Identification and Synthesis of an

Unknown Compound
Department of Chemistry, Michigan State University
East Lansing, MI 48823
November 10th, 2016

In fulfillment of the General Chemistry Laboratory project report requirements under

supervision of Dr. Joseph Ward
Abstract:

The topic of this project is to experimentally determine the identity of an unknown substance.

This can be done through various tests which will identify the properties of the substance, and

this will make it easy to determine the overall identity. It is important to be able to determine the

identity of unknown substances for safety reasons to the public, as well as many chemical

processes that could take place as a result of not knowing how chemicals will react. The group

was able to use solubility tests, as well as pH tests and testing against various acids, to determine

the substance given contained a Carbonate. After further testing and the use of HCl, it was

determined that the identity of the substance was Sodium Carbonate. This was solidified when

taking known Sodium Carbonate and running tests against the unknown compound. The results

of this will be discussed throughout the report, but it can be seen that Sodium Carbonate reacted

almost identically in every test to the unknown compound that was given to the group.
Introduction:

Throughout the duration of this experiment, there was several overall goals. The group was given

approximately 5 grams of an unknown substance. The first part of the experiment was to

determine the identity of the unknown substance. This was able to be accomplished through

multiple rounds of testing and compound mixing, creating reactions that would lead to the

discovery of the different components that make up the unknown substance. Initially, a table

with potential identities of the unknown substance was given and series of testing would help

narrow this list to a few compounds that the unknown substance could be.

Once the identity of the substance is determined by the group, the next part of the experiment

consisted of running further tests in order to confirm or deny the identity previously discovered.

These tests were all different than the original tests used to initially determine the identity of the

compound. The group was able to obtain an amount of the known substance to test against the

unknown substance in order to determine if the compounds reacted the same given the various

tests. This method of identifying unknown substances is essential to various aspects of working

in an analytical chemistry profession. There are various substances unknown to the common

person and these series of tests are important in being able to identify the substance. If one can

identify the substance, they are then able to determine whether the substance is hazardous to

human health or not and determine the proper action that must be taken as a result. Furthermore,

mixing chemicals can be very dangerous to the overall health of society as they could create

potentially dangerous reactions that could result in poison or even death. These reasons are

crucial in understanding the importance of being able to identify unknown substances.

Experimental Details:

To begin procedures for this project, the group was initially given only 5 grams of an

unknown substance. The goal of the first week was to try and identify the substance. A

preliminary table of potential substance identities was given in order to give a starting point

in the process, as shown below:

Table 1: Potential Substance Identities

NaCl KCl Na2SO4 CaCl2 MgSO4

Na2CO3 K2SO4 KNO3 Ca(NO3)2 NH4CO3
NH4Cl (NH4)2SO4 CaCO3 MgCO3 CH3CO2Na

To begin, the group first performed a visual test in order to gain some qualitative information

about the substance. It was seen that the substance is very white and somewhat fine, almost

clumped in little grains. The next step the group took to identify the substance was to test the

solubility. To do this, one member of the group – Cameron – added a small amount of the

substance was added to 1 mL of water and stirred thoroughly in order to see whether or not

the substance forms a homogeneous solution with the water. The next test the group used was

the flame test. Using a Bunsen burner and some wet, thin wood sticks, the other group

member – Taylor – took an amount of the substance and stuck it onto the wood stick and held

it over the flame. The color of the flame and also the flammability of the substance can

further be used to narrow down the identity of the compounds that make up the substance.

Further testing included looking at the pH of the substance. This was done by using an

amount of distilled water to mix with the substance, and then applying a pH strip to the

mixture and watching to see what color the strip turns. The pH test determines whether the
unknown substance is acidic or basic, which will further help narrow down the list of possible

known substances given in table 1.

The tests that followed once these three tests were complete included mixing the unknown

substance with various liquid compounds and determining if a reaction takes place. The first

liquid was 1M Sodium Hydroxide (NaOH). This was followed by 6M Hydrochloric Acid

(HCl). Once all these tests were performed, the given list of possible compounds was then

narrowed down to a specific group of compounds containing the same elements. The final

step in identifying the unknown compound was to gain from the lab each of the possible

known compounds and react them with the 6M HCl. The reason that HCl was used instead of

the other liquids was that this reacted the quickest with the unknown compound since it is a

very strong acid. After going through all of these tests, the group was able to narrow down to

one compound, which will be discussed in the results.

The week that followed included various steps taken in order to confirm the identity that the

group established for the unknown compound. Once a potential identity for the substance is

found, the group obtained an amount of the known substance in order to test it against the

unknown substance and compare the results. The tests for this week varied from the tests

performed in the previous week. The first test was a quantitative solubility test, which tests

the maximum amount of the substance that can be dissolved in 1 mL of water. The following

two tests included using mixing an amount of the unknown substance with two different acid

solutions. These solutions were 6M Nitric Acid (HNO3) and 18M Sulfuric Acid (H2SO4),

which are both very strong acids and will cause a quick reaction with the unknown substance.

For the nitric acid, 10 drops was mixed with 0.5 grams of each of the substances. Similarly,

10 drops of the sulfuric acid was mixed with 0.3 grams of the substances. The overall goal of
running these tests is to see if the known substance reacts the same with the acids as the

unknown substance.

Results:

The general solubility test determined that the substance was completely water soluble, for

the whole substance dissolved after stirring for a sufficient period of time (~2 minutes). To

gain more qualitative data on the substance, the group recognized that the mixture had no

smell, and the color was slightly cloudier. The next test performed was the flame test. The

substance made the flame turn an orange color, and the substance did not burn at all. Given

the outcome of this test, the group was able to determine that the substance was not

flammable on its own. Furthermore, the use of the pH strip determined the pH of the

unknown substance in distilled water. This showed a 9-10 on the pH, proving the substance to

be basic. This helped us narrow down the list of potential known compounds to those that

were mainly basic.

The next tests executed included mixing the substance with different liquid concentrated

compounds to show whether a reaction takes place or not. In 1M sodium hydroxide, the

substance dissolved and was clear in color. Since our substance was shown to be basic by the

pH test, this test was rather inconclusive. Next, in 6M nitric acid, the substance underwent a

chemical reaction. This was shown by condensation on the tube; however, the substance did

not dissolve fully. Not a strong enough test to prove the identity of our substance or narrow

the list any further, the group moved on to Hydrochloric Acid. In 6 molar HCl, the substance

reacted very rapidly in a bubbling manner. Not only did the substance dissolve completely in
a matter of seconds, but it also had a very pungent smell. This helped the group to determine

that there is carbonate in the substance.

The group was then able to narrow down the list of potential substances to 4 main

possibilities: Ammonium Carbonate ((NH4)2CO3), Sodium Carbonate (Na2CO3), Calcium

Carbonate (CaCO3), and Magnesium Carbonate (MgCO3). The group then acquired an

amount of all the substances that contain Carbonate (except Ammonium Carbonate, ruled out

due to the initial smell) and reacted them with three drops of HCl to see which of the

substances had a similar reaction. With MgCO3, there was little reaction. Only a little bit of

bubbling occurred, but no smell was produced. Next, with CaCO3, similar to the Magnesium

Carbonate, the solution bubbled a little bit; however, no smell was produced. The group also

noticed that the solution had a yellow hue to it, which immediately ruled this out as a

possibility. Finally, there was Na2CO3, which produced the most immediate and active

reaction. This solution bubbled all the way up in seconds, while fully dissolving the initial

amount of the substance into it. A very pungent smell then arose from the test tube, which

was identical to what happened when the group mixed the unknown substance into the HCl.

Given this result, the group was able to determine that Sodium Carbonate was the identity of

our unknown substance.

Further testing was to be done in order to confirm the identity of the substance to be what the

group had found experimentally. The first of these tests was the quantitative solubility test.

This test ultimately showed how much of each substance was able to be dissolved in water,

which resulted in the figures given below:

 Table 2: Quantitative Solubility Test

Substance (amount 0.1g 0.3g 0.5g

put in distilled water)
Unknown Substance Fully dissolved Cloudy, not fully N/A
dissolved
Sodium Carbonate Fully dissolved Cloudy, not fully N/A
dissolved

Through these results, one is able to see that the same amount of both the unknown substance

and the sodium carbonate had a threshold of less than 0.3g in the water before it was not able

to fully dissolve. Testing of the sodium carbonate and the unknown compounds in strong

acids showed very much similar results. For the unknown substance in nitric acid, a very foul

smell was produced. The reaction caused the mixture to get very warm and also to bubble up

fast. After a short period of time, Sodium Nitrate began to form on the sides of the test tube.

Similarly, the Sodium Carbonate reacted quickly and produced a warm temperature, as well

as a pungent smell. Also, a solid precipitate which appeared to be Sodium Nitrate began to

form around the sides of the test tube. The third test, mixing Sulfuric Acid with the

substances, produced identical results. The unknown substance turned very hot when added to

the acid. Though there was little bubbling, after a period of time one could notice a crystalline

substance forming around the edges of the test tube. This was the same as the way in which

Sodium Carbonate reacted with the acid. There was not much bubbling, but one could see a

precipitate forming along the sides of the tube and could also feel the heat that was being

produced and radiating from the tube as well.

Discussion:

The overall objectives of this experiment were to determine the identity of the unknown

substance and to prove this using a variety of tests which show the elements that make up the

substance. The group began by using the solubility test. This is a useful test because it shows

the ability of the compound to be broken down and whether the molecules of the substance

can attach to water molecules. Our substance was easily soluble, which showed that the bonds

between molecules were not unbreakable. The flame test is also important in identifying the

compound. Flammability is a very important aspect to know of every compound because it

can be very hazardous given the conditions the compound are exposed to. Since our

substance did not burn when held to the flame, this showed that flammability is not an issue

with this unknown substance. This also enables us to run a wider variety of tests because

heating the substance over flame will not cause any hazardous reactions to occur.

Testing for pH of the substance was necessary in order to narrow down the given list of

potential compounds. A pH test can determine the acidic or basic qualities of the substance.

For the purpose of this experiment, a pH strip was used to determine the overall pH of the

substance in distilled water. One limitation to using a pH strip is that it is not the most

accurate way to measure pH. The use of a pH meter would have been more efficient in

determining the exact pH of the substance. The group was able to determine a pH of around

9-10, proving the substance to be basic. The use of pH testing in very crucial to identifying

whether a substance is safe or not when contaminating water or soil[1]. A very high or a very

low pH could result in various abnormalities occurring. Since the pH obtained was in the

basic range, the group was able to narrow the list down to only those compounds which were

basic.
The mixing of the unknown substance with various liquid solutions was helpful in

determining the ions present in the substance, whether they were anions or cations. A great

majority of the tests run were to determine the presence of anions in the substance. The main

concern of our group was to determine whether there was Ammonia, Carbonate, or Sulfate

present in the compound. Our first test with Sodium Hydroxide was to test for Ammonia.

Since very little reaction occurred, along with the fact that our substance was basic, this was

enough for us to rule out the presence of Ammonia. Our next test was with Hydrochloric

Acid in order to determine the presence of either Sulfate or Carbonate. First, a small amount

of Barium Dichloride (BaCl2) was added to a small amount of HCl and then mixed with our

unknown substance. The formation of a precipitate would have indicated the presence of a

sulfate; however, no precipitate was formed. The group then added the substance to only HCl

to observe if a reaction would take place. This yielded a great and rapid reaction, containing a

lot of fizzing and bubbling, and this indicated to us that there was a carbonate ion present in

the solution.

After narrowing the list of potential compounds to only the ones that contained carbonate, the

group was then able to test each carbonate and see which had the same reaction as our

substance. This was a great advantage to the group because it determined which of the

substances would react exactly the same as our unknown substance. Since Ammonium

Carbonate initially had a smell, this was enough to rule it out as the unknown compound

since it was odorless. There was not much of a fizzing reaction when HCl mixed with both

Magnesium and Calcium Carbonate and this was the main factor that helped us determine

that carbonate was present. Magnesium is often used to neutralize an acid and this explains

why there was little reaction occurring[2]. Calcium has the same effect; however, this is not
the case with Sodium Carbonate. This is because this contains sodium, which is a strong acid.

Ultimately, this aided the strong reaction occurring between the unknown substance and the

HCl. These results were enough to confirm to the group the Sodium Carbonate was the

identity of our unknown substance. It is also important to note that the pH of Sodium

Carbonate is about 10.5[3], which is the same as our unknown compound, further solidifying

the identity that was obtained by the group.

Conclusion:

To conclude the experiment, it is important to state that the identity obtained for the unknown

substance was determined to be Sodium Carbonate. This is due to the results of all of the tests

previously run, which helped decompose the substance into its ions and showed what was

present in the substance. First, the pH test determined that the substance had a very high pH

of around 10. Furthermore, the addition of HCl resulted in a fizzy chemical reaction that

ultimately led to the realization that the substance contained Carbonate. Once the list of

possible substances was narrowed down, that left the group with four potential substances.

After testing each of those substances in HCl, it was determined that Sodium Carbonate had

the most similar of a reaction (almost identical) to our unknown compound. The results of the

various tests was enough to conclude that our substance, determined to be Sodium Carbonate,

was the same as the known substance Sodium Carbonate. Through the first test, determining

solubility, both amounts of substance dissolved in water up to around 0.3 grams each and

then dissolved no further. Both of the other tests, reaction of the compounds with each of

sulfuric acid and nitric acid, produced the same reaction in both the known and unknown

compounds. Given the results of all three of these tests, the group was ultimately able to
conclude that Sodium Carbonate was the identity of our unknown compound. The group was

unable to run further tests due to lack of resources in the lab; however, the number of tests

that were run was sufficient to confirm that Sodium Carbonate was the unknown substance.

References:

[1] Singer, M.J., H.A. George, C.D. Childers, and M.L. Merrill-Davies. What Is PH and Why

Do We Care? (n.d.): n. pag. Agriculture and Natural Resources. University of

California, Oct. 2012. Web. 18 Oct. 2016.

[2] "Acids, Bases, and Metals." KS3 Bitesize Science. BBC, 2014. Web. 18 Oct. 2016.

[3] "PH of Common Acids and Bases." PH of Common Acids and Bases. Aquion, 20 Apr.

2016. Web. 18 Oct. 2016. <http://www.aqion.de/site/191>.

Ward, Dr. Joseph. "Dealing with Unknown Compounds." LabArchives MSU Edition.

Michigan State University, 29 June 2015. Web. 18 Oct. 2016.

Ward, Dr. Joseph. "Project 3: Identification and Synthesis of an Unknown Ionic

Compound." LabArchives MSU Edition. Michigan State University, n.d. Web.

18 Oct. 2016.