EHA 3001 การจัดการส้วมสาธารณะ · eha 3001 การจัดการส้วมสาธารณะ ที่มา : ส านักอนามัยสิ่งแวดล้อม
Quiz Time 05:00 04:0003:0002:0001:3001:0000:4500:3000:1500:00.
-
date post
19-Dec-2015 -
Category
Documents
-
view
220 -
download
2
Transcript of Quiz Time 05:00 04:0003:0002:0001:3001:0000:4500:3000:1500:00.
Last Week Synthesized chloropentaaminocobalt
chloride [Co(NH3)5Cl]Cl2 Determine theoretical yield (mass) of
product
Goals for This Week Determine % yield of product Analyze product by cation exchange
column chromatography to determine charge
Analyze product by Atomic Absorption Spectroscopy (AAS) to determine its % mass composition of cobalt
The Analyses Three types
%Yield Charge analysis – _______________________ Amount of cobalt present - ____________
What will they tell us? %Yield Charge
Mass% Co
% Yield What does it tell?
%Yield= Theoretical yield
Weigh amount of ____________________ Change grams to moles Determine how many moles of product this
could make Take into account ______________
For this expt: ___________________ Change to __________ of product
Ion Exchange Chromatography (IEC)
Absorption column chromatography OR Affinity Chromatography
Chromatography – _____ ______ – separation of mixture based on specific property of mixture In our case, the property that we want to study is
the ________, therefore the separation is based on the ________
Cobalt is a cation Therefore, we use _____ exchange chromatography Cation exchange chrom. uses exchangeable cations Anion exchange chrom. uses exchangeable anions
IEC continued Columns packed with synthetic
polymeric resin Cations are able to displace the
H+ ions What happens to pH of effluent (the stuff coming off of the
column) when H+ goes into solution?
IEC continuedNumber of H+s “kicked off” is dependent on
number of positive charges replacing them If cation has +1 charge, will kick off 1 H+s If cation has +2 charge, will kick off 2 H+s
[Co(NH3)5Cl)]2
+
IEC continued Therefore, if you can tell how many H+s
are kicked off and you know how much of the substance you added to the column, you can tell how many complex charges stick
How do you determine how many H+s? What is the indicator?
IEC Column Prep Choose a column that has at least ½” of yellow bed NEVER allow column bed to get dry Never trust anyone who used equipment before you Columns will still have Co and may still have HCl on
column How does this affect us?
How do you get rid of HCl? Wash column with deionized (d.i.) water You must remove cork in order for column to drain Check effluent with pH paper until same pH as d.i. water
IEC Analysis Weigh sample (only using 0.2g (very small
%)) of sample Dilute sample Apply aliquot of sample to column Flush column with d.i. water Collect effluent in flask (to be titrated) Continue collecting until pH paper turns
same color as d.i. Water to be sure that all sample binds and all H+s are collected
Titrate the effluent with standardized NaOH
IEC Results Theoretically
Final product had +2 charge Can you get something else?
What does the charge that you get depend on?
HCl:NaOH = 1:1 molar ratio In expected complex, Comp:HCl = 1:2 Therefore, expect NaOH:Comp = 2:1
Ionic charge = MNaOH*Vtitrated
(masssample/mwcomplex)*dilution = mol NaOH/mol complex
If ratio is not 2.00, you should explain why
Atomic Absorption Spectrometry Finding mass% of Cobalt atoms in
sample UV-vis spectrometer was used in sports
drink lab Similar guiding principles
Be sure to use d.i. water so no ion
interference
How Does AAS Work? Instrument heats sample to change into vapor
state Flame causes decomposition into elements
Elements = atom = Co for us Light travels through sample that is in gaseous
phase, each element has specific that it will absorb
Electromagnetic radiation is absorbed by atoms of interest
Absorbance is determined in similar fashion as in UV-vis spec
How Does AAS Determine Concentration?
Using standards, you can make _____________
___________ just like in sports drink experiment
Then, sample is run and computer uses ______
__________________ to indicate concentration Given in ppm (parts per million) = 1/106 =
10-6 = mg/L
Advantages of AAS Quick
Standards ~ 5 minutes Samples ~ 1 minute each
Very sensitive Can detect trace amounts of atoms in sample
Very small amount of sample needed None of the other atoms in complex
interferes Therefore, impurities, etc. do not get detected
AAS Results Theoretical %Co
[Co] = (atomic mass Co/mw complex)* 100%
Actual %Co Your value will be given in mg/L or ppm 0.2xxxg of sample in 100mL dilution Diluted again, 5mL to 500mL
%100mL1000
L1
mg1000
g1
mL5
mL500
)g(samplemass
mL100Co/L ??mg %Co
Compare actual value to theoretical value of the expected product (and different intermediates) and tell what it means about what you have for your “product”
Results Summary What does %yield tell you?
What could cause this value to be other than 100%? What should the final charge be for the product?
Can you get something else?
What does the charge that you get depend on?
How much cobalt should be in the product?
You know how to calculate expected mass% when given chemical formula
What if you determine that it is not the calculated value?
Applications of Methods Column Chromatography
Useful step in many types of purifications or analyses You must know some physical characteristics of the
substance (ie charge) Example: Protein purifications
AAS Used to detect trace quantities of metals Can be used when not enough present to perform
titrations, etc. because of sensitivity Example: can be used to monitor drinking water to
ensure that levels of lead, arsenic, etc. are within limits