CHE029

MODULE 1-3– Analytical Chemistry 1. Spatula - to scoop small amounts of a solid substance
Lesson title: Laboratory Lessons and to scrape something
2. Glass Funnel - used to channel liquid or finegrained
Coverage: substances into containers with a small opening
• Laboratory Equipments 3. Stirring/Glass Rod - used to mix chemicals and liquids
• Techniques and Operations for laboratory purposes
• Identification of Ion metals 4. Thistle Tube - to add liquid to an existing system of
apparatus.
5. Dropper/Pasteur Pipette - used to transport a
INTRODUCTION
measured volume of liquid
ANALYTICAL CHEMISTRY
6. Volumetric Flask - used to measure one specific
- Is a scientific discipline that develops and applies
volume.
methods, instruments and strategies to gain
7. Mohr Burette - used to measure the volume of the
information about the composition and nature of
liquid dispensed
matter
8. Geissler/Acid Burette - used especially in laboratory
- An interdisciplinary branch of science which plays an
procedures for accurate fluid dispensing and
important role in nearly streams of chemistry such as
measurement
inorganic, organic, physical, industrial, and
9. Volumetric Pipette - a tool for measuring precise
biochemistry
volumes of a liquid
- Embraces a wide range of manual, chemical, and
10. Serological Pipette - used in the same way as Mohr
instrumental techniques
pipettes except all the solution must be forced out in the
LABORATORIES
receiving container to deliver required volumes.
- are places where scientists and medical professionals
11. Graduated Cylinder - used to accurately measure the
conduct studies to perform other work relevant fields
volume of a liquid
CLASSIFICATION OF USES OF LABORATORY EQUIPMENTS
12. Beaker - Used to hold and heat liquids.
• USED TO MEASURE VOLUME
13. Florence Flask - used for heating substances that
• Graduated cylinders
needs to be heated evenly
• Volumetric flasks
14. Erlenmeyer flask - used to heat and store liquid
• Burettes 15. Iodine Flask - used for the wet chemical analysis
• Pipettes 16. Evaporating Dish - used to heat and evaporate liquids.
• USED TO MEASURE WEIGHT 17. Porcelain Casserole
• Analytical balance 18. Watch Glass - used to hold solids when being weighed
• Top loading balances or transported
• Triple Beam balances 19. Ignition Tube - primarily used to hold small quantities
• USED TO MEASURE LENGTH of substances which are undergoing direct heating by a
• Rulers Bunsen burner or other heat source.
• Tape measures 20. Porcelain Crucible - used to heat small quantities to
• Micrometer very high temperatures
• Vernier Caliper (most precise) 21. Crucible Tong – Used to hold the crucible
CLASSIFICATION OF USES OF GLASSWARE 22. Distilling Flask - used for distillation processes.
• Used to Contain 23. Condenser - used in distillation
- Glassware that are used to contain samples as long as 24. Adapter - a device that connects the condenser and
it can contain the samples the receiving flask in a distillation process
• Used to Deliver 25. Test Tube - used by chemists to hold, mix, or heat
- Used to measure and deliver specific amounts of small quantities of solid or liquid chemicals, especially for
samples qualitative experiments and assays
26. Test Tube Rack - is used to hold test tubes while
LABORATORY APPARATUS reactions happen in them or while they are not needed
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27. Iron Stand – used to hold the iron ring and supports 52. Triple Beam Balance - used in the laboratory to
28. Iron Ring – used to hold or support beakers during determine the mass (by weight comparison) of samples
experiments while connected to the iron stand 53. Analytical Balance - measures masses to within
29. Tripod – three-legged support equipment used to 0.0001 g
place above the bunsen burner in the science lab to 54. Hot Plate – Used for heating beakers, Erlenmeyer
heat/boil anything flasks, hot water baths, and other flat-bottomed
30. Burette Clamp - used to fasten glassware into place on containers
a ring stand 55. pH meter – Used to measure acidity of solutions
31. Clay Triangle - used to hold crucibles when they are 56. Wash Bottle – Used for dispensing small quantities of
being heated distilled water
32. Clamp Holder - used to secure an extension-type
utility clamp to a support stand (or ring stand)
33. Mortar & Pestle - used to crush solids into powders
for experiments, usually to better dissolve the solids
34. Bunsen Burner - used for heating and exposing items
to flame
35. Alcohol Lamp – Used to heat things
36. Wing Top/Fish Tail - used to bend glass as it spread
out the heat over a larger area, making it more uniform.
37. Wire Gauze - used to spread heat of a burner flame
38. Cork Borer - tool for cutting a hole in a cork or rubber
stopper to insert glass tubing
39. Thermometer - used to take temperature of solids,
liquids, and gases.
40. Desiccators - used for preserving moisture-sensitive
items
41. Weighing Bottle - used when you're making up a
standard solution
42. Triangular File - used for many cuts, such as cutting
angles less than 90 degrees
43. Petri Dish - use to culture cells, which can be bacteria,
animal, plant, or fungus
44. Spot Plate – Used for observing small amounts of
solids
45. Test Tube brush - used to easily clean the inside of a
test tube
46. Pinchcock - used to regulate or close a flexible tube,
especially in laboratory apparatus
47. Rubber Aspirator – used for moving air, fluids, etc. by
suction
48. Rubber Tubing - is used to connect two openings
49. Separatory Funnel - used in liquid-liquid extractions
to separate (partition) the components of a mixture
between two immiscible solvent phases of different
densities.
50. Buchner Funnel - used in suction filtration
51. Filtering Flask - holds the sample isolated from the
suction by a layer of filter paper.
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LAB TECHNIQUES AND OPERATIONS VOLUMETRIC WARE

BUNSEN BURNER PIPETTE & BURETTE
Successfully
Transferred Liquid = Initial Volume – Remaining Volume

Error In Volume = Successfully transferred liquid -

Volume using the mark of the container

FORMULA TO FIND PERCENT OF ERROR:

Error in Volume
% Error X100
Successfully Delivered Liquid

PRECISION
- Measures how close results are to one another
GAS CONTROL VALVE ACCURACY
- Controls the amount of gas entering the Bunsen - Measures how close results are to the true or known
burner value
- Allowing more gas to enter the Bunsen burner creates
a larger flame DECANTATION
AIR VENTS SUPERNATANT LIQUID
- Increase air flow to the burner producing more - Refers to the liquid lying above a sediment during it
complete combustion and hotter flame settels
LUMINOUS FLAME (YELLOW) SEDIMENT
- Color of the flame when the air vents are closed - Refers to ta substance that lies or settles at the
NONLUMINOUS FLAME (BLUE) bottom
- Color of the flame when the air vents are open FILTRATION
FILTRATE
LAB MEASUREMENTS - A liquid that is obtained after filtering out
• VOLUME RESIDUE
FORMULA TO FIND ERROR IN VOLUME: - Refers to the solid particles that remains after
Error in Volume = Volume by graduated cylinder filtration is performed
– Volume using the mark of container

FORMULA TO FIND PERCENTAGE OF ERROR:

Error in Volume
% Error X100
Volume by graduted cylinder

• MASS
- Grams (g) to Miligrams (mg) = x1000
- Miligrams (mg) to Grams (g) = ÷1000
• LENGTH
- Area of Rectangle = lxw

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GROUP IB METALS (COINAGE/NOBLE)

• Copper (Cu)
IDENTIFICATION OF SELECTED IONS AND METALS • Silver (Ag) (Light-reflective)
QUALITATIVE ANALYSIS • Gold (Au)
- Common experimental method used to identify ions - Group 11 metals (d-block or Transition metals)
in a mixture - Relatively inert and corrosion-resistant metals
- Ions in a mixture are separated by selective (suitable for coin production)
precipitation - Ineffective as weapons because of their malleability
SYSTEMATIC WAYS FOR SEPARATING IONS OR DETERMINING
PRESENCE OF SPECIFIC IONS:
GROUP IIB METALS (ZINC GROUP)
• Selective precipitation
• Zinc (Zn)
• Acid-base reactions
• Cadmium (Cd)
• Oxidation-reduction reactions
• Mercury (Hg)
• Formation of complex ions
• Copernicum (Cn)
- Group 12 in periodic table
GROUP IA METALS (ALKALI METALS)
- Zinc, Cadmium, Mercury are metals with a silvery-
• Lithium (Li)
white appearance and relatively low melting and
• Sodium (Na)
boiling points
• Potassium (K)
- More electropositive
• Rubidium (Rb) - Less noble and always found in nature combine with
• Caesium (Cs) sulfur
• Francium (Fr)
- Found in Group IA of the periodic table TRACE ELEMENTS/IONS
- One valence electron in outer shell (S-block) - Are minute levels of which are found in living tissues
- Lose valence electron to form cation with charge 1+ - Function primarily as catalysts in enzyme systems
(stable)
- Malleable, ductile, good conductors of heat and
electricity
- Shiny and soft metals
- Found naturally only in salts
- Stored under oil to prevent reaction with air

GROUP IIA METALS (ALKALINE-EARTH METALS)

• Beryllium (Be)
• Magnesium (Mg)
• Calcium (Ca)
• Strontium (Sr)
• Barium (Ba)
• Radium (Ra)
- Found in Group IIA of the periodic table
- Many compounds of these metals are basic or Alkaline
- Many compounds are insoluble in water
- Be and Mg are active metals
- Lose two electrons to form 2+ ions
- Less reactive metals

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IDENTIFICATION TESTS FOR GROUP IA AND IIA IDENTIFICATION TESTS FOR GROUP IB AND IIB
METALS METALS
TEST / REAGENT THEORETICAL RESULTS TEST / REAGENT THEORETICAL RESULTS
TS 1 LEMON/PALE YELLOW TS 1 - Refer to the
Magnesium Uranyl precipitate Ammonium color/precipitate
Acetate - Sodium is present Hydroxide produced
TS 2 WHITE precipitate - If no change; add 1-2
Lead Nitrate (II) - Sodium is present mL of Nitric acid

TS 3 YELLOW precipitate ION/METAL PRESENT RESULT

Lead Nitrate (II) - Potassium is present Copper (Cu) Azure Blue Solution
Zinc (Zn) White precipitate
TS 4 WHITE CRYSTALLINE Cadmium (Cd) Colorless Solution
Tartaric Acid precipitate Aluminum (Al) White gelatinous Solution
- Potassium is present Nickel Bluish Green Solution
TS 5 WHITE precipitate Cobalt Pink Solution
Sodium Bicarbonate - Lithium is present Iron Reddish Brown

TS 6 WHITE precipitate IDENTIFICATION TESTS FOR GROUP IB AND IIB

Sulfuric Acid - Lithium is present METALS
TEST / REAGENT THEORETICAL RESULTS
TS 7 WHITE OCTAHEDRAL
TS 2 - Refer to the
Acetic + Oxalic Acid precipitate
Potassium color/precipitate
- Calcium is present
Ferrocyanide produced (Table
TS 8 WHITE precipitate
below)
Potassium Oxalate - Magnesium is present

ION/METAL PRESENT RESULT

TS 9 YELLOW precipitate
Copper (Cu) Brick red or brown precipitate
Potassium Chromate - Barium is present
Zinc (Zn) White precipitate
Cadmium (Cd) White flocculent precipitate
TS 10: FLAME TEST - Refer to the Color of
Iron (Fe) Prussian blue precipitate
the flame

FLAME TEST
ION/METAL PRESENT COLOR OF FLAME
Sodium (Na) Golden Yellow
Potassium (K) Violet/ Purple
Lithium (Li) Carmine Red
Calcium (Ca) Brick Red
Magnesium (Mg) Colorless (No change)
Barium (Ba) Apple Green

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IDENTIFICATION TESTS FOR GROUP IB AND IIB • Cu2+

METALS • Cd2+)
TEST / REAGENT THEORETICAL RESULTS
ARSENIC SUBGROUP CATIONS (Form acidic sulfide and
TS 3 PALE GREEN/DEEP RED COLOR Soluble in KOH)
Acetic Acid - Ferrous 2+ /Ferric ion • Hg2+
3+ • Pb2+
TS 4 BLUE-GREEN COLOR • Bi3+
Sodium Flouride + - Cobalt is present • Cu2+
Alcoholic • Cd2+)
Ammonium
GROUP III:
Thiocyanate - Form insoluble hydroxides in basic solution
TS 5 FADING BLUE COLOR These cations include:
Hydrochloric acid + - Chromium is present • Aluminum (Al3+)
Hydrogen peroxide • Chromium (Cr3+)
• Iron (Fe2+ and Fe3+)
• Nickel (Ni2+)
• Cobalt (Co2+)
ANALYSIS OF GROUP I AND II CATIONS • Zinc (Zn2+)
• Manganese (Mn2+)
- The systematic analysis of cations is an essential
component of salt analysis (or systematic Group IV:
qualitative analysis - Form volatile compounds with ammonium
hydroxide
GROUP I: These cations include:
- Form insoluble Chlorides in acidic solution • Magnesium (Mg2+)
- Cations are those that selectively precipitate as • Calcium (Ca2+)
chlorides when diluted hydrochloric acid is added • Strontium (Sr2+)
- These metals are less reactive than their alkali • Barium (Ba2+)
metal neighbors
These cations include: Group V:
• Silver (Ag+) - Cations that do not fit into the previous four
• Lead (Pb2+) groups.
• Mercury (Hg𝟐 +𝟐+ ) These cations include:
• Sodium (Na+)
GROUP II: • Potassium (K+)
- Form insoluble Sulfides in acidic solution • Ammonium (NH4+)
(Hydrochloric acid) • Lithium (Li+)
• Rubidium (Rb+)
CATIONS REACT WITH H2S :(Form insoluble sulfides) • Cesium (Cs+)
- Mercuric Sulfide (HgS)
- Lead Sulfide (PbS)
- Bismuth Sulfide (Bi2S3)
- Cupric Sulfide (CuS)
- Cadmium Sulfide (CdS)
- Arsenic Trisulfide (As2S3)
- Tin Sulfide (SnS2)
- Antimony (Sb2S)

COPPER SUBGROUP CATIONS: (Not soluble in KOH)

• Hg2+
• Pb2+
• Bi3+
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IDENTIFICATION TESTS FOR GROUP I CATIONS PREPARATION AND STANDARDIZATION OF

TEST / REAGENT THEORETICAL RESULTS O.1 N SULFURIC ACID
VOLUMETRIC ANALYSIS (Titrimetric Analysis)
TS 1 YELLOW precipitate - Is the determination of the volume of a solution of
6M Acetic Acid + 1M - Lead (II) Pb2+ ion known concentration required to react with a given
Potassium Chromate BRICK RED precipitate substance to be analyzed
- Silver (Ag+) ion - An analytical method in which the volume of known
TS 2 WHITE precipitate concentration consumed during the analysis is taken
Sodium carbonate - Lead (II) Pb2+ ion as a measure of the amount of active constituent om
a sample being analyzed
TS 3 WHITE CURDY precipitate TYPES OF TITRATION:
6M Hydrochloric - Silver (Ag+) ion (In • Direct titration
acid (HCl) Acidic solution) • Residual or Back titration
• Blank titration
TS 4 METALLIC SILVER color THE REQUIREMENTS FOR TITRIMETRIC ANALYSIS ARE
Ammonium - Silver (Ag+) ion THE FOLLOWING:
Hydroxide + Formic • Reaction must be complete
acid • Must have an end point detecting device
• Must be rapid
• Must have a sharp endpoint
TS 5 GRAY TO BLACK color
Ammonium - Mercury Hg2+ ion NEUTRALIZATION REACTION
Hydroxide - Is a chemical process in which an acid (proton
donor) reacts with a base (proton acceptor)
- The products are Salt and Water
- This is a reaction which is applicable both in
aqueous and non-aqueous solvents
IDENTIFICATION TESTS FOR GROUP II CATIONS
- The substances in aqueous neutralization
TEST / REAGENT THEORETICAL RESULTS reactions are soluble in water and the acid
TS 1 WHITE/GRAY precipitate solutions used have almost equal strengths in
water
Stannous Chloride - Merucry (Hg2+)
Solution ion
STANDARDIZING A SOLUTION
- Refers to the process of determining an
TS 2 IMMEDIATE BLACKENING
unknown concentration of substance within a
Conc. Ammonium - Bismuth(Bi3+) ion solution
hydroxide + H20 +
STANDARD SOLUTION (TITRANT)
Potassium stannite - The solution (0.1 N Sulfuric acid)
solution - A standard reagent of known concentration
TS 3 REDDISH BROWN precipitate - Solution in the burette
Conc. Nitric acid + - Arsenic (As3+) ion
silver nitrate + PRIMARY STANDARD
sodium acetate - a highly pure reagent, representative of the
number of moles the substance contains that
TS 4 BLACK DEPOSITS in peso coin
can be easily measured or dissolved in a
Tin + 1-peso coin - Arsenic (As3+) ion known volume of solvent to produce a primary
standard solution for titration
TS 5 Conversion of Rhodamine B - The primary standard used in the experiment is
Sodium nitrite + dye’s RED TO LAVENDER anhydrous sodium carbonate
conc. HCl - Antimony (Sb3+) ion
TS 6 WHITE/GRAY precipitate
3N HCI+Mg ribbon + - Tin (Sn4+) ion
Mercuric Chloride
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INDICATOR
- Substance that provides a visible sign of the
presence or absence of a particular chemical
substance or condition
- The indicator used in the experiment is
methyl red
END POINT
- Point of chemical equivalence
- Is signaled by an color change or a change in an
instrumental response

ANALYTE (UNKNOWN CONCENTRATION)

- Components of a sample that are to be
determined
- Substance that is being analyze whose
concentration is unknown in the solution

CHEMICAL REACTION IN THE EXPERIMENT

Na2CO3 + H2SO4 ---> Na2CO4 + H2CO3

- The experiment involves double displacement

reaction wherein the Sodium Carbonate
(Na2CO3) and the Sulfuric acid (H2SO4) react
together which produces Sodium Sulfate
(Na2SO4) and Carbonic acid (H2CO3)

FORMULA OF NORMALITY
N
𝑔 𝑜𝑓 𝑁𝑎2𝐶03
=
(𝑣𝑜𝑙𝑜𝑚𝑒 𝑜𝑓 𝐻2𝑆04)(𝑚𝐸𝑞 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑁𝑎2𝐶03)

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