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1
Quantitative Analysis of Cobalt (II) Ions
Collect
◼ One test tube and six 50 mL Erlenmeyer
flasks (wash clean, oven dry, and cool to r.t.)
◼ Test tube (take 8 mL Co2+ standard soln)
◼ 10 mL Volumetric flask
◼ 2 mL Graduated pipet and pipet filler
◼ Cork stoppers (6)
◼ Cuvette (rinse with water, do not brush it;
return after class)
◼ Dropper
◼ Lens tissue (2)
◼ Take ca. 80 mL of D.I. water with 100 mL
beaker
◼ Unknown cobalt(II) ion solution: give by TA
2021/01/24 revised
2
Objective & Skills
Objective
▪ Determine trace amounts of cobalt(II) ions by quantitative
analysis of [Co(SCN)42-] with spectrophotometer
max: 620 nm
Skills◼ Pipet, volumetric flask, spectrophotometer, and plotting
Light pink
Co2+(aq)
Blue
+ 4SCN-(aq) [Co(SCN)4]2-(aq)
3
absorbed
Transmitted
Absorption Spectrum and Color
Absorption spectrum of Co(SCN)42-(aq)
Complementary color
Beer’s Law
▪ Transmittance: T = P/P0
▪ Absorbance:
A = - logT = e b cA: Measured absorbance
e : Extinction coefficient
b: Path length
c: Concentration of the absorbing substance
▪ Concentration is directly proportional to absorbance for
dilute solution
▪ Calibration curve: Abs (y axis) vs. c (x axis)
4x
x
x
x
x
y = mx + b
A1
C1
5
Step 1: Prepare Blank Solution (without Co2+)
(1) 0.80 mL 6 M HCl
(2) 2.0 mL 50% KSCN
(3) 4.8 mL acetone
Add to volumetric flask from dispenser
◼ Firmly stopper the
flask
◼ Invert repeatedly
◼ Assure mixing well
and solids disappear
◼ Transfer soln into
clean Erlenmeyer
flask
◼ Stopper to prevent
evaporation
Add D.I. water
to 10 mL mark
Dropper
Mark
Pre-set
volume of
disperser
White ppt.
appears
6
Step 2: Prepare Cobalt(II) Sample Solution with Standard Solution
II. Unknown analysis:
Accurately measure x mL unknown
Co2+ soln with 2 mL pipet
* 0.5 ≦ x ≦ 2.0
I. Calibration curve:
Accurately measure indicated volume of 0.10
mg/mL Co2+ standard soln with 2 mL pipet
1) 0.50; 2) 1.00; 3) 1.50; 4) 2.00 mL
To 10 mL volumetric flask
A clean Erlenmeyer flask with stopper on
Add D.I. water till 10 mL mark
Mix thoroughly
Transfer to
Add 0.80 mL 6 M HCl
2.0 mL 50% KSCN
4.8 mL acetone
To 10 mL volumetric flask
Add 0.80 mL 6 M HCl
2.0 mL 50% KSCN
4.8 mL acetone
A clean Erlenmeyer flask with stopper on
Add water till 10 mL mark
Mix thoroughly
Transfer to
Standard sample solutions
• Color intensity increases with concentration
• Transparent without white precipitate
• Checked by TA 7
Formula of Standard Cobalt(II) Sample Solution
Sample
No.
0.10 mg/mL
Co2+ (mL)6 M HCl
50%
KSCNAcetone
0 0
0.8 mL 2.0 mL 4.8 mL
1 0.50
2 1.00
3 1.50
4 2.00
Unknown 0.5 ≦ x ≦ 2.0
0 1 2 3 4 Transparent blue
sample solution
(1) Turn on power and warm up for 20 min.
(2) Empty cuvette holder
(3) Press “Mode” button and set to A (Absorbance)
(4) Set the analytical wavelength (i.e. 620 nm)
(5) Press “BLANK” button to zero set
8
(4) Wavelength
setting
(2) Cuvette
holder
(5) Blank
(3) A/T/C Mode
(1) Power
switch
Step 3: Calibration of Spectrophotometer
9
Calibration: Blank Adjust
Notice:
• Hold the top of cuvette
• Rinse with water
• Do not brush it
• Do not use a test tube
1) Align cuvette in same
direction to control the
path of the light
2) Close lid
3) Press “Blank” button to
blank adjust
Blank soln
1) Rinse cuvette twice
with blank soln
2) Add soln until 1/2 height
3) Wipe with lens tissue
10
Step 4: Absorbance of Standard and Unknown Cobalt(II) Sample Solution
◼ Start testing from lower concentration
◼ Rinse cuvette with test solution twice
◼ Fill cuvette with soln at 1/2 height
◼ Wipe cuvette with lens tissue
◼ Place cuvette in cuvette holder
◼ Align cuvette in same direction
◼ Close lid and read the Absorbance
* Use same cuvette to make whole measurements
0 1 2 3 4
11
Notice of Experiment
◆ Familiar with the operation of pipet, volumetric flask, and
spectrophotometer first.
◆ Use 2 mL graduated pipet to measure 0.10 mg/mL Co2+
standard solution accurately. Do not use graduated cylinder
instead.
◆ Write down all the observation such as color, precipitate, endo-
or exothermic… etc.
◆ After class, waste solution contains heavy metals and organic
solvent that must be recycled.
◆ Wash the Erlenmeyer flasks used and put into oven to dry.
◆ Wash and clean up all the apparatus including pipet.
◆ Hand the cuvette to TA; do not leave in the spectrophotometer.
◆ Turn off the spectrophotometer and put dust cover on.
12
Plot the Calibration Curve
▪ 5-points plot (blank soln included)
▪ X-Y scattering plot (label x,y axes)
▪ Show linear regression (y = mx + b) and R2
▪ The absorbance of the unknown solution should be in
the range of the calibration curve
y = 32.5x + 0.0052
R² = 0.9997
00.1
0.2
0.3
0.4
0.5
0.6
0.7
0 0.005 0.01 0.015 0.02 0.025
Ab
so
rba
nc
e
[Co2+] mg/ mL
Cobalt Solution Calibration Curve
Ax
C
Full version report
13
In your report, it should include
1) Make and print out chart 1
2) Make and print out diagram 1
3) Calculate original Co2+ concentration of unknown with suitable
significant figures and units
Note: Concentration of unknown solution should take into account
its dilution factor (x mL diluted to 10.0 mL)
Chart 1
2[Co ]
2.0 mL0.10 mg/mL
10.0 mL
0.020 mg/mL
+
=
=
Diagram 1
Linear regression
R2
EXCEL X-Y scattering plot and add regression line
Notice of Results
13
Ex. Deliver 5.00 mL solution:
▪ Wash a 10 mL pipet thoroughly.
▪ Rinse twice with small portion of sample solution.
▪ Press valve A of pipet filler and squeeze bulb to
expel the air inside and create a vacuum.
▪ Insert the top of pipet into pipet filler, press valve S
to draw liquid to pass the graduation mark.
▪ Remove pipet filler and quickly cover the top of
pipet with index finger and adjust liquid level to the
mark of 5.00 mL.
▪ Hold pipet vertically and transfer liquid into
container. (One hand hold pipet and the other
hand hold container to operate.)
▪ Remove index finger and free fall the drop on tip
by touching it to the wall of the flask.
▪ Stay for 15 s to drain the solution.
▪ Do not blow out remaining liquid, pipet is calibrated
for this to remain.
▪ Wash thoroughly after use. 14
0 1
2
3
4
5
6
7
8 9
10 ml Ex
20
C
o
25 ml
EX 20
C
o o
0 1
2
3
4
6
7
8 9
0 1
2
3
4
5
6
7
8 9
安全吸球
排氣閥
吸液閥
A
SE
排液閥
安全吸球
5
6
7
8
9
10
Totally Delivery
Aspirate
valve
Bulb
Suction
valve
Empty
valve
Pipette
filler
T12 - Graduated Pipet
Transfer
pipetPipet
15
T13 - Volumetric Flask
▪ Wash a 10 mL volumetric flask thoroughly
and rinse with D.I. water.
▪ Transfer the solution to flask with the help of
a funnel.
▪ Fill the flask about half-full and swirl the
contents to achieve solution.
▪ Bring the liquid level almost to the mark.
▪ Use a dropper to add solvent drop by drop
to the mark.
▪ Stopper the flask and invert repeatedly to
assure homogeneous.
▪ Pour the solution in flask for later use.
▪ Wash immediately after use.
標線刻度
100 ml
±0.15 In
20oC
Mark
16
Dispenser
1. Check if the pre-set volume is
correct, do not change the
volume setting afterwards.
2. Position the volumetric flask
under the tip of dispenser.
3. Lightly pull the piston pump up
and down several times to get
rid of the bubbles (done by TA).
4. Lightly pull piston pump up to
the top, then slowly push down
to obtain the measured solution.
(2)
(1)
(3)
(4)
I. Prelab report
✓ Objective
✓ Principle
✓ Chemicals
✓ Procedures
17
II. Exp. Records
✓ Observation
✓ Operation
✓ Reaction condition
✓ Data and results
III. Final report
✓ Data analysis
✓ Error analysis
✓ Questions and
discussion
✓ Feedback and
suggestion
Full Version Report (within 4 pages)
▪ Submit your lab report at the class next week.
▪ Hand in lab report on time, including prelab report,
records, and final report.
▪ Late submission: -5 points within a week; get 0 point over a
week.
▪ Miss contents: -5 points per category
Category Guidelines
I. Prelab
report
1. Indicate the main principles and chemical equations in summary.
2. List the chemicals’ physical, chemical properties, and toxicity.
3. Use the flow chart to explain the procedures concisely.
II. Lab
record
4. Record the data with correct significant figures and units.
5. Record the observations, operation, and reaction condition in
details.
III. Results
&
discussion
6. Process the data correctly, including the equations and calculation.
7. Indicate the final results with correct significant figures and units.
8. Analyze the results and make the appropriate discussion.
9. Plot the results with appropriate XY axis and indicate each curves.
10. Provide the concrete outcome and constructive suggestion.
18
Scoring Rubrics for Lab Report