Materials
-0.5 to 1g of hair sample (kept at ambient temperature)
-Inductively coupled plasma mass spectrometer
-Analytical balance
-Temperature adjustable hot plate (kept at 95°C)
-Mortar and pestle
-Polypropylene sieve, 5-mesh
-Gravity convection drying oven with thermostatic control (maintain at 105°C)
-Glassware
-Pipettes
-Watch glasses
-Evaporating dishes
-Quality control sample
-Laboratory fortified blank
-Reagent and standards:
•Nitric acid, concentrated and diluted
•Hydrochloric acid, concentrated and diluted
•Ammonium hydroxide, concentrated
•Reagent grade water
•Stock standard solution
-Blanks:
•Calibration blank (1% [v/v] nitric acid in reagent water)
•Laboratory reagent blank
•Rinse blanks (2% [v/v] nitric acid in reagent water)
Procedure
Preparation of standard stock solution
1. Dissolve 0.1320g of As2O3 in a mixture of 10mL reagent water and 2mL concentrated ammonium hydroxide.
2. Heat gently to dissolve.
3. Cool and acidify solution with 2mL concentrated nitric acid.
4. Dilute to 100mL with reagent grade water and mix.
5. Repeat step 4 to obtain standard solutions of different concentrations (e.g. 10% (v/v), 20% (v/v),40% (v/v), 70% (v/v)). (external standard method)
6. Extract approximately 1.5mL of the different standards into autosampler vials (working solutions) and run it for analysis.
Sample preparation
1. Weigh hair sample and record wet weight (WW). Dry sample to constant weight at 60°C and record dry weight (DW).
2. Sieve dried sample using a 5-mesh polypropylene sieve and grind in a mortar and pestle. Transfer ground sample to a 250mL beaker for acid extraction.
3. Add 4mL of HNO3 and 10mL OF HCl. Cover lip of beaker with a watch glass. Place beaker on a hot plate at 95°C, located in a fume hood.
4. Heat sample and gently reflux for 30 minutes.
5. Let sample cool and quantitatively transfer extract to a 100mL volumetric flask. Dilute with reagent water, stopper and mix.
6. Perform centrifugation to separate insoluble material. Filter if necessary.
7. Adjust the chloride concentration by pipetting 20mL of the prepared solution into a 100mL volumetric flask, dilute with reagent water and mix.
8. Add approximately 1.5mL of prepared solution into an autosampler vial (sample solution) and run it for analysis.
Results
Normal concentration: 0.08 to 0.25 mcg/g
Lethal concentration: >1mcg/g
1. Round off solution analyte concentrations in analysis solution to appropriate significant figures.
2.Construct a calibration graph of peak area against concentration.
3. Using the equation from the graph, calculate concentration of sample by multiplying dilution factor.
3. Calculate dry weight by this equation:
4. Convert to mcg/g.
5. Check if quantity in sample is within normal concentration or lethal concentration.
Conclusion
During Mary Ann Cotton's time, there were only primitive techniques of detection available. This could have contributed to the delay of the conviction of Mary Ann Cotton even when she committed a whopping amount of murders. ICP-MS can detect the presence of substance and also the amount. Despite this, results are still tentative and needs to be further confirmed with methods like HPLC or even ICP-MS coupled with HPLC or ion chromatography to improve the accuracy of analysis. With ever-advancing rapid methods being discovered, detection of substances is made easier in solving cases and also in many other areas.
References
Done by:
Koh Siew Lian
Lee Huan Ting
2F01
David Wilson. (2012). She poisoned 21 people including her own mother, children and husbands. So why has no-one heard of Britain's FIRST serial killer, Mary Ann Cotton? . Available: http://www.dailymail.co.uk/femail/article-2096423/Mary-Ann-Cotton--Britains-FIRST-serial-killer-poisoned-21-people-including-mother.html#axzz2JoDWH4e5. Last accessed 3rd Feb 2013.
Alan White. (Jul 26). The Story of Mary Anne Cotton. Available: http://aljwhite.com/?p=11. Last accessed 3rd Feb 2013.
Mayo Clinic. (). Test ID: ASHA8651 Arsenic, Hair. Available: http://www.mayomedicallaboratories.com/test-catalog/print/8651. Last accessed 3rd Feb 2013.
California State University Northridge. (). Chemistry 322L Manual.Available: http://www.csun.edu/~hcchm003/322l/322lmicp.pdf. Last accessed 3rd Feb 2013.
J.T. Creed, C.A. Brockhoff, and T.D. Martin. (1994). DETERMINATION OF TRACE ELEMENTS IN WATERS AND WASTES BY INDUCTIVELY COUPLED PLASMA - MASS SPECTROMETRY. Available: http://www.caslab.com/EPA-Methods/PDF/200_8.pdf. Last accessed 3rd Feb 2013.
Jorge Ya´n˜ez, Vladimir Fierro, Hector Mansilla, Leonardo Figueroa, Lorena Cornejo and Ramon M. Barnes . (2005). Arsenic speciation in human hair: a new perspective for epidemiological assessment in chronic arsenicism.Available: http://www.ispch.cl/actualidad/doc/Peper%20As%20Jorge%20Ya%F1ez.pdf. Last accessed 3rd Feb 2013.
J.T. Creed, C.A. Brockhoff, and T.D. Martin. (1994). DETERMINATION OF TRACE ELEMENTS IN WATERS AND WASTES BY INDUCTIVELY COUPLED PLASMA - MASS SPECTROMETRY. Available: http://www.caslab.com/EPA-Methods/PDF/200_8.pdf. Last accessed 3rd Feb 2013.
MedicalHealthTests ©. (2012). Reasons, Preparation & Procedure For Conducting a Arsenic Hair Test. Available: http://www.medicalhealthtests.com/pathology-test/arsenic-hair.html. Last accessed 3rd Feb 2013.
Smith, A. and Heitkemper, D.T., et al.. (2001). Arsenic Analysis and Speciation by ICPMS. Available: http://www.wcaslab.com/tech/arsenic.htm. Last accessed 3rd Feb 2013.
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