Description This application report describes the general procedure for the titer determination of EDTA solutions. As reference material CaCO3 or Zink is used. The titer is a dimensionless number about 1 for correcting the indicated concentration. In the software of ® the titration devices and application reports from SI Analytics , the term “Titer“ describes the exact concentration in mol/l and not the dimensionless factor.
Instruments Titrator TL 5000 or higher Exchangeable Unit WA 20 (only for TL 7000 or higher) Electrode Cu 1100 Cable L1A Reference electrode B 2920+ Cable L1N Stirrer Magnetic stirrer TM 235 or similar Lab accessoires Glas beaker 150 ml Magnetic stirrer bar 30 mm
Reagents 1 Na2EDTA - solution 2 Calcium carbonate certified reference material, volumetric standard 3 Zink certified reference material, volumetric standard 4 Ammonia solution 25% 5 Ammonium chloride 6 Copper-EDTA solution 0.1 mol/l (Cu(NH4)2-EDTA) 7 Hydrochloric acid 25% 8 Distilled water 9 Elektrolyt solution L300 All reagents should be in analytical grade or better.
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Titration procedure Reagents Buffer solution pH 10 Dissolve 54.0 g of ammonium chloride in a little water, add 350 ml of ammonia solution 25% and make up to 1.0 liter with water.
The CaCO3 or Zn volumetric standard is dried as described in the corresponding certificate of analysis.
Cleaning and storage of the electrode
The electrodes are cleaned with distilled water. The Cu 1100 is stored clean and dry, for the storage of the reference electrode use electrolyte solution L300.
Sample preparation The CaCO3 or Zn volumetric standard is dried as described in the corresponding certificate of analysis.
The amount of volumetric standard depends on the size of the burette and the concentration of the EDTA. The amount should be chosen so that about half of the burette volume is consumed. The most common is the 20 ml burette. The required quantity of CaCO3 can be estimated according to this rule of thumb:
𝑊 [𝑔] = 1 ∗ 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛[𝑚𝑜𝑙/𝑙]
At lower concentrations than 0.1 mol/l, the required amount of reference material is very small and difficult to weigh. Here it is usefull to use a liquid Ca-standard (e.g. 1000mg/l).
To determine the titer of a 0.1 mol/l EDTA- solution, about 0.1 g CaCO3 (or Zinc) volumetric standard are weighed into a 150 ml beaker and 4 ml HCl 25% are added. After complete dissolution of the reference material, the solution is made up to 60 ml with distilled water and the pH is adjusted to weak acid – neutral with Ammonia. 5 ml buffer solution pH 10 and 1 ml of Cu-EDTA 0.1 mol / l are added. The titration is done with the EDTA - solution to an equivalence point. The consumption should be about 5 - 15 ml.
If the specified assay of the volumetric standard is significantly different from 100%, the weight for calculating the concentration must be corrected:
𝑊𝑒𝑖𝑔ℎ𝑡 ∗ 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑒𝑑 𝑎𝑠𝑠𝑎𝑦 %
𝑊= 100
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Titration parameter
Default method Titer EDTA
Method type Automatic titration Modus Dynamic Measured value mV Measuring speed / drift User defined Minimum holding time 5s Maximum holding time 15 s Measuring time 3s Drift 5 mV/min Initial waiting time 0s Dynamic flat Max step size 0.5 ml Slope max ml 10 Min. step size 0.05 ml Slope min. ml 120 Damping none Titration direction decrease Pretitration off Delay time 0s End value off EQ On (1) Slope value 120 Max. titration volume 20 ml Dosing speed 100% Filling speed 30 s
When titrating with very low concentrated EDTA – solution, the potential jump at the EQ is flatter. In this case the slope value for the EQ should be decreased.
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Calculation: 𝑊 ∗ 𝐹2 𝑇 [𝑚𝑜𝑙/𝑙] = (𝐸𝑄 − 𝐵) ∗ 𝑀 ∗ 𝐹1
B 0 Blank value W man Weight of the sample [g] F2 1000 Conversion factor EQ1 Consumption of titrant until first Equivalence point M 100,09 Molecular mass of KIO3 F1 1 Conversion factor
If Zinc is used as reference material instead of CaCO3, the molar mass of Zinc with M = 65.38 must be used for M. We recommend to write the exact concentration T to the Exchangable Unit (WA) automatically.
Any questions? Please contact the application team:
Xylem Analytics Germany Sales GmbH & Co. KG, SI Analytics
