User:Moira M. Esson/Notebook/CHEM-571/2014/04/09

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==Objectives==
 
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#UV-vis analysis of both N2 reactions prepared on [[User:Moira M. Esson/Notebook/CHEM-571/2014/04/02|04/02/2014]]
 
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#DSC of any remaining samples needed for analysis
 
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#Sample preparation using the sonicator and oven method
 
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<br>
 
-
 
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==UV/vis==
 
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*Please refer to Trisha Ibeh's notebook for all UV/vis data
 
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<br>
 
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==DSC==
 
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*The general protocol described on [[User:Moira M. Esson/Notebook/CHEM-571/2014/04/08|04/08/2014]] was followed.
 
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Table 1. Crystallization and Melting temps for 13500:1 Mag:BSA N2 prep
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Crystallization temperature (°C)'''
 
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| align="center" style="background:#f0f0f0;"|'''Melting point (°C)'''
 
-
|-
 
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| 121.3138||131.0097
 
-
|-
 
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| 117.9636||129.6897
 
-
|-
 
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| 117.3508||
 
-
|-
 
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| -37.45993||
 
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|}
 
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<br>
 
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Figure 1. DSC 13500:1 Mag:BSA N2 prep
 
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[[Image:Differential Scanning Calorimetry analysis of 13500-1 Mag-BSA prepared using Schlenk line method .png]]
 
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<br>
 
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Figure 2. DSC of sonicator and oven prep
 
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[[Image:Differential Scanning Calorimetry 13000-1 Magnetite-BSA sonicator prep vs. oven prep .png]]
 
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<br>
 
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Figure 3. DSC of sample with gold
 
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[[Image:Differential Scanning Calorimetry analysis of 13000-1 Magnetite-BSA with 130-1 Gold-BSA prepared using the oven .png]]
 
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<br>
 
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Table 2. Recrystallization and Melting temps for sonicator method and oven method
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Sample Name'''
 
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| align="center" style="background:#f0f0f0;"|'''Crystallization temperature (°C)'''
 
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| align="center" style="background:#f0f0f0;"|'''Melting point (°C)'''
 
-
|-
 
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| 13000:1 Magnetite:BSA oven preparation||115.5866||132.246
 
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|-
 
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| 13000:1 Magnetite BSA Sonicator preparation||118.914||131.4689
 
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|}
 
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Table 3. Recrystallization and Melting temps for sample prepared with gold
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Recrystallization temperature (°C)'''
 
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| align="center" style="background:#f0f0f0;"|'''Melting Point (°C)'''
 
-
|-
 
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| 117.6786||131.1519
 
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|-
 
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| 118.1845||129.0052
 
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|-
 
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| -37.52146||11.15457
 
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|-
 
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| -37.48928||11.24656
 
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|}
 
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*Circular shape in gold spectra is due to some form of interference (electrical effect)
 
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<br>
 
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==Sample preparations==
 
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*All of the general protocols for the sonicator method and the oven method were followed.
 
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<br>
 
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'''Sample preparation of magnetite only samples in the sonicator'''
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration BSA'''
 
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| align="center" style="background:#f0f0f0;"|'''Volume BSA Added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
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|-
 
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| 13000||2.30769E-06||0.881472149||1||0.909090909||4.444444444||2.764992498
 
-
|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration Hemoglobin'''
 
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| align="center" style="background:#f0f0f0;"|'''Volume Hemoglobin Added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
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|-
 
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| 16500||1.81818E-06||1.178620375||1||0.909090909||4.444444444||2.467844272
 
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|}
 
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<br>
 
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'''Sample preparation of all samples prepared in the oven'''
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration BSA'''
 
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| align="center" style="background:#f0f0f0;"|'''Volume BSA Added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
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|-
 
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| 13000||2.30769E-06||0.747970622||0.5||0.454545455||0.555555556||2.741928368
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration Hemoglobin'''
 
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| align="center" style="background:#f0f0f0;"|'''Volume Hemoglobin Added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of FeSO4 added(mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KOH added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''amount of KNO3 added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Water added (mL)'''
 
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|-
 
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| 16500||1.81818E-06||0.589310187||0.5||0.454545455||0.555555556||2.900588803
 
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|}
 
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<br>
 
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Gold sample preparation for the addition to the magnetite samples
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration BSA (M)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume BSA added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume water added (mL)'''
 
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|-
 
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| 130||0.340447787||1.92308E-06||0.367280062||4.292272151
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Ratio'''
 
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| align="center" style="background:#f0f0f0;"|'''Amount of gold added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''Concentration Heme (M)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume Heme added (mL)'''
 
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| align="center" style="background:#f0f0f0;"|'''volume water added (mL)'''
 
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|-
 
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| 165||0.340447787||1.51515E-06||0.491091823||4.16846039
 
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|}
 
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<br>
 
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'''All stock solution preparations''':
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of FeSO4 stock'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular Weight (g/mol)||278.01
 
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|-
 
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| mass(g)||0.83403
 
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|-
 
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| volume stock (L)||0.01
 
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|-
 
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| Concentration (M)||0.3
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of BSA stock'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular weight (g/mol)||66463
 
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|-
 
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| mass (g)||0.0174
 
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|-
 
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| volume stock (L)||0.01
 
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|-
 
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| Concentration (M)||2.618E-05
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of hemoglobin Stock solution'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular weight (g/mol)||64500
 
-
|-
 
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| mass hemglobin (g)||0.0995
 
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|-
 
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| volume solution (L)||0.1
 
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|-
 
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| Concentration (M)||1.54264E-05
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of KNO3'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular Weight (g/mol)||101.1
 
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|-
 
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| mass(g)||0.9099
 
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|-
 
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| volume stock (L)||0.01
 
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|-
 
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| Concentration (M)||0.9
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation of KOH stock'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular Weight (g/mol)||56.11
 
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|-
 
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| mass(g)||0.61721
 
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|-
 
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| volume stock (L)||0.01
 
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|-
 
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| Concentration (M)||1.1
 
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|}
 
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<br>
 
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{| {{table}}
 
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| align="center" style="background:#f0f0f0;"|'''Preparation gold stock'''
 
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| align="center" style="background:#f0f0f0;"|''''''
 
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|-
 
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| Molecular weight Au (g/mol)||393.83
 
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|-
 
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| mass Au(g)||0.01446
 
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|-
 
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| volume stock(L)||0.01
 
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|-
 
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| Concentration (M)||0.003671635
 
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|}
 
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<br>
 
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