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Lead Rubidium
Limitations
- Can’t detect all metals - some metals don’t produce colours
- Some are unsafe to test
- Some produce similarly coloured flames, difficult to distinguish them
- Only for metal cations
- People perceive colour in different ways
- Destructive test
✵ Precipitation - Get solution, put it in a beaker
- Add solutions of anions and see if precipitates form (in a particular order, so we can use the process of
elimination to work it out)
- Precipitate the most insoluble cations
- Add HCL (Chloride ions)- if there's a precipitate, it could only be Pb or Ag
- Filter to remove the precipitate and add NaOH
- a white precipitate will be lead ions
- brown will be silver ions
- Add Na2SO4 (Sulfate ions) - precipitate will be barium or calcium, both white
- Flame test - green flame is barium, red flame is calcium
- Add NaOH
- copper will have a blue precipitate, can confirm this with a flame test
- iron II will have a pale green precipitate (over time it will oxidise and go brown)
- iron III will have a brown precipitate
- aluminium and magnesium will have a white precipitate
- Add NaOH in excess - aluminium will form a clear solution, but magnesium will stay white
3 - Complexing - adding a chemical to a reagent/formed precipitate to further distinguish what it is
- Colours might be similar
- Cl- Br- and I- form similar precipitates with silver - white cream and yellow
- Add ammonia - Cl and Br precipitates dissolve but not I-
- Forms a complex
- AgCl(s) + NH3 → [Ag(NH3)2] + CL-(aq).
- 6 water ligands - lone pair of electrons forms a covalent bond with the Cu
- Responsible for colour in solution
- Silver halides often form complexes which make them soluble
- Can be used to distinguish between lead and silver chloride, between silver halides, confirm transition metal
cations
Reliable - did we get the same answers
Accurate - how good of a colour can we get
Valid - there could be misleading colours, perhaps from a mix of substances, can be hard to analyse.
Calorimetry - absorption of light
- Directly proportional to its concentration
- Linear relationship
- anions: chloride (Cl–), bromide (Br–), iodide (I–), hydroxide (OH–), acetate (CH3COO–), carbonate
(CO32–), sulfate (SO42–), phosphate (PO43–)
✵ Can’t do cation and anion - you need cations to test anions and anions to test cations
- Only precipitation tests
✵ Precipitation test ((: for everything except hydroxide (indicator)
- Add HNO3 (nitric acid) - if there are bubbles a carbonate is present (carbon
dioxide, as its an acid carbonate reaction)
- Must be in excess, to ensure no precipitates form
- Add Ba(NO3)2 - could be sulfate or phosphate
- Since our solution is slightly acidic from the nitric acid, if a precipitate
forms it will likely be sulfate. This is because phosphate is more soluble in
acidic conditions
- Double check this - get a clean sample, add barium nitrate to
create basic conditions, and if the precipitate forms its sulfate.
- Add AgNO3 - white precipitate could be chloride - add dilute ammonia to check
- Yellow precipitate - bromide - add concentrated ammonia
- No precipitate from any ammonia - iodide.
- Brown precipitate - hydroxide ions
- Add iron (III) chloride - acetate ions will form a red precipitate
- No precipitate is nitrate. Though it also could be pure water
- Test conductivity, see if there are any ions at all
✵ Interpreting results of precipitation tests - work backwards of solubility rules
-
- This is fine - NaCl means that Ag, Pb and Hg are not present
- Add sulfate - means there’s Ca or Ba
- Flame test - Ba
conduct
investigations and/or process data involving:
When there is a point of change - from there you can measure
- Adding till you see a precipitate, excess the solubility products
- How much sulfate in a fertiliser - naturally lowers pH
- gravimetric analysis
✵ Analysing the mass of substances to make measurements. Weighing to four significant figures. Quantitative.
- Perhaps the substance is mixed with the solute and other substances, and we cannot weigh it.
- So we have to isolate stuff using precipitation reactions.
- Find a precipitating agent, will form a precipitate with the substance (but make sure to weigh the whole
thing before). Ensure it's added in excess, perhaps using a beaker.
- If we have chloride ions, add silver nitrate to form silver chloride.
- Filter the precipitate out using a filter paper (weighed) and funnel, into a conical flask.
- Dry out the filter paper - very important as extra solution will make us overestimate the weight.
- Air dry over a few days, or use an oven.
- Then weight the paper, subtracting the filter paper weight. Now we have some Grams
- Cl- + AgNO3 → NO3- + AgCl(s)
- Moles of AgCl = 5.6g/10787+35.45 = 0.0390734… = Cl- moles
- Mass Cl- = 0.03090734 x 35.45 = 1.38515203g
- Limitations - drying process isn’t perfect, there will be an overestimation of the substance, possibly
decrease accuracy
- Precipitate could be too fine and go through the filter paper, underestimation of the substance.
- Use more accurate filters such as glass sintered filters
- Deciding when the precipitation reaction has finished is a qualitative observation - the tester may
stop the reaction before it has reached completion, reducing precipitate mass
- Not suitable to analyse all salts, some are soluble with all ions
- Only salts that form a stable precipitate can be analysed
- Precipitates may form other ions that aren’t being tested - silver can also form silver sulfate ions
which are not soluble
- Add excess barium sulfate to ensure all sulfate is precipitated out as barium sulfate.
- precipitation titrations
✵ Difference between gravimetric - this is volumetric analysis
- Accurately measure the amount of substance based on its volume
- Testing fertilisers - could test how much of sulfate ion is in a sample
- Known sample taken → includes some parts that we need to measure → dissolve it, it now is in ion form →
precipitate it
- Often done with halides, and silver nitrate as the standard
- Measures volumes reacting, not masses of precipitates
- Colour change titrations - colour change occurs at the equivalence point due to a precipitate forming
- Mohr’s method apparently - unknown solution of NaOH titrated against AgNO3.
- At the equivalence point, all the chloride should be precipitated out as silver chloride. If we know
how much silver nitrate we add to reach this point, we can calculate the amount of chloride present.
- Use a potassium chromate indicator to assist, and change from yellow to red
- Silver will react very readily with the chloride ions, and will precipitate out
- Once no more precipitate can be formed, the silver ions will react with
the indicator, forming reddish precipitate silver chromate.
- Then we measure the mean titre, do normal calculations
- The precipitate is filtered and washed, so no other ions are collected
with it, and then dried and weighed.
- However, you must add something that will only precipitate out the desired
substance, not the other ions.
- Reats selectively.
- Precipitate must be highly insoluble
- May have to add other ions before to get rid of other possible ions,
like carbonates and hydroxides
- Validity, assume that only and all analyte precipitates out and none is lost
✵ Conductometric titrations - monitoring electrical conductivity, as ions allow electricity to flow through
- If forming precipitates, there are fewer ions as they are solids, meaning conductivity will decrease
- If more stuff is added (used to form the precipitate, barium acetate to sodium sulfate) it will increase again,
as they have a charge with no one to match with
- So the equivalence point is when the conductivity is lowest
- We can observe the conductivity falling as barium acetate is added
- At a point it increases again, after equivalence point
- Can use volume and stoichiometric calculations to work out the concentration of sulfate ions
- Sharpness of this change differs, as different ions have different conductivities
- Ion added in excess, not precipitating
- Barium acetate is more bulky, less conductive than smaller sulfates,
which is why the conductivity decreased.
- Use Cl- instead, a less steep curve
Hence, the steepness depends on the ions added!
conduct investigations and/or process data to determine the concentration of
coloured species and/or metal ions in aqueous solution, including but not
limited to, the use of:
- colourimetry
✵ Analyse the concentration of any coloured species in a sample - colour
intensity
- Can analyse metals and non metals that emit visible light
- Phosphate - react it to make it purple
- Colour intensity is proportional to concentration
- Colour identified, intensity of colour is how concentrated,
how much
- Hence qual and quant
- The more intense the colour, the higher concentration
-
- They are the same species because they're the same colour. They have different concentrations
because they have different intensities
- Choose what we’re testing for
- Instead of having a different lamp for each element, we have different filters. A filter is chosen
based on what we’re looking for
- Specifically chosen light is passed through a filter (we have already chosen what we’re testing for)
- Filter contains complimentary colour to the solution
- Sample is contained in glass cuvette, light passes through it
- Complimentary colours?
- Light sensor detects the percentage absorbed - the higher it is, the more there was present
- Blank - do the same with deionised water to zero the colorimeter
- ultraviolet-visible spectrophotometry
✵ same principle as AAs and colourimetry
- UV spectrum - 190-400nm wavelength
- Uses UV and visible light spectrum - 190-800nm wavelengths
- Many organic molecules absorb UV-vis light and appear colourless - chromophores
- Deuterium/tungsten lamp emits visible and UV light
- Monochromator selects and splits the light, so it can go to the sample and a reference
- Goes to a detector/spectrophotometer records the wavelength when absorbance occurs and the amount of
absorption occurs
- Qual and quant
- Wavelength that is absorbed identifies if the chemical is present, and the amount that is absorbed tells us
how much is in the sample
- Wavelength identifies, absorption quantifies
✵ Wavelength max - when the most absorption occurs
- Each element has one, like a fingerprint, stored in a database
- If a sample matches the one in a database, the chemical would be present
- A UV vis spectrum can be compared to this
- Chromophore - functional group!
- Most have C-H bond, so this is very low, however those with a functional group have a higher WM
- The more functional groups the more complex (more peaks)
- The higher the concentration the higher the peaks/absorbance
- atomic absorption spectroscopy
✵ Atomic absorption spectroscopy - measure the concentration of metals in a sample
- Have to know what you’re looking for first, so we can set up which lamp to use
- Testing for mercury, use a mercury cathode lamp
-
- Set up a lamp of the metal that we’re testing for - radiates the wavelength of light that the metal will
absorb, its electrons gets excited
- Light will pass through the sample (in the flame)
- Some light will pass through, and some may be absorbed by the sample. (only the metal tested for)
- If the metal is not there, the sample will not absorb the wavelength and it'll just pass straight through
- Measures the element’s wavelength
- Detector measures how much light passes through the flame, not absorbed by atoms
-
- The amount of light absorbed depends on how many
atoms there are, as if there are any metals that we’re
testing for present, they would be absorbed by the flame
and not pass in through the detector. Therefore we can
find out how much of the sample didn’t go through the
detector and hence how much of the metal is present.
- Gives us an absorbance number
- Absorption is proportional to concentration -if there is lots of the metal present the absorbance will be
high, not much will get through
- The type/wavelength of light absorbed depends on the types atoms
✵ Limitations - can only be used to detect metals, as the cathode lamp only works if the element can conduct
electricity. Non metals are typically bad conductors.
- Only works if the metal is chosen before starting, as the lamp needs to emit the right wavelength
- Can only detect one element at a time
- Amount of light absorbed is directly proportional to the ppm concentration of atoms
- Can plot the absorbance of different standard solutions
- Concentration is independent, since they cause changes (also
1mg/kg - 1mg/L)
- Application - used to measure trace concentrations - very small
element quantities
- Monitor pollutants in air and soil
- Check if there are toxic metals in food and water eg. mercury
- Check if there are toxic metals in the body eg, mercury,
aluminium, cobalt
- Limitation - Can accurately measure absorption, however you can lose
energy in other ways hence it can be hard to measure emission
conduct qualitative investigations to test for the presence in organic molecules of the following functional groups:
- carbon–carbon double bonds
✵ Alkanes - saturated - only C-C. Alkenes are not saturated
Experiment: (need to use high mass hydrocarbons so they are liquid at room temperature)
1. Add 3mL of cyclohexene and cyclohexane to two test tubes
2. Add a few drops of bromine water (originally orange) to each test tube and mix gently
3. Cyclohexene will turn clear, but cyclohexane will stay orange. This is because the alkene is unsaturated, and
will break its double bond to bond with bromine, forming 1,2-dibromocyclohexane
Risk assessment:
However, alkanes can also do this in UV light, doing a substitution reaction
- UV light will form bromine free radicals that will swap with a hydrogen in the alkane. The solution will
decolourise.
- hydroxyl groups
✵ Metal + alcohol → metal alkoxide (salt, conjugate bASE of alcohol) + hydrogen gas
- Butanol - butoxide, ethanol - ethoxide
- Redox - switching electrons
✵ Sodium test - qualitative test, if there is a hydroxyl group
-
- First add calcium chloride to ensure any water is removed
- Put sodium into a test tube with 5mL of alcohol
- Bubbles show that hydrogen gas has been produced
- 2C2H5OH(l) + 2Na(s) → 2NaC2H3O(non aq) + H2 (g).
- Ethanol + sodium metal = sodium methoxide + hydrogen gas
- Non Aq - dissolved in a solvent that isn’t water (ethanol).
- H2 can be confirmed with a pop test
- Na is a strong reducing agent - makes other species reduce.
- So its oxidised and has lost electrons
-
✵ Tertiary alcohol testing - oxidation
- Same catalysts - acidified potassium dichromate or acidified
potassium permanganate
- See if these strong oxidising agent cause a reaction
Experiment:
1. Put 3mL of acidified potassium dichromate with 3mL of the primary alcohol (1-butanol) in a test tube
2. Repeat in 2 more test tubes with the secondary (2-butanol) and tertiatry (3-butanol) alcohols.
3. Place all in a 30oC heated water bath
4. Primary and secondary test tubes will turn green, the tertiary will stay
Same with permanganate, except its purple originally, and turns colourless in primary and secondary
- This is because primary and secondary will undergo oxidation, tertiary will not
- Primary will form aldehydes (1-butanal) and secondary will form ketones (butanone)
- Tertiary will not, because oxidation of alcohols involves breaking a C-H bond on the carbon holding the
hydroxyl group. There are no C-H bonds to break
- The color change - reduction of acidified thing
- Orange dichromate ions become green chromium ions.
- Purple permanganate chromium ions become clear manganese ions
✵ Primary/secondary - Benedict’s/fehling’s solution test
- Keep the ketones and aldehydes form the previous reaction, and distill the mixture.
- Add a small amount of this to either Benedict’s or Fehling’s solution, which are both blue
- Put into a hot water bath
- Aldehydes will form a red precipitate and a ketone will stay blue
- carboxylic acids
✵ Acid carbonate reaction - produces salt, water and carbon dioxide
- (donates proton) CH3COOH(aq) + NaHCO3 (aq) → CH3COONa(s) + H2O(l) + CO2 (g).
- Qualitative, detects if there is any carboxylic acid
- Test CO2 through limewater test
Experiment: Sodium bicarbonate test
1. Add 1mL of NaHCO3 to the test tube
2. Add 2-3 drops of carboxylic acid
3. Seal test tube with stopper, with a delivery tube in
it
4. Bubbles indicate carbon dioxide - test for this using limewater test
5. Fill the second test tube with calcium hydroxide (limewater)
6. Place the tube into the limewater tube. If it turns cloudy, it's carbon dioxide.
a. CO2 (g) + Ca(OH)2 (aq) → CaCO3 (s) + H2O(l).
b. Solid is a white precipitate, which makes the solution cloudy
In this reaction, sodium bicarbonate acts as a base, as the hydrogen ion from the acetic acid molecule bonds with
the hydrogen carbonate ion
- So boom, carbon dioxide and water products w/ the rest, and ofc the salt.
Limitations - it tests for the presence of any acid, not just carboxylic ones. Further testing is needed.
- Esterification reaction - if a sweet smell is produced then we have a carboxylic acid.
investigate the processes used to analyse the structure of simple organic compounds addressed in the course,
including but not limited to:
- proton and carbon-13 NMR
✵ NMR spectroscopy - nuclear magnetic resonance
- Instead of electrons absorbing energy, it’s nuclei, absorbing radio waves and
emitting them characteristically
- Must be the exact amount required for what we’re testing
- Energy into the system (radio waves), excited, and gives off energy that can be
measured
- Low energy radio waves - don't make the molecules change shape, structure or
fragment, good for studying behaviour of nuclei
- If the molecule is surrounded by electrons/other atoms, it will require more
energy to flip as they shield it
- In ethane, all the H atoms have the same chemical environment
- All Hs are equally shielded. H1 spectrum could have only 1 line
- But propanal - the H near the C=O is a lot less shielded, plus oxygen is very electronegative and will pull
H’s electrons toward it - so it's going to be more easily spun
- More electronegative, the more easily its own electrons are taken in
- TMS (tetramethylsilane) is the most shielded compound, as there is very little electronegativity
- Is zero, used as a reference. Requires lots of energy to flip, very symmetrical
- Everything needs less energy than TMS
- The closer to an electronegative boi, the less shielded bc it will take the electrons
- The further from zero, the less shielded, as zero is TMS which is the most shielded compound and we’re
comparing it to that.
- 1 peak = 1 chemical environment
- Ethane - all Hs have the same chemical environment. So there will only be 1 peak
- Its close to zero - not affected by anything polar
-
- The heaviest is furthest to the right
- Lines are fragment ions
- Y axis - proportion of the total ions detected that were recorded at a particular m/z value
- Largest m/z value will belong to the original big molecular ion, with only one electron knocked off (at 60)
- Heaviest. It’s m/z value is it’s molar mass.
- OTHER FRAGMENTS - cracked/broken off pieces of the parent molecule that broke off along the way
under the stress of electron bombardment. Poor guys
- Base peak (41) - most abundant fragment ions in the sample. Can be given a relative abundance of 100%,
so all the other ions can be measured relative to it??????
-
- The location of the line on the x axis determines what the molecule is (qualitative)
- The height of the peak determines how much there is (quantitative)
Example: what produced the base peak (43) in hexanone
-
- Must have 3 carbons or less, as 4 x 12 = 48, higher mass
- Could be the C3H7 fragment (mass of 43) or C3H5O fragment (mass of 57, too high)
- So it's the C3H7 fragment.
- Thousands of trials have resulted in a mass spectra of each molecule, data bank, can be compared when
analysing substances.
- Small peaks beside the base peak are isotopes, having an extra neutron, making the mass go up by 1
- Usually rare
- Chlorine however has isotopes 33 and 37, 3:1 ratio
- Will have a few different peaks containing their isotopes
-
- Work out the structure of the peak at m/z 65
-
- In organic analysis, the molecular ion peak/base peak is what we’re interested in, determining the identity of
the organic compound by providing information about their molecular mass and formula.
- Molecular ion will then have a charge of +1, so z in m/z will = 1
- So the value will equal the mass of the original molecule.
Molecular mass of the original = 58
Alkane formula = CnH2n + 2.
58 = 12n + 1(2n + 2) (using periodic table, most common isotopes, as the peak is produced using only these
isotopes)
= 12n + 2n + 2
56 = 14n
N = 4
Alkane = C4H2x4 + 4 = C4H12 = butane
- infrared spectroscopy
✵ determines the concentration and nature of polyatomic molecules. How it interacts with organic molecules
- Infrared - between visible light and microwave radiation
- Visible light - makes electrons excited, jump energy states
- Infrared - Bond vibrations affected, make their energy increase
-
- Different bonds absorb different amounts of energy
- Heavier atoms require more energy, and absorb lower frequencies
- Double bonds require more energy, and absorb higher frequencies
- Stronger bonds absorb high frequency radiation and weaker ones absorb lower frequency radiation
- The same bonds on different areas of a molecule can absorb different frequencies
- Like AAS - IR light is put into a sample, we measure how much is absorbed. If energy is absorbed in the
sample, less energy makes it to the detector, troughs in energy
- If there is 100% transmittance then all the light passed through the sample.
- If there is less, then some of it has been absorbed, and we can guess what the sample is
- Measuring the absorbance can help to identify what bonds are present
- Transmittance - basically above, how much light is absorbed and doesn't make it to the detector
N2 H2
78% of air contains nitrogen, however there is also 21% More difficult to source, however it can be sourced
oxygen, which will react explosively with hydrogen from CH4 at high temperatures
React methane with steam
Reacting air with methane will remove the oxygen Use a nickel catalyst, and high temperatures
CH4 (g) + 2O2 (g) ⇋ CO2 (g) + H2O(g) CH4 (g) + H2O(g) ⇋ CO(g) + 3H2 (g)