Lab Report

Lab Practical: Identifying an Unknown Salt

Unknown: 17

Due: 11/16/2011

By: Stephen Kinney

Monday-Wednesday Lab

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Summary- This experiment had us use the majority of the skills we have developed so far

to identify an unknown salt that was assigned to us in lab. We had to do several qualitative

tests to identify the cation and anion in each of our salts. After the ions were identified in

each of the compounds, we had to perform a quantitative test to prove that our salt would

react as predicted based on its formula. When all the tests were finished, I came to the

conclusion that my compound (unknown 17) was potassium iodide (KI).

Procedure- The first part of my experiment consisted of all qualitative tests. The first

experiment I did when I received my salt was a flame test. When I did my flame test, the

compound I was given burned a light violet color. This was a tell tale sign of the cation in my

salt. Next, I did a solubility test to see if my compound was soluble in water. After I tested

the compound’s solubility rate, I checked with the CRC Handbook of Chemistry and Physics1

to see what cations burn violet during a flame test. The CRC Handbook gave me a good idea

of what element my cation was. It was one of three different elements: potassium, rubidium,

or cesium. The next thing test I did was to check and see if my compound was a hydrate. For

this experiment, I added some of my compound to a large test tube and heated it over the

Bunsen burner to see if any water would condense on the side of the test tube. When I heated

my compound with the Bunsen burner, nothing happened, which proved my compound was

not a hydrate. The next thing I did was mix some of my unknown in a beaker filled with

distilled water and added the solution to 6 test tubes. After I had added the solution to the 6

different test tubes, I gathered some solutions to mix with my unknown solution to see if a

precipitate would form. Fortunately, silver nitrate (AgNO 3) was the first and only solution I

mixed with my unknown, and when I mixed these two solutions together, a bright yellow

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Foot note to be replaced.
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precipitate formed. This finding was a very important one in the identification process of my

compound, for earlier in the semester we did an experiment where we had to identify an

unknown halide in a salt by mixing it with AgNO 3. The unknown halide in my previous

experiment turned out to be Bromine, which formed a yellow precipitate when mixed with

silver nitrate. Based on the information from the previous lab I decided my anion could be

either bromine or iodine. The next thing I did in my experiment was identify which anion

was in my compound. To identify my anion I placed 1 mL of my unknown solution, sodium

bromide, and sodium iodide into three separate test tubes, then I added about 1 mL of a

solution containing elemental chlorine and 1mL of mineral oil. When I added the chlorine

and mineral oil to the test tubes containing the sodium bromide and sodium iodide, the test

tube containing the sodium bromide turned a yellowish red color, and the solution containing

the sodium iodide turned a brownish color. I then added the chlorine water to my unknown

solution, which turned dark brown too. I then took all the test tubes and mixed the solutions

with the vortex stirrer to ensure the reaction had gone to completion. After I stirred with the

vortex stirrer, I let the tubes sit for a couple minutes. Several minutes later the solutions

separated from the oil leaving two test tubes with burgundy red solutions on top of the oil

and one with a yellow solution on top. The sodium iodide and my unknown solution

produced a burgundy red solution when mixed with the chlorine water, which led me to the

conclusion that my anion was iodine. The next thing I did in my experiment was identify my

cation by mixing my unknown solution with a solution of Na 3Co(NO2)6, which was supposed

to produce a solid if potassium was my cation. When I mixed my unknown solution with the

Na3Co(NO2)6, the yellow precipitate K3Co(NO2)6 formed, which proved the cation in my

solution was potassium. Based on all my tests I came to the final conclusion that my

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compound was potassium iodide and proceeded on with the quantitative part of the

experiment. The first thing I did was calculate the amount KI and AgNO 3 I would need to

carry out my reaction. I found that I would need about 0.217g of AgNO 3 and 0.212g of my

unknown (KI) to perform this small-scale precipitation reaction. I then measured out about

0.212g of KI and 0.300g of AgNO3, which was more than I calculated because I wanted to

ensure I had enough to complete the reaction. After I had mixed each of the solids in test

tubes with distilled water, I added the solution containing AgNO3 to the solution of KI 1 mL

at a time. When the reaction was completely finished and no precipitate would form with the

addition of more AgNO3, I centrifuged my solid for 5 minutes and decanted the supernatent

liquid when it was done. I then rinsed the solid and repeated the above process twice, and

when the rinsing process was completed I placed my solid in the oven to dry for 2 days.

When I came back, I recoded the mass of my solid AgI to be 0.314g. I then did calculations

to find my percent error.

Observations-

Qualitative tests:

1. Performed a flame test with my unknown compound.

a. My unknown burned a light violet color.

2. Dissolved my substance in water to check its solubility rate.

a. My unknown dissolved immediately and completely.

3. Placed some on my unknown in a test tube and heated it with a Bunsen burner see if it was

a hydrate.

a. When the unknown was heated, there was no condensation that formed on the

side of the tube, which meant it was not a hydrate.

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4. Placed AgNO3 in a test tube and added my unknown in solution form to see what would

happen.

a. When these two solutions were mixed, a bright yellow precipitate formed.

5. Added NaI, NaBr, and my unknown to three different test tubes and mixed them all with

chlorine water and mineral oil on the vortex stirrer. When the solutions separated, there

were distinct color differences between two of the solutions.

a. The NaBr formed a yellowish orange solution.

b. The NaI formed a burgundy red solution.

c. My unknown formed a burgundy red solution.

d. Based on the observations above my unknown anion was I-.

6. Added a solution of Na3Co(NO2)6 to my unknown solution to see if K+ was my cation.

a. When the solution of Na3Co(NO2)6 added to my unknown solution, a dark

yellow precipitate formed, which was K 3Co(NO2)6 and proved my cation was

potassium.

Quantitative test:

7. Measured out KI.

a. 0.215g KI

8. Measured out AgNO3.

a. 0.300g AgNO3.

9. Mixed both solids with distilled water in separate test tubes.

a. Both solids completely dissolved in the water.

10. Added AgNO3 1 mL at a time to the KI.

a. A bright yellow precipitate formed.

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11. Centrifuged and rinsed the solid 2 times.

12. Placed the solid AgI in the oven to dry for 2 days.

13. Removed the solid from the oven and recorded the mass.

a. Mass of solid AgI: 0.314g AgI.

Calculations-

Amount of KI and AgNO3 needed for quantitative precipitation reaction.

Calculations based on the data collected from the precipitation reaction.

Data Collected From Small Scale Precipitation Reaction

Mass unknown 17(KI) 0.215g
   
Mass AgNO3 0.305g
   
Actual Yield AgI 0.314g
   
Theoretical yield AgI 0.304g
   
Experimental Error 3.29%

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Conclusion- To figure out what unknown 17 was I did several qualitative tests to get and

idea of what the cation and anion were in my salt compound. After observing the bright

violet flame during my flame test, I knew my cation had to be K +, Rb+, or Cs+. This led me to

do the Na3Co(NO2)6 test to see if a precipitate would form, which would be K 3Co(NO2)6 and

would identify my cation as K+. Next I identified my anion by mixing my unknown solution

with AgNO3, which formed a bright yellow precipitate. I knew it had to be either I - or Br -, so

I did the chlorine water test with NaI, NaBr, and my unknown to see which ones would look

the same. The NaI and my unknown solution looked identical, which led me to conclude that

my unknown anion was I-. Unknown 17 ended up being KI (potassium iodide). After I

identified my compound, I did the small-scale precipitation reaction to support my

conclusions. When the precipitation reaction was done, I did all the calculations to find out I

had a 3.29% error, which I believed was in part because I did not rinse the solid good enough

leaving trace amounts of the supernatent AgNO3 in test tube. This allowed the AgNO3 to add

to the weight of my solid during the drying process. Next time I do a precipitation reaction I

will be sure to rinse the solid more thoroughly to ensure all the supernatant fluid is removed

for better measurements.