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Chem 1LC S17 - Andrew Phan

Expt 2/Lab Report


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Andrew Phan
on
Apr 20, 2017 @05:25 PM PDT

Table of Contents
Table of Contents 1
Lab Report 2
Lab Report/ 2 of 11

Lab Report

Kim Edwards Jan 22, 2016 @11:15 AM PST

Assigned to
Assignment Status
Student
Assignment # 2a
Name Expt 2 Pre/In Lab
Description

Andrew Phan Apr 12, 2017 @09:44 PM PDT

Chemical Equilibrium
Andrew Phan Apr 12, 2017 @09:44 PM PDT

Objectives
Andrew Phan Apr 18, 2017 @06:22 PM PDT

This experiment will be about chemical equilibrium, and will be about finding the equilibrium between the forward and reverse reactions of

Fe3+(aq) + SCN-(aq) ⇄ FeNCS2+(aq)

While Fe3+ and SCN- are colorless when dissolved in water, their product is a red-orange solution that follows Beer's Law (A = εCl); therefore, the product will
absorb certain wavelengths of light. We will use a spectrometer to measure the absorbance of multiple concentrations of FeNCS2+ by measuring the amount of
light able to pass through the substance. Because FeNCS2+ is the only substance that absorbs light, the amount of light absorbed measured by the spectrometer
will help to indicate how much FeNCS2+ was formed in the reaction.

This experiment also uses Le Chatlier's principle, that if a reaction in equilibrium is disturbed, then equilibrium will shift to reduce the disturbance's effect. In this
experiment's case, the disturbances are the different concentrations of Fe3+ and SCN-. Therefore, each test tube will have a different equilibrium concentration.

Andrew Phan Apr 13, 2017 @04:43 PM PDT

Equipment and Chemical Tables


Andrew Phan Apr 19, 2017 @08:08 PM PDT

Equipment Description Equipment Image

LabQuest2 and Computer

Spectrometer and Cuvette

Kimwipes

10mL Volumetric Flask


Lab Report/ 3 of 11

25mL Volumetric Flask

1mL Graduated (Mohr) Pipet

5mL Volumetric Pipet

1L Beaker (for waste)

4 Test Tubes and "Rack"

Scale

Image Sources (in order, from top to bottom):

https://www.vernier.com/products/interfaces/labq2/

http://www.vernier.com/products/sensors/spectrometers/visible-range/svis-pl/

http://makezine.com/2012/05/15/tool-review-kimwipes-delicate-task-wipers/

http://www.capitolscientific.com/Corning-5640-10-PYREX-10mL-Class-A-Volumetric-Flask-with-Glass-ST-Stopper

https://www.amazon.com/Volumetric-Flask-Break-Resistant-Class/dp/B004K9M7EE

http://www.capitolscientific.com/Dynalon-302765-0001-Graduated-1mL-Mohr-Measuring-Pipet-Class-B-Disposable-Translucent-PP-Non-St

http://www.capitolscientific.com/Kimble-37004-5-KIMAX-5mL-Volumetric-Pipet-TD-Class-A-White-Color-Band
Lab Report/ 4 of 11
http://www.capitolscientific.com/Corning-1000-1L-PYREX-1L-Low-Form-Griffin-Beaker-Double-Scale-Graduated

https://www.montessoribymom.com/store/products/test-tube-rack-wooden/

https://www.alibaba.com/showroom/electronic-scale-connect-to-computer.html

Chemicals
Molar Mass (g mol-1) Other Fire Diamond
H2O 18.015 DI: Distilled?
Fe(NO3 )3 241.86 9 Waters of Hydration
HNO 3 63.01
KSCN 97.181

(For future reference, would it be okay to exclude this table, and write the information inside the fire diamond descriptions instead?)

Andrew Phan Apr 18, 2017 @03:45 PM PDT

Description:

0 H2O
Molar Mass: 18.015g/mol

0 0
DI water is used in this experiment.

Click each diamond division to enter values.

Andrew Phan Apr 18, 2017 @04:32 PM PDT

Description:

0 Fe(NO3)3
Molar Mass: 241.86g/mol

3 0
9 waters of hydration: 162.135g/mol
Combined Molar Mass: 404.00g/mol

Click each diamond division to enter values.

Andrew Phan Apr 18, 2017 @03:46 PM PDT

Description:

0 HNO3
Molar Mass: 63.01g/mol

2 0
Click each diamond division to enter values.

Andrew Phan Apr 18, 2017 @03:46 PM PDT

Description:

0 KSCN
Molar Mass: 97.181g/mol

2 0
Click each diamond division to enter values.
Lab Report/ 5 of 11
Andrew Phan Apr 19, 2017 @08:34 PM PDT

Dilution Plan
Andrew Phan Apr 19, 2017 @08:44 PM PDT

Step five in part B requires us to fill three test tubes with 5.0mL of the dilute solution. We will also need some solution for a blank cuvette to calibrate the
spectrometer. Since we need more than 10mL, we should make 25mL, which will be enough for 15mL plus extra.

M1 V1 = M2 V2

(0.20M) (x) = (0.0020M) (0.025L) → x = (0.0020) (0.025) / (0.200) = 0.00025L 0.20M Fe(NO3 )3

We shall transfer 0.25mL Fe(NO3 )3 solution into a 25mL volumetric flask, using a graduated pipet.

Andrew Phan Apr 19, 2017 @08:34 PM PDT

Procedure
Andrew Phan Apr 19, 2017 @09:22 PM PDT

Part A.

1. Wear lab coat, goggles, and gloves.

2. Measure out about 0.8g Fe(NO3 )3 ·9H 2 O. Prerinse 10mL volumetric flask with 0.1M HNO3 solution, then pour Fe(NO3 )3 in. Dissolve up to 10mL line with 0.1M
HNO 3 solution.

3. Use dilution plan above to create 25mL 0.0020M Fe(NO3 )3 solution. Fill up to 25mL line with DI water.

4. Stockroom already prepared KSCN for us. Mass and concentration will be shown below.

Part B.

5. Label four test tubes 1 to 4. Mix each solution thoroughly.

- Test Tube 1: 5mL dilute Fe(NO3 )3 solution, 2mL KSCN solution, 3mL DI water

- Test Tube 2: 5mL dilute Fe(NO3 )3 solution, 3mL KSCN solution, 2mL DI water

- Test Tube 3: 5mL dilute Fe(NO3 )3 solution, 4mL KSCN solution, 1mL DI water

- Test Tube 4: 9mL 0.20M Fe(NO3 )3 solution, 1mL KSCN solution

6. Table in observations.

7. Temperature of solution recorded in observations.

8. Get LabQuest2, SpectroVis Plus spectrometer, and cuvette from stockroom. Connect spectrometer to LabQuest2 with provided USB cable.

9. Fill cuvette three quarters full with dilute Fe(NO3 )3 solution, and wipe down sides with kimwipes. Place in designated spot in spectrometer. Calibrate
spectrometer; let lamp warm up first.

10. Pour out cuvette into a waste beaker, and prerinse with solution one. Fill cuvette three quarters full with test tube one solution. Wipe the outside with
kimwipe, and place in spectrometer. Record data.

11. Repeat step 10 with the other three test tubes. Email test data to our own email.

12. Pour waste beaker into designated waste bottle in hood. Record another group's data table.

Andrew Phan Apr 13, 2017 @06:07 PM PDT

Observations
Andrew Phan Apr 20, 2017 @05:14 PM PDT

Part A.

- Fe(NO3 )3 looked like a white powder, but not quite perfectly white. Its particles did not look very fine either.

- HNO3 looked like a clear liquid, with water-like appearance and viscosity.

- When the Fe(NO3 )3 was dissolved into HNO3 , the ensuing solution was orange in color. It was very viscous, and slowly slid flowed down the flask's neck. Over
time, as the solute dissolved, the solution looked more yellow than orange; the solution was still quite clear.

- The diluted Fe(NO3 )3 solution was clearer than the other solution.

- The KSCN solution prepared was .38772g KSCN dissolved in 2L de-ionized H2 O. I shall find the concentration later.

Part B.

- The temperature was 22°C.

- KSCN was also clear like water.

- When pouring KSCN into our flasks of Fe(NO3 )3 , the solution turned more orange again, more than before.

- Each test tube was successively more orange than its others.

Our Group's Data Table


Lab Report/ 6 of 11
Test Tube Number Volume Fe(NO3 )3 (mL) Concentration Fe(NO3 )3 (M) Volume of 1.99(10)-3 M KSCN (mL) Volume of H2 O (mL) Absorbance (λmax = 444.5 nm)

1 5 0.00198 2 3 0.237

2 5 0.00198 3 2 0.550

3 5 0.00198 4 1 0.749

4 9 0.198 1 0 1.472

Graph

(in order, from bottom to top):

Calibration, Test Tube 1, Test Tube 2, Test Tube 3, Test Tube 4 (standard)

Other Group's Data Table

Test Tube Number Volume Fe(NO3 )3 (mL) Concentration Fe(NO3 )3 (M) Volume of 1.99(10)-3 M KSCN (mL) Volume of H2 O (mL) Absorbance (λmax = 446.9 nm)

1 5 0.002 2 3 0.336

2 5 0.002 3 2 0.498

3 5 0.002 4 1 0.697

4 9 0.2 1 0 1.136

Andrew Phan Apr 18, 2017 @04:24 PM PDT

Calculations
Andrew Phan Apr 18, 2017 @05:31 PM PDT

1. For all trials (including those trials from the other pair of students), calculate the initial
concentrations of the reactants, [Fe3+]i and [SCN–]i.
Lab Report/ 7 of 11
Andrew Phan Apr 20, 2017 @04:33 PM PDT

All groups used the same solutions and materials, so all concentrations will be the same.

10mL Volumetric Flask of Fe(NO3 )3

Solute: 0.800g Fe(NO3 )3 ·9H2O

9 waters of hydration

Molar Mass Fe(NO3 )3 : 241.86g mol-1

Molar Mass 9H2 O: 162.14g mol-1

Molar Mass Fe(NO3 )3 ·9H2O: 404.00g mol-1

Moles Fe(NO3 )3 : 0.800g / (404.00g mol-1) = 0.00198mol

Solvent: 0.010L HNO3

M = (mol solute)/(L solvent) = 0.00198mol / 0.010L = 0.198M Fe(NO3 )3

25mL Volumetric Flask of Dilute Fe(NO3 )3

Solute: Fe(NO3 )3

Volume of Initial (10mL) Solution: 0.00025L

Solvent: HNO3

Total Volume of New Solution: 0.025L

M = 0.00198M Fe(NO3 )3

Prepared Solution of KSCN

Solute: 0.38772g KSCN

Molar Mass KSCN: 97.181g mol-1

Moles KSCN: 0.38772g / (97.181g mol-1) = 0.003989mol KSCN

Solvent: 2.00L H2 O

M = 0.00199M KSCN

Test Tube One

Volume Fe(NO3 )3 0.00198M solution: 0.005L

Volume Test Tube: 0.010L

M 1 V1 = M 2 V2

(0.00198M) (0.005L) = ([Fe3+]i) (0.010L) → [Fe3+]i =(0.00198) ( 0.005) / (0.010) = 0.00495M Fe(NO3 )3

Volume KSCN 0.00199M solution: 0.002L

(0.00199M) (0.002L) = ([SCN-]i) (0.010L) → [SCN-]i = (0.00199) (0.002) / (0.010) = 0.000398M SCN-

Our Group

Test Tube Number Volume Test Tube (L) Volume Fe3+(L) [Fe3+]i (M) Volume SCN- (L) [SCN -]i (M)

1 0.010 0.005 (dilute) 0.000990 0.002 0.000398

2 0.010 0.005 (dilute) 0.000990 0.003 0.000597

3 0.010 0.005 (dilute) 0.000990 0.004 0.000796

4 0.010 0.009 (non-dilute) 0.178 0.001 0.000199

Other Group

Test Tube Number Volume Test Tube (L) Volume Fe3+(L) [Fe3+]i (M) Volume SCN- (L) [SCN -]i (M)

1 0.010 0.005 (dilute) 0.00100 0.002 0.000400

2 0.010 0.005 (dilute) 0.00100 0.003 0.000600

3 0.010 0.005 (dilute) 0.00100 0.004 0.000800

4 0.010 0.009 (non-dilute) 0.180 0.001 0.000200


Lab Report/ 8 of 11
Andrew Phan Apr 18, 2017 @05:31 PM PDT

2. Show the derivation of equation (2).


Andrew Phan Apr 18, 2017 @05:41 PM PDT

Beer's Law: A = εCl

A: Absorbance

ε: Molar Absorptivity Constant (constant with material in sample: FeSCN2+)

C: Concentration

l: Path length of light through solution (constant with spectrometer used)

Because ε and l are constant, we can rewrite the equation to A/C = εl

Because εl are the same across all samples used, Aeq/Ceq = Astd/Cstd

Rewriting the equation gets us: Ceq = (Aeq/Astd) Cstd

Andrew Phan Apr 18, 2017 @05:46 PM PDT

3. Show the derivation of equations (3) and (4) by creating an ICE chart (Initial Change
Equilibrium).
Andrew Phan Apr 19, 2017 @09:35 PM PDT

Fe3+(aq) + SCN-(aq) ⇄ FeNCS2+(aq)

Equation (3) [Fe3+]eq [Fe3+]i [FeSCN 2+]eq

Initial 0 x 0

Change +x -x +x

Equilibrium x 0 x

[Fe3+]i = [Fe3+]eq + [FeSCN2+]eq → [Fe3+]eq = [Fe3+]i - [FeSCN2+]eq

Equation (4) [SCN -]eq [SCN -]i [FeSCN 2+]eq

Initial 0 x 0

Change +x -x +x

Equilibrium x 0 x

[SCN -]i = [SCN-]eq + [FeSCN2+]eq → [SCN-]eq = [SCN-]i - [FeSCN2+]eq

Andrew Phan Apr 18, 2017 @04:24 PM PDT

Andrew Phan Apr 18, 2017 @05:58 PM PDT

4. Calculate [FeNCS2+]std.
Andrew Phan Apr 19, 2017 @10:50 PM PDT

The standard solution contains a large amount of Fe3+ and a small amount of SCN-. Due to Le Chatelier's Principle, one can expect that by having such a large
imbalance of reactants, equilibrium will be shifted far to the right, with almost all of the SCN - reacting. Therefore, for every mole of SCN- reacting, a mole of
FeSCN2+ is formed. Therefore, one can assume that [FeSCN2+]std = [SCN-]i. [FeSCN2+]std = 0.000199M

Andrew Phan Apr 18, 2017 @06:11 PM PDT

5. For all trials (yours and the other pair’s), calculate the equilibrium concentrations of
the reactants and products, [Fe3+]eq, [SCN–]eq, and [FeNCS2+]eq.
Lab Report/ 9 of 11
Andrew Phan Apr 20, 2017 @10:36 AM PDT

Test Tube One

C eq = (Aeq/Astd) Cstd

Aeq = 0.237

Astd = 1.472

C std = 0.000199M FeSCN2+

C eq = (0.237/1.472) (0.000199M) =0.0000320M → 3.20 (10)-5

[Fe3+]eq = [Fe3+]i - [FeSCN2+]eq

[Fe3+]i = 0.000990M

[Fe3+]eq = 0.000990M - 0.000320M = 0.000958M → 9.58 (10)-4

[SCN -]eq = [SCN-]i - [FeSCN2+]eq

[SCN -]i = 0.000398M

[SCN -]eq = 0.000398 - 0.0000320M = 0.000366M → 3.66 (10)-4

Our Group

Test Tube Number [FeSCN 2+]std (M) [FeSCN 2+]eq (M) [Fe3+]eq (M) [SCN -]eq (M)

1 0.000199 3.20 (10)-5​ 9.58 (10)-4 3.66 (10)-4​

2 0.000199 7.44 (10)-5 9.16 (10)-4 5.23 (10)-4

3 0.000199 1.01 (10)-4 8.89 (10)-4 6.95 (10)-4

4 0.000199 1.99 (10)-4 1.78 (10)-1 0.00

Other Group

Test Tube Number [FeSCN 2+]std (M) [FeSCN 2+]eq (M) [Fe3+]eq (M) [SCN -]eq (M)

1 0.000200 5.92 (10)-5 9.41 (10)-4 3.41 (10)-4

2 0.000200 8.77 (10)-5 9.12 (10)-4 5.12 (10)-4

3 0.000200 1.23 (10)-4 8.77 (10)-4 6.77 (10)-4

4 0.000200 2.00 (10)-4 1.80 (10)-1 0.00

Andrew Phan Apr 20, 2017 @10:37 AM PDT

6. For all trials (yours and the other pair’s), calculate Kc.
Lab Report/ 10 of 11
Andrew Phan Apr 20, 2017 @05:20 PM PDT

Fe3+(aq) + SCN-(aq) ⇄ FeNCS2+(aq)

Test Tube One

Kc = [FeNCS2+]eq / ([Fe3+]eq [SCN-]eq)

Kc = (0.0000320) / (0.000958) (0.000366) = 91.3

Our Group

Test Tube Number Kc (M-1)

1 91.3

2 155

3 163

Other Group

Test Tube Number Kc (M-1)

1 184

2 188

3 207

Andrew Phan Apr 20, 2017 @04:34 PM PDT

Error Analysis
Andrew Phan Apr 20, 2017 @04:35 PM PDT

1. Perform a Q-test on either the lowest or highest K value (choose the one most likely to
be an outlier). If the data point fails the test, throw it out. Then, determine an average
value for Kc and the estimated standard deviation.
Andrew Phan Apr 20, 2017 @04:54 PM PDT

Test tube one seems to be the most likely outlier.

Q = gap / range = (155- 91.3) / (207 - 91.3) = 0.551

Because this 0.551 < 0.560, we cannot say with 90% certainty that this value is an outlier.

Average Kc = (91.3 + 155 + 163 + 184 + 188 + 207) / 6 = 165M-1

Standard Deviation = [((91.3 - 165)2 + (155 - 165)2 + (163 - 165)2 + (184 - 165)2 + (188 - 165)2 + (207 - 165)2 ) / 6]1/2 = 36.9

Andrew Phan Apr 20, 2017 @04:54 PM PDT

2. What modifications could be made to the procedure to better account for random
(indeterminate) errors?
Andrew Phan Apr 20, 2017 @05:00 PM PDT

- The glassware used by the class was wet with water; the glassware had been previously used by another lab, and were still wet from being rinsed. This volume
of water can lead to errors that the class was unable to avoid for sake of time. To fix this, we could have used drier glassware for the experiment.

- Through the transportation of Fe(NO3 )3 (s) powder from the back of the lab to our stations, there could have been a small loss of powder to the wind; the powder
may have remained stuck to the paper we carried it as well. To adjust for this, we could have moved closer to the station to prevent the powder from being
exposed to open air as much as possible.

Andrew Phan Apr 20, 2017 @05:00 PM PDT

3. List three potential systematic (instrumental, methodological, or personal) errors that


could be made in this experiment.
Lab Report/ 11 of 11
Andrew Phan Apr 20, 2017 @05:10 PM PDT

- The class did not use all volumetric glassware; the class had to use graduated pipets to transfer very small volumes of solution to other glassware. Because this
glassware was not volumetric, it was less accurate than the volumetric glassware by a small degree. However, all glassware, volumetric or not, are not exactly
accurate to the values they claim to contain; therefore, the glassware we use will always include a bit of instrumental error.

- DI water, while very pure, may still contain some non-ionic chemicals within it. These chemicals may affect our experiment's results, if just a little bit.

- While volumetric glassware is very accurate, the lines still have a width to them. Therefore, the meniscus, while touching the line, may not align exactly with the
line as to equal the volumetric glassware's intended volume. Because the student reading the glassware's measurements cannot observe exactly where the
meniscus is, there may be some error with the volumes held by the glassware.

Andrew Phan Apr 20, 2017 @05:10 PM PDT

4a. Why did you blank with the 0.0020 M Fe(NO3)3 solution as opposed to just DI water?
What does it do to your spectrum?
Andrew Phan Apr 20, 2017 @05:13 PM PDT

The Fe(NO3 )3 solution is more similar to our test tubes than DI water would be. This would calibrate the spectrum towards Fe(NO
3 )3 rather than DI water, which
may reduce the gap between the calibration and actual values.

Andrew Phan Apr 20, 2017 @05:14 PM PDT

4b. What chemicals create the absorbance you observe from the standard solution (Test
Tube #4)?
Andrew Phan Apr 20, 2017 @05:16 PM PDT

The FeSCN2+ and Fe 3+ create absorbance from the standard solution; this is due to the fact that both have color.

Andrew Phan Apr 20, 2017 @05:16 PM PDT

4c. How can you find the absorption of only the FeNCS2+ in the standard solution?
Andrew Phan Apr 20, 2017 @05:17 PM PDT

The blank cuvette's absorbance is essentially the Fe3+'s absorbance. Therefore, by subtracting the graphs, one could find the absorbance of only FeSCN2+.

Andrew Phan Apr 20, 2017 @05:18 PM PDT

5. Did any gross errors occur? Did you mess up? Did the equipment or instrumentation
fail?
Andrew Phan Apr 20, 2017 @05:19 PM PDT

Towards the end of the experiment, our group was running out of 0.200M Fe(NO3 )3 solution, so we were unable to fully rinse cuvette after the first test. There
may have been some contamination left from previous tests that we were unable to rinse out, and that may have affected our results for test tubes 2, 3, and 4.

Andrew Phan Apr 18, 2017 @06:16 PM PDT

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