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Pharmaceutical Calcium in Tablets - kyoto-kem.com

Pharmaceutical Calcium in Tablets Chelatometric titration by Automatic Potentiometric Titrator Standard The amount of Calcium in Tablets is quantified first by preparing test sample liquid. Crush the sample tablet, and add pure water with 10% Hydrochloric acid. Warm the liquid in bath at 80 C, and cool. Then, filter, and add water to make test sample liquid. Further, add water with 10% Potassium hydroxide and Potassium cyanide for titration with EDTA. The endpoint is determined by the color change of indicator on titration curve. Calcium is calculated from titration volume of EDTA.

Pharmaceutical Calcium in Tablets Chelatometric titration by Automatic Potentiometric Titrator Standard 1.Abstract The amount of calcium in tablets is quantified first by preparing test sample liquid.

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Transcription of Pharmaceutical Calcium in Tablets - kyoto-kem.com

1 Pharmaceutical Calcium in Tablets Chelatometric titration by Automatic Potentiometric Titrator Standard The amount of Calcium in Tablets is quantified first by preparing test sample liquid. Crush the sample tablet, and add pure water with 10% Hydrochloric acid. Warm the liquid in bath at 80 C, and cool. Then, filter, and add water to make test sample liquid. Further, add water with 10% Potassium hydroxide and Potassium cyanide for titration with EDTA. The endpoint is determined by the color change of indicator on titration curve. Calcium is calculated from titration volume of EDTA.

2 1) Chelatometry by Kagehira Ueno from Nankodo 2) Experiment and Calculation for Quantitative Analysis by Seiji Takagi from Kyoritsu Publishing Company in measurement 1) Handle with care when you work on chemicals. 2) Reactivity of sample and titrant may change depending on H in chelatometry. Therefore, Adjust it to the optimal pH before titration. TIC-97003 1/4 TIC-97003 2/4 care After a series of measurements is over, rinse the photo sensor with pure water, and keep it dipped in water in a beaker. equipment Main unit Automatic potentiometric titrator (Option photometric amplifier PTA- Detector Option Photo sensor (Filter wavelength:630nm) Reagent / EDTA solution Solvent Pure water Additive 10% Potassium hydroxide, Potassium cyanide 1g/10mL Indicator procedure Pretreatment 1) Crush sample Tablets , and dry at 105 C for 3 hours.

3 Then, cool it in desiccator. 2) Weigh in dried sample at 3 , and add 200mL water and 30mL of 10 HCl. 3) Warm in bath at 80 C for about an hour while shaking occasionally. 4) After warmed, cool and filer. 5) Add water to make it 1 in total. Measurement 1) Deliver sample in a 100mL beaker, and add 50mL water. 2) Add 15mL of 10 Potassium hydroxide and 3 drops of Potassium cyanide 1g/10mL . 3) Add 10 drops of indicator. 4) Titrate with EDTA to obtain the concentration of Calcium . Calcium ( % ) = ( EP1 BL1 ) FA1 C1 K1 / SIZE EP1 : Titration volume ( mL ) BL1 : Blank level ( ) FA1 : Factor of titrant ( ) C1 : Concentration conversion coefficient ( 2mg/mL ) ( EDTA 1mL 2mg Ca ) K1 : Unit conversion coefficient Dilution ratio ( 100 10 ) SIZE.

4 Sample size ( g ) of measurement Ambient condition Room temperature 26 C Humidity 55 Weather Cloudy -Titration parameter- Titration parameter Titration mode Auto cut-off Titration reagent EDTA Detector No. 3 Max. titration volume Titration direction Auto Titration form EP Stop Burette No. 1 Potential unit %T Wait time before titration 0s Control parameter Number of endpoints 1 EP sense potential EP sense differential Over-titration Gain 1 Simulation Off Data sampling potential Stability check potential Delay time before stability 1s Stability check time 30s Data sampling

5 Volume Separate potential setup Off -Titration curve- (The above printout data were obtained from titration by AT-400 WIN) TIC-97003 3/4 Measurement results n Sample (g) Titration (mL) Calcium (%) Concentration of Calcium 1 2 3 Mean SD RSD % % % The above test results were obtained by 3 tests of the same sample. 10. Summary Tablets mean Pharmaceutical pills containing active ingredients added with fillers and formed into given shape. Calcium belongs to the second group of alkaline earth metal in periodic table of the elements, and its proton number is 20 with chemical symbol Ca.

6 It is an essential element in human body, weighing approximately 1kg, and 99% of our bones and teeth are made from Calcium . The measurement results show a favorable repeatability with les than relative standard deviation. Precise and reliable measurement is assured by the automated potentiometry. The analysis of Calcium can be perfectly made by any of the following titration systems manufactured by Kyoto Electronics (KEM). AT-510 Compact and cost performance model PC card expands data memory for convenience and versatility. AT-500N-1 Low cost and high performance Easy view with back light LCD GLP/GMP conformed model AT-610 Awarded Product of Supreme Technology from Kyoto City Easy key entry by touch panel of large color LCD 8-inch wide Simultaneous titration in parallel Both potentiometric and Karl Fischer moisture titration (coulometric volumetric can be performed at a time.)

7 TIC-97003 4/4


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