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Exp 05 Qualitative Analysis of Anions PDF
Exp 05 Qualitative Analysis of Anions PDF
Introduction
In qualitative analysis we determine which chemical substance is present whereas in quantitative analysis
we determine how much of a given chemical substance is present.. The qualitative analysis, or
identification, of the common anions is markedly simpler than the analysis of the cations. One reason is
that there are many fewer possibilities for the anions. Another is that analysis of anions usually relies on
spot tests of the anions rather than separations followed by Confirmatory tests. For these reasons, the study
of qualitative analysis often begins with the anions. The common anions you will test for are carbonate,
phosphate, sulfate, bromide, chloride, iodide, acetate, thiocyanate, and nitrate. Before beginning this
experiment, you should review the formulas and structures of these ions from your textbook.
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III. The Silver Precipitate Group.
This group includes the halides: iodide, bromide, and chloride, and also the thiocyanate ion, which is often
called a pseudohalide. All of these form light-colored precipitates with excess Ag+ ion. The precipitates
vary slightly in appearance, which helps to distinguish them.
Ag+(aq) + X-(aq) AgX(s) (X- = Br-, Cl-, l-, SCN-)
The thiocyanate ion is readily confirmed by the blood-red complex it forms with Fe+3.
Fe+3(aq) + SCN−(aq) → [Fe(SCN)]2+ (aq)
The halides can be oxidized to the halogens, then extracted into an organic layer and identified by color.
For example, when reacting with “chlorine water (Cl2 dissolved in water), the Cl2 oxidizes (takes away an
electron) the Br− to Br2 which can be extracted into hexane layer.
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Safety Precautions
Handle all the chemicals in this experiment with care. Avoid getting AgNO3 on skin or clothing; it will
stain dark-brown or black. Be especially careful when handling concentrated sulfuric acid, H2SO4. It is one
of the strongest and most corrosive concentrated acids. If any skin contact occurs, wash with large amounts
of water. If instructed to sample odors, do not inhale deeply, gently waft the fumes toward your nose. Wear
your safety glasses at all times which is required for all experiments in which you use chemicals.
Experimental Procedure
Tests on Known Anions
Carefully follow the procedures given below that follow to identify each of the known anions provided.
Confirmatory test: Add 6 drops 6 M HCl to the above precipitate and stir. Does the precipitate dissolve?
Record your observation in the laboratory data sheet.
3. Test for PO43−
Place 10 drops of 1 M Na3PO4 solution in a small test tube and dilute slightly. Add 6 drops of 1 M BaCl 2
and mix well. Allow the precipitate to settle and decant the supernatant.
Confirmatory test: Add 7 drops of 6 M HCl to the above precipitate and stir. Is the solid soluble in HCl?
Record all observations.
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In a small test tube mix 5 drops of 1 M KSCN (or NaSCN) with 2 drops AgNO 3. Record the results. Save
the precipitate for later comparison to your unknown.
Confirmatory test: Place 5 drops of 1 M KSCN (or NaSCN) in a test tube and slightly dilute it. Add 2
drops of 0.1 M Fe(NO3)3 and record the results. Dilute the complex with water until the test tube is nearly
full. Notice that the color is still detectable, even at very dilute concentrations.
5. Test for Cl−
Place 12 drops of 1 M NaCl in a test tube and add 8 drops of 0.2 M AgNO 3. Note the appearance of the
precipitate and set it aside.
Confirmatory test for Cl−. In another test tube add 12 drops of 1 M NaCl and acidify with 8 drops of 6 M
HCl. Dilute with 6 drops of distilled water. Add 2 mL hexanes gently over the aqueous solution. Dropwise
add chlorine water (provided). After adding about 2 mL of chlorine water, shake vigorously and observe
any colour change. The color will be extremely pale, if it is visible at all. You are not actually producing
chlorine here, only trapping the free Cl2 present in the chlorine water. Stopper the test tube and set it aside
for later comparison.
6. Test for I−
Place 10 drops of 1 M NaI solution in a test tube and add 8 drops of 0.2 M AgNO3. Note the appearance
(colour) of the precipitate and set it aside.
Confirmatory test for I−: In another test tube place 10 drops of 1 M NaI, add 10 drops of 6 M acetic acid,
CH3COOH. Dilute the solution with 5 drops of distilled water. Add 2 mL of hexanes gently down the side
of the test tube. Add 4 drops of chlorine water. The Cl2 reacts with the I– to form free iodine, I2. The
nonpolar I2 will dissolve readily in the upper organic layer. Shake or agitate briefly. Record the color of
two layers.
7. Test for Br–
Place 12 drops of 1 M NaBr solution in a test tube and add 8 drops of 0.2 M AgNO 3. Note the appearance
(colour) of the precipitate, and set it aside for later comparison.
Confirmatory test for Br–: Place 12 drops of 1 M NaBr in a small test tube and acidify with 8 drops of 6 M
HCl. Dilute slightly by adding 5 drops of distilled water. Add 2 mL of hexanes gently down the side of the
test tube. Add 4 drops of chlorine water to the test tube with NaBr and hexanes and note the yellow
appearance as Br2 is absorbed into the upper, organic hexane layer. Shake the test tube gently. Continue
adding the chlorine water dropwise and stir vigorously or agitate. A darker color will develop in the hexane
layer as the reaction continues. Record the color of the two layers and set aside the test tube.
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Experimental General Chemistry 1 Experiment 5: Qualitative Analysis of Anions
SCN– + Ag+
SCN-
SCN– + Fe3+
I– + Ag+
I-
I– + Cl2
NO3-
Soluble
Group
CH3COO-
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