Chem 211 Tools - 1
Basic Lab Equipment
Handling of Chemicals and Waste
- must always wear safety goggles
should not wear contacts in the lab
plastic gloves are available
a lab coat is recommended
hazardous waste buckets in the fume hood at the back of the room
- if you feel that anything that you are asked to do is dangerous please ask
Lab Notebook
- title, date, partner etc
unknown numbers
write down all observations
note the time that anything is done
Analytical Balance
- these are sensitive instruments
hygroscopic chemicals must be dried and cooled before weighing
weigh a capped bottle of reagent on the balance
then pour some of the weighed chemical into the container to be used
reweigh the capped bottle the difference is how much chemical was used
if the chemical had to be dried before weighing takes ~ 30 min to come back to RT
the general uncertainty is + or – the last digit given on the scale
1. reagents usually can use a top loading balance not as accurate
most reagents are added in excess, slight differences from batch to batch are not NB
especially if you use the same reagents on samples and standards
2. standards all your data depends on your standardization procedure, which starts with weighing out
your standard chemical on the balance
common mistakes are not giving the balance time to settle, leaving the door open to air currents, leaving
volatile samples open to the air, not drying the sample prior to weighing etc
Volumetric Glassware
1. Burettes for titrations
if the tolerance is 0.05 mL eg for a 50 mL burette: the true volume of say 30.0 mL is really somewhere
between 29.95 mL and 30.05 mL
to use a burette properly, it must be vertical
when you read it your eye should be at the same height as the top of the liquid
aquatic solutions will form a concave meniscus
measure to the bottom of the meniscus
estimate the reading to the nearest 10th of a division between marks
read to either the top or the bottom of the painted marks
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1 drop from a 50 mL burette is ~ 0.05 mL
as you get near the endpoint try to add < 1 drop at a time
Burette Usage Tips
1. rinse burette with new solution
2. eliminate any air bubbles
3. drain liquid slowly
4. deliver fractions of drops near the end point
5. read the bottom of a concave meniscus
6. estimate reading to 1/10 of a division
7. avoid parallax (ie read at same height as marking)
8. account for thickness of graduation marks
2. Volumetric Flasks
- calibrated to contain a volume of solution at 20C
flasks are to be filled to the line when the bottom of the meniscus is adjusted to the centre of the mark
on the neck
- to make up solution in volumetric flask:
dissolve the solute in less than the required amt of water (fluid)
once it is completely dissolved and brought back to RT then make up to the mark
3. Pipettes and Syringes
1. transfer pipettes are calibrated to deliver a fixed volume
the last drop of liquid is not blown out
2. measuring pipette delivers a variable volume
3. blow out pipettes rarely encountered where the specific volume must be blown out
- the transfer pipette is the most accurate
the tolerance is the allowed uncertainty in the volume delivered
Using Transfer Pipettes
- use a rubber bulb to draw liquid up the pipette
rinse the pipette with your new solution
overfill the pipette and replace the bulb with your index finger
then wipe the outside of the pipette with a kimwipe
the pipette is calibrated to deliver against the side of a glass beaker
so touch the side of a beaker before releasing your finger
drain against the side of a flask until the bottom of the meniscus just reaches the centre of the mark
then transfer the pipette to the volumetric flask or other container
again touch the side of vessel drain by gravity
after the liquid stops wait a few sec to drain it completely
do not blow out
Micropipettes
- deliver volumes of 1 to 1000 L with accuracies of 1-2% and precisions of 0.5%
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Using Micropipettes
- put fresh tip on the barrel tips have a limited usage
if the pipette is adjustable, set the desired volume with the knob at the top
depress the plunger to the first stop
holding the pipettor vertically, dip it into the
slowly release the plunger to suck up the liquid
remove the pipettor from the solution, but drag the tip along the side of the vessel as you do so this
removes any drops from the outside of the tip
put the pipettor in the new vessel touch the side of the vessel and gently depress the plunger to the first
stop
wait while the liquid drains from the tip then depress the plunger to the second stop to force out any
remaining liquid
rinse the tip with solution first
Syringes
- microlitre syringes are used for very small volumes
1 to 500 L accuracy and precision ~ 1%
syringe should always be rinsed with reagent before use
these are delicate do not throw around
Filtration
- in gravimetric analyses the mass of a product from a reaction is measured
precipitates are collected by filtration, washed, dried and weighed
fritted glass funnel aka filter crucible
suction pulls the solution through
weigh the dried crucible before use and then again after collecting and drying the precipitate
filtrate liquid that passes through a filter
- ordinary filtration can be done using filter paper in a glass funnel or a buchner funnel
Drying
- dry in an oven at ~ 110C
put watch glass over beaker to prevent contamination, but allow drying
must cool before weighing takes around 30 min to reach room temperature
weigh the crucible/flask
ideally you then reheat it and recool it and then reweigh it until a constant mass is obtained (ie 0.3 mg)
Calibration of Volumetric Glassware
- measure out several aliquots and weigh them using the density of water, convert to volume
Calibration of Micropipettes
- these are fairly delicate instruments because they are so abused by students, it’s a good idea to do a
quick calibration at the start of the lab
eg for a 500 L pipette place a 25 mL beaker on the balance and tare it
correctly pipette 10 aliquots into the beaker note the weight convert to volume using density
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Sample Prep
- usually need a homogenized sample can grind to a fine powder using a mortar and pestle or a
mechanical grinder
Acid Digestion of Inorganic materials
most metals dissolve in acid
often dissolve in strong acids such as HCl, HBr, HF, HNO3, H3PO4 and H2SO4
use a Teflon-lined bomb in a microwave
sample is sealed in the bomb and heated to ~200C
Fusion
inorganic substances that do not dissolve in acid can be dissolved by a hot molten inorganic flux
eg lithium tetraborate or NaOH
the unknown substance is powdered and mixed with 2-20 x its mass of solid flux
the mixture is then used in a Pt-Au alloy crucible at 300 to 1200C in a muffle furnace
when it is homogeneous poured into a beaker containing an acid solution to dissolve the product
Digestion of Organic Substances
digestion a reactive liquid such as H2SO4 is added to the substances and boiled or heated in a bomb for
10 to 20 min until everything is more or less dissolved
after cooling, H2O2 is added to discharge the dark colour and then reheated
the sample is then analyzed after this section digestion
Extraction
- an analyte is dissolved in a solvent that does not dissolve the entire sample
often an organic solvent is used
Rules for Significant Figures
1. Leading zeros do not count. 0.0031 is 2 sf
2. Tailing zeros do count. 0.00310 is 3 sf
3. Tailing zeros without decimal point, have no idea. 350,000 ?
4. Use scientific notation: 3.500 x 105 is 4 sf
5. Addition and subtraction: Answer has no more decimal places after the decimal point than the original
number with the fewest significant figures after the decimal point.
eg 14.3
+ 6.2497
20.5497
if numbers are in scientific notation, must first express all of them with the same exponent
6. Multiplication and division: Answer has no more significant figures than the original number with the
fewest significant figures.
eg 12 x 528 = 1593.561368 = 1600 = 1.6 x 102
3.976
7. Rounding < 5 unchanged
> 5 round up
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= 5 round to the nearest even digit
when rounding always look at all digits beyond the last significant digit
eg 1.3499999 to 2 sf = 1.3
8. Logs and antilogs: The number of digits in the mantissa (decimal part) of the log should equal the number
of digits in the original number that was logged
eg log 5.109 x 10-6 = -5.2917
for antilogs, the number of digits in the antilog should equal the number of digits in the mantissa of the
number for which the antilog was taken
eg antilog (-8.39) = 10-8.39 = 4.1 x 10-9
carry as many significant figures as your calculator will permit and only round off when you have
the final answer.
Accuracy vs Precision
Accuracy the extent to which a measured value coincides with the true or accepted value of the
measured quantity.
Precision how closely the individual measurements agree with each other
Errors Systematic and Random
1. Systematic (Determinate) Errors
accuracy is a measure of how close your measurement is to the true value, µ
determinate or systematic error errors affecting the accuracy of an analysis characterized by a
systematic deviation from the true value ie all the individual measurements are either too large or too small
constant determinate error the magnitude is the same for all samples and is more significant when
analyzing smaller samples
proportional determinate error the magnitude depends on the amount of sample and is more difficult
to detect since the result of an analysis is independent of the amount of sample
- to measure. analyze standard reference material in a matrix similar to that of the samples of interest
2. Random (Indeterminate) Error
- affect the precision of an analysis
due to difficulty in measuring things
equal probability that the error is positive or negative
need not affect the accuracy of an analysis
repeatability the precision when all measurements are made by the same analyst during a single period,
using the same reagents and equip
reproducibility precision under any other set of conditions, including between analysts, or between lab
sessions for a single analyst
Error vs Uncertainty
error = the difference between a single measurement and the true value
can be determinate (systematic) or indeterminate (random)
uncertainty = the range of possible values that a measurement might be reasonably expected to have
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uncertainty accounts for all errors that could possibly affect the measurement, both determinate and
indeterminate error
absolute uncertainty expresses the uncertainty in a measurement eg 21.8 0.1 cm
absolute error must always be expressed to one significant figure only.
relative uncertainty compares size of absolute uncertainty to the magnitude of the measurement
eg 0.1 X 100% = 0.5% ie 21.8 0.5 %
21.8
To convert relative error to absolute error
21.8 x 0.5 = 0.109 = 0.1
100
Propagation of Uncertainty
- suppose you had to add a reagent to a flask by several successive transfers using a 10 mL glass pipette
the pipette has been calibrated to deliver 9.992 mL with a standard deviation of 0.006 mL
the standard deviation from the calibration can be used as a measure of uncertainty
this uncertainty tells us that the volumes actually delivered are randomly scattered around the mean of
9.992 mL
if the uncertainty in using the pipette once is 9.992 0.006, what is the uncertainty of using it twice?
we could add the uncertainties together: (9.992 + 9.992) (0.006 + 0.006) = 19.984 0.012 mL
but in doing this, you are assuming that both volumes are either > 9.992 mL or < 9.992 mL
this would be an overestimate of uncertainty
this is as incorrect as assuming that the 2 pipettings were on opposite sides of the pipette’s mean volume:
(9.992 + 9.992) (0.006 - 0.006) = 19.984 0.000 mL
this would be an underestimate of uncertainty
so we use mathematical techniques, which depend on which mathematical operation is being carried out
Addition and Subtraction
the absolute uncertainty is the square root of the sum of the squares of the absolute uncertainties of the
individual measurements
so, for R = x + y + z where x, y, and z are individual measurements and R is the final result:
the uncertainty in R, eR, is given by:
e R = √ e 2x + e 2y + e 2z
Multiplication and Division
the relative uncertainty is the square root of the sum of the squares of the relative uncertainties of the
individual measurements
2 2 2
eR ex ey ez
R
=
√( x) ( ) ( )
+
y
+
z
Mixed Operations treat each operation separately using the equations above
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Other Math Functions
Function eR
R = kA e R= ke A
R=A+B e R = √ e 2A + e 2B
R=A–B e R = √ e 2A + e 2B
R=AxB 2 2
eR eA e
R = A/B
R
eR
=
√( A
eA
) ( )
2
+ B
B
eB 2
R = ln (A)
R
=
eA
√( A ) ( )
+
B
eR =
A
R = log (A) eA
e R = 0 . 4343 x
A
R = eA eR
= eA
R
R = 10A eR
= 2 .303 e A
R
R = Ak eR e
=k A
R A
