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| AN-U-021 |
Traces of nitrate in concentrated phosphoric acid with UV detection |
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| Determination of nitrate in concentrated phosphoric acid using anion chromatography with UV detection. |
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| AN-S-024 |
Fluoride, chloride and nitrate in an acidic nickel/zinc bath |
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| Determination of fluoride, chloride and nitrate in a solution of NiSO4, ZnSO4 in sulfuric acid using anion chromatography with conductivity detection after chemical suppression. |
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| AN-N-028 |
Traces of bromide in hydrochloric acid (32%) using amperometric detection |
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| Determination of traces of bromide in HCl (32%) using anion chromatography with amperometric detection at the silver electrode. |
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| AN-N-022 |
Traces of iodide in hydrochloric acid (25%) using amperometric detection |
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| Determination of traces of iodide in HCl (25%) using anion chromatography with amperometric detection at a silver electrode. |
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| AN-N-003 |
Five anions in solder paste |
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| Determination of anions in solder paste after alcoholic extraction using anion chromatography with direct conductivity detection. |
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| AN-H-084 |
Determination of sulfuric, phosphoric and nitric acid mixtures |
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| Determination of mixtures of sulfuric, phosphoric, and nitric acids. The procedure is suitable for automated analysis using an 814 Sample Processor. |
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| AN-H-080 |
Determination of total sodium in sodium aluminate liquors by aluminum titration |
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| Determination of the total sodium content of sodium aluminate liquors, such as Bayer Process liquor. This method is suitable for the analysis of all sodium aluminate solutions down to at least 1 g/L as Na2CO3. The determination may be automated by adding an 814 USB sample processor to an 859 Titrotherm |
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| AN-H-075 |
Standardization of tetrasodium EDTA solutions |
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| Standardization of ~1mol/L tetrasodium EDTA solutions for thermometric complexometric analysis. |
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| AN-H-074 |
Determination of calcium and magnesium in sea water |
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| Determination of calcium and magnesium in sea water. The method is suitable for determining the effect of caustic soda and alumina refinery aluminate solutions on the calcium and magnesium content of sea water. |
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| AN-H-070 |
Determination of ferric and cupric Ions in copper refining solutions |
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| Determination of Fe3+ and Cu2+ in copper refining solutions by thermometric titration. It was found that the conventional approach of masking Fe3+ to permit the iodometric determination of Cu2+ is not possible in some copper refining solutions. |
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| AN-H-069 |
Determination of ferric ion by titration with fluoride |
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| Determination of Fe3+ by thermometric titration. Al 3+ must be absent. Useful for determination of Fe3+ in the presence of Cu2+ and Fe2+ in copper refining solutions. |
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| AN-H-068 |
Determination of ferric ion by iodometric titration |
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| Determination of Fe3+ by iodometric titration. Useful if Fe3+ is accompanied by Al3+, Mg2+, Ca2+ and Fe2+. |
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| AN-H-067 |
Determination of chloride in Bayer process liquor |
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| Determination of chloride in Bayer process liquor. |
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| AN-H-057 |
Standardization of sodium fluoride for aluminum titrations |
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| Standardization of sodium fluoride titrant for determination of aluminum. |
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| AN-H-053 |
Determination of aluminum by fluoride titration |
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| Determination of aluminum in acidic, basic and neutral solutions; including aluminum chloride, aluminum chlorohydrate (also in anti-perspirant formulations), alum, etching solutions and aluminate solutions. |
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| AN-H-047 |
Determination of nickel by EDTA back-titration |
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Determination of nickel in refinery and plating solutions. When other metals capable of being complexed by EDTA
are present, these will interfere and enhance the result for nickel. |
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| AN-H-046 |
Standardization of copper back-titrant by EDTA |
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| Standardization of copper back-titrant using standard tetrasodium EDTA titrant in the determination of metals. |
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| AN-H-045 |
Standardization of EDTA titrant by magnesium |
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| Standardization of tetrasodium EDTA titrant for use in the determination of magnesium. |
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| AN-H-044 |
Standardization of EDTA titrant by copper |
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| Standardization of tetrasodium EDTA titrant for use in the determination of metals. |
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| AN-H-043 |
Determination of copper by iodometric titration |
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Determination of copper, principally in copper mining and refining solutions. The method may also be used for
determination of purity of copper metal. Optimal results are obtained when aliquots containing copper in the range
approximately 3 – 6 mmol Cu are titrated. |
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| AN-H-027 |
Determination of organic soda in Bayer aluminate liquors |
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| Determination of total basicity of extractable organic compounds of acidic character in Bayer process refinery liquors. |
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| AN-H-026 |
Determination of caustic, carbonate and alumina in Bayer Process liquors |
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Determination of caustic, carbonate and alumina in Bayer Process liquors using a method based on procedures developed by Watts-Utley1 and VanDalen-Ward2.
1 H. L. Watts and D. W. Utley, Anal. Chem. 28, 1731 (1956)
2 E. VanDalen and L. G. Ward, Anal. Chem. 45, 2248 (1973)
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| AN-H-023 |
Determination of nickel by dimethylglyoxime titration |
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| Determination of nickel in the absence of cobalt and other interferences. |
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| AN-H-021 |
Determination of free acid in copper refining solutions |
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| Determination of free acid in copper refining solutions. |
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| AN-H-014 |
Determination of free acid content of solutions containing Fe(III) |
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| Determination of free acid in solutions containing metal ions, particularly Fe(III). |
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| AN-H-005 |
Determination of cuprous ions in the presence of ferrous ions |
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| Determination of cuprous ions in the presence of ferrous ions in electrochemical copper leaching solutions. |
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| AN-C-061 |
Zinc and manganese in the presence of standard cations in an extract of a zinc compound |
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| Determination of zinc, sodium, ammonium and manganese in the presence of magnesium and calcium in an extract of a zinc compound using cation chromatography with direct conductivity detection. |
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| AB-300 |
Determination of cyanide in process water of the steel industry |
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The production of steel involves many different materials and procedures. In order to achieve a smooth, reliable production process and obtain a good product quality, the materials and procedures have to be controlled very thoroughly. One important component in the steel production is process water that is used for cooling the blast
furnace and for washing and cleaning the top gases (blast-furnace gases). After top gas purification the scrubbing water contains dissolved cyanide and the water can only be returned to the public sewage system if the cyanide concentration is below the legal limits.
The ProcessLab setup described here offers a measurement and monitoring solution and provides various options for reacting to any situation. With the aid of the input/output controller, the measured analytical values are easily transferred to the process control center in the form of 4…20 mA analog signals. On the basis of these values, all further process steps are initiated and controlled automatically in the process control center. |
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| AB-295 |
Determination of Fe2+, Fe3+, total and free acid in an etching bath (steel industry) |
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Acid etching baths are used for oxide removal and cleaning of the surface of different types of steel. To keep the bath in an optimum condition the Fe2+/Fe3+ and free acid/total acid ratios must be maintained within certain limits. Auxiliary substances like hydrogen peroxide are added to influence the Fe2+/Fe3+ ratio, which is responsible for a constant activity of the bath.
The quality of the end products depends directly on the correct composition of the etching bath. Keeping these parameters in an optimum range results in a permanently higher quality and at the same time lowers costs due to lower reagent consumptions. This bulletin describes the monitoring of an etching bath in the steel industry. ProcessLab offers a solution that automatically evaluates the desired bath parameters (free acid, total acid, Fe2+ and Fe3+). Due to the flexibility offered by ProcessLab the determination of hydrogen peroxide can be integrated very easily. |
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| AB-293 |
Analysis of Bayer Aluminate Liquors with 859 Titrotherm |
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The purpose of this manual is to assist the analyst engaged in the determination of sodium aluminate liquor to quickly set up the 859 Titrotherm titration system to perform this task. While every effort has been made to make this easy, it is not
possible to provide for every situation. The analyst must be prepared to make modifications to the procedures where appropriate.
The two complexant method described in this manual is based on the procedure originally developed by Watts and Utley1, and modified for use in thermometric titrimetry by VanDalen and Ward2. It is arguably the fastest and most reliable determination for the analysis of Bayer Process liquor. This manual is dedicated to an explanation of the application of the Van Dalen-Ward method to the 859 Titrotherm titration system. However, the method as presented has a considerable number of refinements and improvements over VanDalen and Ward’s original work; not the least
in the ability to measure the carbonate content of the liquor. This method has been designated as the “Bayer Classic” method, in reference to the origins of the analytical chemistry involved.
This manual is a component of a package of files which assists the analyst in rapidly setting up Titrotherm to perform analyses on Bayer liquors. The other components of this package comprise:
- Pre-optimized titration files which can be converted to titration methods.
- An Excel worksheet template which is linked to the titration methods, and automatically calculates results for caustic, alumina and carbonate in both American and European alumina refining conventions.
References (1) H.L. Watts and D.W. Utley, Anal. Chem. 28,1731 (1956). (2) E. VanDalen and L.G. Ward, Anal. Chem. 45, 2248 (1973). |
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| AB-183 |
Fully automatic analysis of Bayer liquors |
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Determination of free alkali and total alkali as well as aluminum in a sample.
By the addition of sodium gluconate the OH- ions of the aluminate complex are released and determined by titration with HCl. After the titration the aluminum hydroxide is recomplexed with potassium fluoride; the released OH- ions can either be titrated with acid or the excess acid can be titrated with alkali. |
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| AB-176 |
Simultaneous determination of lead and tin by anodic stripping voltammetry |
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In most electrolytes the peak potentials of lead and tin are so close together that a voltammetric determination is impossible. Difficulties occur especially if one of the metals is present in excess. Method 1 describes the determination of Pb and Sn. Differential pulse anodic stripping voltammetry (DPASV) is used under addition of cetyltrimethylammonium bromide. This method is used when:
- one is mainly interested in Pb
- Pb is in excess
- the Sn:Pb ratio is not higher than 200:1
According to method 1, Sn and Pb can be determined simultaneously if the difference in the concentrations is not too high and Cd is absent.
Method 2 is applied when traces of Sn and Pb are found or interfering TI and/or Cd ions are present. This method also uses DPASV in an oxalate buffer with methylene blue addition.
Method 3 in this Bulletin describes the determination of Sn(II) in presence of Sn(IV) by DPASV. Using an electrolyte containing fluoride, Sn(IV) gives no signal, so that a speciation is possible. |
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| AB-132 |
Polarographic determination of molybdenum in strongly ferruginous materials |
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| A method is described in this Bulletin that allows molybdenum to be determined in steel and other materials containing a high iron concentration. Mo(VI) is determined at the dropping mercury electrode by catalytic polarography. The determination limit is approx. 10 μg/L Mo(VI). |
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| AB-101 |
Complexometric titrations with the Cu ISE |
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| This Bulletin describes the complexometric potentiometric titration of metal ions. An ion-selective copper electrode is used to indicate the endpoint of the titration. Since this electrode does not respond directly to complexing agents, the corresponding Cu complex is added to the solution. With the described electrode it is possible to determine water hardness and to analyze metal concentrations in electroplating baths, metal salts, minerals and ores. The following metal ions have been determined: Al3+, Ba2+, Bi3+, Ca2+, Co2+, Fe3+, Mg2+, Ni2+, Pb2+, Sr2+ and Zn2+. |
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| AB-093 |
Potentiometric analysis of cadmium plating baths |
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| This Bulletin describes titrimetric methods for the determination of cadmium, free sodium hydroxide, sodium carbonate and total cyanide. The free cyanide can be calculated from the total cyanide and the Cd content. |
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| AB-092 |
Potentiometric analysis of lead plating baths |
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| This Bulletin describes the potentiometric determination of lead, tin(II) and free fluoroboric acid. |
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| AB-091 |
Potentiometric analysis of brass and bronze plating baths |
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Methods are described for the potentiometric analysis of the following bath components: Brass plating bath: copper, zinc, free cyanide, ammonium, carbonate and sulfite
Bronze plating bath: copper, tin and free cyanide |
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| AB-090 |
Potentiometric analysis of tin plating baths |
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| Potentiometric titration methods for the analysis of acid and alkaline tin plating baths are presented. The following methods are described: tin(lI) / tin(IV) / total tin, free fluoroboric acid or free sulfuric acid, chloride in acidic tin baths, free hydroxide and carbonate in alkaline tin baths. |
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| AB-061 |
Potentiometric determination of silver |
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| This Bulletin describes a potentiometric method for the determination of silver in fine silver, silver alloys and silver plating baths. After digestion of the sample with nitric acid, titration is performed with potassium bromide solution using the Ag Titrode with AgBr coating. |
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| AB-049 |
Colorimetric determination of copper |
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Application Bulletin no. 43 describes the polarographic determination of copper. For copper concentrations of 10 mg/L and below, however, colorimetric methods are also used, particularly in water analysis.
The method using sodium diethyldithiocarbamate can be employed down to a minimum limit of 0.01 mg/L Cu, but suffers from the drawback that the determination can also be affected by other metal ions.
The method using neocuproine has a minimum concentration limit of 0.1 mg/L Cu, but has the advantage of being unaffected by ions of other metals.
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| AB-046 |
Potentiometric determination of cyanide |
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The determination of cyanide is very important not only in electroplating baths and when decontaminating wastewater but, due to its high toxicity, also in water samples in general. Concentrations of 0.05 mg/L CN- can already be lethal for fish. This Bulletin describes the determination of cyanide in samples of different concentrations by means of potentiometric titration. Chemical reactions: 2 CN- + Ag+ → [Ag(CN)2]- [Ag(CN)2]- + Ag+ → 2 AgCN |
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| AB-037 |
Determination of chromium in iron and steel |
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| Two methods are described for the determination of chromium: a biamperometric titration and a polarographic analysis. |
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| AB-036 |
Polarographic analysis - half-wave potentials of inorganic substances |
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| In the following tables the half-wave potentials or peak potentials of 90 metal ions are listed. The half-wave potentials (listed in volts) are measured at the dropping mercury electrode (DME) at 25 °C unless indicated otherwise. |
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| AB-030 |
Photometric determination of chromium(VI) |
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With chromates and dichromates, diphenylcarbazide gives a red-violet coloration which can be measured with the 662 Photometer. The reaction is extremely sensitive, enabling concentrations of ρ(Cr) < 0.1 mg/L to be measured without difficulty. In electroplating effluents, chromium occurs as the Cr(VI) ion. It must first be reduced to Cr(III) and then precipitated as the hydroxide. With incomplete reduction, hexavalent chromium remains in solution in the effluent water. For this reason, periodic checks for chromium in the effluent are necessary. |
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| AB-024 |
Potentiometric determination of aluminum |
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Aluminum compounds dissolved in water are treated with an organic complexing agent (gluconate or tartrate) and the pH is adjusted with NaOH to 11.5...12. The free alkali is now titrated and the solution is treated with potassium fluoride. After the reaction has been completed the released alkali, which is proportional to the aluminum content, is back-titrated with HCl. Al(OH)3 + KF → K3AlF6 + 3 OH- |
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| AB-21 |
Bibliography concerning the polarographic determination of lead in different materials |
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| Bibliography concerning the polarographic determination of lead in different materials |
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| AB-016 |
Routine determination of copper in brass, bronze, German silver and in electroplating baths |
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| A routine method for the determination of copper is described. After dissolving the sample and adding a KI/KCNS solution, the released iodine is back-titrated with thiosulfate. The endpoint indication is potentiometric. |
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| AB-014 |
Determination of nickel by potentiometric titration |
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A potentiometric method for the determination of nickel in gold and silver electroplating baths is described. The titration is carried out with KCN. Gold and silver are removed before titration by a reduction process. It is also possible to determine nickel in steel alloys, etc. (see the literature reference). Ni2+ + 4 KCN + 2NH4+ -> (NH4)2[Ni(CN)4] + 4 K+ |
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| AB-011 |
Determination of zinc by bi-amperometric titration with potassium hexacyanoferrate(II) |
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Zinc, such as that occurring as a constituent of light alloys, can be determined by precipitation titration with potentiometric endpoint indication. The determination of zinc in the presence of cadmium is also possible. 2 K4[Fe(CN)6] + 3 ZnCl2 → K2Zn3[Fe(CN)6]2 + 6 KCl. |
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| AB-004 |
Biamperometric titration method for the determination of antimony in lead |
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| An automatic titration method is described using biamperometric endpoint indication for the determination of antimony in antimony-alloyed cable lead (approx. 1% Sb). A 0.01 mol/L KBrO3 solution is used as the titrant. |
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