mod 8 Flashcards
how does IR work
- solution of the unknown sample to be tested is placed in cuvette and a sample of solvent by itself is placed in another cuvette (reference)
- the IR source is split into 2 beams using mirrors and passed through both cuvettes
- the beams pass through a monochromator to isolate wavelengths to analyse
- the difference in the absorbance between both cuvettes is due to IR absorbed by the substances
- the beam hits the detector which converts the information into a digital signal
choice of reactants
retrosynthetic analysis is the method by which scientists begin with the desired product and work backwards to determine required reactants
- e.g in organic compounds –> break long chains and consider which functional groups react
UV visible spectrophotometry
is based on the same principles as colorimetry, but it can also measure UV spectrum (190nm-380nm) absorbance
- no complementary absorbance but we take the peak absorbance
- select wavelength to test using UV spectrophotometer (uses monochromator not colour filter)
compound purity
spectrometric techniques (IR, NMR, MS) can be used to determine purity
- additional peaks
- missing peaks
- overlapping peaks when -CH2- are buried in long alkyl chains
hydrogen chemical environment
look at:
- what the hydrogen atom is bonded to
- what the atom the H is bonded to is bonded to
if they are the same = same carbon environment
- H atoms attached to the same C atom are identical
- OH has its own H environment
pH test
if it has acidic properties –> blue litmus will turn red
chemical shifts
to record C and H shifts, they are compared to the reference compound tetramethylsilane (TMS)
- TMS is chemically inert with 1 C and H environment hence strong baseline
fragmentation in MS
high energy electrons strike molecular ions and fragment them into smaller parts:
molecular ion –> cation + radical
- cation will be deflected and hit detector to form another peak
- fragments (m/z) < parent molecular ion
important complexes
memorise table
emission and absorption
emission = black background with coloured lines
absorption = coloured background with black lines
reaction conditions for exo equilibrium reactions
- too high temp = equation shifts left decreasing yield + safety concerns
- too low temp = reduces ROR
- need modernate-high temp
how AAS works steps
- hollow cathode lamp has a filament composed of element to be analysed
- the lamp is heated to emit the specific wavelength of the elements specific to the wavelengths absorbed by the element
- the solution is sprayed into the flame to atomise the substance (converts ions to free neutral gas atoms)
- light leaving the flame passes through a monochromator, separating and selecting a single wavelength
- the selected wavelength strikes a detector which determines the intensity and calculates he absorbance (by comparing to lamp’s intensity)
testing for sulfate and phosphate ions
- test for SO4(2-) by first adding acid then Ba2+ ions
- test for PO4(2-) by first adding base then Ba2+ ions
principles of infrared spectroscopy
molecules absorb infrared radiation and transition from lower to higher vibration levels
- vibrational levels are called modes (i.e stretching, bending)
- only modes that change the dipole moment (polarity through magnitude or direction) of molecular with be infrared active
reaction conditions for gas equilibrium reactions
- too high pressure = safety
- too low pressure = reduces ROR
- need to decide based on pressure conditions
isotopes
additional very small peaks due to the presence of isotopes
- usually have very small abundance
performing colorimetry in a school lab
- filtered light beam passes through analyte
- light beam strikes the detector which converts light into electricity
- the final result is an absorbance value
- absorbance must be compared o those of standard solutions
- machine must be calibrated (using blank with only solvent to set baseline at 0) by testing standard solutions = graph should be linear
bromine water test
test for C=C (carbon carbon double bonds)
- unsaturated carbons undergo addition reactions with hydrogen or hydrogen halides
- bromine water contains:
Br2(aq) + H2O(l) –><— HOBr(aq) + H+(aq) + Br-(aq)
- bromine is brown and will decolourise when reacted with unsaturated hydrocarbons
advantages of MS
- used for quantitative and qualitative analysis
- identify isotopes
- very sensitive, requires small sample
- accurate and fast
precipitation titration: equations
- Ag reacts with unknown anion to precipitate
Ag(aq) + X(-) –> AgX(s) - Ag reactions with dichromate to precipitate
2Ag(aq) + CrO4(2-)(aq) –> Ag2CrO4(s)
chemical shift formula
sample frequency - reference (TMS) frequency / spectrometer frequency
fertilisers
have nitrates and phosphates, causing:
- algae growth (eutrophication)
- decreases O2 in water
- algae blocks sunlight - limiting photosynthesis
stretching mode
2 atoms oscillate back and forth, stretching the bond between them
- at ground level a molecule stretches to a certain degree
- with infrared energy, the molecule stretches to a greater extent –> higher energy stretching mode
IR graph
- xaxis plots wave numbers –> higher wave no. = higher frequency = shorter wavelength = higher energy
- yaxis plots transmittance
= 10^-absorbance x 10%
= light leaving cuvette/light entering cuvette x100% - if no light absorbed, transmittance = 100% (baseline)
availability of reactants
chemical production facilities are best located near the production site of the raw materials it uses:
- reduce cost of transportation (e.g ethanol produced near farms supplying sugar cane)
- unless material is abundant (e.g haber process uses NaCl from ocean)
reading IR
- remove fingerprint region (right of 1500)
- look at wave number on reference sheet
- memorise table about depth and breadth
nucleus spins for NMR
- applied external magnetic field splits nucleus into 2 levels (parallel/low = poles align with magnetic field) (antiparallel/high = poles don’t align with magnetic field)
- when radio-wave pulse of correct frequency is applied –> aligned will absorb energy and transition to higher unaligned state
- nucleus oscillates between the levels called resonance
reaction conditions for endo equilibrium reactions
- need high temp but safe