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laboratory_exercises:determination_of_low_solubilities [2023-07-24 15:02]
Gennaro Nesso
laboratory_exercises:determination_of_low_solubilities [2023-09-16 15:43] (current)
Susanna Salmien-Paatero
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 ==== Learning Goals ==== ==== Learning Goals ====
-Here the learning goals and purpose of the exercise should be presented in a reasonable way.+In this exercise, the students learn how to determine solubility of strontium sulphate by means of LSC and find out possible uncertainty sources in this determination method.
  
 \\ \\
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 Therefore, an A* activity is produced by:\\ Therefore, an A* activity is produced by:\\
-{{:laboratory_exercises:eq.7.png?100|}}+{{:laboratory_exercises:eq.7.png?70|}} 
 + 
 +and the solubility is:\\ 
 +{{:laboratory_exercises:eq.8.png?150|}}\\ 
 + 
 +Certain errors may arise in this type of determination.\\ 
 +For example, it may be necessary to correct for the self-absorption of the active solid, or to arrange the experimental procedure so that this may be avoided.\\ 
 +Care must also be taken to avoid errors due to absorption on apparatus. 
 + 
 +In this experiment the solubility of strontium sulphate is determined and at the same time errors likely to arise are investigated.\\ 
 +<sup>35</sup>S (T1/2 = 87 days) will be used. Alternatively <sup>89</sup>Sr (T1/2 = 54 days) would also be suitable. 
 + 
 +\\ 
 + 
 +=== Experimental Procedure === 
 +  -Take two 2 cm<sup>3</sup> aliquots of <sup>35</sup>S-spiked strontium nitrate solution and place in separate 15 mL centrifuge tubes, add excess 2.5 M sulphuric acid (approx. 4-5 cm<sup>3</sup>). A white precipitate will rapidly form. 
 +  -Centrifuge at 5000 rpm for 5 min and then pour off supernatant into the waste beaker provided. 
 +  -Wash repeatedly with distilled water using at least 100 cm<sup>3</sup>. Carefully pour off wash water into the waste beaker leaving the precipitate in the centrifuge tube each time. 
 +  -Add 10 cm<sup>3</sup> of distilled water to the washed precipitate and leave to stand for 10-30 min, shaking periodically. This allows time for precipitate and water to equilibrate (see //step 9//). 
 +  -Meanwhile dilute the strontium nitrate solution by a factor of 100 in the volumetric flask with distilled water– use 0.25 cm<sup>3</sup> in 25 cm<sup>3</sup>
 +  -Add 10 cm<sup>3</sup> of scintillation fluid to 5 plastic scintillation vials. 
 +  -Add 1 cm<sup>3</sup> of original undiluted solution to the 1<sup>st</sup> vial. 
 +  -Add 1 mL of the 100x diluted solution to a 2<sup>nd</sup> vial. 
 +  -Once the strontium sulphate has equilibrated, centrifuge off the precipitate and add 1 cm<sup>3</sup> of the supernatant from 1<sup>st</sup> precipitated sample to a 3<sup>rd</sup> vial. 
 +  -Add 1 cm<sup>3</sup> of the supernatant from the 2<sup>nd</sup> precipitated sample to a 4<sup>th</sup> vial. 
 +  -The 5<sup>th</sup> vial has no activity added and is the background sample. 
 +  -Count all 5 vials on liquid scintillation counter using <sup>14</sup>C channel (Protocol 2). \\ Press button F2 to start the run. 
 + 
 +\\ 
 + 
 +As the majority of the activity is in the precipitate, it is clear that a minute amount of this in the supernatant may cause a gross error in the determination.\\ 
 + 
 +From the results obtained the solubility of strontium sulphate may be determined as follows:\\  
 + 
 +  *Let count of 1 cm<sup>3</sup> original solution diluted 1/100th=z cpm 
 +  *Let count of 1 cm<sup>3</sup> of SrSO<sub>4</sub> = y cpm 
 +  *Thus, 100 z cpm is equivalent to 0.1 g Sr(NO<sub>3</sub>)<sub>2</sub>: {{:laboratory_exercises:eq.9.png?140|}} 
 +  *y cpm is equivalent to:{{:laboratory_exercises:eq.10.png?140|}} 
 +  *Solution of SrSO<sub>4</sub>={{:laboratory_exercises:eq.11.png?340|}} 
 + 
 +\\ 
 + 
 +==== Questions for the Students ==== 
 +  -What are the sources of error? 
 +  -Highlight the potential problems of using <sup>90</sup>Sr for this experiment. 
 + 
 +\\ 
 + 
 +====Safety Aspects=== 
 +  *A lab coat, gloves and safety spectacles must be worn.\\ <sup>35</sup>S is a soft beta emitter which means that it is not readily detected.\\ When checking the bench, hands, lab coat, etc for contamination it is necessary to use a sensitive instrument. 
 +  *DO NOT dispose of any liquid or solid waste down sinks or in waste bins.\\ Place in the waste buckets provided. 
 + 
 +\\ 
 + 
 +====Work report==== 
 +The work report about this exercise should contain clear description of the performed work presenting the original theory, used equipment with settings, radionuclides with their activities and reference dates, answers to the two questions above, and finally the calculated results. 
 + 
 +\\ 
 +====Preparation for the Lab Supervisor==== 
 + 
 +===Equipment=== 
 +  *Centrifuge\\ 
 +  *Liquid scintillation counter\\ 
 +  *1 mL autopipette\\ 
 + 
 +\\ 
 + 
 +=== Consumables === 
 +  *4-5 mL of 2 M sulphuric acid 
 +  *15 mL centrifuge tubes x 2 
 +  *> 100 mL of H<sub>2</sub>
 +  *Scintillation vials x 5 
 +  *50 mL of scintillation cocktail 
 +  *1 mL tips 
 +  *Waste beaker\\ 
 +  *Glass beaker x 2 for H<sub>2</sub>O\\ 
 +  * Polystyrene or other type of base to stand centrifuge tubes in 25 mL volumetric flask\\ 
 + 
 +\\ 
 + 
 +=== Source === 
 +4 mL of <sup>35</sup>S strontium nitrate 0.28 kBq/mL 
 + 
 + 
 + 
 + 
 + 
 + 
 + 
  
  
  
  
laboratory_exercises/determination_of_low_solubilities.1690203770.txt.gz · Last modified: 2023-08-28 22:10 (external edit)