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Formal Lab Report

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Submitted By zeynoire
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Identification and Synthesis of an Unknown
Ionic Compound
3/24/16

Department of College of Natural Science, Michigan
State University, Farm Lane, East Lansing, MI 48825
Chemistry 161, Section 10
Dr. Joseph Ward

Abstract
The goal of this experiment is to identify an unknown compound. To identify this compound a series of test were performed to find the chemical and physical properties of the unknown compound. The test performed; flame test, solubility test, halide test, acetate test, ammonium test, nitrate test, sulfur test, carbonate test, calcium test and pH test.
When the flame test of the unknown resulted in a brick red color, it was determined that the unknown contained calcium. Another calcium test was tested and proved that the unknown was calcium. Since the unknown is dissolvable in water, CaCO3 was no longer a possible candidate because it is insoluble. The pH test for the unknown was 5 whereas the pH for calcium chloride is 8 and the unknown tested negative for halide, therefor calcium chloride was not an option for the unknown as well. The last calcium compound left was calcium nitrate which also had a pH of 5 and a brick red flame test color.

Introduction
There was an unidentified white compound found in the lab. The goal of the experiment was to identify what the unknown compound is and how to dispose of it safely. In order to find this information, the compounds chemical and physical properties needed to be determined. This was a given table of possible compounds the unknown might be:
NaCl
KCl
Na2SO4
CaCl2
MgSO4
Na2CO3
K2SO4
KNO3
Ca(NO3)2
NH4CO3
NH4Cl
(NH4)2SO4
CaCO3
MgCO3
CH3CO2Na
To narrow the possibilities down there were a list of test to run. The first test ran was the solubility test on unknown compound, to see if it dissolved in water. This determined a physical property that is easy to compare to the possible known compound. After that there were multiple test ran, searching for cations and anions. The flame test, determined a chemical property, the color the unknown burned, which shortens the possible compounds significantly. To test for carbonate, a carbonate test was ran on the unknown.
A halide test was also completed to detect the presence of chloride, bromide or iodide.
The remainder of test were a sulfate test, nitrate test, ammonium test, and a pH test. All of these test helped detect what the chemical and physical properties of the unknown.

Experimental Details
Week 1: To constrict the list of potential compounds a soluble test was ran (2). The materials used during this test were; 30mL beaker, 100mL graduated cylinder, scale. To conduct this experiment there was 15mL of distill water mixed with 50mg of the unknown compound and stirred. Then the carbonate test was performed (1). The materials needed for this experiment included; 2 test tubes, 10mL graduated cylinder, distilled water. To pursue this test 5mL of HCl was poured into a test tube and mixed with 2mL of the unknown. After, the flame test was ran(3). The materials required for this experiment were; spatula, wet wood splint, Bunsen burner. A wet wood splint got two particles of the unknown sprinkled on the end of it and then held over the Bunsen burner until the unknown burned its color. Next, a series of ion test were performed (4).
The ammonium test consists of measuring 1mL of the unknown assorted with 1mL of 6M

NAOH (4). The halides assessment mixed 1mL of the unknown with 1mL of 6M HNO3 and 1mL of .1M AgNO3 (4). The sulfate test combined 1mL of the unknown with 1mL of 6M HCL and 1mL of .1BaC12 (4). The nitrate test tested a solution of 3mL of the unknown with 3mL of H2SO4, cooled. After cooling, 2mL of FeSO4 was poured into the solution with the solution tilted at a 45-degree angle (4). Lastly, the acetate. To test acetate, take 2mL of the unknown and add one drop of sulfuric acid and 1mL of ethanol, then heat the mixture (4).
Week 2: All the experiments from week 1 were repeated but in comparison with Calcium
Chloride and Calcium Nitrate, each test and the comparisons were ran by the same person it was ran by in week 1. A new experiment testing for calcium was performed during week 2 (1). To complete this test, 4 drops of sodium hydroxide was mixed with 3 mL of the unknown. This test was repeated but with Calcium nitrate and a separate one with
Calcium Chloride (1). A pH test was also completed during week 2 (2). The pH was performed by mixing 100mg of the unknown with 15mL of distilled and dipping a pH stick in it. The same experiment was performed with Calcium Nitrate and Calcium
Chloride (2).

Results
Week 1: The solubility test came back positive; the unknown compound dissolved in water. The carbonate test was negative because it formed no precipitate. Similarly, when testing for the ions such as Ammonium, Halides, Sulfate, no precipitate was formed. No brown ring was formed around the top of the Nitrite test indicating no presence of Nitrite.
The Acetate test came back positive with a fruity smell. The unknown compound burned brick red during the flame test.
Table 1:
Test
Result
Solubility
Soluble
Flame Test
Brick Red
Ammonium Test
Negative
Carbonate Test
Negative
Nitrate Test
Negative
Sulfate Test
Negative
Halide Test
Negative
Acetate Test
Positive
Week 2: All the results for the unknown came back the same as the previous week. The additional calcium test on the unknown came back positive, with a precipitate. The flame test for CaCl was a orange-red and the flame test for (Ca(NO3)2) burned brick red.
(Ca(NO3)2) was positive for Nitrate and CaCl had a positive Halide test. The pH for the unknown was 5. The pH of (Ca(NO3)2) was 5 and the pH for CaCl was 8.
Table 2:
Test
Results

pH (unknown) pH (CaCl) pH (Ca(NO3)2)
Flame Test (unknown)
Flame Test (CaCl)
Flame Test (Ca(NO3)2)
Calcium Test (unknown)
Calcium Test (CaCl)/ (Ca(NO3)2)
Halide Test (unknown)
Halide Test (CaCl)
Nitrate Test (Unknown)
Nitrate Test (Ca(NO3)2)
Solubility (unknown)
Solubility (Ca(NO3)2)
Solubility (CaCl)

5
8
5
Brick Red
Red/orange
Brick Red
Positive
Positive
Negative (no precipitate)
Positive (precipitate)
Negative
Positive
Soluble
Soluble
Soluble

Discussion
Week 1: The results from the flame test indicated that the unknown contained calcium.
Calcium burns brick red such as our unknown. The reference page “dealing with an
Unknown” in LabArchives (5) help to determine what compound the flame color indicated. There were only three compounds that contained Calcium; CaCO3, (Ca(NO3)2), and CaCl. Since the unknown was soluble in water and the carbonate test came back negative, it could easily be determined that the unknown was not CaCO3. Both the Halide test and the Nitrate test also came back negative, so both were still strong candidates to possibly be the unknown. The negative test results may have been due to contamination.
Week 2: The positive result of the additional Calcium test added to week 2 proved that the unknown compound contained Calcium. The Halide test came back negative for the unknown compound and (Ca(NO3)2) whereas it came back positive in CaCl. The Nitrate test also came back negative for the unknown compound and CaCl but positive for
(Ca(NO3)2). The pH of the unknown compound concluded to be 5 as well as in
(Ca(NO3)2). The pH for CaCl was 8. The difference in pH, the color of the flame test and the negative for Halide, made it clear that the unknown compound was not CaCl. Though the Nitrate test for the unknown compound was negative, a nitrate test is very complicated test to run and is often not ran correctly or contaminated, indication the unknown could still be (Ca(NO3)2).

Conclusion
In closure, the unknown compound was concluded to be Calcium Nitrate. The flame test of the unknown burned brick red as well as Calcium Nitrate (3). The Unknown compound and Calcium Nitrate were soluble in water (2). The pH of the unknown and
Calcium Nitrate were 5 (2). The Nitrate came back negative for the unknown compound

and positive for Calcium Nitrate, which is believed to be due to contamination and error.
The unknown compound could not be CaCl because they burned different shades of red
(3) and the halide test came back negative for the unknown compound (4). The pH levels were very different as well (2). The unknown compound could not be CaCO3 either because the unknown dissolved in water completely and the carbonate test results were negative for the unknown compound. After group collaboration, the unknown compound was determined to be Calcium Nitrate.

References:
1. Anderson, Z. Michigan State University, East Lansing. Personal Communication
2016.
2. Croteau, K. Michigan State University, East Lansing Personal Communication.
2016
3. Bender, V. Michigan State University, East Lansing.. Personal Communication
2016.
4. Burns, M. Michigan State University, East Lansing. Personal Communication
2016.
5. Ward, J. Michigan State University. Lab Archives: Dealing With Unknown
Compounds. 2016

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