GIST 

Anal Chem 9/10/2016

2. TOOLS OF THE TRADE

GIST Analytical Chemistry by Kim, Tae-Young

Why do we need to study this chapter?

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Analytical Chemistry

Measurement

Lab Safety Lab Notebook

Concentration

Mass Volume
Analytical balance Buret
Buoyance Volumetric flask
Filtration Pipet
Oven/Desiccator Syringe

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1. Safe, Ethical Handling of Chemicals & Waste

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 Safety Rule: Familiarize yourself with the hazards & do nothing that you consider to be
dangerous.
 Wear goggles or safety glasses at all times in the lab.
 Wear a flame-resistant lab coat & gloves.
 DO NOT eat or drink in the lab.
 Proper use of a fume hood.
 Clean up spills immediately.
 Label all vessels to indicate what they contain.

 Green Chemistry
 Minimize waste production & dispose of chemical waste in a responsible manner.
 Recycling of chemicals, if economically feasible.

2. The Lab Notebook

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 Lab notebook must:

 State what was done.
 State what was observed.
 Be understandable to someone else (Reproducible!).

 Benefits of writing a complete & legible lab notebook.

 Grounds for filing a patent: Anything of potential importance should be signed & dated by a second
person.
 Good resources for writing a scientific paper.
 A systematic way to find & fix the errors made during experiments.

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3. Analytical Balance
: Terms
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 Readability: The smallest increment of mass that can be

indicated.
 Microbalance: Weighs mg quantities with a readability of
1 μg.
 Tare: The mass of the empty vessel.
 Weighing by difference: Hygroscopic reagents.
 Step 1. Weigh a capped bottle containing dry reagent.
 Step 2. Quickly pour some reagent from the weighing bottle into a
receiver.
 Step 3: Cap the weighing bottle & weigh it again.
The difference = the mass of reagent delivered
An electronic analytical balance.
Hygroscopic: Rapidly absorb moisture from the air

Analytical balance
: How an electronic balance works?
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Analytical balance
: Preventing weighing errors
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 Samples must be at ambient temperature to prevent errors due to convective air currents.
 A sample that has been dried in an oven takes about 30 min to cool to room temperature.
 Place the sample in a desiccator during cooling to prevent accumulation of moisture.
 Use tweezers or a tissue to place objects on a balance.
 The warmth of your hand & your fingerprints can affect the apparent mass of an object.
 Close the glass door of the balance to prevent drafts from affecting the reading.
 Should be located on a heavy table to minimize vibrations.
 Keep the balance leveled with adjustable feet & a bubble meter.
 Keep the object to be weighed close to the center of the pan.
 Use a spacer (e.g., an upside-down beaker) in weighing magnetic objects to minimize
magnetic attraction.

Calibration of an analytical balance

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Linearity error.

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Analytical balance
: Buoyancy error
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 Buoyancy: The upward force exerted on an object in a liquid or gaseous fluid.

 The mass of an object weighed in air = the actual mass − the mass of air that it displaces

 If mass m′ is read on a balance, the true mass m of the object weighed in vacuum is

 da: The density of air (0.0012 g/mL near 1 bar & 25ºC).
 dw The density of the calibration weights (8.0 g/mL).
Buoyancy correction.
 d: The density of the object being weighed.

4. Burets
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 Buret: A precisely manufactured glass tube with graduations

enabling you to measure the volume of liquid delivered
through the stopcock (the valve) at the bottom.
 Parallax: The error that occurs when your eye is not at the
same height as the liquid.

 Operating a buret.

Wash buret with new solution Read bottom of concave meniscus

Eliminate air bubble before use Estimate reading to 1/10 of a division
Drain liquid slowly Deliver fraction of a drop near end point
Avoid parallax Account for graduation thickness in readings

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Autotitrator
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 Deliver reagent from the bottle at the left to

the beaker at the right.

 The electrode immersed in the beaker

monitors pH or the concentrations of
specific ions.

 Volume & pH readings can go directly to a

computer for manipulation in a spreadsheet.

5. Volumetric Flasks
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 Volumetric flask: A glassware calibrated

to contain a particular volume of solution
at 20ºC when the bottom of the meniscus
is adjusted to the center of the mark on
the neck of the flask.

 Most flasks bear the label “TC 20ºC,”

which means
“To contain at 20ºC”
 Pipets and burets are calibrated to deliver,
“TD,” their indicated volume.

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Acid washing of glassware

: Remove trace of chemicals
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 Glass is notorious for adsorbing traces of chemicals−especially cations.

 For critical work, you should acid wash glassware: Replace low concentrations of cations
on the surface with H+.
 Soak already thoroughly cleaned glassware in 3-6 M HCl or HNO3 in a fume hood for > 1h.
 Rinse it well with distilled water.
 Finally, soak it in distilled water.
cf. This acid solution can be reused many times, as long as it is only used for clean glassware.

6. Pipets & Syringes

: Pipets
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 Pipet: Deliver known volumes of liquid.

 (a) Transfer pipet: Deliver one fixed volume.

Do not blow the last drop out of a transfer pipet!!!
 (b) Measuring (Mohr) pipet: Deliver a variable volume.

 The transfer pipet is more accurate. (why?)

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Micropipets
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 Micropipets: Deliver volumes of 1 to 1000 μL.

 Sources of error for micropipettes

 Use tip recommended by manufacturer. Other tips might
make inadequate seal.
 Take up & expel liquid 3X before delivery to wet pipet tip &
equilibrate the inside with vapor.
 Unnecessary wiping of the tip can cause loss of sample.
 Liquid must be at the same temperature as pipet.
 Micropipets are calibrated at sea level pressure: They are out
of calibration at higher elevations. Errors are greatest for
smallest volumes.

Tolerances for micropipets

: Most accurate volume delivery
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Syringes
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 Microsyringes: Used for sample injection in gas or liquid chromatography.

 Exist in sizes from 1 to 500 μL & have an accuracy and precision near 1%.
 The steel needle is attacked by strong acid and will contaminate strongly acidic solutions with iron.
 A syringe is more reliable than a micropipet, but the syringe requires more care in handling and cleaning.

7. Filtration
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 Precipitates from gravimetric analyses are collected by filtration.

 Mother liquid: Liquid from which a substance precipitates or crystalizes.
 Filtrate: Liquid that pass through the filter.

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8. Drying
: Oven & desiccator
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 Oven: Dry reagent, precipitates, and glassware at

110ºC (Some chemicals require other temperature).
 Use a beaker & watchglass to minimize contamination by
dust during drying.
 Cover all vessels whenever possible!

 Desiccator: A closed chamber containing a drying

agent (desiccant).
 The lid is greased to make an airtight seal.
 Desiccant is placed in the bottom.
 To open, slide the lid sideways, not pull it straight up.

Ordinary desiccator. Vacuum desiccator.

Desiccants
: Drying agents
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9. Calibration of Volumetric Glassware

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 Calibration: The process of measuring the actual quantity mass, volume, force, or electric
current that corresponds to an indicated quantity on the scale of an instrument.

 Calibration of volumetric glassware

 Measure the mass of water contained or delivered by the vessel.
 Convert mass into volume using the density of water.

 Corrections for thermal expansion of solutions & glassware

 c′ & d′: The concentration & density at temperature T′.
 c & d: The concentration & density at temperature T.

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