ANALYTICAL CHEMISTRY LAB QUESTIONS

LAB 1: Introduction

FIRST 2 GENERAL QUESTIONS ARE FROM LAB 1 INTRODUCTION

1. What is the function of each glassware: Beaker, volumetric/ graduate pipette,

cylinder, Erlenmeyer flask, volumetric flask, weighing boat...?

No Equipments Functions
.

1. Beaker Use for contain, dissolve and heating chemical

2.
Weighting boat, Weight the solid chemical.
Weighting
bottle

3. Stirring rod Stirring to dissolve solid chemical.

4. Spatula Mixing, scraping, transferring materials

5. Magnetic bar Stir liquids in a sealed container

and stirrer

6. Pipette Use for transfer or deliver specific, accurate amount of chemical

(Graduated
pipet,
Volumetric
pipet)

7. Pipette Use for suck up small volume of chemical (approximately

(Pasteur pipette, amount, a droplet or a bulb)
Glass pasteur
pipet)

8. Pump Take up chemical solution by pipette

9. Test tube
Observe chemical reaction, temporary storage of chemical

10. Clamp / holder Hold a container of any given substance during an experiment
that often involves heating the substance

11. Test tube rack Hold multiple test tubes upright at the same time
Provide protective storage for test tubes and make transporting
and cleaning test tubes much easier
 12. Volumetric flask Precise volume of chemical for preparation of solution dilution

13. Duran bottle

Contain chemical solution

Media and reagent preparation, media sterilization, liquid

handling and dispensing, filtration, shipping and transport, sample
collection, sterile media storage, sample storage, frozen storage,
long-term archival storage, tissue culturing, microbial culturing,
heating and cooling samples, preparation of bulk intermediates,
and shipping of APIs (active pharmaceutical ingredients).

14. Amber bottle Contain chemical solution

Protect contents from UV rays and are ideal for light sensitive
products
Help eliminate waste and help to insure product integrity for long
term storage

15. Erlenmeyer flask Mixing

16. Burette Measure volume of chemical in titration

17. Balance Determine weight or mass of object

(Analytical
balance,
Electronic
balance)

18. Fume Hood Reduce exposures to hazardous fumes, vapors and volatile gases.

2. What is the function of the datasheet?

 Used as a diary, record:
 All results
 All phenomena of reaction
 All notice or change in procedure
 Provide data to write the final report
 Suggest any error could happen

3. List some safety regulations of the Chemistry lab.

● Be respectful and responsible for your own personal and others safety: googles, gloves, lab
coat, shoes

● No food or drink in lab

● No running or horseplay

● No contact lens in this area

● Find it then ask it

● Clean before and after use

● Check chemical label carefully before use

● Do not touch any equipment, chemicals or other material in lab until you are instructed to
do so

● Unauthorized experiments are not allowed

● Dispose chemical waste, broken glass properly

● When diluting concentrated acid or base, WATER always first

● Keep your face AWAY chemical reaction

● Immediately REPORT any accidents

● NEVER return unused chemical to the stock bottle

● WASH your hand with water if chemicals contact to your skin

● Know where the SAFETY FEATURES or the lab: fire extinguisher, safety shower and first
aid kits...

 Don’t under or overreact

5 QUESTIONS FROM 5 REMAINING LABS

LAB 2: Acid-Base Titration

1. Principle of acid-base titration. What, When, How...
_ Laboratory method of quantitative chemical analysis to determine the unknown
concentration solution (an identified analyte) by using a known concentration solution
(standard solution / titrant). Using indicator to determine the end-point of a titration.
Including 2 parts: standardize a standard solution and then use standard solution to titrate
an unknown solution.

2. Why do we need to contain NaOH in a plastic bottle, not a glass container?

The solution should be stored in a polyethylene bottle since sodium hydroxide can react with
silica from glass containers
 3. What is the purpose of re-standardization?
Since there are a couple of titrants such as NaOH and Na2S2O3 that are unstable, which
means that they can cause error and the solution themselves tend to degrade with time.
Hence, re-standardization is utilized to re-check the concentration of the solution which is
used as standard solution to reduce the error in the subsequence part.

4. Why do we use KHP to re-standardize NaOH? What properties of chemicals are

used as a standard solution?
Not all the time the concentration labeled on the bottle is correct, due to the time, external
factors such as light, temperature, vaporization, etc. contribute to increasing or decreasing the
concentration of the titrant, so, re-standardization will specify titrant concentration again and
reduce errors. Potassium hydrogen phthalate (KHP) is used as a primary standard due to its
stability in air and its large molecular weight for minimizing relative error in weighing.
Properties of chemicals are used as a standard solution:
 High purity
 High stability
 Low moisture absorption
 Readily available and inexpensive
 Not change its size if exposed to air
 Large in size (mass) to minimize weighing errors

5. What is the purpose of adding distilled water into the Erlenmeyer flask before
titration?
Adding distilled water into the Erlenmeyer flask before titration aids to increase the voume
(thickness) of solution to observe color changes easier.

6. In titration, what should we do to improve the accuracy of the result?

• Set up a burette, clean with distilled water and chemicals a few times.
• No leaking and air bubble left in burette
• Label all chemicals (name and concentration) and waste beaker
• Put waste container (beaker) under burette
• Remove funnel after fill up solution
• Using white paper for clear view
• Using wrist to spin the erlen flask, not whole arm
• Start titration at 0 – 2ml level
• Initial reading is always be no decimal number (such as 9ml or 10 ml, not 8.5ml or 8.7ml)
• No interfere between initial reading with final reading of previous titration trial.
• Read the bottom of meniscus
• Record all initial and final reading (with 2 decimal number)
• Record all phenomenon of chemical reaction
• Be careful with all tall and long to break glassware. Keep them on a stable surface and away
from the edge of the table.

7. How to prepare a chemical solution?

_ Calculate the mass

_ Weigh the chemical solid by analytical balance

_ Dissolve in beaker with stirring rod / magnetic stirrer in 50% volume of distilled
water

_ Transfer dissolved liquid into volumetric flask (rinse all glassware few times with
DI water each transferring step)

_ Fill up to mark with distilled water.

_ Mix the solution by flip upside down.

_ Put into container and label

8. List equipment for Chemical preparation / titration technique

● 100ml and 50ml Burette

● Burette clamp and stand

● Stopcock

● 250ml Erlenmeyer flask

● 250ml Volumetric flask

● Beaker

● Volumetric pipette

● Pump

● White papers

● Distilled water bottle

● Funnel

● Plastic bottle
● Analytical balance

● Weighing bottle

● Spatula

● Stirring rod

● Beaker

● Pasteur pipette / Plastic pipette

● Plastic container

LAB 3: Complexometric Titration

1. What is the function of NH3-NH4Cl pH 10 buffer?
NH3-NH4Cl pH 10 buffer is utilized to maintain the optimal pH for EDTA and the whole
reactions as well as provide the suitable environment for EBT to change its color (EBT
changes its color with the pH ranging from 6.3 to 11.5).

2. What is the properties of standard solution?

_ High purity
_ High stability
_ Low moisture absorption
_ Readily available and inexpensive
_ Not change its size if exposed to air
_ Large in size (mass) to minimize weighing errors

3. What is the normal hardness of the water in safe-drinking water?

The hardness of drinking water should not be higher than 170mg/L

4. Why colour of indicator change from pink to blue in this titration?

EBT originally has a blue color. When it reacts with metal ions (Ca2+ or Mg2+) to form a
metal-EBT complex, the solution turns to pink. The metal-EBT complex is then titrated with
EDTA. EDTA can react with metal ions, and the metal-EDTA complex is also more stable
than metal-EBT complex. Once all EBT is replaced by EDTA in the complex, it is released,
and thus the solution turns to the original color of EBT which is blue.

5. Positive and negative effect of water hardness?

• Hard water containing a lot of Mg will taste bitter
• Irritated or dry skin and thin hair, cause eczema, cause dandruff
• When boiled, CaCO3 or MgCO3 precipitates are formed.
• Faded clothes
• Equipment that is often in contact with water is also prone to rust, white residue
• React badly with soap

LAB 4: Redox Titration of Vitamin C (abscorbic acid)

1. What is reducing/ oxidizing agent/ oxidation / reduction process/ redox
reaction/iodometric titration?
 Reducing agent: a compound that loses electrons
 Oxidizing agent: a compound that gains electrons
 Reduction process: a half-reaction in which a chemical species decreases its oxidation
number, done usually by gaining electrons
 Redox reaction (Oxidation - Reduction Reaction): A reaction in which electrons are
transferred between species or in which atoms change oxidation number
 Iodometric titration: a method of volumetric chemical analysis, a redox titration where
the appearance or disappearance of elementary iodine indicates the endpoint

1. When will we use back titration/redox titration?

 Back titration: instead of titrating the original sample, a known excess of standard
reagent is added to the solution, and the excess is titrated. Back titrations are used
when the reaction between the analyte and the titrant is very slow, or when the analyte
is in an insoluble solid.
 Redox titration is used to determine concentration of a solution, based on a redox
reaction between the analyte and titrant. It can be used when we want to analyze for
any oxidizing or reducing agent.

2. Why is H2SO4 added for the titration?

When you do redox reactions involving reagents such as permanganate or chromate, the acid
is there to provide H+ ions to convert the oxygen from the oxidizing agent into water
molecules. A typical half-reaction involving permanganate looks like this:
MnO*4- + 8 H+ + 5 e- -----> Mn2+ + 4 H2*O
It also provides charge balancing. The permanganate begins as K+ and MnO*4- ions and
ends up as K+ and Mn2+ ions. Obvious charge discrepancy there. So the residual SO4*2-
ions from the sulfuric acid help to balance that out.

3. What gives the blue color of the titration

Complex of Iodine + Starch

4. Why do not add starch from the beginning of the titration process? Why do we
have to add starch just before the endpoint?
If you add starch solution at the beginning, excess I3− (triiodide ion) would destroy the starch
structure. That's why you need to titrate dark color to yellow color with thiosulfate solution
first before the addition of starch. That time, I3− concentration is dilute enough, yet give a
dark blue color by making the I3-starch complex. The end point would be dark blue to very
pale pink becace of the presence of Mn2+Mn2+ ions.
In the presence of large amounts of triiodide ion, the iodine may bet rapped in large
aggregates of the iodine-starch complex and not be accessible for reaction with titrant. For
this reason, we add the starch indicator just before the end-point is reached.
During the titration, iodine is slowly released. It could pass the equilibrium point with still
some slow-reacting iodine adsorped to the starch, giving it a black color. That introduces
errors
5. Why do we need to contain KI and KIO3 in the brown Duran?
to protect light-sensitive chemical compounds from visible light, ultraviolet and infrared
radiation which may alter them. To prevent the degradation of light-reactive substances,
maintaining their stability and efficacy.
LAB 5: Spectrophotometric detection of iron
1. What conditions that Beer’s Law can be used to determine the concentration of a
sample?

The equation for Beer’s law is a straight line with the general form of y = mx +b.

Beer’s Law: A = (l)c

with the general form y = (m)x

where the slope, m, is equal to l. In this case, use the absorbance found for your unknown,
along with the slope of your best fit line, to determine c, the concentration of the unknown
solution.

2. Absorbance range from 0.1- 0.9. Why? What should be done if the absorbance of
a sample is out range?
 As the logarithm for absorbance is linearity and the amount of radiation absorbed may
be measured in which calculating the transmission. Absorbance can range from 0 to
infinity such that an absorbance of 0 means the material does not absorb any light, an
absorbance of 1 means the material absorbs 90 percent of the light, an absorbance of 2
means the material absorbs 99 percent of the light. So if the absorbance range is
outside 0.1 to 0.9 it would be unmeaningful
 If the absorbance is higher than 0.9 means that the concentration of samples is too
high. A dilution is needed
 If the absorbance is below 0.1 means that the concentration of samples is too low. An
action on increasing concentration is needed.
3. 2 types of dilution? Conditions to choose suitable type of dilution?
 2 types of dilution: Serial dilution, parallel dilution
 Small volume of stock, a constant dilution factor: serial dilution
 Small volume of stock, a inconstant dilution factor: both
 Large volume of stock, a constant dilution factor: both
 Large volume of stock, an inconstant dilution factor: parallel dilution

4. Function of all agents in reaction: sodium acetate, NH2OH.HCl or

phenanthroline
_ Hydroxylamine hydrochloride (NH2OH.HCl): reducing agent (Fe 3+ => Fe 2+)
_ Penanthroline: color indicator (colorless => red orange)
_ Sodium acetate: maintain Fe 2+ when Fe 3+ => Fe 2+; maintain pH around 3.5

5. What is spectrophotometer?
Spectrophotometer is a device that can measure a light beam's intensity as it passes through a
sample solution.

6. Why should use the wavelength that give maximum absorbance?

 According to the beer-lambert law: c = A/eb +d/eb
 If there is an error (d) in the measurement of absorbance (A), then the concentration
calculation would also contain an error. If d is independent of A, then we can write
c=(A+d)/eb
c = A/eb +d/eb
 Since d is independent, so The absorptivity reaches a maximum at the peak in an
absorbance spectrum which wavelength is the wavelength at which the error in
concentration will be lowest.

7. What should we do to dilute 0.01, 0.02, 0.03 and 0.05M from 1ml of 0.2M H2
SO4?

LAB 6: Thin Layer Chromatography

1. Which pigments, if any, were present in both vegetation? Explain
Carotenoids, including both carotene and xanthophylls, are involved in both carrot and
spinach. Carotenoids absorb wavelengths of violet and blue-green light, so we will
perceive vegetables containing carotene as the opposite colors in the color wheel, which
are yellow and red-orange, respectively. Carrots usually appear to be orange, because this
is a middle color between yellow and red. Spinach contains both chlorophyll (green
pigment) and carotenoids. However, only the green color is observed since chlorophyll
masks the bright color of carotenoids.

2. Why have to use pencil to draw in TLC plate?

The pen ink becomes mobile on the plate and travels up the TLC plate with TLC solvent.
But the solid particles of graphite in the pencil won't get dissolved and hence can be used
to mark TLC plates.

3. What are functions of Acetone and Hexane in extraction step?

The extraction of chlorophylls and carotenoids from water-containing plant materials requires
polar solvents, such as acetone, methanol, or ethanol, that can take up water

The chlorophyll extract will fluoresce when its electrons are excited with light energy.

1. and chromatography step (mobile phase) the experiment?

1. Why spot the sample 1cm above the edge of plate? 1cm away from side of plate?
Distance between 2 spot (1.5cm)?
-Spotting the sample 1cm above the edge of plate to prevent contact with the level of solvent
in the chamber.

-The spots should be marked 1cm away from the side of the plate to have enough space to
move up to the plate. Otherwise, the movements of spots can be impeded since mobile phase
can be washed near the side.

-Distance between 2 spots is 1.5 cm to make sufficient surface areas for the spots to move
along the plate

What is chromatography? How many type of Chromatography? What is TLC / mobile/

stationary phase?

 Chromatography is a laboratory technique that is used to separate components of a

mixture compound.
 4 different types of chromatography:
 According to stationary phase:
 Thin layer chromatography (TLC)
 Column chromatography
 According to mobile phase:
 Gas chromatography (GC)
 High pressure liquid chromatography (HPLC)
 Thin-layer chromatography (TLC) is a chromatography technique used to separate
non-volatile mixtures.
 Mobile phase: an solvent mostly are organic solvent
 Polar solvent: methanol, ethanol, acetone.
 Non-polar solvent: hexane and toluene
 Stationary phase: a thin layer of adsorbent particles, usually silica gel or
aluminum oxide, coated onto a solid plate (glass, aluminum or plastic)

1. Function of buffer?
 Function on reaction
 Create good condition to reaction
 Catalyze reaction speed
 => pH increase solubility EDTA, enhance the ability of ion to bind to EDTA, keep EDTA stable

Properties of standard solution

 DS must react with the analyze
 Must have indicator to reveal equivalent point
Small stock volume, DF constant: serial
Large stock volume, DF constant: parallel
Large, DF not constant use parallel
Small, DF not constant: can use serial with dilution by C1V1=C2V2
For using parallel: we dilute to smaller molar => increase volume of stock by dilution