Experiment 32 Lab Proposal

Devin Dustman

Katie Nolan

Lab Section #202

3/22/17
Introduction

Chemistry can be used to identify substances in many differing ways. From emission

spectroscopy, to freezing point depressions, the unique attributes of different compounds can be

used to identify said compounds. This experiment will identify an unknown substance using all

of the skills gained during lab. In this case, the unknown will be identified from a list of 12

chemicals using solubility, conductivity, emission spectrography, pH, absorption spectrography,

density and freezing point depressions. These techniques, in coordination with our knowledge

about these compound’s chemical properties will answer the question, what chemical is in this

container.

This experiment will be used to identify an unknown substance found in a drawer. This

unidentified substance was found by an inspector, who gave the lab 3 hours to identify this

unknown, to avoid a large fine. This is important because unidentified substances can lead to

major issues as it can create identification issues, as well as major problems with mixing

chemicals that may not be what we think they are. As well as this, this experiment is significant

because it will show the many skills we have gained over our two semesters in lab, skills that

will be required to correctly and thoroughly identify the substance. As well as this, this

experiment is important because it shows our understanding of many different chemical

attributes, and our ability to use these in a real world scenario.

In this experiment, we will be largely using a flowchart, created to identify what chemical

substance is in the jar. In this flowchart, found on the next page, a variety of experiments will be

followed in such a fashion as to use the information used in the experiments just completed as to

minimize the amount of work required to successfully identify a compound. As well as this, this
flowchart will help to simply give structure to the experiments, and help avoid wasteful, and

unnecessary tests. This specific flow chart was made in draw.io, with the flowchart function, and

was made with information we largely learned in many earlier experiments. Though as well as

this the peak emission spectrums of these ions were found online (GSU, 2012).
 The first chemical test that will be used to narrow down the identity of the unknown

substance is a basic solubility test in water. This is a very similar test, and simply involves taking

a small amount of either solid, or liquid and mixing it in water, mixing the solution, than

examining the liquid, and seeing if the solute is fully dissolved. For many of the 12 substances

this will be repetitive, as 5 of the chemicals are already diluted in water.

The next chemical test that will be performed is a simple pH test, and this is tested with

the MeasureNet pH probe. All that this process involves is simply putting the pH probe in an

aqueous solution of the compound. For some compounds the substance will be given aqueous,

but for some (solids), they will need to be dissolved into distilled water and then tested. The

compound is acidic if the pH is less than 7.00, basic if the pH is greater than 7.00, and neutral if

it is at or close to 7.00.

After the pH has been calculated is completed, testing conductivity will be the next step

in identifying this compound. Once again conductivity can only be tested if the compound is in

liquid form, as a major part of conductivity is running electricity through something, which can

only be tested for effectively while in liquid form. Once you have an either aqueous solution or a

pure mixture of substance, put a small amount of the liquid onto a watch glass. Once the solution

is in the watch glass, place the dual electrodes of the conductivity detectors into the solution, and

record the amount of light produced. If there is a weak light produced, the substance is a weak

electrolyte, if there is a bright light, it is a strong electrolyte, but if there is no light at all, then it

does not act as an electrolyte at all.

The MeasureNet spectrophotometer will be used in both parts of the experiment for

emission and absorption spectroscopy. Emission spectroscopy will involve the process of

burning the unknown compound in liquid form, and recording the emission spectra with the
MeasureNet. The graphs the data of the wavelengths given off by the known solutions will be

compared to that of the known chemicals they could be associated with. This can be used to

determine which compound is found in the jar. This will not work for all substances, and should

be used sparingly.

Depending on the substance calculated using the flowchart a variety of differing tactics

will be used to confirm the identity of the unknown substance. For example, the density of

substance will be tested if it is a pure liquid, but if it is a soluble solid this test will be nearly

impossible to do, and if the substance is a liquid with an unknown amount of the unidentified

substance, it will once again be impossible to identify. Some more important additional

identification tactics for identifying these known substance are freezing point depression for

soluble solids, testing pH for some liquids, and using a titration curve. As well as this, for some

solutions mixing them with another solution can prove it’s identity. This is true with potassium

sulfate, which when mixed with barium chloride will form a precipitate, as well as with sodium

hydroxide and iron nitrate which will once again form a precipitate, and barium chloride with

silver nitrate which will also form a precipitate.

Experimental

Reagents

A..1 M Hydrochloric acid solution

B.pH 4 and pH 7 buffer solutions

C..1 M Sodium hydroxide solution

D.Silver Nitrate solution

E..1M Barium chloride solution

F..1 M Iron(III) nitrate solution

 G..1 M Sodium chloride solution

H..1 M Potassium chloride solution

I.Distilled water

Equipment

A.MeasureNet Temperature Probe

B.Styrofoam Lids

C.Styrofoam Cups

D.Magnetic Stirrer

E.Stir Bar

F.Hot Plate

G.MeasureNet pH probe

H.Conductivity detector

I.Kimwipes

J.Crucible

K.Crucible Lid

L.MeasureNet drop counter

M.Volumetric Flasks
Setup

Procedures

Part 1: Determination of Solubility in Water

Firstly, collect either 1 gram of solid, or around 15 drops of liquid, and place the unknown in an

empty glass vial. Then squirt around 20 mL of distilled water into the glass vial, and swirl the

mixture around, either manually or with a mixer machine. Once it has been mixed for about 1

minute, examine the mixture and try to identify any non-diluted liquid or any solid that did not

dissolve into the mixture. If there is either of these, the compound is insoluble, if there are none

visible, it is likely soluble.

Part 2: pH of Unknown Substance

For this portion of the experiment the first step is to convert the unknown into a liquid form, this

section will only be completed if the unknown is a solid. Firstly take about 1.00 gram of the

substance, and mix it with around 50 mL of distilled water until all solid particles are dissolved

into the solution. Now that the substance is in liquid form, set up the MeasureNet for recording

pH, and then input the pH probe into the liquid solution, if it began as a liquid, simply input the

probe into the chemical solution. This will display the pH of the solution on the MeasureNet.

Part 3: Conductivity of the Unknown

The conductivity of the unknown substance will be determined using a basic conductivity

detector which is a simple batter connected to a light and 2 electrodes. Once again the first step is

to convert the unknown substance into a liquid if it is not already. For this, measure out about

0.50 grams of solid, and mix it with about 20 mL of distilled water. Put this solution, or the liquid

chemical, if given in that form, into a watchglass, and take out the conductivity detector. Next,

place the two electrodes of the conductivity detector into the liquid in the watch glass

simultaneously, and record the amount of light produced.

Part 4: Emission Spectrography

Firstly, either prepare a solution of the unknown chemical or, this step can be ignored if the

solution is given in liquid form to begin with. This will be done by mixing some of the solid with

an amount of water, the amount mixed is pretty irrelevant, just make sure it is a reasonably high

amount of substance. Now, the bunsen burner must be cleaned, this is done by simply filling the

watch glass with water, heating up the nichrome wire until it is red hot, then pressing the wire

into the water at an angle, as to fill the bunsen burners intake valve with sputtered water vapour,

and water. Repeat this a few times as to clean the bunsen burner thoroughly. Next, repeat this

with the created aqueous solution, or with the given liquid, making sure to correctly sputter the

solution into the intake valve. This will be recorded using the MeasureNet spectrophotometer.

Part 5: Absorbance Spectrography

Once again, if the solution is a solid, it must be dissolved into water, in this case the molarity of

the solution is irrelevant. Once the solution is in liquid form, put the liquid into a small cuvette,

make certain that the cap stays on well. Next, place the cuvette into the MeasureNet absorbance

spectrometer, and save the results to examine later. In this case, getting multiple different
concentrations is irrelevant because you are simply using the absorbance to identify the ion

present, rather than using it for identifying the amount of ion within the solution.

Part 6: Further Confirmation

After following the flowchart to completion, it is important to confirm the identity of the

chemical to a greater degree. This is done differently for different substances, but some important

means of further confirmation are with gravimetric analysis, chemical reactions with certain

aqueous solutions, precise pH, and freezing point depression. It is very important, that once you

have a general idea of what the unknown substance is, to further confirm the identity of the

unknown, this should be done until you confirm the identity in any way available to the

substance at hand, that have not already been performed. Though if time does not allow, simply

just confirm with the basic flowchart.

Results

Unknown:

Solubility in Water Y / N

pH Acidic / Basic

Conductivity Strong / Weak / Nonelectrolyte

Emission Spectroscopy Wavelength at peaks:

Absorption Spectroscopy � Max:

Density Mass: Volume:

Freezing point depression New freezing Mass/volume of Mass of Water:

point: unknown:

Trial 1

Calculations:

Titration Volume of Volume of Equivalence pKb

Unknown reagent Point
(depends on pH
of unknown)

Trial 1

Trial 2

Discussion
 The results of this experiment shows that the unknown substance that was found in the jar

was ammonia. This was shown by the fact that the substance was a non-electrolyte, soluble in

water, slightly soluble, and smelled much like ammonia in high concentrations. All of these facts

come together, and can be used to confirm the fact that the substance, unknown 13, we were

given was very likely ammonia. This makes our identification even more important, as ammonia

is of course both toxic and corrosive, so therefore leaving this substance unidentified could lead

to serious lab accidents, that could possibly be highly dangerous.

Some of the largest errors that could have been made in this experiment comes from the

conductivity test, which gave somewhat shaky results. This is because the liquid we tested was

dim, but when distilled water was tested, the light shown with a similar dimness, indicating a

solution with no ions to conduct the electric current. Because of this, we concluded that the

solution was a non-electrolyte, but this process is not foolproof, and may indicate a mistake.

Another possible error comes from the lack of complete confirmation, coming from our failure to

send over our freezing point depression, which would have provided complete confirmation. But

outside of this our largely quantitative results did provide fairly comprehensive confirmation. As

well as this, an error could have very easily come from the fact that in the experiment all of the

substances that were given were given in solid form, despite what was written in the lab manual,

which identified some of the compounds as liquids. This simple fact threw off the flowchart that

was used, and this could have easily created some pretty major issues in identification.

Conclusion

This experiment was run in order to determine what unknown substance was present in a

container, given three hours to perform as many chemical tests as needed to avoid paying a large

fine. The results from this experiment show that the substance was a non-electrolyte, water
soluble, and created a slightly basic solution when dissolved in water. Through the use of a

titration, the molar mass was found to be. This data shows that the unknown substance in the

container was ammonia.

Bibliography

Sodium Energy Levels. (n.d.). Retrieved March 28, 2017, from http://hyperphysics.phy-

astr.gsu.edu/hbase/quantum/sodium.html

Stanton, B., Zhu, L., & Atwood, C. H. (2006). Experiments in general chemistry

featuring McomparieasureNet. Belmont, CA: Thomson Brooks/Cole.