Titration automatic titrators

Derivative methods work well only when sufficient data are recorded during the sharp rise in plT occurring near the equivalence point. This is usually not a problem when the titration is conducted with an automatic titrator, particularly when operated under computer control. Manual titrations, however, often contain only a few data points in the equivalence point region, due to the limited range of volumes over which the transition in plT occurs. Manual titrations are, however, information-rich during the more gently rising portions of the titration curve before and after the equivalence point. 

The following data were collected with an automatic titrator during the titration of a monoprotic weak acid with a strong base. Prepare normal, first-derivative, second-derivative, and Gran plot titration curves for this data, and locate the equivalence point for each. 

Phosphoms content usually is measured by a double end point titration method in which a 1.0-g sample is dissolved in a hot HNO —H2SO4—HCIO4 mixture. The pH is adjusted to 2.5 with NaOH, and the resulting H PO is titrated with 0.5-A[ NaOH, using an automatic titrator. The titer between the first and second end points is used to quantify the phosphoms as H PO. ... 

The use of "fixed" automation, automation designed to perform a specific task, is already widespread ia the analytical laboratory as exemplified by autosamplers and microprocessors for sample processiag and instmment control (see also Automated instrumentation) (1). The laboratory robot origiaated ia devices coastmcted to perform specific and generally repetitive mechanical tasks ia the laboratory. Examples of automatioa employing robotics iaclude automatic titrators, sample preparatioa devices, and autoanalyzers. These devices have a place within the quality control (qv) laboratory, because they can be optimized for a specific repetitive task. AppHcation of fixed automation within the analytical research function, however, is limited. These devices can only perform the specific tasks for which they were designed (2). 

Small amounts of moisture (up to about 0.5%) in crystalline sugars can be determined chemically by titration with Kad Fisher reagent. A volumetric Kad Fisher titration procedure for moisture in molasses is accepted by AO AC. Automatic Kad Fisher titrators are available, and as acceptance of pyddine-free reagents increases, their use may increase. 

Assay of beryUium metal and beryUium compounds is usuaUy accompHshed by titration. The sample is dissolved in sulfuric acid. Solution pH is adjusted to 8.5 using sodium hydroxide. The beryUium hydroxide precipitate is redissolved by addition of excess sodium fluoride. Liberated hydroxide is titrated with sulfuric acid. The beryUium content of the sample is calculated from the titration volume. Standards containing known beryUium concentrations must be analyzed along with the samples, as complexation of beryUium by fluoride is not quantitative. Titration rate and hold times ate critical therefore use of an automatic titrator is recommended. Other fluotide-complexing elements such as aluminum, sUicon, zirconium, hafnium, uranium, thorium, and rate earth elements must be absent, or must be corrected for if present in smaU amounts. Copper-beryUium and nickel—beryUium aUoys can be analyzed by titration if the beryUium is first separated from copper, nickel, and cobalt by ammonium hydroxide precipitation (15,16). 

It was indicated that the original method can be extended on systems where two or three analytes can be determined from a single titration curve. The shifts DpH affected by j-th PT addition should be sufficiently high it depends on pH value, a kind and concentration of the buffer chosen and its properties. The criterion of choice of the related conditions of analysis has been proposed. A computer program (written in MATLAB and DELPHI languages), that enables the pH-static titration to be done automatically, has also been prepared. 

There are two types of fluoride lon-selective electrodes available [27] Onon model 96-09-00, a combination fluoride electrode, and model 94-09-00, which requires a reference electrode The author prefers to use Onon model 94-09-00 because it has a longer operational life and is less expensive When an electrode fails, the reference electrode is usually less expensive to replace The Fisher Accumet pH meter, model 825 MP, automatically computes and corrects the electrode slope It gives a direct reading for pH, electrode potential, and concentra tion in parts per million The fluoride lon-specific electrode can be used for direct measurement [2S, 29] or for potenPometric titration with Th" or nitrate solutions, with the electrode as an end point indicator... 

The methods dependent upon measurement of an electrical property, and those based upon determination of the extent to which radiation is absorbed or upon assessment of the intensity of emitted radiation, all require the use of a suitable instrument, e.g. polarograph, spectrophotometer, etc., and in consequence such methods are referred to as instrumental methods . Instrumental methods are usually much faster than purely chemical procedures, they are normally applicable at concentrations far too small to be amenable to determination by classical methods, and they find wide application in industry. In most cases a microcomputer can be interfaced to the instrument so that absorption curves, polarograms, titration curves, etc., can be plotted automatically, and in fact, by the incorporation of appropriate servo-mechanisms, the whole analytical process may, in suitable cases, be completely automated. 

In piston burettes, the delivery of the liquid is controlled by movement of a tightly fitting plunger within a graduated tube of uniform bore. They are particularly useful when the piston is coupled to a motor drive, and in this form serve as the basis of automatic titrators. These instruments can provide automatic plotting of titration curves, and provision is made for a variable rate of delivery as the end point is approached so that there is no danger of overshooting the end point. 

The method (which is largely electrical in nature) is readily adapted to remote control this is significant in the titration of radioactive or dangerous materials. It may also be adapted to automatic control because of the relative ease of the automatic control of current. 

A minor disadvantage of external generation of titrant is the dilution of the contents of the titration cell care is therefore necessary in suitably adjusting the rate of flow and the concentration of the generator solution. The procedure is, however, admirably suited for automatic control. 

Unless the curve has been plotted automatically, the accuracy of the results obtained by any of the above procedures will be dependent upon the skill with which the titration curve has been drawn through the points plotted on the... 

As has been indicated, if suitable automatic titrators are used, then the derivative curve may be plotted directly and there is no need to undertake the calculations described above. 

With this simplified procedure it is much easier to protect the system from atmospheric moisture, which must obviously be excluded. Modem K-F Titrators are equipped with special titration vessels which are designed to prevent the ingress of atmospheric moisture. Many also have microprocessors attached which will carry out the requisite operations automatically and will often provide a print-out of the results including the percentage moisture content. 

A 3 litre bioreactor with a working volume of 2 litre is inoculated with the three shaking flasks. The pH is maintained at 5.5 by automatic titration with 5mol l 1 NH4OH and the temperature is held at 37°C. 

FIG. 11 Titration plot of alkanesulfonates. Sample 60 wt % of Hostapur SAS 60, monosulfonates fraction contents ca. 140 mg/100 ml (10% MeOH) solution to be titrated 10 ml, 5 ml buffer pH 3 (Merck), 5 ml MeOH, diluted to 100 ml with water titrant 0.004 mol/l TEGOtrant A 100 (l,3-didecyl-2-methyl-imidazolium chloride, Metrohm 6.2317.000) titrator Titrino 716 DMS with automatic titrator 727 and propellant stirrer titration mode dynamic end point titration (DET), high-sense electrode Metrohm 6.0504.15Q, reference electrode Ag/AgCl Metrohm 6.0733.100, EP = end point. 

Physical methods for endpoint detection have been suggested. Hellsten [226] proposed an instrumental turbidimetric method to determine the endpoint, which does not need indicators. Since chloroform is emulsified by the anionic surfactant, changes in the optical density can be followed by a colorimeter thus detecting the endpoint when the emulsion breaks. Another turbidimetric method based on commercially available automatic titrators has also been proposed [227],... 

A plot of the pH of the analyte solution against the volume of titrant added during a titration is called a pH curve. The shape of the pH curve in Fig. 11.4 is typical of titrations in which a strong acid is added to a strong base. Initially, the pH falls slowly. Then, at the stoichiometric point, there is a sudden decrease in pH through 7. At this point, an indicator changes color or an automatic titrator responds electronically to the sudden change in pH. Titrations typically end at this point. However, if we were to continue the titration, we would find that the pH... 

A simple, reliable, and fast method of determining the pH of a solution and of monitoring a titration is with a pH meter, which uses a special electrode to measure H 0+ concentration. An automatic titrator monitors the pH of the analyte solution continuously. It detects the stoichiometric point by responding to the characteristic rapid change in pH (Fig. 11.9). Another common technique is to use an indicator to detect the stoichiometric point. An acid-base indicator is a water-soluble organic dye with a color that depends on the pH. The sudden change in pH... 

FIGURE 11.9 A commercially available automatic titrator. The stoichiometric point of the titration is detected by the sudden change in pH that occurs in its vicinity the pH is monitored electronically. The pH curve can be plotted as the reaction proceeds, as shown on the monitor screen. 

Endgroup analyses were carried out with an automatic potentiometer. The [-NH2] and [-C00H] were determined simultaneously. The polymer was dissolved in o-cresol/chloroform mixture (70/30), excess alcoholic KOH added and titrated with alcoholic HCl (0.1 N). The inherent viscosities were determined in0.5% solutions... 

FIGURE 3 Effect of the amount of cholesterol on the particle size. Phosphatidylcholine/cholesterol liposomes were prepared by the octyl glucoside dilution technique. The begin concentration of the mixed micelles was 150 mM octyl glucoside and 10 mM phosphatidylcholine in 10 mM tris(hydroxymethyl)aminomethane and 0.9% NaCl, pH 7.4. Dilution was performed with an automatic titration unit at a dilution rate (= dilution factor, relative to the initial volume, per unit of time) of 0.026 sec"l ( a and ) or 0.69 sec l ( and o). Mean diameters after dilution and ) and after filtration ( L and q) are repi sented. (Adapted from Jiskoot et al, 1986a.)... 

Cotlove, E. and Nishi, H. H. Automatic titration with direct read-out of chloride concentration. Clin. 

After 24 h of reaction, the catalytic bed was retrieved and sieved to separate the catalyst from the diluent. The used catalyst particles were placed in a Soxhlet apparatus, washed with n-hexane for 8 hours and then dried overnight at 393 K. Their carbon content was determined by automatic titration of the CO2 formed by burning the washed sample, in a Strohlein Coulomat 702 apparatus. 

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