Вы находитесь на странице: 1из 10

QUALITATIVE ANALYSIS

The medical field uses a variety of rapid diagnostic tests, including tests for urine, premature
rupturing of membranes, and occult blood in stools. These test all rely on simply chemical
reactions that produce a visible change in color. Many of these tests can be purchased by anyone
without a prescription, such as pregnancy urine tests.
This type of rapid testing is generally qualitative, which give a visible positive or negative result,
but without a specific quantity. For example, a pregnancy urine test can be positive due to the
presence of the hCG hormone, but it does not indicate anything about how much hormone is
present. A blood hCG test can give a specific concentration of hCG, or a quantitative result, but it
requires more time, and often more sophisticated instrumentation.
In some cases, qualitative tests are looking for a positive or negative result. For example, an occult
blood test will be positive if there is blood in the stool, but negative in any other case. How much
blood is not important at that point. The same argument can be made for a pregnancy test.
However, in many cases, qualitative tests require a standard to compare to. One form of a standard
is a standard curve, which was used during the CAD experiment. Another can be a pre-printed
standard, such as those used for urine tests. This standard can provide an approximate
concentration of a substrate to provide additional diagnostic information.
No matter which qualitative test is performed, it is essential to know what a positive and negative
result looks like. Imagine giving a pregnancy test and not knowing what a positive result looked
like—the data is useless! In this experiment you will be identifying an unknown salt solution. As
a comparison, you will first need to test known compounds to recognize a positive test when you
see it. Since salts are a mix of a cation and an anion, it will be essential to identify both parts
independently, looking for both positive and negative results.
Positive results can be in the form of gas evolution (bubbles), precipitates, color changes, or
temperature changes. Negative results are the lack of a visual change (which does not mean nothing
is happening, just nothing is happening visually). It is also important to pay close attention to the
speed of a reaction—some happen very quickly, and some will take a few minutes. Negative results
are just as important as positive results, as false positives happen, and additional data helps support
the correct answer.
To further avoid false positives (or false negatives), it is important to understand the predictive
nature of chemistry. When reactivity rules or trends are understood, the observations (and,
subsequently, the chemistry) makes sense. In that vein, this experiment also requires an
understanding of what is going on. Why does a solid form? Because the product is insoluble. Why
do bubbles appear? Because there is a reaction that forms a gas. Understanding the chemistry
greatly reduces false positives or false negatives, because understanding eliminates guess-work.
These patterns can be found in solubility tables, reactivity tables, and other tables that have been
printed in textbooks for generations.
For this lab, you will be given one of the following unknowns. By identifying both the cation and
anion portion (by comparison to known compounds), it is possible to identify the unknown. The
potential cations are aluminum, ammonium, barium, calcium, iron, magnesium, potassium,
sodium, or zinc, and the potential anions are bromide, carbonate, chloride, hydroxide, iodide,
oxide, phosphate, or sulfate.

|1
2 | Qualitative Analysis

Name Formula Source/Description


Aluminum hydroxide Al(OH)3 Active ingredient in antacid tablets
Aluminum oxide Al2O3 Metal and rock polishing compound
Aluminum sulfate Al2(SO4)3 Antiperspirant
Ammonium hydroxide NH4OH Household cleaner
Ammonium bromide NH4Br Used in fireproofing of wood and corrosion inhibitors
Ammonium carbonate (NH4)2CO3 Active ingredient in "smelling salts"
Ammonium chloride NH4Cl Fertilizer, expectorant (cough syrup)
Ammonium phosphate (NH4)3PO4 Fertilizer
Ammonium sulfate (NH4)2SO4 Fertilizer, pH adjuster for soil
Barium carbonate BaCO3 Used in glazes for pottery and ceramics
Barium sulfate BaSO4 Radio contrast agent for x-rays and CAT scans
Calcium carbonate CaCO3 Marble and limestone
Calcium chloride CaCl2 Desiccant (removes moisture from a room)
Calcium hydroxide Ca(OH)2 Used to reduce acidity in soil
Calcium oxide CaO Used by builders to make plaster
Calcium phosphate Ca3(PO4)2 Naturally occurring source of calcium in cow's milk
Calcium sulfate CaSO4 Blackboard chalk, plaster of Paris
Ferric chloride FeCl3 Wastewater treatment
Iron(III) oxide Fe2O3 Common rust
Iron(II) sulfate FeSO4 Used in wool dyeing
Magnesium carbonate MgCO3 Antacid, athlete's chalk
Magnesium hydroxide Mg(OH)2 Antacid (Milk of Magnesia)
Magnesium sulfate MgSO4•7H2O Epsom Salt
Magnesium chloride MgCl2 Deicer, used in the preparation of tofu from soy milk
Potassium carbonate K2CO3 Water softener
Potassium bromide KBr Used for black-and-white photo development
Potassium chloride KCl Road deicer, salt substitute
Potassium hydroxide KOH Drain cleaner
Potassium iodide KI Radiation pills, film development
Sodium bromide NaBr Disinfectant in swimming pools
Sodium carbonate Na2CO3 Washing soda (water softener for laundering)
Sodium chloride NaCl Table salt
Sodium hydroxide NaOH Lye, drain cleaner
Sodium phosphate Na3PO4 Used to clean walls prior to painting
Sodium sulfate Na2SO4 Filler in powdered laundry detergent, drying agent
Zinc oxide ZnO Component of calamine lotion (not active ingredient)
Zinc sulfate ZnSO4 Used in the production of rayon
Qualitative Analysis | 3

PURPOSE AND ILLUSTRATED PROCEDURE


In your own words, write the purpose and goal of this experiment in the space below.

Use pictures to illustrate the procedure required for this experiment in the space below.
4 | Qualitative Analysis

MATERIALS AND EQUIPMENT


• 13 – small test tube • 1 – watch glass
• 1 – test tube holder • plastic pipet
• 1 – test tube rack • litmus paper
• 1 – 24-well plate • Bunsen burner
• 2 – beaker • coding dots or labeling tape
• 1 – glass stir rod • hot plate (2 per section)
• 1 – nichrome wire

CHEMICALS
• 0.1 M aluminum nitrate, Al(NO3)3 • 0.1 M sodium phosphate, Na3PO4
• 0.1 M barium nitrate, Ba(NO3)2 • 6 M nitric acid, HNO3
• 0.1 M calcium nitrate, Ca(NO3)2 • 0.5 M ammonium molybdate,
• 0.1 M ferric nitrate, Fe(NO3)3 (NH4)2MoO4
• 0.3 M potassium nitrate, KNO3 • 0.5 M sodium sulfate, Na2SO4
• 0.1 M magnesium nitrate, Mg(NO3)2 • 0.1 M sodium iodide, NaI
• 0.1 M sodium nitrate, NaNO3 • 0.1 M sodium bromide, NaBr
• 0.1 M ammonium nitrate, NH4NO3 • 6 M acetic acid, CH3COOH
• 0.1 M zinc nitrate, Zn(NO3)2 • cyclohexane
• 6 M sodium hydroxide, NaOH • 0.5 M sodium hypochlorite, NaOCl
• 1 M sodium carbonate, Na2CO3 • 0.1 M sodium chloride, NaCl
• 6 M hydrochloric acid, HCl • 0.1 M silver nitrate, AgNO3

HAZARDS
Acids and bases can be corrosive and cause severe burns. Gloves, goggles, and proper clothing
are required. In case of contact, affected clothing should be removed immediately and skin rinsed
with abundant amounts of water until medical help arrives. Use the safety shower if necessary.
Other solutions may be toxic or corrosive. Silver nitrate will stain skin and clothes. Refer to the
applicable SDS for additional information regarding the chemicals used in this experiment.

PROCEDURE & DATA


Perform each test in a well plate or small test tube, as directed. Quantities do not have to be exact
(20 drops ~1 mL).
To manage possible interfering species, it is important to follow directions carefully. Reagents for
the tests are located in dropper bottles at several stations in the lab. Take only the reagent dropper
bottles needed for one test at a time to your station. When finished with a test, return dropper
bottles to the same station and get the next bottles you will need (be courteous!). Before handling
bottles, make sure they are clean, the tops are on securely, and that you have read and re-read the
labels. Negative tests are just as important as positive tests.
When testing knowns, you do not need to go in order—use the chemicals no one else is using!
Qualitative Analysis | 5

TECHNIQUES
This experiment requires the use of a variety of techniques, which are explained below. Please
refer to these instructions before attempting this experiment.
Heating
Your TA will set up a hot water bath with a large beaker at the end of the bench near the windows
or in a fume hood. Make sure the beaker does not boil to dryness—alert your TA if the water gets
low. Use the bath carefully as needed.
Mixing
Small amounts in a test tube may be mixed by carefully tapping a finger against the side of the
tube near the bottom. Never point the open mouth of a test tube toward yourself or others.
Indicator/Litmus Paper
Use a small amount of solution on the end of a glass stirring rod and touch it to the paper. Do not
dip the paper into your test tube.

PART A: IDENTIFYING CATIONS


Solution Color
Observe and record the color of each solution. Colors are often associated with atoms where the
electrons can easily change energy levels, such as many transition metals.
Flame tests
Use the following salt solutions: Al(NO3)3, Ba(NO3)2, Ca(NO3)2, Fe(NO3)3, KNO3, Mg(NO3)2,
NaNO3, NH4NO3, and Zn(NO3)2 (or unknown).
Place a small drop of salt solution (or unknown) on the edge of the watch glass. Light a burner,
and heat a nichrome wire in the flame until it is red. Bring the watch glass to the burner, putting
the drop of solution right next to the air inlet. Place the hot nichrome wire in the solution and
observe the flame color. Record the color and duration.
Cation Precipitation with NaOH
To a small test tube containing 1 mL 0.1 M Zn(NO3)2, add 6 M NaOH dropwise. Note if a
precipitate forms. Continue adding 6 M NaOH dropwise and note if the solid begins to dissolve.
Repeat procedure using Al(NO3)3, Ba(NO3)2, Ca(NO3)2, Fe(NO3)3, KNO3, Mg(NO3)2, NaNO3,
NH4NO3 (or unknown).
Ammonium Test
To a small test tube containing 1 mL 0.1 M NH4NO3 (or unknown) add 3–5 drops 6 M NaOH.
Heat the test tube gently in a water bath in a fume hood. The evolution of NH3 gas can be detected
using a moist piece of litmus paper held near the mouth of the test tube. Note: If you touch the
litmus paper to the edge of the tube you may get a false positive.
6 | Qualitative Analysis

Solutions Color Test Flame Test NaOH Test Ammonium Test

Al(NO3)3 –

Ba(NO3)2 –

Ca(NO3)2 –

Fe(NO3)3 –

KNO3 –

Mg(NO3)2 –

NaNO3 –

NH4NO3

Zn(NO3)2 –

Unknown
Qualitative Analysis | 7

PART B: IDENTIFYING ANIONS


Carbonate
To a 24-well plate, add 2 drops 1 M Na2CO3 (or unknown). The add 6 M HCl dropwise until you
see a reaction. Record your observations.
Phosphate
To a 24-well plate, add 2 drops 6 M HNO3, 2 drops 0.5 M (NH4)2MoO4, and 2 drops 0.1 M Na3PO4
(or unknown). The precipitate, (NH4)3PO4•12MoO3, may form slowly.
Sulfate
To a 24-well plate, add 2 drops 0.5 M Na2SO4 (or unknown), 2 drops 6 M HCl and 2 drops 0.1 M
Ba(NO3)2. You may need a different color background to see the precipitate.
Hydroxide
Place 1 drop of 6 M NaOH (or unknown) on a piece of red litmus paper. Phosphate and carbonate
may also show a positive result.
Iodide or Bromide
To a small test tube containing 1 mL 0.1 M NaI add 5 drops 6 M acetic acid and 1 mL cyclohexane.
After mixing well, add 2 drops 0.5 M NaOCl and mix. The NaOCl oxidizes the iodide into iodine,
which causes a lavender color in the cyclohexane layer. The lavender color may be difficult to
detect, and holding the test tube in front of a sheet of white paper may help.
Repeat using 1 mL NaBr (or unknown). The NaOCl oxidizes the bromide into bromine, which
causes an orange color in the cyclohexane layer.
Chloride
To a 24-well plate, add 2 drops 0.1 M NaCl (or unknown) and 2 drops 0.1 M AgNO3.
Perform the iodide or bromide test on your unknown first, because the presence of iodide or
bromide will result in a false positive for this test.
Oxide
If all of the anion tests are negative, the anion is oxide.

Question 1. Why might phosphate or carbonate show a positive result in the hydroxide
test? Include appropriate chemical reactions in your explanation.
8 | Qualitative Analysis

Test Known Unknown

Carbonate

Phosphate

Sulfate

Hydroxide

Iodide

Bromide

Chloride

Oxide

PART C: IDENTIFYING AN UNKNOWN


You will be given 6 mL of an unknown salt solution. You will repeat the methods described in
above to identify the cation and anion of your assigned salt. Make sure that your procedure is clear
and detailed and that your logic and conclusions are sound. If you need more unknown, you may
lose points. Fill in the unknown data in the appropriate tables.

Question 2. Why would the presence of bromide or iodide show up as a false positive
in the test for chloride? Include appropriate chemical reactions in your explanation.
QUALITATIVE ANALYSIS
Name:________________________________
Section:_______________________________
Date:_________________________________

POST LABORATORY QUESTIONS


1. Your unknown was found on a patient that was just brought into the ER. Come up with a short
story describing how they ended up in the ER with that chemical on them. Creativity is
encouraged, and identical answers will not receive credit. Note: You may look up more uses of
the chemical than just the ones listed herein.

2. Using your data, solubility tables, and your understanding of chemical reactivity, write the
products and the state of matter for the products (solid, aqueous, or gas) that form when the
following compounds are mixed with aqueous NaOH.

Al(NO3)3 BaCl2 CaCl2

Fe(NO3)3 KCl Mg(NO3)2

NaCl NH4NO3 Zn(NO3)2

|9
10 | Qualitative Analysis

3. Write balanced net ionic equations (remember states) for the each of the reactions below.

Reaction Net Ionic Equation


NH4NO3 + NaOH
with heat

Na2CO3 + HCl

Na2SO4 + BaCl2

NaCl + AgNO3

4. Based on your experimental results, write a conclusion for this experiment. This should be in
paragraph format and include the purpose, your results, and the identification of your unknown.
Support your claims with experimental evidence (but do not restate the procedure). Be sure to
include an any errors that may have affected your experimentation.

Upload all procedure and data pages (pages 3, 6–10) as a single PDF document to Canvas within 24 hours from
the end of lab. A PDF image of each page can be obtained using an app on your phone, a scanner at the library,
or another method of your choice.