Chem2 Laboratory Manual MLS - LA1 7 - Prelim

Qualitative-Quantitative Chemistry
Laboratory Manual
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Chemistry Department
Revised 2019
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UNIVERSITY OF THE IMMACULATE CONCEPTION
MEDICAL TECHNOLOGY/MEDICAL LABORATORY SCIENCE
Fr. Selga St. Bankerohan, Davao City
Tel. No: (082)-2218181 loc 188
INTRODUCTION TO THE LABORATORY
TERMINOLOGY
REACTION – Any process in which a new chemical substance is formed.
REAGENT – The substance used to bring about a reaction.
PRECIPITATE – Any insoluble substance produced in the reaction.
RESIDUE – The solid remaining after evaporating a mixture or solution to dryness.
CLEAR SOLUTION – A solution that is not turbid or cloudy
COLORLESS SOLUTION – A solution that is not colored.
NOTE: Do not use “clear” to mean “colorless”. For example, cupric sulfate solution is a clear solution and
colored blue.
TEST – A laboratory operation to show the presence or absence of some substances, usually some ionic
species.
NOTE: A test is said to be positive or negative, depending on whether it indicates that the substance is
present or absent.
A positive test maybe indicated by the:
1. Formation of a precipitate.
2. Dissolution of a precipitate.
3. Appearance or disappearance of a color in a solution or in a flame.
4. Evolution of a gas.
5. Development of a characteristic odor.
CONFIRMATORY TEST – A test used to identify the ion since the ion is the only one that would give a
characteristic result.
TEST SOLUTION – A solution that contains the ion or substance for which test are made.
NOTE: Test solution of cations (positive ions) are prepared from their nitrates. When the metal nitrates
are unavailable, the chloride are used. Test solutions of anions (negative ions) are prepared from the
corresponding sodium or potassium salts.
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Basic Rules and Regulations in the Laboratory
1. Be sure the science teacher is present in the laboratory when you work.
2. Know the location of all emergency equipment (e.g. fire extinguishers, eye washes, and fire blankets)
in the laboratory and be sure that you know how to use it.
3. Wear goggles and other safety garment at all time when you are in the laboratory. Do not wear
contact lenses because there is always danger of volatile or corrosive material dissolving in the
lenses or getting beneath them.
4. Tie back long hair and remove coats. Do not wear open-toed shoes or sandals in the laboratory.
5. Read each activity carefully before starting work to become familiar with the experimental procedure
and safety precautions.
6. Perform only those procedures directed by your teacher. Use only the recommended amounts of
chemicals and no more.
7. Always keep your working area clean and orderly. Keep materials away from the edge of the
laboratory bench or worktable.
8. When instructed to test for the odor of a substance, follow the instructions in the procedure. Hold
the container away from you and fan a small amount of the vapor toward you with your hand.
9. When heating in a test tube, hold it at an angle and move it through the flame: point the mouth of
the test tube away from others and from yourself.
10. Handle hot glassware with tongs, test tube holders, or potholders as directed in the procedure.
Remember that hot glass looks like cold glass.
11. Extinguish all burner flames before using flammable materials, such as alcohol and ether.
12. Turn off burners that are not in use.
13. Note carefully the method of disposal of chemical in each activity and follow directions given by your
teacher. Never put solid chemicals, solutions, or liquids in the sink unless directed to do so.
14. Corrosive substances spilled on skin must be washed off promptly with plenty of water. Clothes
spilled with chemicals must be removed immediately.
15. Eating, drinking, and smoking are strictly prohibited inside the laboratory.
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Tel. No: (082)-2218181 loc 188
GENERAL LABORATORY TECHNIQUES
FILTRATION. In semi-micro work, filter paper- funnel method of filtration in seldom used.
The use of centrifuge makes filtration more rapid and more convenient with the volume of the reagent.
The centrifuge is a device which makes use of centrifugal force for speeding up the rate of
settling of solids. The steps are:
1. The mixture is placed in a small test tube or centrifuge tube and placed in one of the cups inside
the centrifuge.
2. The centrifuge should be balanced symmetrically to avoid vibration. This is done by placing
another test tube containing water opposite the test tube containing the mixture of liquids. Two
test tubes should have approximately the same amounts of liquid and should not be more than
three-fourths full.
3. Turn on the switch for 20-30 seconds, then turn it off and allow the machine to stop by itself.
PRECIPITATION. This may be accomplished by using either a centrifuge or a round bottomed test tube.
The precipitating reagent is added dropwise to treat solution with constant stirring until precipitate
seems to be complete.
TEST FOR COMPLETENESS OF PRECIPITATION. After centrifugation, add to the clear supernatant liquid 1-
2 drops of the precipitating reagent. If no more precipitate is formed, precipitate is complete. If more
precipitate are formed, add a few drops more, stir and centrifuge again. The procedure is repeated until
the solution fails to give a precipitate.
DECANTATION. After centrifugation, the supernatant liquid ( or the centrifuge 0 is separated from the
precipitate using a pipette. First compress the bulb and insert the tip of the pipette slightly below the
level of the liquid and slowly release the bulb. Lower the tip level as the level of the solution drops and
when the solution level is near the precipitate, slowly tilt the test tube so as to express the additional
solution to the surface.
WASHING OF THE PRECIPITATE. After decantation, the precipitate retains some of the centrifugate which
contains some ions that may interfere in the analysis of the precipitate. To remove these impurities, the
precipitate is washed. The washed liquid is distilled water unless other liquid is specified. Washing is
accomplished by adding the required amount of distilled water or washed solution to the solid. Bring the
solid into suspension by agitating it with a stirring ro. Then centrifuge and decant the washed liquid. The
first portion if the washed liquid is often combined with the supernatant liquid. The second portion is
usually discarded.
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TEST FOR SOLUBILITY OF THE PRECIPITATE. Remove the centrifugate by decantation after centrifugation,
add 1-2 drops of specified reagent at a time, stirring the
USE OF THE WATER BATH: A solution contained in a small test tube should never be heated over a direct
flame since bumping causes the loss of part or all of the solution. A more appropriate way is to use a
water bath. A 100 mL beaker about 2/3 full of water is suitable for the purpose.
EVAPORATION: This should be carried out in an evaporating dish and heating over wire gauze using a
small flame. It should be rotated slowly with a motion that allows the liquid to come in contact with the
hot walls of the evaporating dish, thereby facilitating evaporation. Evaporation should be conducted
without boiling since boiling is always accompanied by spattering. In evaporating to dryness, remove the
evaporating dish from the flame while there is still a drop or two of the liquid left. The heat in the vessel
is usually sufficient to complete the evaporation.
PRECIPITATION OF THE HYDROGEN SULFIDE GAS (H2S). The sources of the hydrogen sulphide gas are:
1. Reaction of HCl with ferrous sulfide (pyrite) in the Kipps-type generator. The equation involved
is: FeS + 2HCl = FeCl2 + H2S
A pipette is connected to the generator by means of rubber tubing. The tip of the pipette is
immersed below the surface of the solution to be saturated and lowered gradually to the bottom
of the tube. It takes 20-30 seconds for the solution to be saturated.
2. Hydrolysis of thioacetamide in a slightly acidic or basic media at elevated temperature. The

equation is: CH3CSNH2 + H2O = CH3CONH2 + H2S ↑
About 10 drops of a 10% thioacetamide solution is added to the solution to be saturated with
hydrogen sulphide. The mixture is stirred thoroughly then it is placed in a boiling water bath for
about 10 minutes.
FLAME TEST: Treat the solution with a few drops of 6M HCl. This converts the ion to its chloride which is
more volatile in the flame. Make a small loop at the end of the platinum wire or nichrome wire. Clean
the loop by alternately dipping it into a small amount of 12M HCl and holding it in the oxidizing zone of
the non-luminous flame. The loop is then immersed into the solution to be tested and placed in the
hottest portion of the oxidizing zone of the non-luminous flame moving towards the edge of the flame.
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A Guide to Proper Pipetting
Following these guidelines can improve the accuracy of manual liquid
17 Ways to Stop Pipetting Errors From Ruining Your Experiments

If you work at the bench, accurate pipetting is crucial. Without accurate pipetting, your experiments
would not be reproducible, your stock solutions would be inaccurate, and your assays would have such
large errors that comparing them would be meaningless. But luckily, there’s no need to worry—your
trusty, precision micropipettes take care of that for you.
Precision instruments they may be, but the accuracy of your micropipettes depends on you. You need to
maintain your pipettes, practice good technique, and have an understanding of how they work. Only
once you have mastered those aspects can you claim to have anything like precision instruments at your
disposal.
Know How Your Pipette Works
1. You Use an Air Displacement Pipette, Most Likely

An air displacement pipette works a bit like a syringe, except that there is an air-filled cushion between
the piston and the sample. The air cushion prevents the piston from coming into contact with the
solutions. Keeping the solution and the pipette barrel apart is good, but it also puts some limitations on
the pipette.
Temperature and pressure affects the volume of the air cushion, which affects pipetting accuracy. Also,
volatile solvents can evaporate into the air cushion, which leads to an inaccurate and lower dispensed
volume than what is displayed on the pipette. The barrel of air displacement pipettes is also vulnerable
to contamination by the pipetted solution. If you are working with corrosives or bio-hazardous material,
this can be a problem.
2. Don’t Use an Air Displacement Pipette (depending on your application)

Most of the information in this article relates to air displacement pipettes, but in certain situations a
positive displacement pipette may be a better option. Positive displacement pipettes also work like a
syringe, but they don’t have an air cushion—unlike air displacement pipettes. This makes them more
accurate for pipetting volatile solvents because there is no place (air cushion) for the solvent to
evaporate. The lack of air cushion also decreases the chance of contamination when pipetting corrosives
and bio-hazardous material, which makes positive displacement pipettes more suitable to working with
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those reagents. These pipettes are expensive because the barrel and the tip are a unit and both are
replaced when pipetting. A cheaper alternative is to use an air displacement pipette with barrier tips, but
these only address some of the problems.
This Gilson information guide provides further on how air displacement and positive displacement
pipettes work.
Take Care of Your Pipette
3. Have Your Pipette Serviced Every 6-12 Months…

However, you made need to have it serviced more often depending on your requirements for
accuracy. The service should include re-calibration, greasing of the moving parts, and replacement of any
worn out seals or other parts. It’s best to have this done by an experienced pipette doctor. If you work in
university or large company, there may be pipette clinics you can use. In other cases, you can send your
pipettes off to companies who will do it for you.
4. Check Your Pipettes Daily for Damage

Examine the nose of the barrel (where the tip is fitted) for any obvious damage. If there is a problem,
have it serviced—because it is unlikely to be fit for the job.
5. Clean Your Pipettes Each Day Before Use

Wiping your pipette with some 70% ethanol should do it.
6. Store Your Pipette Vertically, Using a Pipette Holder

Storing your pipette this way prevents any liquids that are in the pipette barrel from getting any further
inside and causing corrosion.
7. Never Put Your Pipette on Its Side With Liquid in the Tip
There’s nothing preventing the liquid from rolling down and into the pipette barrel (remember only air
separates the liquid from the pipette barrel). Any liquid inside the pipette barrel results in contamination
at the least and can cause some serious corrosion damage.
8. Use Well-Fitting Tips

Poorly fitting tips allow air to escape when drawing up and dispensing liquid, leading to inaccurate
results. This technical note from Biohit goes into more depth on how poorly selected tips can cause
major errors in accuracy.
Practice Good Pipetting Technique
9. Make Sure You Know How to Pipette Properly

For the basics, take a look at Gilson’s pipetting technique manual. The most important rules to follow
are:
 Pipette with a slow, smooth action
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 Hold the pipette vertically when drawing liquid in
 Only immerse the tip slightly when drawing liquid in—otherwise you will coat the outside of the
tip with liquid, which will be transferred along with the volume inside the pipette
 When dispensing the liquid, hold the pipette vertically but keep the sidewall of the receiving
vessel at 45 degrees. Pipette against the sidewall or into the liquid that’s already there.
10. Test Your Accuracy

Check the accuracy of your pipetting technique by dispensing 100 µL onto a fine balance. The mass of
the droplet you make should be around 0.1 g. Now do the same thing 10 times and record the masses
you obtain. If the variation is more than +/- 0.5%, then you either need to re-evaluate your pipetting
technique or practice more!
Know the Tricks That Increase Your Accuracy
11. Pre-Wetting the Pipette Tip

When you dispense liquid from your pipette, a coating of the liquid is left on the tip and makes the
dispensed volume slightly less than what is displayed on the pipette. Pre-wetting the tip before you
pipette will help increase your accuracy. To pre-wet your tip, draw up the liquid into your pipette and
then dispense back into the original vessel. The coating is on the tip. Now, when you draw up the liquid
again and dispense it into the receiving vessel, none of it will be left on the tip and lost to wetting. This is
only recommended for volumes greater than 10 µL.
12. Reverse Pipetting

Use this technique when pipetting viscous liquids or volatile solvents. Reverse pipetting also helps when
pipetting ultra-micro samples of 0.5 µL or less. Push the piston down to the purge position (the second
stop), then draw the liquid up. There is too much liquid in the tip at this point. However, when the liquid
is dispensed by pushing the piston to the aspirate position (the first stop), the extra liquid is left inside
the tip. Using this method, the tip is “automatically” pre-wetted. The extra liquid also helps when
pipetting volatile solvents, because some of the solvent will tend to evaporate into the air cushion.
13. Take the Ambient Temperature Into Account

The person or company that calibrated your pipette likely did so at room temperature. If you are working
at a different temperature (e.g., in a cold room), then your pipette will not dispense the displayed
volumes.
14. Take the Sample Temperature Into Account

In a recent Nature Methods publication, Millet and Barthlen observed a strange phenomenon. When
repeatedly pipetting cold samples, the first dispensed volume is always larger than expected, but
subsequent pipetting with the same tip gave the correct volume. The same was true for hot samples,
except that the first dispensed volume was smaller than expected. Their solution was simple—dispense
the first volume back into the original vessel, then start pipetting.
15. Use a Sensible Pipette for the Volume You Want to Dispense
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The accuracy of your pipette decreases as the dispensed volume approaches the minimum the pipette
can handle. For example, if you are dispensing 15 µL, then a 1 mL pipette would be terrible, a 200 µL
pipette not so good, and 20 µL pipette ideal.
16. Use the Largest Volume Possible

Large volumes are easier to pipette accurately than small. Say you are performing an assay where you
have to accurately pipette 5 µL. Pipetting that small amount accurately is not easy and will likely
contribute greatly to the statistical error in your results. On the other hand, you could dilute the stock
solution 10 times and pipette 50 µL of the solution. You could easily and accurately pipette this amount,
which would yield much tighter error bars.
17. And Finally, Here’s How to Get Maximum Accuracy

An analytical balance is more accurate than any pipette. For maximum accuracy, use your pipette to
dispense the volume you need but do it into a tared container on a balance. Then, calculate the actual
pipetted volume from the mass (using the formula volume=mass/density). Of course, this only works for
solutions of known density—but for aqueous solutions that have a density of 1, this is not a problem.
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TABLE OF CONTENTS
Learning TITLE Rating
Activity
1
SEPARATION OF THE BASIC CONSTITUENTS INTO GROUPS
2
REACTIONS OF THE SILVER GROUP
3
REACTIONS OF THE HYDROGEN SULFIDE GROUP
4
REACTION OF THE AMMONIUM SULFIDE GROUP
5
REACTIONS OF THE ALKALINE EARTH GROUP
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REACTIONS OF THE ALKALI GROUP
ANALYSIS OF CATION IN A SOLUTION CONTAINING ONLY ONE INORGANIC
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COMPOUND
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THE CHEMISTRY OF THE ACIDIC CONSTITUENTS
ANALYSIS OF AN ANION IN A SOLUTION CONTAINING ONLY ONE INORGANIC
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COMPOUND
10 PREPARATION AND STANDARDIZATION OF HYDROCHLORIC ACID SOLUTION
11 PREPARATION AND STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION
STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION WITH POTASSIUM ACID

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PHTHALATE
13
DETERMINATION OF ACETIC ACID CONTENT IN VINEGAR
14
PREPARATION AND STANDARDIZATION OF EDTA
15
DETERMINATION OF THE TOTAL HARDNESS OF WATER
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PREPARATION AND STANDARDIZATION OF IODINE SOLUTION
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DETERMINATION OF VITAMIN C
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GRAVIMETRIC METHOD: DETERMINATION OF SOLUBLE CHLORIDE
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THE CHEMISTRY ANALYZER (SPECTROPHOTOMETER)
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THE CHEMISTRY ANALYZER (SPECTROPHOTOMETER)
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Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______

Year & Section: __________________ Date Performed: _________
Group No. : _____________________ Date Submitted: _________
Learning Activity No. 1

SEPARATION OF THE BASIC CONSTITUENTS INTO GROUPS
o LEARNING OBJECTIVES: At the end of the experiment, the students can:

1. separate basic constituents into groups according to the reactions and properties of their
ions; and
2. identify the precipitating reagent of each group of cation.
o DISCUSSIONS
The elements in the periodic table can be classified in two different ways:
1. according to their atomic numbers.
2. according to the reactions and properties of their ions.
In the laboratory, we follow the second classification in which the ions that form compounds having
similar properties are placed in a single group. This classification makes use of group precipitants
facilitating the separation of each group and the subsequent identification of the ions.
o LEARNING RESOURCES
Small test tubes Centrifuge Tripod Stirring rod
Droppers Aspirator Water bath Red litmus paper
Evaporating dish Burner Wire gauze
o LEARNING STRATEGIES
1.1. Place in a test tube 5 drops of each of the following test solutions containing: Ag +, Cu2+, Zn2+,
Ba2+ and Na+.
1.2. Add 1-2 drops of 2N HCl at a time until precipitation seems complete. Stir and centrifuge.
Test for completeness of precipitation by adding 2 drops of 2N HCl to the supernatant liquid.
If no precipitate or turbidity is formed, precipitation is complete. If more precipitate is
formed, add a few drops more, stir and centrifuge again. Transfer the filtrate into another
test tube.
What is the color of the precipitate? ____________. What ion is precipitated? ______
1.3. Place the filtrate obtained in 1-2 in an evaporating dish and evaporate almost to
dryness. Add 1 drop of concentrated HCl to the residue and sufficient water to make 39
drops. Stir and transfer into a test tube. Saturate the solution with H 2S. Stir and centrifuge.
Transfer the filtrate into another test tube.
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What is the color of the precipitate? ____________ .What ion is precipitated? ______
To the filtrate obtained in 1-3, add 5 drops of NH 4Cl and make alkaline with concentrated NH4OH.
Saturate with H2S. Stir and centrifuge. Transfer the filtrate into another test tube.
What is the color of the precipitate?__________ What ion is precipitated?_________
Place the filtrate obtained in 1-4 in an evaporating dish and evaporate almost to dryness. Add 3 drops of
6N NH4OH and heat on a water bath for 3-5 minutes. Add 15 drops of (NH 4)2CO3 and 15drops of 95%
ethyl alcohol. Stir and centrifuge.
What is the color or the precipitate?___________ What ion is precipitated?____________
What ion is left in the filtrate?__________
IV. COMPLETE THE TABLE.
Ions
Group No.
Precipitating
reagent
Equation
Name and
color of the
precipitate
V. CONCLUSION
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Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______


REACTIONS OF SILVER GROUP
(Ions Separated as Chlorides)
I. LEARNING OBJECTIVES: At the end of the experiment, the students can:

1. test the reaction of the Silver Group I cations; and
2. write equations about the reactions of the Silver Group.
II. DISCUSSIONS
Precipitating Reagent (or Group Reagent): Dilute solution of HCI

The metals of this group all form chlorides on addition of HCI solution. The group reagent furnishes both
H+ and Cl- which is the actual precipitant. The chlorides formed are insoluble or slightly soluble in water
or dilute acids. This group is sometimes called the chloride group after its precipitating reagent.
The members of the group are: Ag+ - silver

Pb2+ - lead
Hg22+ - mercurous mercury
SILVER
The Ion. Silver forms the colorless univalent Ag+ ion. Its is an oxidizing agent and is reduced by strong
reducing agents to metallic silver which is usually black.
Compounds of Silver
1. Silver nitrate, AgNO3. This salt is formed by dissolving the metal in HNO3. It is the most soluble salts
of silver.
2. Silver chloride , AgCl. It is a white, curdyprecipitate formed with HCl or a soluble chloride the
precipitant. The precipitant darkens on exposureto light, but this does not affect its analytical
properties.
AgNO3 + HCl  AgCl ↓ + HNO3
AgNO3 + NH4Cl  AgCl ↓ + NH4NO3
The precipitate formed is only slightly soluble in hot water and in acids, but somewhat soluble in higher
concentrations of Cl ions forming complex ion which is relatively unstable.
On the hand, AgCl is readily soluble in aqueous ammonia, alkali cyanide, and sodium thiosulfate
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solutions owing to the formation of complex ions.
AgCl + 2NH4OH  Ag(NH3) 2Cl + 2H20
AgCl + 2KCN  KAg(CN) 2 + KCl
AgCl + Na2S2O3  NaAgS2O3 + NaCl
Silver chloride is only slightly soluble in HNO 3 even on prolonged boiling.
3. Other Silver Halides. The other halide ions, Br - and I- combine with Ag+ forming AgBr and AgI,
respectively, which resembles AgCl in their chemical properties.
AgBr is a cream, curdy precipitate slightly soluble in NH 3.
AgI is a yellow, curdy precipitate very slightly soluble in NH 3.
4. Silver-ammonia complex ion, Ag(NH3) 2+ . The Ag+ combines directly with ammonia molecules forming
the silver-ammonia complex cation which is very stable. Its dissociation into Ag + and NH3 is a good
trap for silver ion.
5. Silver hydroxide, AgOH. In the presence of OH - ions, AgOH is precipitated from solutions containing
silver ions. This compound is very unstable even at ordinary temperatures. It decomposes yielding
Ag2O. AgOH is not appreciable soluble in excess alkali hydroxide and does not have pronounced
amphoteric properties.
AgNO3 + NaOH  AgOH + NaNO3
2AgOH  Ag2O + H2O
NH4OH also precipitates AgOH, but the compound formed is soluble in excess of the reagent forming
silver-ammonia complex.
AgNO3 + NaOH  AgOH + NH4 NO3
AgOH + (excess) 2 NH4OH  Ag(NH3) 2OH + 2 H2O
6. Silver cyanide, AgCN. It is a white precipitate formed when a silver soluble salt reacts with an alkali
cyanide. The compound is insoluble in dilute acids but readily soluble in excess of the reagent
forming a stable argenticyanide complex.
AgNO3 + KCN  AgCN + KNO3
AgCN + KCN (excess)  KAg(CN)2
7. Silver chromate, AgCrO4. A brownish-red precipitate obtained when Ag + and CrO42- ions combine. The
compound is soluble in acids, KCN and NH 4OH.
2 AgNO3 + K2CrO4  AgCrO4 + 2KNO3
AgCrO4 + 2 KCN  2 AgCN + K2CrO4
AgCrO4 + 6 NH4OH  2 Ag(NH3)2OH + (NH4)2CrO4 + 6 H2O
LEAD
The Ion. Lead forms two positive ions: Pb+ (plumbous) and Pb4+ (plumbic).
Compounds of Lead
1. Lead nitrate, Pb(NO3)2. This is the most important of all lead salts. It is formed when metallic lead is
dissolved in dilute HNO3.
2. Lead sulfate, PbSO4. It is a white precipitate formed from aqueous or dilute acid solutions of lead
with H2SO4 or soluble sulfates.
Pb(NO3)2 + H2SO4  PbSO4 + 2 HNO3
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The HNO3 formed exerts a solvent action on the precipitate. Thus, if PbSO 4 is to be completely
precipitated, HNO3 must be removed by evaporation.
PbSO4 is soluble in ammonium acetate due to the formation of the soluble weakly ionized lead acetate.
PbSO4 + 2 NH4C2H3O2  Pb(C2H3O2)2 + (NH4)2SO4
PbSO4 is also soluble in alkali hydroxides with the formation of plumbites.
PbSO4 + 4 NaOH  Na2PbO2 + Na2SO4 + 2 H2O
3. Lead chromate, PbCrO4. This is a yellow precipitate which is insoluble in acetic acid but soluble in
HNO3 and in caustic alkali.
Pb(NO3)2 + K2CrO4  PbCrO4 + 2 KNO3
PbCrO4 + 4 NaOH  Na2PbO2 + Na2CrO4
PbCrO4 + 2 HNO3  Pb(NO3)2 + H2CrO4
chromic acid
4. Lead sulfate, PbS. Hydrogen sulfide precipitates the black lead sulfide in solutions of lead salts. It is
soluble in acid, but insoluble in caustic alkali.
Pb(NO3)2 + H2S  PbS + 2 HNO3
3 PbS + 8 HNO3  3 Pb(NO3)2
If the precipitate is carried out in HCl solutions, an orange-red precipitate of lead sulfochloride is first
formed which readily decomposes into black PbS with more H2S.
Pb(NO3)2 + 2 HCl  PbCl2 + 2 HNO3
PbCl2 + H2S  Pb2Cl2S ( or PbCl2.PbS)

Lead sulfochloride
Pb2Cl2S + H2S  2 PbS + 2 HCl
Lead sulfide is also precipitated by H2S from alkaline solutions containing the plumbite ion, HPbO 2.
NaHPbO2 + H2S  2 PbS + H2O
5. Lead Hydroxide, Pb(OH)2. This is a white precipitate formed when a solution of a lead salt is made to
react with an alkali hydroxide, possessing amphoteric properties, in that pumbites are readily formed
in an excess of the reagent.
Pb(NO3)2 + 2 NaOH  Pb(OH)2 + 2NaNO3
Pb(OH)2 + 2 NaOH (conc.)  Na2PbO2 + 2H2O
Pb(OH)2 + 2 NaOH (dilute)  2 NaHPbO2 + 2H2O
Ammonium hydroxide also gives thePb(OH)2 ppt. but it is insoluble in the excess of the reagent which
makes difference from silver.
Pb(NO3)2 + 2 NH4OH  Pb(OH)2 + 2 NH4NO3
6. Lead chloride, PbCl2. This is a white crystalline precipitate formed when a moderately concentrated
solution of a lead salt is treated with HCl or soluble chlorides.
Pb(NO3)2 + 2 HCl  PbCl2 + 2 HNO3
The precipitate is difficultly soluble in the cold, but much more soluble in hot water. Upon cooling, the
PbCl2 will precipitate in the form of glistening needles or plates. It is much more soluble in conc. HCl and
in the solution of an alkali chloride than in water, forming complex compounds.
MERCUROUS MERCURY
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The Ion. Mercury forms two ions: Hg2+, mercuric and Hg22+, mercurous. Both ions differ in their properties
very distinctly, the reason why they belong to different analytical groups.
Compounds of Mercurous Mercury

1. Mercurous nitrate, Hg2(NO3)2. This is the most important of all soluble salts of this ion.
2. Mercurous chloride, Hg2Cl2. This compound is also called calomel, it is a white precipitate obtained
by the reaction between mercurous nitrate and ammonia chloride.
Hg2Cl2 + SnCl2 = Hg2Cl2 + Sn(NO3)2
The precipitate turns gray or black in excess of the reagent with the reduction of Hg 22+ to metallic
mercury.
Hg2Cl2 + SnCl2 = 2 Hg + SnCl4
Mercurous chloride is basically precipitated from a solution of mercurous salt by the group reagent HCl.
The precipitate formed is insoluble in water and dilute acids but soluble in NH 4OH forming an insoluble
white amino-basic salt: (mercuric amino chloride) mixed with black finely- divided metallic mercury.
Hg2(NO3)2 + 2 HCl  Hg2CL2 + 2 HNO3
Hg2(NO3)2 + 2 NH4Cl  Hg2Cl2 + 2 NH4NO3
Hg2Cl2 + 2 NH4OH  HgNH2Cl + Hg + 2 H2O + NH4Cl
Mercuric amino- chloride
III. LEARNING STRATEGIES

2-1. In 3 separate test tubes, place 5 drops each of the test solutions for Ag +, Pb2+, and Hg22+.
2-2. Place 2-3 drops of 2N HCl. Note the color of the precipitate.Ag + ______________,
Pb2+ __________, Hg22+___________
For each test tube, stir and divide into 2 portion in 2 tes tubes. Centrifuge the 2 test tubes and separate
the centrifuge by decantation and use the precipitate to test the following:
a) Test the solubility of the precipitate by adding 5 drops of boiling water and heating the test
tube in the water bath. Write soluble, slightly soluble, or insoluble in row 2-2a in Table 2.
b) To another portion, add 5 drops of 6N NH 4OH. Describe the solubility of the precipitate and
write down the results in row 2-2b in Table 2.
2-3. Repeat step 2-1 and add 1 drop of 6N NH 4OH to each test tube. Stir. Note the color of the
precipitate. Ag+ , ____________ Pb2+ ___________ Hg22+ ____________
a) Continue adding NH4OH until precipitation have reached the maximum and add 3-5 drops
more in excess. Note in what test tubes the precipitate dissolves. Write down your
observations in Table 2.
2-4. Repeat step 2-1 and add 1 drop of 6N NaOH to each test tube. Stir. Note the color of the
precipitate. Ag+___________, Pb2+____________, Hg22+______________
a) Continue adding of NaOH until precipitate seems complete. Add 4 drops more in excess of
NaOH and note in what test tubes the precipitate dissolves. Write down your observations in
row 2-4a in Table 2.
2-5. Repeat step 2-1 and add 1 drop of K 2CrO4. Note the color of the precipitate.
Ag+___________, Pb2+____________, Hg22+_____________.
Centrifuge each test tube and separate the centrifugate. To the precipitate.
16
a) Add 3 drops of 6N NaOH. Write your observation in row 2-5a in Table 2.
2-6. Repeat step 2-1 and add 3-5 drops of KI. Note the color of the precipitate.
Ag+___________, Pb2+____________, Hg22+______________.
a) Add 3 drops more in excess of KI. Observe the solubility of the precipitate. Write down your
observations in row 2-6a in Table 2.
TABLE 2
Ions Ag+ (silver) Pb2+ (lead III) Hg22+ (mercurous

mercury)
Test Solution AgNO3 Pb(NO3)2 Hg2(NO3)2
2-2.TS and HCI: color,

name and formula of
ppt
2-2a. solubility of the

ppt in boiling water
2-2b. solubility of the

ppt in NH4OH
2-3. TS and NH4OH:

Color, name and
formula of ppt

ppt in excess of NH4OH
(if soluble write the
name and formula of
the product)
2-4. TS and NaOH:

Color, name and formla
of the ppt.
17
ppt in excess of NaOH
(if soluble write the
name and formula of
the product)
2-5. TS and K2CrO4:

color, name and
formula of the ppt.

ppt in NaOH (if soluble,
write the name and
formula of the product)
2-6. TS and KI:

color, name and
formula of the ppt.

ppt. in excess KI
Write equations to show the reactions of the following procedures:
1) 2-2
2) 2-3
3) 2-4
4) 2-5
5) 2-6
18
V. CONCLUSION:
19
Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______


REACTIONS OF THE HYDROGEN SULFIDE GROUP
(Ions Are Separated as Sulfides In their Acid Solutions)
I. LEARNING OBJECTIVES: At the end of the experiment, the students can:

1. test the reactions of the Hydrogen Sulfide Group or Group II cations.
2. write equations about the reactions of the Hydrogen Sulfide Group.
II. DISCUSSIONS
Precipitating Reagent: Hydrogen Sulfide

The metals of this group form chlorides that are soluble in water and in dilute acids but their sulfides are
precipitated by hydrogen sulfide in dilute (0.2-0.3 M H +) HCl solutions. It is necessary to maintain the H +
at this concentration for it in turn regulates the concentration of the sulfide ions. The higher the
concentration of the H+ ion, the lower the concentration of the sulfide ion would be as may be seen
following the equilibrium for the saturated solution of the H 2S.
[H+]2 [S-2] = 1.1 x 10-23
If the concentration of the [H+] is at 0.3M, it follows from the foregoing expression that the S -2
concentration in the same solution is approximately 1.2 x 10 -22 moles per liter which condition is most
favorable for the precipitation of the sulfides of this group. Too high H + concentration would fail to
precipitate cadmium and lead. On the hand, if the concentration is considerably lower than 0.2M, the
sulfides of zinc, nickel and cobalt which belong to the next group will precipitate if they are present in
the solution.
Treatment of the sulfide precipitates with sodium sulfide dissolves some ions of the group while the
others are left unaffected. Thus, the group is eventually split into 2 subgroups namely:
1. Copper Subgroup- whose sulfides are insoluble in sodium sulfide reagent
2. Tin Subgroup- whose sulfides are soluble in sodium sulfide reagent
Members of the group are:

Group II-A (Copper Subgroup) Group II-B (Tin Subgroup)
Hg2+ - mercuric mercury As3+ - arsenious
Pb2+ - lead (II) As5+ - arsenic
20
Bi3+ - bismuth Sb3+ - antimonious
Cu2+ - copper (II) Sn2+ - stannous
Cd2+ - cadmium Sn4+ - stannic
COPPER SUBGROUP (Group II-A Cations)
As described earlier, these ions do not dissolve in sodium sulphide, thus, separating them from the other
subgroup. These sulphides are, however, soluble in hot dilute HNO 3 except for mercuric mercury which
dissolves only in hot conc. HNO3.
MERCURIC MERCURY
The ions Hg2+ is a colorless ion and all its compounds are exceedingly poisonous. It forms complex ions
with the halogens, cyanide, ammonia, but its reaction appears to be somewhat irregular.
Compounds of Mercury
a. Mercuric nitrate, Hg(NO3)2. This is the important salt of mercuric mercury and is formed when
the metal is dissolved in hot, concentrated HNO 3.
b. Mercuric chloride, HgCl2. This is a white precipitate, soluble in water and alcohol. Stannous
chloride reduces mercuric salts, first to white mercurous chloride ppt, then it slowly turns to gray
metallic mercury, when excess of this reagent is added.
2HgCl2 + SnCl2  Hg2Cl2 + SnCl4
Hg2Cl2 + SnCl2  2Hg + SnCl4

c. Mercuric iodide, HgI2. This compound is a scarlet precipitate formed by the reaction of a
mercuric salt with an alkali iodide, soluble in an excess of the reagent.
2HgCl2 + 2KI  HgI2 + 2KCl
HgI2 + 2KI (excess)  K2HgI4
d. Mercuric sulphide, HgS. Hydrogen sulphide, alkali, or ammonium sulphide precipitate black
mercuric sulphide from solutions of mercurous or mercuric salts.
Hg2(NO3)2 + H2S  HgS + Hg + 2HNO3
Hg(NO3)2 + H2S  HgS + 2HNO3
Mercuric sulphide is insoluble in HCl and boiling dilute HNO 3. It is insoluble in ammonium
sulphide but readily soluble in alkali sulphide. It is readily soluble in aqua regia.
LEAD
The nature of lead ion and its reactions involved are given under Group I cations, Their presence in
Group II may be taken into account since they interfere with the test for the other ions namely: bismuth,
copper, and cadmium ions.
21
BISMUTH
The ion. Bismuth forms two ions: the trivalent Bi 3+ and the pentavalent Bi5+ which forms the bismuthate
compounds. The bismuthate are rather relatively unstable and are vigorous oxidizing agents.
Compounds of Bismuth
a. Bismuth sulfide, Bi2S3. It is a brown precipitate produced by the reaction of H 2S on solution of a
bismuth salt.
2Bi(NO3)2 + 3H2S  Bi2S3 + 6HNO3
Bismuth sulfide is insoluble in dilute acids and in alkali or ammonium sulfide. However, it is
readily soluble in hot, dilute HNO3 and in hot, conc. HCL
Bi2S3 + 8HNO3  2Bi(NO3)3 + 3S + 2NO + 4H2O

Bi2S3 + 6HCl  BiCl3 + 3H2S
b. Bismuth. A compound of bismuth will blacken instantaneously when treated with sodium
stannite reagent due to the formation of metallic bismuth.
Bi(NO3)3 + 3NaOH  Bi(OH)3 + 3NaNO3

2 Bi(OH)3 + 3NaSnO2  2Bi + 6NaNO3 + 3NaSnO3 + 3H2O
COPPER
The ion. Copper forms 2 series of compounds: cuprous, Cu + and cupric, Cu2+. Cuprous salts are found to
be quite insoluble and show a marked tendency to be oxidized easily into the cupric state even in the
presence of air.
The Cu2+ is characterized by a blue color in water solution which changes with the concentration of the
Cu2+ ion. This property may be due to a change in the extent of the hydration of the ion.
Compounds of Copper
a. Cupric sulfide, CuS. This compound is one of the most insoluble salts of the compounds. A
neutral, ammoniacal or slightly acidic solution of a copper salt readily reacts with H 2S
forming the black precipitate of CuS.
Cu (N03)2 + H2S  CuS + 2HNO3

Cupric sulfide is insoluble in dilute acids and in alkali sulfides and slightly dissolves in yellow ammonium
sulphide forming a brown solution. It is, however ,readily soluble in dilute HNO 3
3CuS + 8HNO3  3 Cu(NO3)2 + 2 NO + 3S + 4H2O
b. Cupric ferrocyanide , Cu2 Fe(CN)6. This amorphous reddish brown precipitate is very insoluble
salt which serves as sensitive test for Cu 2+ ion. Its formation may be represented as follows:
2Cu(NO3)2 + K4Fe(CN)6  Cu2 Fe(CN)6 + 4KNO3
If only a trace of Cu2+ is present , the copper ferrocyanide will appear not as a precipitate but as a rose
-colored solution. This salt is insoluble in dilute or weak acids but soluble in solutions of ammonium
22
hydroxide giving a blue solution of Cu(NH 3)4 2+ , tetraamine complex , which furnishes fewer Cu 2+ ions
than does the saturated solution.
Cu2Fe (CN)6 + 12 NH4OH  2 Cu (NH3)4 (OH)2 + (NH4)4 Fe(CN)6
On acidifying slightly, the copper ferrocyanide is re-precipitated.
2Cu (NH3)4 (OH)2 +(NH4)4 Fe( CN)6 + 12HCL  Cu2 Fe(CN)6 + 12 NH4Cl + H2O
c. Copper –ammonia complex ion, Cu (NH3)4 2+. Ammonium hydroxide added dropwise to a solution of
copper salt, gives first a green basic precipitate which readily dissolves in an excess of the reagent with a
characteristic deep blue solution.
CADMIUM
The ion Cadmium ion,Cd2+ shows a marked tendency to form complex ion with halides and ions. The
halides of cadmium resemble that of Hg 2+ in that they are weakly ionized in solution.
Compounds of Cadmium
a. Cadmium sulphide, CdS. It is yellow precipitate produced by passing through H 2S gas into
solutions containing Cd2+ ions. The color may vary from yellow to orange (or even brown)
depending upon the conditions of precipitation.
Cd(NO3)2 + H2S  CdS + HNO3
b. Cadmium ferrocyanide, Cd2 Fe (CN)6 . Potassium ferrocyanide gives white precipitate of

cadmium ferrocyanide with solution containing Cd2+ ions. The precipitate formed is insoluble in
weak acids such as acetic acid or dilute HNO3. The precipitate is however ,soluble in strong
HNO3.
Cd(NO3)2 + K4Fe(CN)6  Cd2Fe(CN)6 + 4 KNO3
c. Cadmium hydroxide, Cd (OH)2 . Alkali hydroxides give a white precipitate when added to a
solution containing Cd2+ ions.
Cd (NO3)2 + 2NaOH  Cd (OH)2 + 2NaNO3
The precipitate is insoluble in an excess of reagent (difference from zinc and lead)
TIN SUBGROUP (GROUP II-B CATIONS)
As previously mentioned, arsenic , antimony, and tin are precipitated as sulfides together with the ions
of copper subgroup, but differ from them by being soluble in yellow sodium sulfide to form the insoluble
thio-compounds. Yellow sodium sulfide may be regarded as the source of sulphur. When the solution is
acidified, the sulfides of this group are re-precipitated, though not necessarily in their original forms. In
the process of re-precipitation, sulfur is always obtained as white precipitate which if in this color will
indicate the absence of Group II-B cations, it is merely of sulfur. If the precipitate is heavy and colored,
the presence of Group II-B cations may be indicated.
23
ARSENIC
The Ion. The element arsenic forms two series of compounds in which it exhibits the oxidation states of
+3 and +5. The hydroxides of element in two valence states are acidic in character and show little basic
properties. They are amphoteric so that cations and anions are formed in both series, e.g. cation As 3+ ,
anion AsO2 – (arsenite),cation As 5+,anion AsO3 – (arsenate). They are comparatively wealk as acids,
arsenious acid being much weaker than arsenic acid. Their sulfides are also aphoteric in nature forming
thio arsenates and thioarsenates respectively in both oxidation states.
Compounds of Arsenic
1. Reaction with AgNO3
a) Silver nitrate , AgNo3 gives a yellow precipitate of silver orthoarsenate in neutral solution of
arsenates (difference from arsenates).
H3AsO3 + 3 NH4OH + AgNO3 = Ag3AsO3 + 3NH4NO3 + 3H2O
The precipitate formed is soluble in HNO3 or in NH4OH, forming silver ammonia complex with the latter.
b. With arsenic acid, H3AsO4, a chocolate- brown precipitate is obtained with silver nitrate (difference
from arsenites and phosphates.)
H3AsO4 + 3NH4OH + 3AgNO3 = Ag3AsO4↓ + 3NH4NO3 + 3H20
2. Sulfides of Arsenic
a. Arsenious sulfide is precipitated by H2S from acid solutions of arsenites or arsenious salts.
2AsCl3 + 3H2S = As2S3↓ + 6HCl
The precipitate which is yellow is exceedingly insoluble and maybe completely precipitated in
the presence of conc. HCl. However, it dissolves on prolonged boiling with concentrated acid
which may be due to the removal of H2S and the volatilization of the arsenious chloride formed.
3As2S3 + 10HNO3 + 4H20 = 6H3AsO4 + 10NO + 9S ↓
With concentrated HNO3, NO2 is formed.
As2S3 + 28 HNO3 (conc.) = 2H3AsO4 + 3H2SO4 + 28NO2 + 8H2O
b. A cold solution of an arsenate or arsenic acid in 0.3N acid precipitates with H2S very slowly,
allowing the reduction of As5+ to As3+ before precipitation of As2S3 actually occurs.
Na3AsO4 + H2S = Na3AsO3S + H20
Na3AsO3S = Na3AsO3 + S↓
H3AsO3 + 3HCl = AsCl 3 + 3H2O
2AsCl3 + 3H2S = As2S3 ↓ + 6HCl
24
2H3AsO3 + 3H2S = As2S3↓ + 6H2O
However, in strongly acid cold solutions of arsenates, a yellow As 2S5, arsenic sulfide precipitate is
obtained with H2S.
2Na3AsO4 + 6HCl + 5H2S = As2S5 ↓ + 6NaCl
If H2S is passed into a hot solution of an arsenate, a mixture of the two sulfides are formed.
H3AsO4 + 5HCl = AsCl3 + 6NaCl + 8H2O
2AsCl5 + 5H2S = As2S5 ↓ + 10HCl
The sulfide is soluble in hot concentrated HNO3
As2S5 + 10 HNO3 = 2H3AsO4 + 10NO2 +5S↓ +2H2O
ANTIMONY
The Ion. Like arsenic, antimony exists in two oxidation states: +3 and +5. Since antimony falls
below arsenic in the fifth group of the periodic table, it is more electronegative than arsenic.
Consequently, the hydroxides of antimony are more basic than those of arsenic although both are
amphoteric. Even as bases, their hydroxides are weak and their salts are highly hydrolyzed. Strong acids
must be added to their solutions to prevent basic salts from precipitating.
Compounds of Antimony
1. Oxides of Antimony. Sb2O3 and Sb2O5. Both behave very much like the oxides of arsenic, the
small difference may be due to the more basic character of antimony.
Solutions of alkali hydroxides, when added to solutions containing Sb 3+ ions, precipitate the
white hydrated oxide, soluble in the excess of the reagent especially on warming, forming
antimonites displaying its amphoteric nature.
2SbCl3 + 6NaOH = Sb2O3 3H2O (or H3SbO3) + 6NaCl
Sb2O3. 3H2O + 2NaOH = 2NaSbO 2 + 4H2O
With acids:
Sb2O3 . 3H2O + 6HCl = 2SbCl 3 + 6H2O
Sb2O3 . 3 H2O + 2NaOH = 2NaSbO 3 + 4H2O
Sb2O3 . 3H2O + 10HCl = 2 SbCl 5 + 8 H2O
The reactions immediately preceeding show the amphoteric character of the Sb 5+ ion
forming the antimonate ion in its reaction with an alkali hydroxide.
Ammonium hydroxide produces the same effect as NaOH, but the resulting product is
insoluble in the excess of the reagent.
25
SbCl3 + 6NH4OH = Sb2O3 . 3H2O + 6NH4Cl
SbCl5 + 10 NH4OH = Sb2O3.5H2O + 10 NH4Cl
2. Sulfides of Antimony, Sb2S3 and Sb2S3
a. Antimonious sulfide, Sb2S3 may be precipitated from any solution containing Sb 3+ ions provided
+
the H ion concentration is not too great.
2 SbCl3 + 3 H2S = Sb2S3 + 6 HCl
In a saturated solution of SbOCl2, there are sufficient Sb3+ so that addition of H2S will precipitate
the red Sb2S3.
2 SbOCl + 3 H2S = Sb2S3 + 2 HCl + 2 H2O
Antimonious sulfide is soluble in moderately strong HCl solution due to the first that a saturated
solution of the sulfide furnishes sufficient S2- ions to form H2S.
b. Antimonious sulfide is precipitated by H2S in moderately strong solutions of Sb5+ ions. This
precipitate which is orange-red in color, is re-dissolved by the addition of concentrated HCl yielding Sb 3+
ions. In other words, strong HCl reduces Sb 2S5.
2 SbCl5 + 5 H2S = Sb2S5 + 10 HCl
Sb2S5 + 6 HCl = 2SbCl3 + 3 H2S + 2 S
In addition to the redox reaction taking place on the antimony ions, S 2- ion is also reduced to free
sulfur.
3. Reduction of Antimony. Active metals such as zinc, iron, or tin, reduces antimony from its compounds
to metallic antimony.
2 SbCl3 + 3 Sn = 2 Sb + 3 SnCl2
2 SbCl5 + 5 Sn = 2 Sb + 5 SnCl 2
The metallic antimony appears as a black deposit or precipitate which is insoluble in sodium
hypobromite solution (difference from arsenic).
TIN
The Ion. Tin forms two series of compounds with the oxidation states of +2 and +4, stannous and
stannic tin, respectively.
Compounds of Tin.
a. Sulfides of tin, SnS and SnS2. Stannous and stannic sulfides may be prepared by fusing the
elements together but the latter is unstable at high temperature.
26
SnS2 = SnS +S
Hydrogen sulfide precipitates brown stannous and yellow stannic sulfide from dilute acid solutions of
stannous and stannic salts, respectively.
SnCl2 + H2S = SnS + 2 HCl
H2SnCl6 + 2 H2S = SnS2 + 6 HCl
Difference between the 2 sulfides:
SnS is soluble in alkali and ammonium sulfides, while SnS 2 is soluble in these 2 reagents.
b. Reduction of tin.
1. Metals such as zinc, iron, or magnesium ribbon, could be used as reducing agent for stannic
tin.
H2SnCl6 + 2 Zn = SnCl2 + 2 ZnCl2 + H2
H2SnCl6 + 2 Sb = SnCl2 + 2 SbCl2 + 6HCl
H2SnCl6 + 2 Mg = SnCl2 + 2 MgCl2 + H2
2. SnCl2 + 2 HgCl2 = Hg2Cl2 + SnCl4
III. MATERIALS:
test tubes droppers centrifuge
burner tripod water bath
pipette aspirator filter paper
cotton
IV. PROCEDURE
3-1. In 9 separate tes tubes, add 5 drops of each of the following test solutions for Pb 2+, Bi3+, Cu2+, As3+,
Sb3+, Cd2+, Hg2+, Sn2+, and Sn4+.
Note the color of each test solution in its aqueous solution.
Pb2+ _________ As3+ __________ Hg²2+__________
Bi3+ _________ Sb3+ __________ Sn2+ __________
Cu²2+ _________ Cd²3+__________ Sn4+ __________
a. Saturate the solution with hydrogen sulfide. Note the colors of the precipitate and write
them in row 3-1 a on the Table.
27
b. Test the solubility of each precipitate with sodium sulfide. Write the observation in
row 3-1b on the Table.
3-2 Confirmatory test for Pb2+. (Refer to Experiment #2)
31-3 Confirmatory test for Bi3+
Place 5 drops of Bi3+test solution in a test tube, add 5-10 drops of freshly prepared sodium
stannite. Observe the results. _______________________________.
Note: Prepare sodium stannite by adding 6N NaOH to 5 drops of SnCl2 dropwise until the
white precipitate of Sn(OH)2 which first formed, redissolves. Then add a slight excess of NaOH.
3-4 Confirmatory tests for Cu2+
a. Acidify 5 drops of Cu2+ solution with 6N Acetic Acid, CH3COOH. Add 21-3 drops of
b. To 5 drops of Cu2+ solution, add 1 drop of 6N NH4OH. Note the color of the precipitate.
______________
Test the solubility of the precipitate by adding 5-10 drops more of NH4OH. Note your
observations. __________________________________________________________
3-5 Confirmatory test for Cd2+
Add 5 drops of K4Fe(CN)6 to 5 drops of Cd2+ test solution. Note the color of the precipitate.
______________
3-6 Confirmatory test for Hg2+
a. Place 5 drops of Hg2+ test solution, add 3-5 drops of SnCl2 solution. Observe the color
of the precipitate/. ____________
b. Add 1 drop of KI solution to 5 drops of Hg2+ test solution. Note the color of the
precipitate. _________________
Test the solubility of the precipitate in excess of KI. Note your observations.
______________________________________________________________
3-7 Confirmatory test for Sb2+
a. Dilute 5 drops of Sb3+ test solution with 5 drops of distilled water and add a small piece of
aluminum metal and heat on a water bath for 5 minutes. Observe the results.
___________________________________________________________________
b. Pipette out the supernatant liquid and add 2-3 drops of freshly prepared sodium
hypobromite to the precipitate. Note your observations. _______________________
____________________________________________
Note: Sodium hypobromite is prepared by adding 6N NaOH to 56 drops of saturated

Bromine solution dropwise until the mixture becomes colorless or light yellow
then adding 3-5 drops more of NaOH in excess.
28
3-8 Confirmatory test for As3+
Dilute 3 drops of As3+ test solution with 3 drops of distilled water and saturate with H2S.
Dissolve the precipitate with 6N NaOH, add a small piece of aluminum metal. Promptly place a
plug of cotton below the mouth of the test tube and cap the tube with filter paper.
Wet the filter paper over the mouth of the test tube with 1 drop of AgNO3 test solution.
Heat the test tube on a water bath for 5-10 minutes. Note the color produced on the filter
paper. _________________________
3-9 Confirmatory test for Sn2+ and Sn4+
a. To 5 drops of Sn2+ test solution, add 1-2 drops of HgCl2 reagent. Observe the color of the
precipitate. __________________________
b. Reduce Sn4+ to Sn2+ by adding a piece of magnesium ribbon to the Sn4+ test solution. Add 3-
5 drops of hgCl2 reagent. Note your observations.
_________________________________________________________
Table 3
IONS Pb2+ Bi3+ Cu2+ As3+ Sb3+ Cd2+ Hg2+ Sn2+ Sn4+
Test Pb(No3)2 Bi(NO3)3 Cu(NO3)2 AsCl3 SbCl3 Cd(NO3)2 Hg SnCl2 SnCl4
Solution (NO3)2
3-1a. TS
with H2s.
Color,
name and
formula of
the
precipitate.
3-1b.
Solubility
of the
above (3-
1a)
precipitate
with Na2S.
29
Table 3-A
Confirmatory Test Reagent/s Added Color, name and formula of

the precipitate
3-3 for Bi3+ Sodium stannite
3-4 for Cu2+ a. Acidified with acetic acid

and added with potassium
ferrocyanide
b. Ammonium hydroxide in
excess
3-5 for Cd2+ Potassium ferrocyanide
3-6 for Hg2+ a. Stannous chloride
b. KI
3-7 for Sb3+ a. Aluminum metal
b. Solubility of the precipitate

in NaOBr
3-8 for As3+ a. Ammonium hydroxide, silver

nitrate
3-9 for Sn2+ and Sn4+ a. HgCl2
b. Magnesium ribbon, HgCl2
V. CONCLUSION
30
31
Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______


REACTION OF THE AMMONIUM SULFIDE GROUP
(IONS ARE SEPARATED AS SULFIDES IN THEIR ALKALINE SOLUTIONS)
I. OBJECTIVE: At the end of the experiment, the students are expected to
1. Test the reaction of the Ammonium Sulfide Group or the Group III cations.
2. Write equation about the reactions of the Ammonium Sulfide Group.
II. DISCUSSION
Group Reagent: Hydrogen sulfide in the presence of NH₄⁺ ions.
Metals of this group form chlorides that are soluble in water, their sulfides are soluble in dilute acids
but are soluble in ammoniacal solutions. They are separated as sulfides or hydroxide by ammonium
sulfide or hydrogen sulfide in a solution of ammonia and ammonium chloride. This group is also called
Aluminum-Iron Group and is divided into 2 subgroups:
1. Aluminum subgroup – whose hydroxides are soluble in excess NaOH and Na₂O₂.
2. Iron subgroub – whose hydroxides are insoluble in excess NaOH and Na₂O₂.
The members of the group are:
Group III-A (Aluminum subgroup) Group III-B ( Iron subgroup)

Al³⁺ - aluminum Fe²⁺ and Fe³⁺ - ferrous and ferric
Cr³⁺ - chromium Mn²⁺ - manganese (II)
Zn²⁺ - zinc Co²⁺ - cobalt (II)
Ni²⁺ - nickel (II)
ALUMINUM SUBGROUP (GROUP III-A)
Except for zinc ion, the sulfides of this group do not precipitate as such due to hydrolysis. Zinc is
classified under this grouping because, like aluminum and chromium, it forms an amphoteric hydroxide
which is very soluble in NaOH and Na₂O₂ mixture. They form complex ions as aluminate, chromate and
zincate, This property is used to separate aluminum subgroup from the iron subgroup.
ALUMINUM
32
The Ion. Aluminum exhibits only one oxidation state, +3 in its compounds. The common salts of this ion
are colorless and are appreciably soluble in water or dilute acid solution. Its hydroxide is decidedly
amphoteric, hence a series of complex compounds are formed in which aluminum is a part of the
complex as an aluminate, AlO₂⁻ ion.
Compounds of Aluminum
a. Aluminum hydroxide, Al(OH)3
1. NH4OH yields a white gelatinous precipitate of Al(OH)3 which is insoluble in the excess
of the reagent.
Al(OH3)3 + 3 NH4OH = AL(OH)3 + 3 NH4NO3
2. NaOH yields a white gelatinous precipitate of Al(OH) 3 which readily dissolves in the
excess of the reagent forming aluminates.
Al(NO3)3 + 3 NaOH = Al(OH)3 + 3 NaNO3
Al(OH)3 + NaOH = NaAlO2 + H2O
b. “Lake Formation”. Al(OH)3, being a positive colloid (carries a positive electric charge), when
mixed with a salt of a dye, and the mixture made alkaline, an insoluble “lake” with a distinctive color is
formed. Thus, aluminum reagent, an ammonium salt of aurintricarboxylic acid, gives a bright red lake
with Al(OH)3.
c. Cobalt aluminate, Co(AlO2)2. When Al(OH)3 is ignited, aluminum oxide, Al 2O3, is formed and
this compound has acidic properties and combines with certain other oxides at high temperature
forming aluminates. If a mixture of Co(NO3)2 and Al(NO3)3 is fused, their respective oxides are first
formed, then these will unite giving a blue residue called cobalt aluminate.
Co(NO3)2 = CoO
+ Co(AlO2)2
Al(NO3)3 = Al2O3 “Thenard’s blue”
CHROMIUM
The ion. Chromium shows three oxidation states in its various compounds. +2 in chromous
compounds, +3 in chromic, and +6 in chromates and dichromates. Chromous ion, Cr 2+ is easily oxidized
into the chromic condition. Chromic, Cr3+ ion resembles Al3+ ion in several ways. It is readily hydrolyzed
with the formation of Cr(OH)3 which possess amphoteric properties. Oxidation of Cr 3+ ion gives rise to
the formation of chromates, CrO42- and dichromates, Cr2O72- depending on the alkalinity or acidity of the
medium.
33
Compounds of Chromium
a. Chromic oxide, Cr2O3. The hydrolysis of the chromium salts gives rise to a hydrated oxide,
Cr2O3. H2O. this so-called “hydroxide” which is precipitated from chromium solution is described as
hydrated oxide and is formed by the reaction of NH 4OH or (NH4)3S with solutions of chromic salts.
2 Cr(NO3)3 + 6NH4OH = Cr2O3.H2O + 6NH4NO3 + 2H2O

2 Cr(NO3)3 + 3(NH4)2S + 4H2O = Cr2O3.H2O + 6NH4NO3 + 3H2S
In the presence of excess alkali hydroxide, the hydrated oxide dissolves forming another series of
compounds known as chromites.
2 Cr(NO3)3 + 6 NaOH = Cr2O3.H2O + 6 NaOH3 + 2H2O
Cr2O3.H2O + 2 NaOH (excess) = 2NaCrO2 + 2H2O
b. Oxidation to chromates by peroxides. Sodium peroxide or hydrogen peroxide solution in

alkaline medium oxidizes Cr3+ into yellow CrO42-, the chromium ion of which has an oxidation state of +6.
When Na2O3 is added to the chromites solution, the latter is oxidized forming a yellow solution of sodium
chromate.
2 NaCrO2 + 2 Na2O2 + H2O = 2 NaCrO4 + 4 NaOH
ZINC
The ion. Zinc shows only one series of compounds in which the oxidation state is +2. Zinc
hydroxide possesses amphoteric properties forming zincates. Its most stable complex ions are Zn(
NH3)42+, Zn(CN)43-, HZnO2-.
Compounds of Zinc
a. Zinc hydroxide, Zn(OH)2. Zinc hydroxide is separated as a white gelatinous precipitate upon
addition of the OH ions to the solutions of zinc salts.
b. Zinc complexes.
1. Sodium zincates, Na2ZnO2. When an alkali hydroxide is added to a solution of a zinc

salt, a white gelatinous precipitate of Zn(OH)2 is first formed which dissolves upon addition of an excess
reagent.
Zn(NO3)2 + 2 NaOH = Zn(OH)2 + 2 NaNO3
Zn(OH)2 + NaNO2 + 2 NaOH = Na2ZnO2 + NaNO3 + 2 H2O
2. Cobalt zincate, CoZnO2. When a mixture of Zn(NO3)2 and Co(NO3)2 is evaporated to

dryness and the residue ignited, the ZnO and CoO formed will unite forming a green CoZnO 2, cobalt
zincate, also known as Rinmann’s green.
An excess of the Zn(NO3)2 should be added because the an excess of CoO that may be formed, makes the
green color.
34
Zn(NO3)2 + Co(NO3)2 = ZNO + CoO = CoZnO2
c. Zinc Potassium ferrocyanide , Zn3K2[Fe(CN)6]2. Zn2+ ions react with potassium ferrocyanide
forming a white precipitate of zinc- potassium freeocyanide which is insoluble in HCL but soluble in
ammonium hydroxide or other strong bases.
2 Zn(NO3)2 + K4Fe(CN)6 = Zn2Fe(CN)6 + 4KNO3

3 Zn2Fe(CN)6 + K4Fe(CN)6 = 2 Zn3K2[Fe(CN)6]2
d. Zinc sulfide , ZnS . Zinc sulfide is the only common white metallic sulfide. It is precipitated by
the addition of an alkali or ammonium sulfide to the solution of zinc salts.
Zn(NO3)2 + H2S = ZnS + 2 HNO 3
GROUP III-B (IRON SUBGROUP)
The hydroxides of the members of this subgroup do not dissolve in excess sodium hydroxide and Na 2O2 -
the mixture used to separate the 2 subgroups by Group III. This group precipitates as sulfides in the
process of separating these cations from the subsequent groups. Their ions do not display amphoteric
properties.
IRON
The ion iron forms two important series of salts : ferrous, with an oxidation state of +2 and ferric with an
oxidation state of +3. The ferrous salts form green hydrates while the hydrated ferric salts are yellow or
brown in color. The ferrous ion is a strong reducing agent having a pronounced tendency to go to the
ferric state.
Compound of Iron
a. Ferrous and ferric hydroxide, Fe(OH)2 and Fe(OH)3. These hydroxides are precipitated by NH 4OH,
NaOH , or KOH when these reagents are added to neutral solutions of ferrous or ferric salts.
For ferrous salts: FeCl2 + 2 NaOH = Fe(OH)2 + 2NaCl
FeCl2 + 2NH4OH = Fe(OH)2 + 2NH4Cl
Ferrous hydroxide is white when pure is rapidly oxidized in air, undergoing several stages of color
: first, green , then it turns black , and finally reddish- brown when it becomes Fe(OH) 3.
2 Fe(OH)2 + H2O (oxidized in air) = 2 Fe(OH)3

For ferric salts : FeCl3 + 2 NaOH = Fe2S3 + 6NH4NO3
FeCl3 + NH4OH = Fe(OH)3 + 3NH4Cl
Ferric hydroxide is insoluble in excess of the reagent and in this way differs from the hydroxies of
aluminum , chromium and zinc. It also differs from the hydroxides of cobalt and nickel since the latter are
soluble in excess NH4OH forming complex ions.
35
b. Sulfides of iron. FeS and Fe2S3. Ferrous sulfide is a black precipitate formed when soluble sulfides
are added neutral or basic solutions of ferrous salts.
Fe(OH)2 + H2S = FeS + 2 H2O

Fe(OH)2 + Na2S = FeS + 2 NaOH
Fe(OH)2 + (NH4)2S = FeS + 2 NH4OH
Hydrogen sulfide in acid solution reduces ferric to ferrous with the precipitation of sulfur.
Fe(NO3)3 + H2S = Fe2S3 = +

2 2 Fe(NO3) 2 + 2 HNO3 + S
But if ammonium sulfide in alkaline solution used, Fe 2S3 is precipiatated.
2 Fe(NO3) + 3 (NH4)2 S = Fe2S3 + 6NH4 NO3

2 Fe(NO3) + 3 (NH4)2 S = Fe2S3 + 6 NH4OH
c. Complex iron cyanides

1. Ferrous and ferrocyanide . Potassium ferrocyanide yield with solutions of ferrous salts, a white
precipitate of ferrocyanide with complete exclusion of air. In the presence of air, the precipitate
the greenish or light blue in which case Fe 3+ state.
2 FeSO4 + K44 Fe(CN)6 = Fe2Fe(CN)6 + K2 SO4

FERROUS FERROCYANIDE
6 Fe2Fe(CN)6 + 6 H2O +
O2 (air) = Fe4[Fe(CN) 6] 3
3 + 4 Fe(OH) 3
FERRIC FERROCYANIDE
With ferric salts , the same precipitate, ferric ferrocyanide (or Prussian blue) as above , is obtained:
4 Fe(NO) 3 + 3 K44 Fe(CN)6 = Fe4[Fe(CN) 6] 3 + 12 KNO3
PRUSSIAN BLUE
2.ferrous and ferric ferricyanide. Potassium ferricyanide yields with ferrous salts, a blue precipitate
(Turnbull's Blue) of ferrous ferricyanide.
3FeSO4 + Fe3 [Fe(CN)6]2 ↓ + 3 K2SO4

Turnbull's Blue
ferric salts give a brown solution with the same reagent due to the formation of a ferricyanide or simply,
ferric cyanide.
36
Fe (NO3)3 + K3Fe (CN)6 or 2 FeFe (CN)6 + 3 KNO3
Ferric Cyanide (Brown Solution)
d. ferric thiocyanate, Fe(SCN)3. Ammonium or Potassium thiocyanate gives a blood-red coloration

with Ferric ions.
Fe (NO3)3 + 3 KSCN = Fe (SCN)3 + 3 KNO3

Blood-red color
MANGANESE
The ion. Manganese forms several series of compounds with the oxidation states ranging from +2 to +7.
These ions with their corresponding names and compounds are the following:
ION NAME COMPOUND

Mn2 Manganous Mn (OH)2
Mn3 Manganic Mn (OH)3
Mn4 Manganese MnO2
Mn6 Manganate KmnO4
Mn7 Permanganate KmnO4
Compounds of Manganese
a. Manganous Hydroxide, Mn (OH). This is a whit precipitate obtained when ammonium hydroxide or
alkali hydroxide is added to a neutral solution of Mn2 ions. But when in contact with air, it becomes
brown.
b. manganous Sulfide, MnS. Solutions containing Mn2 ions when treated with ammonium sulfide will
produce a salmon-colored precipitate of MnS which is readily soluble in acids even in the weak acetic
acid.
Mn (NO3)2 + (NH4)2S = MnS ↓ + 2 NH4NO3
Mn (OH)2 + (NH4)2S = MnS ↓ + 2 NH4NO
c. Oxidation of Mn2 ion.
1. Manganous Compounds are also oxidized by NaBiO3, Sodium bismuthate, with the development
of a purple or violet or pink coloration (depending on the amount of Mn2 ions present).
2Mn (NO3)2 + 5 NabiO3 + 16 HNO3 = 2 HmnO4 + 5NaNO3 + 5 Bi (NO3)3 + 7 H2O
COBALT
The ion Cobaltous, Co2 form is the only simple ion of Cobalt that is of analytical importance. Hydrated
cobaltous compounds and their dilute solutions are pink in color, while concentrated solutions and the
anhydrous salts are blue.
Compounds of Cobalt
a.Cobalt hydroxide, Co (OH)2. Alkali hydroxides precipitate cobalt hydroxide from solutions of cobalt
salts. The hydroxide is blue in color in cold solutions but pink or rose colore3d in warm solutions.
37
Co (NO3)2 + 2 NaOH = Co (OH)2 ↓ + 2NaNO3
The precipitate formed is only very slightly soluble in excess alakali. On exposure to air, Co
(OH)2 becomes brown in color due to partial oxidation.
b. Oxidation of Cobalt. When Cobalt hydroxide is treated with Na2O2, a brown to black precipitate of
cobaltic hydroxide, Co (OH)3 is formed.
2 Co (OH)2 + Na2O2 + 2 H2O = Co (OH)3 ↓ + 2 NaOH
c. Cobalt Sulfide, CoS. Cobalt sulfide is a black precipitate obtained in an ammoniacal solution of Co2
ions with (NH4)2S.
Co (NO3)2 + (NH4)2S = CoS ↓ + 2NH4NO3
d. Cobalt ammonia complex ion, Co (NH3)42. Ammonium hydroxide when added to solution of
cobalt ions precipitate Co (OH)2, but this is soluble in excess of the reagent
And in an excess of NH4Cl. The dirty yellow ammoniacal solutions gradually turns to reddish in color on
exposure to air due to the formation of the more stable cobalt ammonia complex ion.
e. cobalt nitrite ion Co(NO2)63-. potassium nitrite added to solution of Co which have been acidified with
acetic acid, given a yellow precipitate of potassium cobalt nitrite.
Co(NO3) 2 + 7KNO 2 + 2CH 3 COOH = K 3 CO(NO 2 ) 6 +2 CH 3 COOK + NO↑ +2 KNO 3 H 2 O
NICKEL
The principal oxidation state of nickel is +2. Nickel salts in the hydrated form and in solution are
green in color while anhydrous salts are yellow.
Compounds of nickel
a. Nickel hydroxide, Ni(OH)2 . it is a green precipitate obtained from The reaction between Ni 2+
ions and alkali hydroxide
b. Nickel ammonia complex, Ni(NH3)62+ . ammonium hydroxide in dilute solution and in the absence
of ammonium salts, precipitates a green basic salt soluble in excess of the reagent forming a
series of ammonia complex ions called nickel-ions.
c. Nickel sulfide, NiS. Nickel sulfide is not precipitated by H 2S in solutions of nickel salts containing
mineral acids or much acetic acid, but from solutions made slightly acidic with acetic acid and
containing alkali acetate, or from solutions its ammoniacal solutions in which all nickel ions may
be precipitated as black nickel sulfide.
Ni(NO3 )2 2CH3 COONa + H2 S = NiS ↑ + NaNO3 + CH3 COOH
Ni (NH3)4 (NO3 )2 + H2 S = NiS ↑ + 2 NH2 NO3 + 2NH3
d. Glyoxime derivative of nickel. Dimethyglyoxime in alcohol yields with solution of nickel salts
made alkaline with ammonium hydroxide, a characteristic red precipitate of nickel
dimethygloxime.
38
Ni(NO3)2 + 2 NH3 + 2 C4H6N2O2H2 = Ni(C4H6N2O2H2)2 + 2 NH4NO3
Dimethylglyoxme nickel dimethylglyoxime
III. Materials
Water bath filter paper burner tripod test tubes droppers
IV. PROCEDURE
4-1. In 8 separate test tubes, place 5 drops each of the following test solutions. Al 3+, Cr 3+, Zn2+, Mn 2+, Co
2+
, Ni 2+, Fe2+ and Fe3+ . Note the color of each solution.
. Al 3+ ____________ Zn2+ ____________ Co 2+__________ Fe2+_____________
Cr 3+____________ Mn 2+ ___________ Ni 2+ ____________Fe3+ ____________
4-2. Add 1 drop of (NH4)2S to the test tubes above (4-2) and note the color of the precipitate. Right the
color in row 4-2 in table 4.
a) Add one drop of (NH4)2S to the test tubes above (4-2) and note the color of the precipitate. Write
the color in row 4-2a in table 4
4-3. In 8 separate test tubes, place 5 drops each of the solutions of group III cations and add 1 drop of 6N
NaOH to each test tube until precipitate is formed. Write the color of each precipitate in row 4-3 in table
4.
a) Test the solubility of the precipitate above by adding 2-3 drops more in excess of 6N NaOH.
Write your observations in row 4-3a in table 4.
b) Then add 2 drops of H2 O2 or small amount of Na2O2 . stir and note in what test tubes you have
observed a change. Write your observations in row 4-3b in Table 4.
4-4. Confirmatory test for Al3+

a) Aluminon test, to 2 drops Al3+ test solution, add 6N NH4OH until precipitate is formed. Add one
drop of ammonium 6N acetate and 2 drops of aluminon reagent. Observe the color of the
lake.____________________
b) Thenard’s blue test. To 5 drops of Al3+ test solution, add one drop of Co(No3)2 and 3-4 drops 6N
NH4OH. Filter and ignite the precipitate. Note the color of the ash. ___________________
4-5. Confirmatory test for Cr3+. To 5 drops of Cr3+ test solution, add 6N NaOH until a precipitate which is
first formed dissolves. Then add H2O2 or Na2O2 until a change is observed. Add 6-8 drops of distilled
water. Stir and heat for 5 minutes. Divide into 4 portions in 4 separate test tubes.
a. To the first portion add AgNO3. Observe the color of the precipitate. _____________
b. To the second portion, add BaCl2. Observe the color of the precipitate. ________________
c. c. Acidify the third portion with acetic acid and add 1 drop of lead acetate. Observe the color of the
precipitate._____________
d. d. Reserve the fourth test tube for comparison. Observe the color of the solution.
e. ______________
39
f. 4-6 Confirmatory test for Zn2+
g. a. To 5 drops of Zn 2+test solution, add 3-5 drops of K₄Fe(CN)₆.Note the color of the
precipitate.________________
h. b. Rinmann’s green. To 6 drops of Zn 2+ test solution, add 1-2 droops of cobalt nitrate and a few
drops( about 4-7 drops) of 6N NH₄OH. Filter and ignite the precipitate. Note the color of the
ash.________________
i. 4-7 Confirmatory test for Mn2+To 2 drops of Mn2+ test solution, add 2 drops of 3N HNO₃.
j. Introduce a bit of sodium bismuthate. Note the color of the solution._________________
k. 4-8 Confirmatory test for Fe3+. In 3 separate test tubes, add 3 drops of Fe 3+test solution, and add the
following reagents:
l. a. 3 drops of KCNS to the first test tube. Observe the change.________________
m. b 3 drops of K₄Fe(CN)₆to the second test tube. Observe._______________
n. c. 3 drops of K₃Fe(CN)₆ to the third test tube. Observe________________
o. 4-9 Confirmatory test for Fe2+. Repeat the tests for Fe3+ using instead of Fe2+ test solution.
p. Compare the results.
q. a. To the first test tube, add 3 drops of KCNS.Note the result._______________
r. b. To the second test tube, add 3 drops of K₄Fe(CN)₆. Note the result.______________
s. c. To the third test tube, add 3 drops of K₃Fe(CN)₆. Note the result._________________
t. 4-10 Confirmatory test for Co2+. To 5 drops of Co2+ test solution, add 3 drops of 6N KNO₂ and 1-2
drops of acetic acid. Stir the mixture and heat almost to boiling in a water bath. Note the crystals
produced._____________
u. 4-11 Confirmatory test for Ni2+.To 5 drops of Ni2+ test solution, add 1 drop of concentrated NH₄OH
an 3 drops of alcoholic dimethyl glyoxime. Note the color of the precipitate._________________.
Table 4
IONS Al3+ Cr3+ Zn2+ Mn2+ Co2+ Ni2+ Fe2+ Fe3+

4-2.TS,NH₄OH,
NH₄Cl
4-2a. To the
solution in 4-2,
add (NH₄)₂S
4-3.TS,
NaOH
40
4-3a. Solubility
of the
precipitate in
4-3 in excess
NaOH
4-3b.Solution
in 4-3a, add
Na₂O ₂Or H₂O₂
Table 4-A
CONFIRMATORY TEST COLOR, NAME AND FORMULA OF THE PRECIPITATE

OR SOLUTION
4-4a. Al3+, NH4OH, NH4Ac, Aluminum reagent
4-4b. Al3+, Co(NO3)2, NH4OH
4-5. Cr3+, NaOH, H2O2 or Na2O2
a. Above solution, add AgNO3
4-5b. solution in 4.5 , add BaCl2
4-5c. solution in 4-5, ad PbAC2
4-5d. solution in 4-5
4-6a. Zn2+, K4Fe(CN)6
4-6b. Zn2+, Co(NO3)2, NH4O. Precipitate ignited
4-7 Mn2+, HNO3, Sodium bismuthate
4-8a. Fe3+, KCNS
4-8b. Fe3+, K4Fe(CN)6
4-8c. Fe2+, K3Fe(CN)6
4-9a. Fe2+, KCNS
4-9b. Fe2+, K4Fe(CN)6
4-9c. Fe2+, K3Fe(CN)6
41
4-10. Co2+, KNO2, CH3COOH
4-11. Ni2+, NH4OH, alcoholic dimethylglyoxime
IV. CONCLUSION
42
Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______


REACTIONS OF THE ALKALINE EARTH GROUP
(Ions Are Separated As Carbonate)
I. OBJECTIVE: At the end of the experiment; the students are expected to:
1. Test the reactions of the Alkaline Earth Group or Group IV cations.
2. Write equations involving the reactions of these cations.
II. DISCUSSION
Group Reagent: Ammonium carbonate
Metals of this group form soluble chlorides and sulfides. They are precipitated as carbonates
in the presence of ammonium carbonate and 95% ethyl alcohol. Most of their salts are colorless
and very slightly soluble in water. This group is also known as the Ammonium Carbonate Group
and the members can be differentiated by means of the flame test and confirmed by their
confirmatory tests.
On account of the close resemblances of the elements in regard to their physical and
chemical properties, they are discussed simultaneously. Magnesium ion is, however, discussed
separately for it differs markedly from the other cations of this group in its chemical behavior.
Ba2+ - Barium Sr2+ - Strontium
Ca2+ - Calcium Mg2+ - Magnesium
The Ions of this group all exhibit a single oxidation state of +2. The elements are highly
electropositive and therefore they are excellent reducing agents. The ions are characterized by
forming a relatively large number of slightly soluble salts.
Compound of the Alkaline Earth Metals
*M – represents any of the metal of Group IV
a. Carbonates. Ammonium or alkali carbonates precipitate neutral or alkali solutions of these

ions the corresponding relatively insoluble white carbonates.
43
M(NO3)2 + Na2CO3 = MCO3 + 2NaNO3
M(NO3)2 + (NH4)2CO3 = MCO3 + 2NH4NO3
b. Chromates. Alkali chromates precipitate yellow alkaline earth metal chromates

M(NO₃)₂ + K₂CrO₄ = MCrO₄↓ + 2KNO₃
BaCrO₄ is the least soluble and CaCrO₄ is the most soluble in the group. BaCrO₄ is so insoluble in the
water that a very small CrO₄²¯ io concentration is sufficient for its preparation. SrCrO₄, on the other
hand, is precipitated by a somewhat higher concentration.
Strong acids will dissolve BaCrO₄ hence it cannot be precipitated from solution of high H + ion
concentration. Acetic acid does not furnish sufficient H+ ion concentration to dissolve BaCrO₄. The
situation is somewhat different from CaCrO₄ and SrCrO₄ which are so much more soluble than BaCrO₄.
They furnish considerable quantities of CrO₄²¯ ions in their saturated solutions, high enough that acetic
acid will dissolve the solid chromate. Thus, solutions containing acetic acid, SrCrO₄ and CaCrO₄ will not
precipitate. This serves as a means of separating Ba 2+ ions from Sr2+ and Ca2+ ions.
c. Oxalates. Ammonium oxalate precipitates the alkaline earth ions as white precipitates.
M(NO₃)₂ + (NH₄)₂C₂O₄ = MC₂O₄ + 2NH₄NO₃
Strong acids, and even hot acetic acid, will dissolve BaC₂O₄ readily, so is true of SrC₂O₄. But CaC₂O₄ is
somewhat less soluble and though it is soluble in solutions containing high H+ ion concentration, it fails
to dissolve to a large extend in acetic acid. This result gives a means of separating Ca 2+ from Ba2+ and Sr2+
ions.
d. sulfates. Ammonium sulfate precipitates the alkaline earth ions as white precipitates.
M(NO₃)₂ + Na₂HPO₄ = MHPO₄↓ + 2NH₄NO₃
The precipitates are not appreciably soluble in HCI and HNO₃ of the sulfates, BaSO4 is the least soluble
and CaSO4 is the most soluble.
e. phosphates. In neutral solutions of the alkaline earth ions, sodium hydrogen phosphate solutions
precipitates the corresponding secondary salts of the said ions.
M(NO₃)₂ + Na₂HPO₄ = MHPO₄↓ + 2NaNO₃
In alkaline solutions, for example, in ammonium hydroxide solution, the normal (tertiary salts) sre
precipitated in the following manner
HPO₄2- + OH = PO₄3- + H₂O
3 M2+ + 2 PO₄3+ = M3(PO4)2
f. Flame tests. Volatile compounds of the alkaline earth meatls give characteristics ccolors to the Bunsen
Flame.
Ba2+ - Green(yellowish-green) Ca2+ -Brick-red Sr2+ - Crimson Red
44
MAGNESIUM
The ion. Magnesium ion differs markedly from the alkaline earth ions in that its sulfate and
chromate compounds are highly soluble and its oxalate and carbonate are moderately soluble. It is
therefore apparent that the same reagents cannot precipitate a magnesium salt as for the alkaline earth
metals. The most conspicuous difference from barium, calcium and strontium ions is the most readily
soluble of the MgCO3 in ammonium salt solutions. It is only upon the addition of a reasonable quantity
of alcohol that this salt of magnesium is precipitated. The ion does not impart any color to the Bunsen
flame.
Compounds of magnesium
a. Magnesium oxalate, MgC2O4. In dilute solution, ammonium oxalate does not precipitate with
magnesium ion except in the more concentratedType equation here. solution of the reagent.
Mg(NO3)2 + (NH4)2C2O4 = MgC2O4↓ + 2NH4NO3
Magnesium oxalate is soluble in acetic acid.
b. Magnesium carbonate, MgCO3. Alkali carbonates precipitate magnesium as a white basic
carbonate of somewhat variable composition depending upon the conditions of precipitation.
2Mg(NO3)2 + N2CO3 + H2O(in alcohol) = Mg(OH)2MgCO3↓ + CO2 + 4NH4NO3
Ammonium carbonate, in the absence of other ammonium salts, precipitates a basic salt, the
composition of which varies with temperature and concentration of the solution. In an excess of the
reagent and when an equal volume of alcohol is added, complete precipitation is attained from a cold
concentrated solution of magnesium salt.
Mg(NO3)2 + 2(Na4)2CO3 + 4H2O(in alcohol) = MgCO3.(NH4)2CO3 + 2NH4NO3 + 4H2O
c. Magnesium ammonium phosphate, MgNH4PO4. A solution of sodium biphosphate gives a white

precipitate of magnesium biphosphate with solutions containing magnesium ions.
Mg(NO3)2 + Na2HPO4 + 7 H2O = MgHPO4. 7 H2O + 2NaNO3
In the presence of NH4OH and NH4CI, a characteristic white crystalline precipitate of magnesium
ammonium phosphate is obtained, but only after allowing it to stand for sometimes and rubbing
the sides of the tube with a glass rod.
Mg(NO3)2 + NH4OH + Na2HPO4 = MgNH4PO4↓ + 2NaNO3 + H2O
III. MATERIALS
Nichrome wire Burner Tripod Test tube Water bath Droppers
IV. PROCEDURE
5-1. Flame test
45
a. Make a tiny loop at the end of the nichrome wire and clean it by immersing it successively in
water and in concentrated HCl and heating it in the non-luminous flame until no color is
imparted.
b. Into 4 separate test tubes, place 3 drops each of the test solution for Ba²⁺, Ca²⁺, Sr²⁺ and Mg²⁺.
Add 2 drops of concentrated HCl to each test tube. Dip the loop into the mixture and heat it in
the non-luminous flame. Note the color imparted to the flame. Repeat 5-1a before doing the
flame test with another test solution.
Ba²⁺______________ Ca²⁺______________ Sr²⁺______________ Mg²⁺_____________
5-2. Place in 4 separate test tubes, 1 drop each of the test solutions of group IV and add 3 drops of
(NH₄)₂CO₃ and 3 drops of 95% ethyl alcohol. Stir and let stand for 1 minute. Note the color of the
precipitate to each test tube.
Ba²⁺______________ Ca²⁺______________ Sr²⁺______________ Mg²⁺_____________
5-3. Place 3 drops each test solutions of Group IV in 4 separate test tubes, and add 3-5 drops of K₂CrO₄.
In what test tubes did you produce a precipitate? ____________________________________________.
Write the color of the precipitate. ________________________.
a. Test the solubility of the precipitate in glacial acetic acid. Write your observation in row 5-3a on
the table.
5-4.To each test tube containing 3 drops each of the test solution of Group IV, add 1-3 drops of
potassium oxalate, K₂C₂O₄. Note the color of the precipitate.
Ba²⁺______________ Ca²⁺______________ Sr²⁺______________ Mg²⁺_____________

Test the solubility of the precipitate in acetic acid. Write your observation in row 5-4a on the table.
5-5. To 3 drops of each of the cations of Group IV in separate test tubes, add 1-3 drops of (NH₄)₂SO₄.
Note the color of the precipitate.
Ba²⁺______________ Ca²⁺______________ Sr²⁺______________ Mg²⁺_____________
a. Test the solubility of the precipitate in HCl. Write your observations in row 5-5a on the table.
5-6. To the 4 test tubes containing 3 drops each of the Group IV cations, add 3 drops of NH₄OH and 5-7
drops of Na₂HPO₄. Mix and heat in a water bath. Allow to stand for 5 minutes. Note the color of the
precipitate.
Ba²⁺______________ Ca²⁺______________ Sr²⁺______________ Mg²⁺_____________
46
Table 5
COLOR, NAME AND FORMULA OF THE PRECIPITATE
IONS Ba²ᶧ Ca²ᶧ Sr²ᶧ Mg²ᶧ
5-1 Flame test
5- 2. TS,
(NH₄)₂CO₃,
C₂H₅OH
5-3. TS,K₂CrO₄
5-3a. Solubility
Of the precipitate
in 5-3 in CH₃COOH
5-4. TS, K₂C₂O₄
5-4a. Solubility of
the precipitate in
5-4 in CH₃COOH
5-5 TS,
(NH₄)₂SO₄,
5-5a. Solubility of
the precipitate in
5-5 in HCl
5-6. TS,
NH₄OH,
Na₂HPO₄
V. CONCLUSION
47
Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______


REACTIONS OF THE ALKALI GROUP
(No Group Reagent)
I. OBJECTIVE: at the end of the experiment, the students are expected to:
1. Test the reactions of the Alkali Group or Group V Cations
2. Write equations about the reactions of group V Cations.
II. DISCUSSION
The metals of this group are not precipitated by any of the reagents used for the
precipitation of the other groups, so they are always in the last filtrate, where they can be
identified. They are also called the “soluble group”.
Ammonium, though not a metal is classified under this group, because it shows similar
properties to that of sodium and potassium. Ammonium salts are readily volatilized when
ignited. The salts of the alkali metals are more or less volatile and impart characteristic
colors to the non-luminous flames.
NH₄ᶧ - ammonium Naᶧ - sodium
Kᶧ - potassium Liᶧ - lithium

The Ions. All the ions of this group carry a single positive charge and are highly
electroposiive. Most of their salts are characterized by the general solubility in water. They
form hydroxides ehich are the strongest bases that are not hydrolyzed. The ammonium ion,
however, differs from the alkali metal ions in that it forms a relatively weak base, NH₄OH.
Ammonium ion also is volatilized on ignition and detected by its characteristic smell.
Compounds of the alkali Metals
a. Tartrates. Tartaric acid, H₂C₄H₄O₆, gives a white crystalline precipitate with potassium
and ammonium ions in their neutral or slightly acidic salt solutions. Rubbing the inside
walls of the tube with a glass rod aids in the precipitation.
KCl + H₂C₄H₄O₆ = KHC₄H₄O₆ ↓ + HCl
NH₄Cl + H₂C₄H₄O₆ = NH₄HC₄ H₄O₆ ↓ + HCl
48
b. Cobaltinitrites. Sodius. Sodium cobalnitrites precipitates the yellow potassium sodium
cobaltilitrite and ammonium sodium cobalnitrite from their respective neutral or slightly
acidic soluttions.
Na3Co(N02)6 + 2KCl = K2NaCo(NO2)6↓ + 2 NaCl
Na3Co(NO2)6 + 2 NH4Cl = (NH4)2NaCo(NO2)6 ↓ + 2 NaCl
If both precipitates are ignited, both are decomposed and upon cooling, if more of the reagent is
added, potassium sodium cobaltinitrite is re-precipitated while that of NH4+ ion will not since NH4 is
expelled as NH3 while potassium remains in the residue. This makes difference between the 2 ions.
c. Antimonates and Pyroantimontes. Potassium ions yield no precipitate with potassium animonate or
pyroantimonate, but in neutral or slightly alkaline solution of sodium salts, the reagent produces a heavy
white crystalline precipitate of sodium antimonite or pyroantimonate adhering to the sides of the
reaction tube.
NaCl + KH2SbO4 = NaH 2SbO4 + 2 KCl
Potassium antimonate sodium antimonate
2NaCl + K2H2Sb2O7 = Na2H2SbO7 + 2 KCl
Potassium pyroantimonate sodium pyroantimonate
d. Triple acetate. Sodium salts react with a mixed reagent containing zinc acetate and uranyl acetate
producing an addition product, a light yellow well-crystallized precipitate of the triple acetate: sodium
zinc-uranyl acetate.
NaAc + ZnAc2 + 3UO2Ac2 + 9 H2O = NaAcZnAc2UO2Ac29H2O
e. Flame test. Flame test are not often used as confirmatory test for both the alkaline earth and the alkali
metals. The colors imparted by the chloride salts of the alkali ions with the non-luminous flame are the
following :
Na+ - intense yellow Li+ - carmine-red or crimson
K+ - violet NH4 + - no color
Other Reaction of the Ammonium Ion
Liberation of Ammonia
a) Action of strong bases. When an ammonium salt is heated with KOH, NaOH, or Ca(OH) 2,
ammonia is liberated and this gas is detected by means of the following tests:
1. By its characteristic smell.
NH4Cl + NaOH = NaCl + H2O + NH3↑
49
2. By giving white fumes of NH4Cl when a glass rod maintained with HCl is exposed to its
vapors. NH3 + HCl = NH4 ( white fumes)
3. The vapors turn red litmus to blue.
4. A strip of filter paper moistened with Nessler’s reagent, turns orange when exposed to
its vapors.
b. Reactions on ignition. All ammonium salts decompose when ignited when ignited at moderately high
temperature, but not always with the evolution of ammonia.
1. NH4Cl = NH3 ↑ + HCl

2. (NH4)2CO3 = NH3 ↑ + H2O + CO2 ↑
3. NH4NO3 = N2O + H2O
4. (NH4)2Cr2O7= N2 ↑ + 4 H2O + CrO3 ↓
Other Reactions of Lithium Ion
a. Lithium carbonate. Alkali or ammonium carbonate produces a white precipitate of

lithium carbonate when added to concentrated solutions of lithium salts.
2 LiCl + Na2CO3 = 2 NaCl + Li2CO3 ↓

2 LiCl + (NH4)2CO3 = Li2CO3↓ + 2 NH4Cl
b. Lithium phosphate. It is a white precipitate produced when sodium biphosphate is

added to a solution of a lithium salt and the mixture made alkaline with ammonium
hydroxide.
3 LiCl + Na2HPO4 + NH4OH = Li3PO4↓ + 2 NaCl + NH4Cl + H2O
MATERIALS
Test tube droppers water bath tripod litmus paper(red to blue)
PROCEDURE.
6-1. Confirmatory test for Na+
a. To 3 drops of Na+ test solution, add 3-5 drops of potassium antimonate of pyroantimonate and
let stand for 5 minutes. Observe the color and nature of the precipitate. -
_______________________________________________
50
b. Add 3-5 drops of zinc uranyl acetate (mixture of zinc acetate and uranyl acetate) to 3 drops of
Na+ test solution. Note the color of the precipitate. _______________
6-2 Confirmatory test for K+
a. to 3 drops of K+ test solution, add 3 drops of sodium cobaltinitrite reagent and note the color of
the precipitate. _________________
b. to 3 drops of K+, add 3-5 drops of tartaric acid. Stir and rub the inside walls of the test tube with
a glass rod. Allow to stand for 5 minutes and note the color and nature of the precipitate.
__________________
6-3 Confirmatory test for Li+
Dilute 2 drops of Li+ with an equal volume of water and 2 drops of Na2HPo4 and render the
mixture alkaline with NH4OH. Heat the test tube in water bath for 2-3 minutes. Observe the
results.___________________
a. Test the solubility of the precipitate in HCL.__________________
b. Render the solution alkaline again with NH4OH. Did you produce the precipitate again? _______
6-4 Confirmatory test for NH4+
a. To 1 drop of NH4+ test solution, add 5 drops of distilled water and 1 drop of Nessler’s reagent.
Note the color of the precipitate._____________
b. To 5 drops of NH4+ test solution, add 2 drops of 6N NaOH and heat the mixture in a water bath.
Identify the gas evolved by its odor.____________ Expose a moistened red litmus paper at the
mouth of the test tube. Observe the results.______________
6-5 Flame test. Perform the flame test for the member of group V. (Follow the correct technique on
the flame test given in the “Introduction to the Laboratory”).
Na+________ K+___________ Li+_____________ NH4+____________
Table 6
CONFIRMATORY TEST
COLOR, NAME AND FOMULA F THE PRECIPITATE
51
6-1 a. Na+, potassium antimonite
6-1 b. Na+, zinc uranyl acetate
6-2a. K, sodium cobaltinitrite
6-2b. K+, tartaric acid
6-3. Li+, NaH2PO4, NH4OH
6-3a. solubility of lithium phosphate in HCL
6-3b. solution in 6-3a, NH4OH
6-4a. NH4+, H2O, Nessler’s reagent
6-4b. NH4+, NaOH, heat
V. CONCLUSION
52
Tel. No: (082)-2218181 loc 188
Name: _________________________ Score: ______

Learning Activity #7
ANALYSIS OF A CATION IN A SOLUTION CONTAINING ONLY ONE INORGANIC COMPOUND

I.OBJECTIVE : At the end of the experiment , the student should be able to identify the cation present in
the unknown inorganic compound.
II. MATERIALS : test tube centrifuge water bath burner tripod
III. PROCEDURE
1. To 1 ml of the original sample, add 1 drop of 2N HCL. If a precipitate is formed, Silver Group is present.
Add a few drops more of 2N HCL unil precipitation is complete.
A. Dilute the mixture with water and boil for 1 minute. If the precipitate dissolves, LEAD is indicated.
Confirm by adding potassium chromate to the original sample; yellow precipitate proves LEAD.
B. if the precipitate is insoluble on boiling, allow the mixture to stand. Decant off the supernatant liquid
and treat the precipitate with ammonium hydroxide. If the precipitate dissolves, SILVER is confirmed. If
the precipitate blackens, MERCUROUS MERCURY is confirmed.
2. If the addition of HCL to the original sample in step (1) has produced no precipitate, treat the mixture
with 10 drops of 10% thioacetamide solution. Stir thoroughly and boil in water bath for about 10
minutes. If precipitate is produced, Hydrogen sulfide group is present.
A. Make the mixture from step (2) alkaline with 6N NaOH and add 2 drops of sodium sulfide. Warm the
mixture. If the precipitate is insoluble after warming, Copper Subgroup is present; if soluble, Tin
Subgroup is present.
B. The precipitate from step (2-A) which is insoluble in sodium sulfide contains the Copper Subgroup.
a. If the precipitate is yellow, the cation present is CADMIUM. Confirm by treating a portion of the
original sample with potassium ferrocyanide. White precipitate proves CADMIUM.
b. If the precipitate is black or brown, BISMUTH, LEAD and COPPER are indicated. Treat a portion of the
original sample with potassium chromate and acetic acid, yellow precipitate proves LEAD.
53
c. Treat a portion of the original sample with 6N NaOH and freshly prepared solution of sodium stannite.
Immediate blackening of the precipitate shows BISMUTH.
d. The presence of copper is indicated by the blue color of the original solution. Treat a portion of the
original sample with potassium ferrocyanide. Reddish-brown precipitate proves COPPER.
C. The precipitate from step (2-A) which is soluble in sodium sulfide contains the Tin Subgroup.
a. If the precipitate is black, MERCURIC MERCURY is indicated. To a portion of the sample, add
stannous chloride. White turning gray shows MERCURIC MERCURY.
b. If the precipitate is orange, ANTIMONY is indicated. Drrop a piece of metallic tin portion of the
original sample. Black precipitate on the tin, insoluble in sodium hypobromite shows ANTIMONY.
c. If the precipitate is yellow, ARSENIC and TIN are indicated. To a portion of the original sample, add
HCl and magnesium ribbon. Boil for 2-3 minutes. Filter and to the filtrate, add a few drops of mercuric
chloride. White or gray precipitate shows TIN.
d. To 2 mL of the original sampe, add 1 mL of ammonium hydroxide and 1 ml of hydrogen peroxide.

Warm the mixture on a water bath for 2-3 minutes, then evaporate to dryness in an evaporating dish.
Dissolve the residue in 1 mL of water and 1 mL of concentrated HNO3, add 2 mL of ammonium
molybdate and warm the mixture. yellow precipitate shows ARSENIC.
3. If the hydrogen sulfide in step (2) has produced no precipitate, to 1 mL of the original sample add 10
drops of ammonium chloride and 10 drops of ammonium hydroxide. If a precipitate is formed, the
trivalent cations of the Ammonium Sulfide Group are present.
A. The precipitate in step (3) indicates ALUMINUM, CHROMIUM and FERRIC.
a. If the precipitate is white, ALUMINUM is indicated. Treat 1 mL of the sample with 10 drops each
of ammonium acetate and aluminon reagent solution. Mix well and make alkaline with ammonium
hydroxide. Red lake shows ALUMINUM.
b. If the precipitate is grayish green, CHROMIUM is indicated. Treat 1 mL of the original sample
with sodium hydroxide, add hydrogen peroxide until any green color has disappeared. Boil the mixture
gently for 5 minutes, replacing the water which evaporates. Cool, acidify with acetic acid and lead
acetate. Yellow precipitate shows CHROMIUM.
c. A reddish-brown precipitate indicates FERRIC. Test 1 mL of the original sample with potassium
ferrocyanide. Blue precipitates confirms FERRIC.
54
B. If there was no precipitate formed in step 3, pass hydrogen sulfide to the alkaline
mixture. Formation of precipitate indicates ZINC, MANGANESE, COBALT and
NICKEL.
B-1. If the precipitate is white, ZINC is confirmed.
B-2. If the precipitate is flesh-colored, MANGANESE is indicated.
a. Treat 1 mL of the original sample with HNO₃ and add sodium
bismuthate. Violet coloration proves MANGANESE.
B-3. If the precipitate is black, COBALT and NICKEL are indicated.
a. The presence of COBALT is further indicated by pink color of the
original solution. To 1 mL of the sample, add 1 mL of potassium nitrite
and acidify the mixture acetic acid. Yellow precipitate proves
COBALT.
b. The presence of NICKEL is indicated by the green color of the original
solution. Treat 1 mL of the original sample with a few drops of
dimethylglyoxime reagent and make the solution slightly alkaline with
ammonium hydroxide. Red precipitate proves NICKEL.
4. If no precipitate is produced in steps 3-A and 3-B, to 1mL of the original sample, add a few
drops of sodium carbonate. White precipitate indicates the presence of the Alkaline Earth
Group.
a) To 1 mL of the original sample, add 2-3 drops of acetic acid and 5 drops of potassium
chromate. Yellow precipitate proves BARIUM.
b) If no precipitate in step 4-A, make the mixture alkaline with ammonium hydroxide and add 1
mL of 95% ethyl alcohol.
B-1. Yellow precipitate indicates STRONTIUM.
a. Confirm strontium by performing the flame test with the original
solution. Carmine-red flame coloration confirms STRONTIUM.
55
c) To 1 mL of the original sample, add 1mL of water 5 drops of potassium oxalate and 2-3 drops
of acetic acid. White precipitate shows CALCIUM.
d) To 1 mL of the original sample, add 10 drops of ammonium chloride, 10 drops of sodium

phosphate and make alkaline with ammonium hydroxide. Allow to stand. White crystalline
precipitate shows MAGNESIUM.
5. If no precipitate is obtained in step 4, Alkali Group is indicated.
a) To 1 mL of the original sample, add 1 mL of sodium hydroxide and heat the mixture.
Evolution of ammonia shows AMMONIUM SALTS.
b) To 1 mL of the original sample, add 1 mL of sodium cobaltinitrite. Yellow precipitate proves
POTASSIUM.
c) To 1 mL of the original sample, add 1 mL potassium pyroantimonate. White crystalline
precipitate proves SODIUM.
d) Perform the flame test with the original solution. Carmine-red coloration proves LITHIUM.
IV. CONCLUSION
56

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Qualitative-Quantitative Chemistry

INTRODUCTION TO THE LABORATORY

REACTION – Any process in which a new chemical substance is formed.

REAGENT – The substance used to bring about a reaction.

PRECIPITATE – Any insoluble substance produced in the reaction.

RESIDUE – The solid remaining after evaporating a mixture or solution to dryness.

CLEAR SOLUTION – A solution that is not turbid or cloudy

COLORLESS SOLUTION – A solution that is not colored.

A positive test maybe indicated by the:

12. Turn off burners that are not in use.

GENERAL LABORATORY TECHNIQUES

2. Hydrolysis of thioacetamide in a slightly acidic or basic media at elevated temperature. The

Following these guidelines can improve the accuracy of manual liquid

17 Ways to Stop Pipetting Errors From Ruining Your Experiments

Know How Your Pipette Works

1. You Use an Air Displacement Pipette, Most Likely

2. Don’t Use an Air Displacement Pipette (depending on your application)

Take Care of Your Pipette

3. Have Your Pipette Serviced Every 6-12 Months…

4. Check Your Pipettes Daily for Damage

5. Clean Your Pipettes Each Day Before Use

6. Store Your Pipette Vertically, Using a Pipette Holder

8. Use Well-Fitting Tips

Practice Good Pipetting Technique

9. Make Sure You Know How to Pipette Properly

10. Test Your Accuracy

Know the Tricks That Increase Your Accuracy

11. Pre-Wetting the Pipette Tip

12. Reverse Pipetting

13. Take the Ambient Temperature Into Account

14. Take the Sample Temperature Into Account

16. Use the Largest Volume Possible

17. And Finally, Here’s How to Get Maximum Accuracy

11 PREPARATION AND STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION

STANDARDIZATION OF SODIUM HYDROXIDE SOLUTION WITH POTASSIUM ACID

Name: _________________________ Score: ______

Learning Activity No. 1

o LEARNING OBJECTIVES: At the end of the experiment, the students can:

What is the color of the precipitate?__________ What ion is precipitated?_________

What ion is left in the filtrate?__________

IV. COMPLETE THE TABLE.

Name: _________________________ Score: ______

Learning Activity No. 2

I. LEARNING OBJECTIVES: At the end of the experiment, the students can:

Precipitating Reagent (or Group Reagent): Dilute solution of HCI

The members of the group are: Ag+ - silver

PbCl2 + H2S  Pb2Cl2S ( or PbCl2.PbS)

Pb2Cl2S + H2S  2 PbS + 2 HCl

Compounds of Mercurous Mercury

III. LEARNING STRATEGIES

IV. COMPLETE THE TABLE.

Ions Ag+ (silver) Pb2+ (lead III) Hg22+ (mercurous

2-2.TS and HCI: color,

2-2a. solubility of the

2-2b. solubility of the

2-3. TS and NH4OH:

2-3a. solubility of the

2-4. TS and NaOH:

2-5. TS and K2CrO4:

2-5a. solubility of the

2-6. TS and KI:

2-6a. solubility of the

Write equations to show the reactions of the following procedures:

Name: ___________________ Score:

What is the color of the precipitate?__ What ion is precipitated?_

Name: ___________________ Score:

Name: ___________________ Score:

Pb2+ _ As3+ Hg²2+____

Bi3+ _ Sb3+ Sn2+ ____

Cu²2+ _ Cd²3+ Sn4+ ____