiaturization of the process. The sample and a known, but excess amount of a calibrated reagent solution are injected and propelled into a titration cell, where their reaction takes place. The excess of the reagent is then titrated with a titrant containing an indicator and the end point is monitored photometrically. Since homogeneous mixing in the titration cell is obtained magnetically in the whole process, there is a linear relationship between the analyte's concentration and the volume of the titrant consumed. Nickel in the range of 10-70 g 1(-1) is determined by the above method, in which 30 microl of sample and 500 microl of EDTA are injected and the excess of EDTA is titrated with a standard zinc salt solution containing xylenol orange which could be blocked by nickel ion in a direct titration. This method is characteristic of low sample and reagent consumption, high sampling rate as high as 45 samples h(-1), negligible effect of sample's viscosity, small carry-over effect (lower than 0.14%), and very good precision, whose relative standard deviations are as small as 0.24%.     

自动电位滴定法快速测定钾盐中的钾含量

钾含量的测量常用火焰光度法和四苯硼钾重量法。火焰光度法适用于微量分析 ,对较高含量钾的测定误差较大 ,四苯硼钾重量法的测定准确度高 ,但操作繁琐 ,测定周期长 ,易出错。本文采用四苯硼钠溶液电位滴定法 ,测定高、中含量组分钾 ,测定周期短 ,所用试剂少 ,且不受样品中水不溶物的干扰 ,选择性好 ,测定的准确度和精密度均在 0 .2 %以下 ,适用于钾盐、卤水、复合肥和钾肥中钾的测定。1　实验部分1 .1　仪器和药品ZD 2型自动电位滴定仪 (上海雷磁仪器厂 ) ,PK 1型钾离子选择电极 ,2 1 7型饱和甘汞电极 (双盐桥 )。四苯硼钠标准液 :0 .1mol…     

An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach

An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes.     

Critical comparison of evaluation methods of potentiometric titration data using a microcomputer-controlled automatic potentiometric titration system

A microcomputer-controlled automatic potentiometric titrator withP controlled intelligent auto-sampler has been built for serial analysis. Controlling and evaluating programs have also been written. In order to use the most powerful evaluating method, a comparison was made between the methods. The data of the titration curves were obtained by the implicit relation characterizing the curve. The different evaluating methods were tested by using these data. The effects of random errors stemming from measurements were also investigated. The methods used were: two point differentiating formula, differentiation of interpolating and smoothing spline functions, the Gran method, and implicit regression with the Gauss-Newton-Marquardt method. Regression is outstanding among the methods, but it needs much more computing time compared with others. The second-best method is the differentiation with smoothing spline function with end point determination based on finding the sign reversal of the second derivative. This method is much faster than regression.     

Substitution titration: a new approach to automatic titration : Determination of Acidity in Precipitation Samples

In substitution titrations, a small portion of the sample is repeatedly replaced by an exactly equal volume of titrant, by means of a rotary injection valve. The titration curves obtained in this manner can be linearized by using suitable functions, and hence equivalence volumes can be calculated. The substitution process means that there is no increase in volume during a titration. It is therefore possible to use a completely closed system, which is advantageous for samples that are sensitive to the ambient atmosphere. The principle is demonstrated for the potentiometric titration of hydrochloric acid containing varying amounts of weak acid (acetic acid or ammonium ion) with sodium hydroxide solutions. By the substitution titration, it is possible to determine the strong and weak acid in HCl/NH₄Cl mixtures with an accuracy of ca. 2%, but acetic acid is difficult to determine in the mixture because of partial protolysis at the concentration level examined. Sample concentrations are chosen in the range 125–1000 μM total acidity, to conform with the concentrations normally found in precipitation samples. The development of a procedure for determining the acidity in rain-watet and throughfall samples is described. The substitution titrations are easily automated and provide adequate sensitivity for routine work.     

The automatic titration of primary aromatic amines with nitrous acid

The “dead-stop” and potentiometric systems have been compared as a basis for the automatic titration of primary aromatic amines with nitrous acid; either system can be used but the potentiometric method is more widely applicable and is less subject to interference. Titrations of sulphanilamide and o-anisidine have been made with two commercial titrimeters and with both instruments the results obtained were at least equal in precision to those which would normally be obtained in manual titrations.     

火试金富集--自动电位滴定法测定粗碲中的银含量

粗碲是由铜、铅、锌冶炼带来的副产品,其中含有大量的金、银等贵金属。快速准确检测粗碲中银含量,具有十分重要的意义。样品预先采用硫酸溶解,还原沉淀金、银,过滤分离大部分的铋、硒、碲等元素,经配料、高温熔融,熔融态的金属铅捕集试料中的贵金属形成铅扣,试料的其他物质与熔剂生成易熔性熔渣。将铅扣灰吹,得金银合粒,清除合粒表面粘附的杂质,经硝酸分金,用硫氰酸钾滴定法测定银量。银的加标回收率在99.5%～101%,相对标准偏差(RSD)小于5%。方法速度快,稳定性好,适用于粗碲中银含量的测定。     

Analysis of polymer blends and copolymers by coupled thermogravimetry and automatic titration

A technique coupling automatic titration to thermogravimetry is described. The amount of a selected component in the volatiles produced under precise heating conditions in a DuPont 951 thermogravimetric analyzer is quantitatively determined with a Radiometer recording titration system. With the combined information on temperature, weight loss and chemical compositional changes, the stability and degradation mechanism of a sample are conveniently studied. Of particular interest is the use of such a technique to analyze polymer blends and copolymers in complex systems. Examples will be given to illustrate the various features of this application.     

A simple automatic system using the HP-85 microcomputer for programmed potentiometric titration

A simple way of constructing an automatic titration system is proposed, based on combination of a digital pH-meter and an automatic burette with an HP-85 microcomputer. An inexpensive interface unit based on a MOTOROLA 6800 has been developed, which permits communication of the computer with the pH-meter and the burette. The system constructed is very flexible and can find wide application in potentiometric titration and direct potentiometry with different kinds of ion-selective electrodes.     

An automatic controlled-potential coulometer

The design and operation of an automatic controlled-potential coulometer is described. It was primarily designed for use with mg quantities of uranium, neptunium and plutonium but can in principle be used on any element possessing more than one valency state in solution. It is capable of an accuracy and precision of ±0.25% and can analyse up to 20 samples on a set programme without operator attention.     

An automatic adiabatic low temperature calorimeter

The calorimeter, for use at temperatures from 5° to 330°K, has several novel features. Servoloops have been developed that will maintain the sample environment at a temperature virtually the same as the sample container. All factors necessary for calculation of the results are controlled and recorded automatically as a function of time. Results on n-heptane are presented and serve to establish the reliability of this equipment.     

An isothermal titration calorimetry study of phytate binding to lysozyme

Isothermal titration calorimetry (ITC) was used to detect phytate binding to the protein lysozyme. This binding interaction was driven by electrostatic interaction between the positively charged protein and negatively charged phytate. When two phytate molecules bind to the protein, the charge on the protein is neutralised and no further binding occurs. The stoichiometry of binding provided evidence of phytate–lysozyme complex formation that was temperature dependent, being most extensive at lower temperatures. The initial stage of phytate binding to lysozyme was less exothermic than later injections and had a stoichiometry of 0.5 at 313 K, which was interpreted as phytate crosslinking two lysozyme molecules with corresponding water displacement. ITC could make a valuable in vitro assay to understanding binding interactions and complex formation that normally occur in the stomach of monogastric animals and the relevance of drinking water temperature on the extent of phytate–protein interaction. Interpretation of ITC data in terms of cooperativity is also discussed.     

A simple differential titrator for automatic potentiometric titration at zero current, with two identical indicator electrodes

A simple differential titrator for automatic potentiometric titration at zero current, with two identical indicator electrodes, is described. The autoburette is a normal microburette connected to one tube of a peristaltic pump, and the differentiating system is a closed-flow circuit in a second tube of the pump, this tube containing two electrodes 5 cm apart. The apparatus has been applied to the determination of halides and sulphide-disulphide mixtures, with electrodes coated with an appropriate silver salt.     

The titration error in potentiometric precipitation titration

The titration error can be calculated with the aid of the value of the buffer index determined at the inflection point of the titration curve when a precipitation titration is followed with an ion-selective electrode. When the precipitate is not formed ideally in the titration (i.e., is not formed under equilibrium conditions) the titration error cannot be predicted from the values of the solubility product, nor can the values of the solubility product be calculated from titration data at the inflection point.     

An automatic NAA analyzer for short-lived nuclides

An automatic activation analyzer with sample changer, pneumatic transfer system and fast pulse counting with real time pulse pile-up and dead time compensation is described. Transfer times between 80 and 300 ms from irradiation position to measurement station can be obtained. Counting losses are corrected within 10% up to total count rates of 120 kc/s.